# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Jean-Marie Lehn' _publ_contact_author_email LEHN@ISIS.U-STRASBG.FR _publ_section_title ; Structural features directing the specificity and functionality of metallo-supramolecular grid-type architectures ; loop_ _publ_author_name 'Jean-Marie Lehn' 'M Drillon' 'Jack Harrowfield' 'Guillaume Rogez' 'Artur R. Stefankiewicz' # Attachment 'CIF for CuGridcorr.cif' data_as2 _database_code_depnum_ccdc_archive 'CCDC 711187' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C324.50 H278 B8 Cu4 F32 N50.50 O8 S8' _chemical_formula_weight 6218.09 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 24.3653(10) _cell_length_b 26.5163(10) _cell_length_c 28.1575(10) _cell_angle_alpha 65.201(5) _cell_angle_beta 75.390(5) _cell_angle_gamma 77.363(5) _cell_volume 15847.7(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 47136 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6429 _exptl_absorpt_coefficient_mu 0.402 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD' _diffrn_measurement_method 'phi&omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 111163 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.1846 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.46 _reflns_number_total 71168 _reflns_number_gt 32734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1882P)^2^+69.9855P] 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 71168 _refine_ls_number_parameters 3924 _refine_ls_number_restraints 365 _refine_ls_R_factor_all 0.2929 _refine_ls_R_factor_gt 0.1675 _refine_ls_wR_factor_ref 0.4368 _refine_ls_wR_factor_gt 0.3631 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.031 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7772(4) 0.5536(4) 0.2803(4) 0.048(2) Uani 1 1 d . . . H1 H 0.7843 0.5429 0.3151 0.058 Uiso 1 1 calc R . . C2 C 0.7223(4) 0.5562(4) 0.2744(4) 0.055(2) Uani 1 1 d . . . H2 H 0.6920 0.5482 0.3043 0.066 Uiso 1 1 calc R . . C3 C 0.7121(4) 0.5710(5) 0.2228(5) 0.064(3) Uani 1 1 d . . . H3 H 0.6746 0.5728 0.2174 0.076 Uiso 1 1 calc R . . C4 C 0.7563(4) 0.5828(4) 0.1810(4) 0.053(2) Uani 1 1 d . . . H4 H 0.7503 0.5927 0.1459 0.064 Uiso 1 1 calc R . . C5 C 0.8105(4) 0.5800(3) 0.1902(3) 0.039(2) Uani 1 1 d . . . C6 C 0.8590(4) 0.5930(3) 0.1487(3) 0.039(2) Uani 1 1 d . . . H6 H 0.8560 0.6046 0.1125 0.047 Uiso 1 1 calc R . . C7 C 1.0036(3) 0.5934(3) 0.1501(3) 0.0311(17) Uani 1 1 d . . . C8 C 1.0574(4) 0.6024(3) 0.1200(3) 0.0365(19) Uani 1 1 d . . . H8 H 1.0644 0.6142 0.0824 0.044 Uiso 1 1 calc R . . C9 C 1.1006(3) 0.5932(3) 0.1474(3) 0.0324(17) Uani 1 1 d . . . C10 C 1.0372(4) 0.5720(3) 0.2265(3) 0.0343(18) Uani 1 1 d . . . C11 C 1.0279(4) 0.5607(4) 0.2842(3) 0.0385(19) Uani 1 1 d . . . C12 C 1.0139(4) 0.6059(5) 0.2998(4) 0.057(3) Uani 1 1 d . . . H12 H 1.0096 0.6429 0.2736 0.069 Uiso 1 1 calc R . . C13 C 1.0061(5) 0.5981(7) 0.3522(5) 0.082(4) Uani 1 1 d . . . H13 H 0.9968 0.6295 0.3621 0.098 Uiso 1 1 calc R . . C14 C 1.0114(5) 0.5484(9) 0.3880(6) 0.093(5) Uani 1 1 d . . . H14 H 1.0050 0.5442 0.4241 0.111 Uiso 1 1 calc R . . C15 C 1.0266(5) 0.4980(6) 0.3765(4) 0.084(4) Uani 1 1 d . . . H15 H 1.0309 0.4616 0.4036 0.101 Uiso 1 1 calc R . . C16 C 1.0347(4) 0.5070(5) 0.3207(4) 0.057(3) Uani 1 1 d . . . H16 H 1.0445 0.4762 0.3098 0.068 Uiso 1 1 calc R . . C17 C 1.2465(4) 0.6019(3) 0.1306(3) 0.042(2) Uani 1 1 d . . . H17 H 1.2583 0.6134 0.0931 0.050 Uiso 1 1 calc R . . C18 C 1.2879(4) 0.5947(4) 0.1639(4) 0.042(2) Uani 1 1 d . . . C19 C 1.3438(4) 0.6004(4) 0.1428(4) 0.061(3) Uani 1 1 d . . . H19 H 1.3578 0.6085 0.1060 0.073 Uiso 1 1 calc R . . C20 C 1.3804(5) 0.5939(5) 0.1765(5) 0.075(3) Uani 1 1 d . . . H20 H 1.4200 0.5970 0.1635 0.090 Uiso 1 1 calc R . . C21 C 1.3573(5) 0.5831(5) 0.2290(5) 0.068(3) Uani 1 1 d . . . H21 H 1.3808 0.5803 0.2525 0.082 Uiso 1 1 calc R . . C22 C 1.3009(4) 0.5763(4) 0.2478(4) 0.053(2) Uani 1 1 d . . . H22 H 1.2864 0.5669 0.2847 0.064 Uiso 1 1 calc R . . C23 C 0.9576(4) 0.6189(3) 0.0712(3) 0.042(2) Uani 1 1 d . . . H23A H 0.9352 0.5964 0.0644 0.050 Uiso 1 1 calc R . . H23B H 0.9974 0.6147 0.0523 0.050 Uiso 1 1 calc R . . C24 C 0.9320(4) 0.6806(3) 0.0504(3) 0.0393(19) Uani 1 1 d . . . C25 C 0.8709(4) 0.7511(3) -0.0117(3) 0.044(2) Uani 1 1 d . . . H25A H 0.8736 0.7564 -0.0491 0.053 Uiso 1 1 calc R . . H25B H 0.8937 0.7777 -0.0115 0.053 Uiso 1 1 calc R . . C26 C 0.8088(5) 0.7645(4) 0.0118(4) 0.058(3) Uani 1 1 d . . . H26A H 0.7880 0.7333 0.0187 0.070 Uiso 1 1 calc R . . H26B H 0.7917 0.7985 -0.0150 0.070 Uiso 1 1 calc R . . C27 C 0.7877(5) 0.8535(4) 0.0480(4) 0.056(3) Uani 1 1 d . . . C28 C 0.7857(5) 0.8653(4) 0.0984(4) 0.057(3) Uani 1 1 d . . . C29 C 0.7479(5) 0.8408(4) 0.1445(5) 0.067(3) Uani 1 1 d . . . H29 H 0.7242 0.8161 0.1455 0.081 Uiso 1 1 calc R . . C30 C 0.7439(6) 0.8519(5) 0.1897(5) 0.085(4) Uani 1 1 d . . . H30 H 0.7184 0.8341 0.2215 0.102 Uiso 1 1 calc R . . C31 C 0.7767(7) 0.8881(5) 0.1882(5) 0.085(4) Uani 1 1 d . . . H31 H 0.7741 0.8956 0.2189 0.102 Uiso 1 1 calc R . . C32 C 0.8136(6) 0.9141(4) 0.1422(5) 0.072(3) Uani 1 1 d . . . H32 H 0.8356 0.9400 0.1413 0.087 Uiso 1 1 calc R . . C33 C 0.8190(5) 0.9030(4) 0.0976(4) 0.058(3) Uani 1 1 d . . . H33 H 0.8451 0.9208 0.0663 0.070 Uiso 1 1 calc R . . C34 C 0.7285(5) 0.8799(5) 0.0314(5) 0.074(3) Uani 1 1 d . . . C35 C 0.7162(8) 0.9381(6) 0.0148(7) 0.118(6) Uani 1 1 d . . . H35 H 0.7436 0.9582 0.0156 0.142 Uiso 1 1 calc R . . C36 C 0.6673(10) 0.9673(9) -0.0024(10) 0.181(11) Uani 1 1 d . . . H36 H 0.6613 1.0071 -0.0163 0.217 Uiso 1 1 calc R . . C37 C 0.6243(12) 0.9350(13) 0.0015(14) 0.247(19) Uani 1 1 d . . . H37 H 0.5884 0.9535 -0.0081 0.297 Uiso 1 1 calc R . . C38 C 0.6357(8) 0.8755(11) 0.0196(11) 0.180(11) Uani 1 1 d . . . H38 H 0.6078 0.8538 0.0225 0.216 Uiso 1 1 calc R . . C39 C 0.6897(6) 0.8498(7) 0.0332(7) 0.112(6) Uani 1 1 d . . . H39 H 0.6989 0.8103 0.0438 0.134 Uiso 1 1 calc R . . C40 C 0.8369(5) 0.8743(4) 0.0037(4) 0.061(3) Uani 1 1 d . . . C41 C 0.8920(6) 0.8608(5) 0.0140(5) 0.074(3) Uani 1 1 d . . . H41 H 0.8977 0.8408 0.0497 0.089 Uiso 1 1 calc R . . C42 C 0.9409(8) 0.8760(7) -0.0277(8) 0.114(5) Uani 1 1 d . . . H42 H 0.9787 0.8679 -0.0208 0.137 Uiso 1 1 calc R . . C43 C 0.9287(11) 0.9036(8) -0.0793(8) 0.129(7) Uani 1 1 d . . . H43 H 0.9593 0.9156 -0.1083 0.155 Uiso 1 1 calc R . . C44 C 0.8742(13) 0.9141(7) -0.0896(8) 0.144(8) Uani 1 1 d . . . H44 H 0.8675 0.9307 -0.1251 0.173 Uiso 1 1 calc R . . C45 C 0.8309(8) 0.9003(6) -0.0485(5) 0.106(5) Uani 1 1 d . . . H45 H 0.7933 0.9092 -0.0561 0.127 Uiso 1 1 calc R . . C46 C 1.1743(4) 0.6158(4) 0.0642(3) 0.041(2) Uani 1 1 d . . . H46A H 1.1481 0.6046 0.0496 0.049 Uiso 1 1 calc R . . H46B H 1.2134 0.5972 0.0560 0.049 Uiso 1 1 calc R . . C47 C 1.1737(4) 0.6798(4) 0.0384(3) 0.047(2) Uani 1 1 d . . . C48 C 1.2185(5) 0.7570(4) -0.0337(4) 0.056(3) Uani 1 1 d . . . H48A H 1.1826 0.7792 -0.0237 0.067 Uiso 1 1 calc R . . H48B H 1.2240 0.7663 -0.0724 0.067 Uiso 1 1 calc R . . C49 C 1.2680(5) 0.7736(5) -0.0222(4) 0.066(3) Uani 1 1 d . . . H49A H 1.2714 0.8137 -0.0440 0.079 Uiso 1 1 calc R . . H49B H 1.3042 0.7513 -0.0317 0.079 Uiso 1 1 calc R . . C50 C 1.3082(4) 0.8006(4) 0.0522(4) 0.055(2) Uani 1 1 d . . . C51 C 1.3015(4) 0.8593(4) 0.0072(4) 0.051(2) Uani 1 1 d . . . C52 C 1.2490(5) 0.8926(4) 0.0053(5) 0.067(3) Uani 1 1 d . . . H52 H 1.2170 0.8796 0.0323 0.081 Uiso 1 1 calc R . . C53 C 1.2430(6) 0.9449(5) -0.0358(6) 0.079(4) Uani 1 1 d . . . H53 H 1.2068 0.9673 -0.0364 0.095 Uiso 1 1 calc R . . C54 C 1.2874(6) 0.9644(5) -0.0746(5) 0.081(4) Uani 1 1 d . . . H54 H 1.2831 1.0009 -0.1016 0.098 Uiso 1 1 calc R . . C55 C 1.3394(6) 0.9306(5) -0.0749(5) 0.083(4) Uani 1 1 d . . . H55 H 1.3708 0.9427 -0.1030 0.100 Uiso 1 1 calc R . . C56 C 1.3449(5) 0.8793(4) -0.0337(4) 0.067(3) Uani 1 1 d . . . H56 H 1.3810 0.8566 -0.0338 0.081 Uiso 1 1 calc R . . C57 C 1.3700(5) 0.7714(4) 0.0481(4) 0.060(3) Uani 1 1 d . . . C58 C 1.4104(5) 0.7928(6) 0.0584(5) 0.077(3) Uani 1 1 d . . . H58 H 1.3994 0.8250 0.0671 0.093 Uiso 1 1 calc R . . C59 C 1.4678(6) 0.7677(8) 0.0562(5) 0.098(5) Uani 1 1 d . . . H59 H 1.4956 0.7834 0.0622 0.117 Uiso 1 1 calc R . . C60 C 1.4828(7) 0.7203(8) 0.0453(5) 0.102(5) Uani 1 1 d . . . H60 H 1.5213 0.7027 0.0444 0.123 Uiso 1 1 calc R . . C61 C 1.4430(8) 0.6980(7) 0.0357(7) 0.115(5) Uani 1 1 d . . . H61 H 1.4540 0.6654 0.0278 0.138 Uiso 1 1 calc R . . C62 C 1.3856(6) 0.7236(5) 0.0377(6) 0.089(4) Uani 1 1 d . . . H62 H 1.3579 0.7076 0.0318 0.107 Uiso 1 1 calc R . . C63 C 1.2877(5) 0.8003(5) 0.1081(4) 0.065(3) Uani 1 1 d . . . C64 C 1.2734(7) 0.8493(6) 0.1186(6) 0.094(4) Uani 1 1 d . . . H64 H 1.2750 0.8853 0.0908 0.113 Uiso 1 1 calc R . . C65 C 1.2567(7) 0.8424(8) 0.1727(7) 0.108(5) Uani 1 1 d . . . H65 H 1.2481 0.8750 0.1807 0.130 Uiso 1 1 calc R . . C66 C 1.2524(6) 0.7933(9) 0.2127(6) 0.104(5) Uani 1 1 d . . . H66 H 1.2391 0.7911 0.2482 0.125 Uiso 1 1 calc R . . C67 C 1.2677(6) 0.7445(7) 0.2021(5) 0.090(4) Uani 1 1 d . . . H67 H 1.2666 0.7088 0.2305 0.108 Uiso 1 1 calc R . . C68 C 1.2843(5) 0.7484(5) 0.1510(4) 0.065(3) Uani 1 1 d . . . H68 H 1.2939 0.7150 0.1442 0.078 Uiso 1 1 calc R . . C71 C 0.8837(4) 0.7072(3) 0.1921(4) 0.048(2) Uani 1 1 d . . . H71 H 0.8902 0.7075 0.1572 0.057 Uiso 1 1 calc R . . C72 C 0.8728(5) 0.7583(4) 0.1985(4) 0.056(3) Uani 1 1 d . . . H72 H 0.8708 0.7928 0.1686 0.068 Uiso 1 1 calc R . . C73 C 0.8650(4) 0.7579(3) 0.2482(4) 0.052(2) Uani 1 1 d . . . H73 H 0.8586 0.7923 0.2531 0.062 Uiso 1 1 calc R . . C74 C 0.8666(4) 0.7071(3) 0.2919(3) 0.0382(19) Uani 1 1 d . . . H74 H 0.8612 0.7059 0.3270 0.046 Uiso 1 1 calc R . . C75 C 0.8764(3) 0.6583(3) 0.2821(3) 0.0354(18) Uani 1 1 d . . . C76 C 0.8781(3) 0.6036(3) 0.3261(3) 0.0317(17) Uani 1 1 d . . . H76 H 0.8688 0.6010 0.3618 0.038 Uiso 1 1 calc R . . C77 C 0.9098(3) 0.4621(3) 0.3409(3) 0.0314(17) Uani 1 1 d . . . C78 C 0.9122(3) 0.4077(3) 0.3780(3) 0.0342(18) Uani 1 1 d . . . H78 H 0.9015 0.3993 0.4151 0.041 Uiso 1 1 calc R . . C79 C 0.9310(3) 0.3661(3) 0.3580(3) 0.0339(18) Uani 1 1 d . . . C80 C 0.9377(3) 0.4308(3) 0.2729(3) 0.0310(17) Uani 1 1 d . . . C81 C 0.9474(4) 0.4462(3) 0.2138(3) 0.039(2) Uani 1 1 d . . . C82 C 0.9002(5) 0.4537(3) 0.1909(4) 0.051(2) Uani 1 1 d . . . H82 H 0.8632 0.4486 0.2121 0.061 Uiso 1 1 calc R . . C83 C 0.9091(7) 0.4689(4) 0.1359(5) 0.075(4) Uani 1 1 d . . . H83 H 0.8775 0.4738 0.1197 0.090 Uiso 1 1 calc R . . C84 C 0.9604(8) 0.4766(4) 0.1056(4) 0.082(4) Uani 1 1 d . . . H84 H 0.9650 0.4873 0.0683 0.098 Uiso 1 1 calc R . . C85 C 1.0068(6) 0.4693(4) 0.1283(4) 0.073(4) Uani 1 1 d . . . H85 H 1.0435 0.4748 0.1065 0.088 Uiso 1 1 calc R . . C86 C 1.0005(4) 0.4536(3) 0.1837(4) 0.049(2) Uani 1 1 d . . . H86 H 1.0325 0.4482 0.1996 0.059 Uiso 1 1 calc R . . C87 C 0.9564(4) 0.2208(4) 0.3920(4) 0.049(2) Uani 1 1 d . . . H87 H 0.9492 0.2037 0.4298 0.059 Uiso 1 1 calc R . . C88 C 0.9728(5) 0.1876(4) 0.3582(4) 0.059(3) Uani 1 1 d . . . C89 C 0.9781(6) 0.1290(4) 0.3801(5) 0.074(3) Uani 1 1 d . . . H89 H 0.9729 0.1082 0.4175 0.089 Uiso 1 1 calc R . . C90 C 0.9914(6) 0.1027(4) 0.3441(6) 0.083(4) Uani 1 1 d . . . H90 H 0.9948 0.0631 0.3565 0.099 Uiso 1 1 calc R . . C91 C 0.9996(6) 0.1341(4) 0.2914(5) 0.075(3) Uani 1 1 d . . . H91 H 1.0086 0.1164 0.2667 0.089 Uiso 1 1 calc R . . C92 C 0.9952(4) 0.1904(4) 0.2734(4) 0.054(2) Uani 1 1 d . . . H92 H 1.0023 0.2110 0.2361 0.065 Uiso 1 1 calc R . . C93 C 0.8782(3) 0.5018(3) 0.4110(3) 0.0332(18) Uani 1 1 d . . . H93A H 0.8939 0.5302 0.4161 0.040 Uiso 1 1 calc R . . H93B H 0.8936 0.4642 0.4344 0.040 Uiso 1 1 calc R . . C94 C 0.8136(4) 0.5096(3) 0.4252(3) 0.0357(18) Uani 1 1 d . . . C95 C 0.7305(4) 0.5482(4) 0.4756(3) 0.044(2) Uani 1 1 d . . . H95A H 0.7233 0.5407 0.5141 0.053 Uiso 1 1 calc R . . H95B H 0.7106 0.5222 0.4710 0.053 Uiso 1 1 calc R . . C96 C 0.7057(4) 0.6090(4) 0.4452(3) 0.045(2) Uani 1 1 d . . . H96A H 0.7259 0.6352 0.4491 0.055 Uiso 1 1 calc R . . H96B H 0.6647 0.6152 0.4603 0.055 Uiso 1 1 calc R . . C97 C 0.6623(4) 0.6872(3) 0.3519(4) 0.047(2) Uani 1 1 d . . . C98 C 0.6834(4) 0.7386(4) 0.3494(4) 0.055(2) Uani 1 1 d . . . C99 C 0.7353(5) 0.7377(5) 0.3611(4) 0.063(3) Uani 1 1 d . . . H99 H 0.7598 0.7034 0.3725 0.076 Uiso 1 1 calc R . . C100 C 0.7525(6) 0.7878(7) 0.3564(5) 0.091(4) Uani 1 1 d . . . H100 H 0.7883 0.7862 0.3648 0.109 Uiso 1 1 calc R . . C101 C 0.7195(9) 0.8367(6) 0.3405(6) 0.100(5) Uani 1 1 d . . . H101 H 0.7315 0.8697 0.3378 0.120 Uiso 1 1 calc R . . C102 C 0.6675(8) 0.8388(5) 0.3279(6) 0.098(5) Uani 1 1 d . . . H102 H 0.6435 0.8735 0.3168 0.118 Uiso 1 1 calc R . . C103 C 0.6500(6) 0.7905(5) 0.3314(5) 0.077(3) Uani 1 1 d . . . H103 H 0.6148 0.7930 0.3213 0.093 Uiso 1 1 calc R . . C104 C 0.6058(4) 0.6741(4) 0.3900(4) 0.049(2) Uani 1 1 d . . . C105 C 0.5817(5) 0.7007(5) 0.4245(5) 0.067(3) Uani 1 1 d . . . H105 H 0.5979 0.7311 0.4225 0.080 Uiso 1 1 calc R . . C106 C 0.5328(5) 0.6826(6) 0.4628(5) 0.081(4) Uani 1 1 d . . . H106 H 0.5161 0.7005 0.4871 0.097 Uiso 1 1 calc R . . C107 C 0.5096(5) 0.6386(6) 0.4648(6) 0.083(4) Uani 1 1 d . . . H107 H 0.4769 0.6261 0.4909 0.099 Uiso 1 1 calc R . . C108 C 0.5325(6) 0.6127(5) 0.4304(6) 0.078(3) Uani 1 1 d . . . H108 H 0.5160 0.5826 0.4318 0.094 Uiso 1 1 calc R . . C109 C 0.5800(5) 0.6311(4) 0.3935(4) 0.063(3) Uani 1 1 d . . . H109 H 0.5959 0.6134 0.3690 0.075 Uiso 1 1 calc R . . C110 C 0.6636(5) 0.6945(4) 0.2951(4) 0.057(3) Uani 1 1 d . . . C111 C 0.6142(6) 0.7041(5) 0.2741(5) 0.089(4) Uani 1 1 d . . . H111 H 0.5778 0.7039 0.2965 0.107 Uiso 1 1 calc R . . C112 C 0.6177(8) 0.7139(6) 0.2201(6) 0.111(6) Uani 1 1 d . . . H112 H 0.5842 0.7202 0.2060 0.133 Uiso 1 1 calc R . . C113 C 0.6716(8) 0.7141(6) 0.1883(5) 0.094(4) Uani 1 1 d . . . H113 H 0.6745 0.7204 0.1520 0.112 Uiso 1 1 calc R . . C114 C 0.7198(6) 0.7057(4) 0.2073(4) 0.073(3) Uani 1 1 d . . . H114 H 0.7560 0.7060 0.1846 0.088 Uiso 1 1 calc R . . C115 C 0.7162(5) 0.6967(4) 0.2603(4) 0.055(2) Uani 1 1 d . . . H115 H 0.7503 0.6918 0.2732 0.066 Uiso 1 1 calc R . . C116 C 0.9224(4) 0.2894(3) 0.4493(3) 0.043(2) Uani 1 1 d . . . H11A H 0.9267 0.3179 0.4617 0.052 Uiso 1 1 calc R . . H11B H 0.9479 0.2548 0.4657 0.052 Uiso 1 1 calc R . . C117 C 0.8608(4) 0.2773(4) 0.4663(3) 0.044(2) Uani 1 1 d . . . C118 C 0.7869(5) 0.2363(4) 0.5423(4) 0.065(3) Uani 1 1 d . . . H11C H 0.7699 0.2555 0.5671 0.079 Uiso 1 1 calc R . . H11D H 0.7631 0.2503 0.5144 0.079 Uiso 1 1 calc R . . C119 C 0.7854(6) 0.1760(5) 0.5713(5) 0.083(4) Uani 1 1 d . . . H11E H 0.7466 0.1697 0.5925 0.099 Uiso 1 1 calc R . . H11F H 0.8124 0.1617 0.5966 0.099 Uiso 1 1 calc R . . C120 C 0.7305(7) 0.1212(6) 0.5328(6) 0.098(4) Uani 1 1 d . . . C121 C 0.6948(6) 0.1797(6) 0.5093(6) 0.088(4) Uani 1 1 d . . . C122 C 0.7086(8) 0.2121(8) 0.4572(7) 0.127(6) Uani 1 1 d . . . H122 H 0.7386 0.1986 0.4349 0.152 Uiso 1 1 calc R . . C123 C 0.6789(8) 0.2650(8) 0.4363(7) 0.131(7) Uani 1 1 d . . . H123 H 0.6889 0.2872 0.3995 0.157 Uiso 1 1 calc R . . C124 C 0.6371(7) 0.2855(7) 0.4660(6) 0.103(5) Uani 1 1 d . . . H124 H 0.6164 0.3213 0.4504 0.124 Uiso 1 1 calc R . . C125 C 0.6237(7) 0.2547(6) 0.5197(7) 0.097(4) Uani 1 1 d . . . H125 H 0.5949 0.2700 0.5415 0.117 Uiso 1 1 calc R . . C126 C 0.6520(6) 0.2019(6) 0.5417(5) 0.081(4) Uani 1 1 d . . . H126 H 0.6427 0.1805 0.5788 0.097 Uiso 1 1 calc R . . C127 C 0.7007(7) 0.0858(6) 0.5886(6) 0.090(4) Uani 1 1 d . . . C128 C 0.6479(7) 0.0735(6) 0.5962(8) 0.122(6) Uani 1 1 d . . . H128 H 0.6283 0.0887 0.5670 0.146 Uiso 1 1 calc R . . C129 C 0.6208(8) 0.0391(7) 0.6456(9) 0.123(6) Uani 1 1 d . . . H129 H 0.5832 0.0318 0.6491 0.148 Uiso 1 1 calc R . . C130 C 0.6469(11) 0.0152(8) 0.6894(9) 0.129(6) Uani 1 1 d . . . H130 H 0.6284 -0.0077 0.7234 0.155 Uiso 1 1 calc R . . C131 C 0.7010(11) 0.0268(6) 0.6808(8) 0.132(7) Uani 1 1 d . . . H131 H 0.7196 0.0112 0.7107 0.158 Uiso 1 1 calc R . . C132 C 0.7324(8) 0.0597(6) 0.6320(7) 0.111(5) Uani 1 1 d . . . H132 H 0.7711 0.0644 0.6280 0.134 Uiso 1 1 calc R . . C133 C 0.7383(7) 0.0870(7) 0.4989(7) 0.106(5) Uani 1 1 d . . . C134 C 0.7777(7) 0.0366(7) 0.5124(7) 0.115(5) Uani 1 1 d . . . H134 H 0.8005 0.0282 0.5382 0.138 Uiso 1 1 calc R . . C135 C 0.7823(10) 0.0001(7) 0.4876(8) 0.138(7) Uani 1 1 d . . . H135 H 0.8083 -0.0334 0.4962 0.165 Uiso 1 1 calc R . . C136 C 0.7470(11) 0.0137(13) 0.4483(12) 0.205(13) Uani 1 1 d . . . H136 H 0.7498 -0.0111 0.4311 0.246 Uiso 1 1 calc R . . C137 C 0.7099(10) 0.0621(13) 0.4361(13) 0.237(17) Uani 1 1 d . . . H137 H 0.6867 0.0706 0.4105 0.284 Uiso 1 1 calc R . . C138 C 0.7058(9) 0.0989(11) 0.4603(9) 0.159(9) Uani 1 1 d . . . H138 H 0.6804 0.1328 0.4506 0.190 Uiso 1 1 calc R . . C141 C 1.1455(4) 0.7054(3) 0.1751(4) 0.046(2) Uani 1 1 d . . . H141 H 1.1537 0.7008 0.1423 0.055 Uiso 1 1 calc R . . C142 C 1.1300(5) 0.7604(4) 0.1747(4) 0.060(3) Uani 1 1 d . . . H142 H 1.1279 0.7921 0.1423 0.072 Uiso 1 1 calc R . . C143 C 1.1183(5) 0.7661(4) 0.2223(4) 0.064(3) Uani 1 1 d . . . H143 H 1.1074 0.8023 0.2236 0.076 Uiso 1 1 calc R . . C144 C 1.1222(4) 0.7196(4) 0.2686(4) 0.051(2) Uani 1 1 d . . . H144 H 1.1148 0.7234 0.3018 0.061 Uiso 1 1 calc R . . C145 C 1.1371(4) 0.6679(3) 0.2661(3) 0.040(2) Uani 1 1 d . . . C146 C 1.1426(4) 0.6165(3) 0.3126(3) 0.041(2) Uani 1 1 d . . . H146 H 1.1363 0.6167 0.3472 0.049 Uiso 1 1 calc R . . C147 C 1.1781(3) 0.4748(3) 0.3280(3) 0.0328(17) Uani 1 1 d . . . C148 C 1.1865(3) 0.4195(3) 0.3634(3) 0.0353(18) Uani 1 1 d . . . H148 H 1.1836 0.4101 0.4004 0.042 Uiso 1 1 calc R . . C149 C 1.1992(3) 0.3786(3) 0.3424(3) 0.0334(18) Uani 1 1 d . . . C150 C 1.1985(3) 0.4457(3) 0.2583(3) 0.0335(18) Uani 1 1 d . . . C151 C 1.2097(4) 0.4583(3) 0.2001(3) 0.041(2) Uani 1 1 d . . . C152 C 1.1663(5) 0.4618(4) 0.1750(4) 0.058(3) Uani 1 1 d . . . H152 H 1.1285 0.4571 0.1944 0.069 Uiso 1 1 calc R . . C153 C 1.1789(8) 0.4725(4) 0.1203(5) 0.085(5) Uani 1 1 d . . . H153 H 1.1492 0.4762 0.1023 0.102 Uiso 1 1 calc R . . C154 C 1.2324(9) 0.4774(5) 0.0938(5) 0.096(5) Uani 1 1 d . . . H154 H 1.2404 0.4839 0.0570 0.116 Uiso 1 1 calc R . . C155 C 1.2764(6) 0.4731(5) 0.1185(5) 0.080(4) Uani 1 1 d . . . H155 H 1.3143 0.4765 0.0989 0.095 Uiso 1 1 calc R . . C156 C 1.2648(5) 0.4639(4) 0.1716(4) 0.059(3) Uani 1 1 d . . . H156 H 1.2948 0.4613 0.1888 0.070 Uiso 1 1 calc R . . C157 C 1.2327(4) 0.2338(4) 0.3758(4) 0.048(2) Uani 1 1 d . . . H157 H 1.2320 0.2199 0.4130 0.057 Uiso 1 1 calc R . . C158 C 1.2479(4) 0.1958(4) 0.3471(4) 0.049(2) Uani 1 1 d . . . C159 C 1.2584(6) 0.1384(4) 0.3747(4) 0.073(3) Uani 1 1 d . . . H159 H 1.2561 0.1228 0.4121 0.087 Uiso 1 1 calc R . . C160 C 1.2724(6) 0.1041(4) 0.3457(5) 0.082(4) Uani 1 1 d . . . H160 H 1.2816 0.0647 0.3630 0.099 Uiso 1 1 calc R . . C161 C 1.2726(6) 0.1279(4) 0.2923(5) 0.080(4) Uani 1 1 d . . . H161 H 1.2795 0.1051 0.2722 0.096 Uiso 1 1 calc R . . C162 C 1.2626(5) 0.1855(4) 0.2677(4) 0.061(3) Uani 1 1 d . . . H162 H 1.2651 0.2020 0.2302 0.074 Uiso 1 1 calc R . . C163 C 1.1591(4) 0.5153(4) 0.3980(3) 0.041(2) Uani 1 1 d . . . H16A H 1.1557 0.4762 0.4235 0.049 Uiso 1 1 calc R . . H16B H 1.1248 0.5396 0.4075 0.049 Uiso 1 1 calc R . . C164 C 1.2135(4) 0.5340(3) 0.4011(3) 0.040(2) Uani 1 1 d . . . C165 C 1.2486(4) 0.5893(4) 0.4364(4) 0.047(2) Uani 1 1 d . . . H16C H 1.2846 0.5635 0.4349 0.056 Uiso 1 1 calc R . . H16D H 1.2377 0.5892 0.4728 0.056 Uiso 1 1 calc R . . C166 C 1.2587(4) 0.6475(4) 0.3972(4) 0.053(2) Uani 1 1 d . . . H16E H 1.2758 0.6652 0.4138 0.064 Uiso 1 1 calc R . . H16F H 1.2213 0.6697 0.3898 0.064 Uiso 1 1 calc R . . C167 C 1.3750(4) 0.6588(4) 0.3443(4) 0.059(3) Uani 1 1 d . . . C168 C 1.3848(4) 0.6118(4) 0.3972(4) 0.054(2) Uani 1 1 d . . . C169 C 1.3966(5) 0.5569(4) 0.4015(5) 0.070(3) Uani 1 1 d . . . H169 H 1.3999 0.5485 0.3712 0.084 Uiso 1 1 calc R . . C170 C 1.4037(5) 0.5136(6) 0.4507(7) 0.094(4) Uani 1 1 d . . . H170 H 1.4141 0.4759 0.4536 0.113 Uiso 1 1 calc R . . C171 C 1.3953(5) 0.5267(7) 0.4954(6) 0.093(5) Uani 1 1 d . . . H171 H 1.3994 0.4975 0.5289 0.112 Uiso 1 1 calc R . . C172 C 1.3813(5) 0.5807(6) 0.4916(5) 0.080(3) Uani 1 1 d . . . H172 H 1.3744 0.5891 0.5224 0.095 Uiso 1 1 calc R . . C173 C 1.3771(4) 0.6232(5) 0.4425(4) 0.063(3) Uani 1 1 d . . . H173 H 1.3689 0.6610 0.4397 0.075 Uiso 1 1 calc R . . C174 C 1.4182(5) 0.6540(5) 0.2950(4) 0.064(3) Uani 1 1 d . . . C175 C 1.4057(6) 0.6856(6) 0.2443(5) 0.091(4) Uani 1 1 d . . . H175 H 1.3694 0.7076 0.2403 0.109 Uiso 1 1 calc R . . C176 C 1.4456(9) 0.6853(8) 0.1997(5) 0.115(6) Uani 1 1 d . . . H176 H 1.4361 0.7082 0.1656 0.138 Uiso 1 1 calc R . . C177 C 1.4969(9) 0.6543(8) 0.2021(8) 0.114(6) Uani 1 1 d . . . H177 H 1.5231 0.6541 0.1708 0.137 Uiso 1 1 calc R . . C178 C 1.5102(7) 0.6225(8) 0.2520(7) 0.117(5) Uani 1 1 d . . . H178 H 1.5463 0.6001 0.2557 0.141 Uiso 1 1 calc R . . C179 C 1.4703(6) 0.6236(6) 0.2968(5) 0.086(4) Uani 1 1 d . . . H179 H 1.4804 0.6016 0.3307 0.103 Uiso 1 1 calc R . . C180 C 1.3774(5) 0.7167(4) 0.3414(4) 0.064(3) Uani 1 1 d . . . C181 C 1.4283(6) 0.7292(5) 0.3456(5) 0.080(4) Uani 1 1 d . . . H181 H 1.4591 0.6998 0.3536 0.095 Uiso 1 1 calc R . . C182 C 1.4364(8) 0.7806(8) 0.3391(9) 0.133(7) Uani 1 1 d . . . H182 H 1.4711 0.7867 0.3442 0.160 Uiso 1 1 calc R . . C183 C 1.3922(9) 0.8248(8) 0.3245(8) 0.136(7) Uani 1 1 d . . . H183 H 1.3976 0.8618 0.3176 0.164 Uiso 1 1 calc R . . C184 C 1.3407(8) 0.8148(5) 0.3201(6) 0.107(5) Uani 1 1 d . . . H184 H 1.3107 0.8446 0.3103 0.129 Uiso 1 1 calc R . . C185 C 1.3334(6) 0.7601(5) 0.3302(5) 0.089(4) Uani 1 1 d . . . H185 H 1.2974 0.7526 0.3293 0.107 Uiso 1 1 calc R . . C186 C 1.2024(4) 0.3029(3) 0.4311(3) 0.042(2) Uani 1 1 d . . . H18A H 1.1895 0.2654 0.4490 0.051 Uiso 1 1 calc R . . H18B H 1.1746 0.3287 0.4454 0.051 Uiso 1 1 calc R . . C187 C 1.2623(4) 0.2998(4) 0.4423(4) 0.043(2) Uani 1 1 d . . . C188 C 1.3202(5) 0.2628(5) 0.5113(4) 0.064(3) Uani 1 1 d . . . H18C H 1.3085 0.2625 0.5477 0.076 Uiso 1 1 calc R . . H18D H 1.3390 0.2968 0.4886 0.076 Uiso 1 1 calc R . . C189 C 1.3627(5) 0.2127(5) 0.5126(4) 0.077(3) Uani 1 1 d . . . H18E H 1.3426 0.1795 0.5252 0.093 Uiso 1 1 calc R . . H18F H 1.3881 0.2054 0.5379 0.093 Uiso 1 1 calc R . . C190 C 1.4586(6) 0.1569(6) 0.4606(6) 0.094(4) Uani 1 1 d . . . C191 C 1.4317(6) 0.1153(6) 0.4577(6) 0.086(4) Uani 1 1 d . . . C192 C 1.3756(8) 0.1095(7) 0.4659(6) 0.114(5) Uani 1 1 d . . . H192 H 1.3500 0.1412 0.4687 0.137 Uiso 1 1 calc R . . C193 C 1.3494(12) 0.0671(8) 0.4710(9) 0.173(11) Uani 1 1 d . . . H193 H 1.3089 0.0682 0.4784 0.207 Uiso 1 1 calc R . . C194 C 1.3875(12) 0.0209(10) 0.4641(9) 0.149(8) Uani 1 1 d . . . H194 H 1.3737 -0.0107 0.4656 0.179 Uiso 1 1 calc R . . C195 C 1.4447(13) 0.0236(8) 0.4553(8) 0.144(8) Uani 1 1 d . . . H195 H 1.4705 -0.0068 0.4499 0.173 Uiso 1 1 calc R . . C196 C 1.4672(8) 0.0664(7) 0.4538(6) 0.111(5) Uani 1 1 d . . . H196 H 1.5074 0.0638 0.4501 0.133 Uiso 1 1 calc R . . C197 C 1.4750(6) 0.1439(6) 0.5120(5) 0.085(4) Uani 1 1 d . . . C198 C 1.5044(6) 0.1762(8) 0.5209(6) 0.106(5) Uani 1 1 d . . . H198 H 1.5194 0.2074 0.4918 0.127 Uiso 1 1 calc R . . C199 C 1.5129(7) 0.1648(10) 0.5706(7) 0.146(8) Uani 1 1 d . . . H199 H 1.5353 0.1876 0.5745 0.176 Uiso 1 1 calc R . . C200 C 1.4908(8) 0.1225(7) 0.6151(6) 0.109(5) Uani 1 1 d . . . H200 H 1.4951 0.1175 0.6495 0.131 Uiso 1 1 calc R . . C201 C 1.4628(7) 0.0882(6) 0.6085(5) 0.092(4) Uani 1 1 d . . . H201 H 1.4489 0.0573 0.6389 0.111 Uiso 1 1 calc R . . C202 C 1.4529(6) 0.0961(6) 0.5577(6) 0.088(4) Uani 1 1 d . . . H202 H 1.4330 0.0713 0.5539 0.106 Uiso 1 1 calc R . . C203 C 1.5061(6) 0.1765(7) 0.4123(6) 0.102(5) Uani 1 1 d . . . C204 C 1.4928(8) 0.1948(9) 0.3621(7) 0.140(7) Uani 1 1 d . . . H204 H 1.4548 0.1965 0.3582 0.168 Uiso 1 1 calc R . . C205 C 1.5395(11) 0.2121(11) 0.3138(8) 0.167(9) Uani 1 1 d . . . H205 H 1.5313 0.2263 0.2789 0.201 Uiso 1 1 calc R . . C206 C 1.5933(11) 0.2068(11) 0.3215(9) 0.163(9) Uani 1 1 d . . . H206 H 1.6225 0.2187 0.2912 0.195 Uiso 1 1 calc R . . C207 C 1.6082(10) 0.1851(12) 0.3712(8) 0.175(10) Uani 1 1 d . . . H207 H 1.6468 0.1813 0.3748 0.209 Uiso 1 1 calc R . . C208 C 1.5647(8) 0.1686(9) 0.4164(8) 0.135(7) Uani 1 1 d . . . H208 H 1.5748 0.1518 0.4507 0.162 Uiso 1 1 calc R . . C211 C 0.8250(5) 0.2981(6) 0.3162(5) 0.082(4) Uani 1 1 d . . . H211 H 0.8259 0.2875 0.3527 0.098 Uiso 1 1 calc R . . C212 C 0.7722(6) 0.3044(8) 0.3009(7) 0.121(6) Uani 1 1 d . . . H212 H 0.7383 0.2967 0.3268 0.145 Uiso 1 1 calc R . . C213 C 0.7709(6) 0.3221(8) 0.2470(6) 0.110(5) Uani 1 1 d . . . H213 H 0.7356 0.3282 0.2356 0.132 Uiso 1 1 calc R . . C214 C 0.8198(5) 0.3305(6) 0.2112(5) 0.081(4) Uani 1 1 d . . . H214 H 0.8194 0.3426 0.1744 0.097 Uiso 1 1 calc R . . C215 C 0.8716(5) 0.3213(4) 0.2289(4) 0.060(3) Uani 1 1 d . . . C216 C 0.9242(4) 0.3283(4) 0.1925(4) 0.045(2) Uani 1 1 d . . . H216 H 0.9256 0.3359 0.1561 0.054 Uiso 1 1 calc R . . C217 C 1.0695(4) 0.3254(3) 0.1967(3) 0.0361(19) Uani 1 1 d . . . C218 C 1.1229(4) 0.3301(3) 0.1655(3) 0.040(2) Uani 1 1 d . . . H218 H 1.1296 0.3347 0.1292 0.048 Uiso 1 1 calc R . . C219 C 1.1666(4) 0.3274(3) 0.1905(3) 0.039(2) Uani 1 1 d . . . C220 C 1.1042(4) 0.3133(3) 0.2687(3) 0.0318(18) Uani 1 1 d . . . C221 C 1.0924(4) 0.3009(4) 0.3271(3) 0.046(2) Uani 1 1 d . . . C222 C 1.0748(4) 0.3446(5) 0.3456(4) 0.065(3) Uani 1 1 d . . . H222 H 1.0703 0.3825 0.3212 0.078 Uiso 1 1 calc R . . C223 C 1.0641(5) 0.3314(10) 0.4002(6) 0.108(6) Uani 1 1 d . . . H223 H 1.0529 0.3611 0.4125 0.129 Uiso 1 1 calc R . . C224 C 1.0687(7) 0.2799(12) 0.4354(7) 0.129(9) Uani 1 1 d . . . H224 H 1.0603 0.2725 0.4724 0.154 Uiso 1 1 calc R . . C225 C 1.0859(6) 0.2364(9) 0.4178(6) 0.123(7) Uani 1 1 d . . . H225 H 1.0901 0.1989 0.4431 0.147 Uiso 1 1 calc R . . C226 C 1.0978(5) 0.2465(5) 0.3620(4) 0.069(3) Uani 1 1 d . . . H226 H 1.1087 0.2165 0.3500 0.083 Uiso 1 1 calc R . . C227 C 1.3130(4) 0.3309(4) 0.1732(4) 0.051(2) Uani 1 1 d . . . H227 H 1.3288 0.3351 0.1375 0.062 Uiso 1 1 calc R . . C228 C 1.3485(4) 0.3260(4) 0.2107(4) 0.052(2) Uani 1 1 d . . . C229 C 1.4056(5) 0.3292(6) 0.1963(5) 0.077(3) Uani 1 1 d . . . H229 H 1.4249 0.3346 0.1610 0.092 Uiso 1 1 calc R . . C230 C 1.4351(5) 0.3244(6) 0.2346(6) 0.086(4) Uani 1 1 d . . . H230 H 1.4750 0.3267 0.2258 0.103 Uiso 1 1 calc R . . C231 C 1.4067(5) 0.3166(5) 0.2842(5) 0.077(3) Uani 1 1 d . . . H231 H 1.4265 0.3125 0.3109 0.092 Uiso 1 1 calc R . . C232 C 1.3477(5) 0.3144(4) 0.2962(4) 0.058(3) Uani 1 1 d . . . H232 H 1.3276 0.3097 0.3311 0.070 Uiso 1 1 calc R . . C233 C 1.0252(4) 0.3380(3) 0.1203(3) 0.041(2) Uani 1 1 d . . . H23C H 1.0613 0.3528 0.0984 0.049 Uiso 1 1 calc R . . H23D H 0.9928 0.3650 0.1054 0.049 Uiso 1 1 calc R . . C234 C 1.0237(4) 0.2807(4) 0.1190(4) 0.047(2) Uani 1 1 d . . . C235 C 0.9889(4) 0.2327(4) 0.0768(4) 0.052(2) Uani 1 1 d . . . H23E H 1.0181 0.2018 0.0929 0.062 Uiso 1 1 calc R . . H23F H 0.9960 0.2406 0.0383 0.062 Uiso 1 1 calc R . . C236 C 0.9303(5) 0.2145(4) 0.1018(4) 0.058(3) Uani 1 1 d . . . H23G H 0.9278 0.1814 0.0951 0.070 Uiso 1 1 calc R . . H23H H 0.9010 0.2450 0.0852 0.070 Uiso 1 1 calc R . . C237 C 0.8543(5) 0.1561(4) 0.1977(4) 0.067(3) Uani 1 1 d . . . C238 C 0.8705(5) 0.1118(5) 0.1727(5) 0.070(3) Uani 1 1 d . . . C239 C 0.9213(6) 0.0762(5) 0.1768(8) 0.113(6) Uani 1 1 d . . . H239 H 0.9467 0.0768 0.1972 0.135 Uiso 1 1 calc R . . C240 C 0.9344(9) 0.0406(7) 0.1515(11) 0.159(10) Uani 1 1 d . . . H240 H 0.9696 0.0165 0.1545 0.191 Uiso 1 1 calc R . . C241 C 0.9010(11) 0.0374(8) 0.1227(9) 0.143(9) Uani 1 1 d . . . H241 H 0.9118 0.0108 0.1066 0.172 Uiso 1 1 calc R . . C242 C 0.8512(9) 0.0725(6) 0.1163(6) 0.108(5) Uani 1 1 d . . . H242 H 0.8273 0.0712 0.0950 0.130 Uiso 1 1 calc R . . C243 C 0.8357(7) 0.1097(5) 0.1412(5) 0.088(4) Uani 1 1 d . . . H243 H 0.8009 0.1344 0.1368 0.105 Uiso 1 1 calc R . . C244 C 0.7993(5) 0.1905(6) 0.1899(5) 0.071(3) Uani 1 1 d . . . C245 C 0.7486(8) 0.1649(8) 0.2158(7) 0.119(6) Uani 1 1 d . . . H245 H 0.7496 0.1269 0.2402 0.143 Uiso 1 1 calc R . . C246 C 0.6962(8) 0.1991(13) 0.2033(11) 0.157(9) Uani 1 1 d . . . H246 H 0.6626 0.1812 0.2169 0.189 Uiso 1 1 calc R . . C247 C 0.6902(9) 0.2526(11) 0.1751(10) 0.135(8) Uani 1 1 d . . . H247 H 0.6531 0.2730 0.1721 0.162 Uiso 1 1 calc R . . C248 C 0.7393(8) 0.2801(8) 0.1490(6) 0.109(5) Uani 1 1 d . . . H248 H 0.7367 0.3187 0.1264 0.131 Uiso 1 1 calc R . . C249 C 0.7920(6) 0.2476(6) 0.1581(5) 0.081(4) Uani 1 1 d . . . H249 H 0.8254 0.2658 0.1414 0.098 Uiso 1 1 calc R . . C250 C 0.8532(6) 0.1308(6) 0.2591(5) 0.089(4) Uani 1 1 d . . . C251 C 0.8565(11) 0.0740(8) 0.2890(6) 0.162(9) Uani 1 1 d . . . H251 H 0.8624 0.0482 0.2722 0.194 Uiso 1 1 calc R . . C252 C 0.8511(12) 0.0549(9) 0.3437(8) 0.184(11) Uani 1 1 d . . . H252 H 0.8513 0.0160 0.3647 0.221 Uiso 1 1 calc R . . C253 C 0.8454(14) 0.0920(10) 0.3685(8) 0.204(14) Uani 1 1 d . . . H253 H 0.8432 0.0781 0.4059 0.245 Uiso 1 1 calc R . . C254 C 0.8430(8) 0.1485(9) 0.3392(7) 0.128(6) Uani 1 1 d . . . H254 H 0.8391 0.1741 0.3557 0.153 Uiso 1 1 calc R . . C255 C 0.8464(6) 0.1673(7) 0.2848(5) 0.097(5) Uani 1 1 d . . . H255 H 0.8440 0.2064 0.2643 0.117 Uiso 1 1 calc R . . C256 C 1.2394(4) 0.3396(4) 0.1070(3) 0.049(2) Uani 1 1 d . . . H25C H 1.2715 0.3624 0.0894 0.059 Uiso 1 1 calc R . . H25D H 1.2073 0.3586 0.0875 0.059 Uiso 1 1 calc R . . C257 C 1.2582(4) 0.2824(4) 0.1053(4) 0.049(2) Uani 1 1 d . . . C258 C 1.3166(5) 0.2285(5) 0.0542(4) 0.073(3) Uani 1 1 d . . . H25E H 1.3191 0.2353 0.0163 0.088 Uiso 1 1 calc R . . H25F H 1.2893 0.2011 0.0758 0.088 Uiso 1 1 calc R . . C259 C 1.3755(5) 0.2030(6) 0.0694(4) 0.085(4) Uani 1 1 d . . . H25G H 1.4036 0.2297 0.0477 0.102 Uiso 1 1 calc R . . H25H H 1.3887 0.1683 0.0624 0.102 Uiso 1 1 calc R . . C260 C 1.4459(6) 0.1578(6) 0.1504(5) 0.087(4) Uani 1 1 d . . . C261 C 1.4604(5) 0.1119(5) 0.1288(5) 0.074(3) Uani 1 1 d . . . C262 C 1.4992(5) 0.1180(5) 0.0799(6) 0.082(4) Uani 1 1 d . . . H262 H 1.5155 0.1522 0.0616 0.099 Uiso 1 1 calc R . . C263 C 1.5152(6) 0.0801(6) 0.0570(7) 0.098(4) Uani 1 1 d . . . H263 H 1.5424 0.0868 0.0249 0.118 Uiso 1 1 calc R . . C264 C 1.4887(8) 0.0282(7) 0.0836(9) 0.121(6) Uani 1 1 d . . . H264 H 1.4984 -0.0010 0.0707 0.145 Uiso 1 1 calc R . . C265 C 1.4480(8) 0.0251(7) 0.1295(7) 0.110(5) Uani 1 1 d . . . H265 H 1.4284 -0.0070 0.1473 0.132 Uiso 1 1 calc R . . C266 C 1.4346(8) 0.0663(7) 0.1508(6) 0.108(5) Uani 1 1 d . . . H266 H 1.4061 0.0615 0.1819 0.130 Uiso 1 1 calc R . . C267 C 1.4389(5) 0.1374(7) 0.2106(5) 0.088(4) Uani 1 1 d . . . C268 C 1.4092(6) 0.1716(7) 0.2372(6) 0.098(5) Uani 1 1 d . . . H268 H 1.3882 0.2060 0.2183 0.118 Uiso 1 1 calc R . . C269 C 1.4092(8) 0.1574(10) 0.2897(7) 0.130(6) Uani 1 1 d . . . H269 H 1.3913 0.1834 0.3059 0.155 Uiso 1 1 calc R . . C270 C 1.4347(10) 0.1066(10) 0.3189(7) 0.138(7) Uani 1 1 d . . . H270 H 1.4328 0.0954 0.3560 0.166 Uiso 1 1 calc R . . C271 C 1.4631(9) 0.0720(8) 0.2935(7) 0.129(6) Uani 1 1 d . . . H271 H 1.4819 0.0367 0.3135 0.154 Uiso 1 1 calc R . . C272 C 1.4658(7) 0.0861(6) 0.2395(6) 0.101(5) Uani 1 1 d . . . H272 H 1.4858 0.0609 0.2230 0.121 Uiso 1 1 calc R . . C273 C 1.4859(6) 0.2027(6) 0.1264(5) 0.078(3) Uani 1 1 d . . . C274 C 1.5448(6) 0.1802(7) 0.1348(6) 0.103(5) Uani 1 1 d . . . H274 H 1.5545 0.1408 0.1504 0.124 Uiso 1 1 calc R . . C275 C 1.5850(9) 0.2129(9) 0.1214(7) 0.115(6) Uani 1 1 d . . . H275 H 1.6228 0.1971 0.1275 0.138 Uiso 1 1 calc R . . C276 C 1.5718(10) 0.2670(14) 0.0999(9) 0.143(8) Uani 1 1 d . . . H276 H 1.6007 0.2898 0.0918 0.172 Uiso 1 1 calc R . . C277 C 1.5192(11) 0.2932(8) 0.0882(6) 0.123(6) Uani 1 1 d . . . H277 H 1.5117 0.3326 0.0703 0.147 Uiso 1 1 calc R . . C278 C 1.4763(8) 0.2571(6) 0.1047(6) 0.104(5) Uani 1 1 d . . . H278 H 1.4385 0.2739 0.0995 0.125 Uiso 1 1 calc R . . N1 N 0.8210(3) 0.5653(3) 0.2396(3) 0.0365(16) Uani 1 1 d . . . N2 N 0.9065(3) 0.5882(2) 0.1622(2) 0.0341(15) Uani 1 1 d . . . N3 N 0.9567(3) 0.5988(3) 0.1279(2) 0.0372(16) Uani 1 1 d . . . N4 N 0.9926(3) 0.5775(2) 0.2044(2) 0.0290(14) Uani 1 1 d . . . N5 N 1.0903(3) 0.5780(2) 0.2005(2) 0.0311(15) Uani 1 1 d . . . N6 N 1.1563(3) 0.5982(3) 0.1217(3) 0.0395(16) Uani 1 1 d . . . N7 N 1.1956(3) 0.5927(3) 0.1518(3) 0.0368(15) Uani 1 1 d . . . N8 N 1.2654(3) 0.5823(3) 0.2161(3) 0.0431(17) Uani 1 1 d . . . N9 N 0.8952(3) 0.6938(3) 0.0177(3) 0.0440(18) Uani 1 1 d . . . H9 H 0.8848 0.6663 0.0136 0.053 Uiso 1 1 calc R . . N10 N 1.2127(4) 0.6978(3) -0.0052(3) 0.0498(19) Uani 1 1 d . . . H10 H 1.2356 0.6734 -0.0172 0.060 Uiso 1 1 calc R . . N11 N 0.8853(3) 0.6582(3) 0.2334(3) 0.0369(16) Uani 1 1 d . . . N12 N 0.8922(3) 0.5594(2) 0.3160(2) 0.0299(14) Uani 1 1 d . . . N13 N 0.8949(3) 0.5076(3) 0.3558(2) 0.0351(15) Uani 1 1 d . . . N14 N 0.9223(3) 0.4740(3) 0.2878(2) 0.0343(15) Uani 1 1 d . . . N15 N 0.9439(3) 0.3769(2) 0.3049(2) 0.0303(14) Uani 1 1 d . . . N16 N 0.9388(3) 0.3097(3) 0.3917(3) 0.0367(16) Uani 1 1 d . . . N17 N 0.9526(3) 0.2728(3) 0.3675(3) 0.0419(17) Uani 1 1 d . . . N18 N 0.9814(3) 0.2185(3) 0.3051(3) 0.0459(18) Uani 1 1 d . . . N19 N 0.7917(3) 0.5372(3) 0.4575(2) 0.0356(15) Uani 1 1 d . . . H19A H 0.8153 0.5492 0.4682 0.043 Uiso 1 1 calc R . . N20 N 0.8456(4) 0.2511(3) 0.5170(3) 0.057(2) Uani 1 1 d . . . H20A H 0.8712 0.2416 0.5374 0.069 Uiso 1 1 calc R . . N21 N 1.1488(3) 0.6610(3) 0.2188(3) 0.0389(16) Uani 1 1 d . . . N22 N 1.1563(3) 0.5705(3) 0.3046(2) 0.0326(15) Uani 1 1 d . . . N23 N 1.1624(3) 0.5192(3) 0.3443(2) 0.0355(15) Uani 1 1 d . . . N24 N 1.1830(3) 0.4891(3) 0.2746(2) 0.0328(14) Uani 1 1 d . . . N25 N 1.2051(3) 0.3911(3) 0.2897(3) 0.0363(15) Uani 1 1 d . . . N26 N 1.2049(3) 0.3228(3) 0.3740(3) 0.0370(16) Uani 1 1 d . . . N27 N 1.2206(3) 0.2856(3) 0.3493(3) 0.0373(16) Uani 1 1 d . . . N28 N 1.2498(3) 0.2190(3) 0.2945(3) 0.0476(18) Uani 1 1 d . . . N29 N 1.2039(3) 0.5692(3) 0.4257(3) 0.0398(16) Uani 1 1 d . . . H29A H 1.1681 0.5811 0.4362 0.048 Uiso 1 1 calc R . . N30 N 1.2692(4) 0.2665(3) 0.4915(3) 0.0523(19) Uani 1 1 d . . . H30X H 1.2422 0.2460 0.5128 0.063 Uiso 1 1 calc R . . N31 N 0.8733(4) 0.3066(3) 0.2811(3) 0.054(2) Uani 1 1 d . . . N32 N 0.9696(3) 0.3242(3) 0.2094(3) 0.0395(17) Uani 1 1 d . . . N33 N 1.0214(3) 0.3310(3) 0.1754(3) 0.0416(17) Uani 1 1 d . . . N34 N 1.0589(3) 0.3174(2) 0.2483(2) 0.0327(15) Uani 1 1 d . . . N35 N 1.1577(3) 0.3192(2) 0.2430(3) 0.0353(15) Uani 1 1 d . . . N36 N 1.2213(3) 0.3349(3) 0.1622(3) 0.0409(17) Uani 1 1 d . . . N37 N 1.2604(3) 0.3293(3) 0.1916(3) 0.0392(16) Uani 1 1 d . . . N38 N 1.3193(3) 0.3189(3) 0.2600(3) 0.0467(18) Uani 1 1 d . . . N39 N 0.9949(3) 0.2827(3) 0.0839(3) 0.0457(18) Uani 1 1 d . . . H39A H 0.9788 0.3154 0.0640 0.055 Uiso 1 1 calc R . . N40 N 1.2946(4) 0.2805(4) 0.0617(3) 0.058(2) Uani 1 1 d . . . H40 H 1.3056 0.3119 0.0366 0.069 Uiso 1 1 calc R . . O1 O 0.9468(3) 0.7130(2) 0.0633(3) 0.0556(17) Uani 1 1 d . . . O2 O 1.1391(3) 0.7096(3) 0.0588(3) 0.0583(17) Uani 1 1 d . . . O3 O 0.7850(3) 0.4906(3) 0.4084(2) 0.0517(16) Uani 1 1 d . . . O4 O 0.8300(3) 0.2923(3) 0.4326(3) 0.073(2) Uani 1 1 d . . . O5 O 1.2598(3) 0.5146(3) 0.3840(3) 0.0523(16) Uani 1 1 d . . . O6 O 1.2969(3) 0.3279(3) 0.4084(3) 0.0554(16) Uani 1 1 d . . . O7 O 1.0496(3) 0.2390(3) 0.1474(3) 0.0591(18) Uani 1 1 d . . . O8 O 1.2404(3) 0.2412(3) 0.1422(3) 0.0614(18) Uani 1 1 d . . . F1 F 0.8145(3) 0.6103(2) 0.5068(2) 0.0654(15) Uani 1 1 d . . . F2 F 0.8958(3) 0.6433(4) 0.4964(4) 0.125(3) Uani 1 1 d . . . F3 F 0.8927(4) 0.5850(7) 0.4597(7) 0.223(8) Uani 1 1 d . . . F4 F 0.8538(8) 0.6652(8) 0.4272(5) 0.260(10) Uani 1 1 d . . . F5 F 0.8522(3) 0.6446(2) -0.0372(2) 0.0695(17) Uani 1 1 d . . . F6 F 0.8258(7) 0.5626(3) -0.0187(4) 0.191(7) Uani 1 1 d . . . F7 F 0.8485(4) 0.5770(3) 0.0448(3) 0.099(2) Uani 1 1 d . . . F8 F 0.9142(6) 0.5646(5) -0.0163(5) 0.210(7) Uani 1 1 d . . . F9 F 1.2195(8) 0.1484(4) 0.4923(4) 0.199(7) Uani 1 1 d . . . F10 F 1.1389(14) 0.1329(15) 0.5439(12) 0.41(2) Uani 1 1 d . . . F11 F 1.1968(12) 0.1058(6) 0.5776(4) 0.320(15) Uani 1 1 d . . . F12 F 1.1760(5) 0.1947(4) 0.5429(5) 0.171(5) Uani 1 1 d . . . F13 F 0.6349(5) 0.6587(4) 0.0386(3) 0.135(3) Uani 1 1 d . . . F14 F 0.6160(6) 0.7117(7) 0.0835(6) 0.198(6) Uani 1 1 d . . . F15 F 0.7042(4) 0.6722(5) 0.0722(4) 0.141(4) Uani 1 1 d . . . F16 F 0.6379(5) 0.6185(6) 0.1249(4) 0.176(5) Uani 1 1 d . . . F17 F 1.1154(3) 0.6215(2) 0.4909(2) 0.0633(15) Uani 1 1 d . . . F18 F 1.0281(5) 0.6670(8) 0.4783(6) 0.241(9) Uani 1 1 d . . . F19 F 1.0764(3) 0.6292(4) 0.4237(3) 0.113(3) Uani 1 1 d . . . F20 F 1.0425(9) 0.5813(10) 0.5014(8) 0.386(19) Uani 1 1 d . . . F21 F 0.8713(6) 0.4400(4) -0.0047(5) 0.188(6) Uani 1 1 d . . . F22 F 0.9151(3) 0.3528(3) 0.0133(2) 0.0794(19) Uani 1 1 d . . . F23 F 0.8555(14) 0.3763(10) 0.0719(9) 0.44(2) Uani 1 1 d . . . F24 F 0.9277(11) 0.4011(6) 0.0520(9) 0.361(17) Uani 1 1 d . . . F25 F 1.3715(17) 0.6213(14) -0.0541(10) 0.43(2) Uani 1 1 d D . . F26 F 1.3386(7) 0.6070(7) 0.0271(5) 0.219(7) Uani 1 1 d D . . F27 F 1.3595(7) 0.5397(6) -0.0054(7) 0.220(6) Uani 1 1 d D . . F28 F 1.2863(10) 0.6123(10) -0.0296(11) 0.366(19) Uani 1 1 d D . . F29 F 0.8977(9) 0.1791(15) 0.6165(11) 0.43(2) Uani 1 1 d . . . F30 F 0.8363(13) 0.1475(10) 0.6866(8) 0.316(14) Uani 1 1 d . . . F31 F 0.8375(9) 0.2338(10) 0.6506(8) 0.301(14) Uani 1 1 d . . . F32 F 0.9092(6) 0.1828(5) 0.6878(5) 0.185(6) Uani 1 1 d . . . Cu1 Cu 0.90509(4) 0.56888(4) 0.23804(4) 0.0328(2) Uani 1 1 d . . . Cu2 Cu 1.17145(4) 0.57666(4) 0.23079(4) 0.0351(2) Uani 1 1 d . . . Cu3 Cu 0.96473(4) 0.30256(4) 0.28917(4) 0.0364(3) Uani 1 1 d . . . Cu4 Cu 1.23378(4) 0.31405(4) 0.26809(4) 0.0383(3) Uani 1 1 d . . . B1 B 0.8650(6) 0.6270(6) 0.4737(5) 0.068(4) Uani 1 1 d . . . B2 B 0.8566(8) 0.5867(7) -0.0061(6) 0.080(4) Uani 1 1 d . . . B3 B 1.1915(11) 0.1471(5) 0.5371(9) 0.126(8) Uani 1 1 d . . . B4 B 0.6511(10) 0.6598(12) 0.0811(8) 0.114(7) Uani 1 1 d . . . B5 B 1.0647(8) 0.6261(6) 0.4732(6) 0.077(4) Uani 1 1 d . . . B6 B 0.8937(8) 0.3953(7) 0.0301(6) 0.084(5) Uani 1 1 d . . . B7 B 1.3356(9) 0.5919(6) -0.0117(6) 0.40(5) Uani 1 1 d D . . B8 B 0.8679(13) 0.1883(12) 0.6612(14) 0.150(12) Uani 1 1 d . . . S1 S 0.79794(12) 0.77590(10) 0.07304(10) 0.0570(6) Uani 1 1 d . . . S2 S 1.25635(12) 0.76121(10) 0.04794(10) 0.0559(6) Uani 1 1 d . . . S3 S 0.71373(10) 0.62215(10) 0.37600(9) 0.0471(5) Uani 1 1 d . . . S4 S 0.80352(16) 0.13550(14) 0.53007(15) 0.0869(10) Uani 1 1 d . . . S5 S 1.30479(12) 0.65098(11) 0.33459(10) 0.0607(7) Uani 1 1 d . . . S6 S 1.40512(17) 0.22359(17) 0.44707(14) 0.0965(11) Uani 1 1 d . . . S7 S 0.91611(13) 0.19730(11) 0.17262(10) 0.0610(7) Uani 1 1 d . . . S8 S 1.37085(14) 0.18728(19) 0.13907(13) 0.0954(12) Uani 1 1 d . . . C301 C 1.3418(8) 0.4383(6) 0.3140(9) 0.116(6) Uani 1 1 d . . . C302 C 1.3673(7) 0.4321(7) 0.3584(8) 0.119(6) Uani 1 1 d . . . H30A H 1.3442 0.4568 0.3760 0.179 Uiso 1 1 calc R . . H30B H 1.4062 0.4422 0.3449 0.179 Uiso 1 1 calc R . . H30C H 1.3685 0.3931 0.3840 0.179 Uiso 1 1 calc R . . N41 N 1.3207(6) 0.4439(5) 0.2806(7) 0.119(5) Uani 1 1 d . . . C303 C 0.7707(9) 0.4111(7) 0.3486(11) 0.131(7) Uani 1 1 d . . . C304 C 0.7364(8) 0.3986(6) 0.3957(9) 0.127(6) Uani 1 1 d . . . H30D H 0.7461 0.3592 0.4180 0.191 Uiso 1 1 calc R . . H30E H 0.6966 0.4051 0.3910 0.191 Uiso 1 1 calc R . . H30F H 0.7411 0.4223 0.4129 0.191 Uiso 1 1 calc R . . N42 N 0.8053(6) 0.4219(6) 0.3104(8) 0.130(6) Uani 1 1 d . . . C305 C 0.7352(13) 0.4665(11) 0.1309(9) 0.218(10) Uani 1 1 d DU . . C306 C 0.7284(15) 0.4913(13) 0.0724(9) 0.231(10) Uani 1 1 d DU . . N43 N 0.7507(12) 0.4608(9) 0.1685(8) 0.214(9) Uani 1 1 d DU . . C309 C 0.6062(12) 0.5891(8) -0.0094(7) 0.196(8) Uani 1 1 d DU . . C310 C 0.5720(15) 0.5590(11) 0.0454(8) 0.243(10) Uani 1 1 d DU . . N45 N 0.6253(11) 0.6177(8) -0.0509(6) 0.208(8) Uani 1 1 d DU . . C311 C 1.0174(8) 0.7423(9) 0.1411(8) 0.35(3) Uani 1 1 d D . . C312 C 1.0279(8) 0.7775(10) 0.0814(7) 0.167(9) Uani 1 1 d D . . N46 N 1.0149(7) 0.7039(6) 0.1809(9) 0.203(11) Uani 1 1 d D . . C313 C 1.0219(18) -0.0018(13) 0.2717(15) 0.281(13) Uiso 1 1 d DU . . C314 C 0.9822(18) -0.0191(17) 0.3256(16) 0.312(16) Uiso 1 1 d DU . . N47 N 1.0499(16) 0.0205(15) 0.2317(15) 0.325(14) Uiso 1 1 d DU . . N50 N 0.9791(9) 0.1562(8) 0.5112(9) 0.179(7) Uiso 1 1 d DU . . C319 C 0.9985(16) 0.1328(11) 0.5490(11) 0.261(12) Uiso 1 1 d DU . . C320 C 1.0276(18) 0.0892(15) 0.5944(13) 0.316(16) Uiso 1 1 d DU . . C401 C 0.8910(6) 0.8357(6) 0.3361(5) 0.186(6) Uani 1 1 d GDU . . H401 H 0.8794 0.8154 0.3731 0.224 Uiso 1 1 calc R . . C402 C 0.9362(6) 0.8124(5) 0.3071(5) 0.158(5) Uani 1 1 d GDU . . C403 C 0.9532(6) 0.8420(6) 0.2530(5) 0.182(6) Uani 1 1 d GDU . . H403 H 0.9841 0.8260 0.2332 0.218 Uiso 1 1 calc R . . C404 C 0.9250(7) 0.8949(6) 0.2278(5) 0.193(6) Uani 1 1 d GU . . H404 H 0.9366 0.9151 0.1908 0.232 Uiso 1 1 calc R . . C405 C 0.8798(7) 0.9182(5) 0.2568(7) 0.191(6) Uani 1 1 d GU . . H405 H 0.8605 0.9543 0.2396 0.229 Uiso 1 1 calc R . . C406 C 0.8628(6) 0.8886(7) 0.3109(7) 0.195(6) Uani 1 1 d GU . . H406 H 0.8319 0.9045 0.3308 0.234 Uiso 1 1 calc R . . C407 C 0.9683(6) 0.7545(6) 0.3350(7) 0.172(8) Uani 1 1 d DU . . H40A H 0.9507 0.7392 0.3726 0.257 Uiso 1 1 calc R . . H40B H 1.0084 0.7581 0.3318 0.257 Uiso 1 1 calc R . . H40C H 0.9663 0.7293 0.3182 0.257 Uiso 1 1 calc R . . C408 C 1.0866(8) 0.9422(7) 0.0862(7) 0.117(6) Uani 0.50 1 d PGDU A 1 C409 C 1.0421(9) 0.9099(6) 0.1040(7) 0.123(7) Uani 0.50 1 d PGDU A 1 C410 C 1.0006(8) 0.9230(8) 0.0731(9) 0.127(7) Uani 0.50 1 d PGU A 1 C411 C 1.0036(9) 0.9684(8) 0.0246(9) 0.130(7) Uani 0.50 1 d PGU . 1 C412 C 1.0481(10) 1.0007(7) 0.0068(7) 0.129(7) Uani 0.50 1 d PGU . 1 C413 C 1.0896(8) 0.9876(7) 0.0376(7) 0.124(7) Uani 0.50 1 d PGDU A 1 C414 C 1.1271(12) 0.9332(10) 0.1239(11) 0.129(9) Uani 0.50 1 d PDU A 1 C415 C 1.1910(10) 0.0865(9) 0.1958(11) 0.165(8) Uani 0.50 1 d PGDU B 1 C416 C 1.2439(10) 0.0959(9) 0.1627(10) 0.158(8) Uani 0.50 1 d PGDU B 1 H416 H 1.2551 0.1324 0.1469 0.190 Uiso 0.50 1 calc PR B 1 C417 C 1.2804(9) 0.0518(12) 0.1526(10) 0.151(8) Uani 0.50 1 d PGU B 1 H417 H 1.3165 0.0582 0.1300 0.182 Uiso 0.50 1 calc PR B 1 C418 C 1.2640(11) -0.0016(10) 0.1758(12) 0.159(8) Uani 0.50 1 d PGU B 1 H418 H 1.2890 -0.0317 0.1689 0.191 Uiso 0.50 1 calc PR B 1 C419 C 1.2111(12) -0.0109(8) 0.2089(11) 0.158(8) Uani 0.50 1 d PGU B 1 H419 H 1.1999 -0.0475 0.2247 0.189 Uiso 0.50 1 calc PR B 1 C420 C 1.1746(10) 0.0331(10) 0.2189(10) 0.168(8) Uani 0.50 1 d PGDU B 1 H420 H 1.1385 0.0267 0.2416 0.202 Uiso 0.50 1 calc PR B 1 C421 C 1.1508(13) 0.1353(13) 0.2070(17) 0.142(10) Uani 0.50 1 d PDU B 1 H42A H 1.1153 0.1218 0.2305 0.212 Uiso 0.50 1 calc PR B 1 H42B H 1.1418 0.1647 0.1734 0.212 Uiso 0.50 1 calc PR B 1 H42C H 1.1694 0.1506 0.2241 0.212 Uiso 0.50 1 calc PR B 1 C307 C 1.1386(12) 0.1828(14) 0.2291(12) 0.113(13) Uani 0.50 1 d PD C 2 C308 C 1.157(3) 0.1589(19) 0.1860(15) 0.72(18) Uani 0.50 1 d PD C 2 N44 N 1.1293(11) 0.1927(10) 0.2664(13) 0.126(11) Uani 0.50 1 d PD C 2 C422 C 0.6744(10) 0.0351(8) 0.2589(8) 0.364(15) Uani 1 1 d GDU . . C423 C 0.6244(9) 0.0619(7) 0.2793(10) 0.366(15) Uani 1 1 d GDU . . H423 H 0.5995 0.0877 0.2562 0.439 Uiso 1 1 calc R . . C424 C 0.6107(10) 0.0509(10) 0.3334(11) 0.360(15) Uani 1 1 d GU . . H424 H 0.5765 0.0693 0.3473 0.432 Uiso 1 1 calc R . . C425 C 0.6471(14) 0.0132(10) 0.3672(8) 0.368(16) Uani 1 1 d GU . . H425 H 0.6378 0.0057 0.4042 0.442 Uiso 1 1 calc R . . C426 C 0.6972(12) -0.0136(7) 0.3468(10) 0.362(15) Uani 1 1 d GU . . H426 H 0.7221 -0.0394 0.3699 0.434 Uiso 1 1 calc R . . C427 C 0.7109(10) -0.0027(7) 0.2927(11) 0.352(15) Uani 1 1 d GDU . . H427 H 0.7451 -0.0210 0.2788 0.423 Uiso 1 1 calc R . . C428 C 0.6887(15) 0.0459(13) 0.1994(9) 0.365(17) Uani 1 1 d DU . . H42D H 0.7256 0.0245 0.1917 0.548 Uiso 1 1 calc R . . H42E H 0.6907 0.0859 0.1786 0.548 Uiso 1 1 calc R . . H42F H 0.6588 0.0341 0.1901 0.548 Uiso 1 1 calc R . . C429 C 0.5701(12) 0.4374(16) 0.3582(12) 0.60(3) Uani 1 1 d GDU D 1 C430 C 0.6087(10) 0.4156(17) 0.3237(10) 0.60(3) Uani 1 1 d GDU D 1 H430 H 0.6419 0.4330 0.3034 0.718 Uiso 1 1 calc R D 1 C431 C 0.5989(15) 0.3683(18) 0.3191(12) 0.60(3) Uani 1 1 d GU D 1 H431 H 0.6253 0.3534 0.2955 0.721 Uiso 1 1 calc R D 1 C432 C 0.5504(17) 0.3428(16) 0.3489(16) 0.59(3) Uani 1 1 d GU D 1 H432 H 0.5436 0.3105 0.3457 0.714 Uiso 1 1 calc R D 1 C433 C 0.5117(12) 0.3646(17) 0.3833(13) 0.59(3) Uani 1 1 d GU D 1 H433 H 0.4785 0.3472 0.4037 0.713 Uiso 1 1 calc R D 1 C434 C 0.5215(10) 0.4119(17) 0.3880(10) 0.59(3) Uani 1 1 d GDU D 1 H434 H 0.4951 0.4268 0.4115 0.709 Uiso 1 1 calc R D 1 C435 C 0.5788(18) 0.4919(18) 0.361(2) 0.58(3) Uani 1 1 d DU D 1 H43A H 0.5481 0.5012 0.3868 0.865 Uiso 1 1 calc R D 1 H43B H 0.5783 0.5223 0.3255 0.865 Uiso 1 1 calc R D 1 H43C H 0.6158 0.4868 0.3710 0.865 Uiso 1 1 calc R D 1 C436 C 0.8949(10) -0.0020(10) 0.6041(14) 0.263(18) Uani 0.50 1 d PGDU . . C437 C 0.8699(10) -0.0511(11) 0.6319(14) 0.262(18) Uani 0.50 1 d PGDU . . H437 H 0.8513 -0.0600 0.6679 0.314 Uiso 0.50 1 calc PR . . C438 C 0.8722(11) -0.0874(9) 0.6071(18) 0.269(18) Uani 0.50 1 d PGU . . H438 H 0.8552 -0.1210 0.6262 0.323 Uiso 0.50 1 calc PR . . C439 C 0.8995(12) -0.0744(12) 0.5545(18) 0.268(18) Uani 0.50 1 d PGU . . H439 H 0.9011 -0.0992 0.5376 0.322 Uiso 0.50 1 calc PR . . C440 C 0.9245(11) -0.0253(14) 0.5267(14) 0.266(18) Uani 0.50 1 d PGU . . H440 H 0.9431 -0.0164 0.4907 0.320 Uiso 0.50 1 calc PR . . C441 C 0.9222(10) 0.0109(10) 0.5515(14) 0.263(18) Uani 0.50 1 d PGDU . . H441 H 0.9392 0.0445 0.5325 0.316 Uiso 0.50 1 calc PR . . C442 C 0.8925(17) 0.0379(16) 0.632(2) 0.28(2) Uani 0.50 1 d PDU . . H44A H 0.9131 0.0696 0.6070 0.416 Uiso 0.50 1 calc PR . . H44B H 0.9103 0.0178 0.6632 0.416 Uiso 0.50 1 calc PR . . H44C H 0.8526 0.0517 0.6422 0.416 Uiso 0.50 1 calc PR . . N48 N 1.432(3) 0.9100(14) 0.0919(15) 0.403(19) Uani 1 1 d DU . . C315 C 1.427(3) 0.8780(17) 0.1350(13) 0.397(19) Uani 1 1 d DU . . C316 C 1.419(3) 0.8273(17) 0.1871(15) 0.41(2) Uani 1 1 d DU . . N49 N 1.488(3) 0.462(2) 0.195(3) 0.73(6) Uani 1 1 d DU E 1 C317 C 1.465(2) 0.474(3) 0.160(3) 0.72(6) Uani 1 1 d DU E 1 C318 C 1.444(3) 0.485(2) 0.110(3) 0.71(6) Uani 1 1 d DU E 1 N52 N 1.464(2) 1.070(3) -0.2388(16) 0.60(3) Uani 1 1 d DU F 1 C324 C 1.417(3) 1.110(2) -0.1636(17) 0.61(4) Uani 1 1 d DU F 1 C323 C 1.439(2) 1.090(3) -0.2090(19) 0.61(3) Uani 1 1 d DU F 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.055(6) 0.053(5) 0.047(6) -0.025(4) -0.017(5) -0.008(4) C2 0.046(6) 0.068(6) 0.057(6) -0.030(5) -0.007(5) -0.011(5) C3 0.043(6) 0.086(7) 0.072(8) -0.033(6) -0.021(6) -0.012(5) C4 0.061(7) 0.063(6) 0.043(6) -0.018(5) -0.026(5) -0.009(5) C5 0.053(6) 0.038(4) 0.035(5) -0.017(4) -0.023(4) 0.000(4) C6 0.055(6) 0.044(5) 0.029(4) -0.016(4) -0.024(4) -0.003(4) C7 0.048(5) 0.027(4) 0.023(4) -0.011(3) -0.014(4) -0.001(3) C8 0.052(5) 0.041(4) 0.022(4) -0.014(3) -0.012(4) -0.009(4) C9 0.042(5) 0.029(4) 0.034(4) -0.016(3) -0.005(4) -0.012(3) C10 0.054(6) 0.033(4) 0.021(4) -0.015(3) -0.007(4) -0.006(4) C11 0.037(5) 0.056(5) 0.028(4) -0.020(4) -0.009(4) -0.006(4) C12 0.047(6) 0.093(7) 0.061(6) -0.057(6) -0.010(5) -0.010(5) C13 0.072(8) 0.156(13) 0.052(7) -0.069(9) -0.009(6) -0.026(8) C14 0.053(7) 0.197(17) 0.058(9) -0.074(11) -0.009(6) -0.026(9) C15 0.044(7) 0.135(11) 0.043(6) 0.013(7) -0.019(5) -0.033(7) C16 0.047(6) 0.081(7) 0.039(5) -0.015(5) -0.011(5) -0.013(5) C17 0.070(7) 0.034(4) 0.022(4) -0.010(3) -0.004(4) -0.015(4) C18 0.036(5) 0.049(5) 0.050(5) -0.024(4) -0.009(4) -0.009(4) C19 0.051(6) 0.072(7) 0.066(7) -0.034(6) -0.005(5) -0.012(5) C20 0.045(6) 0.113(9) 0.076(8) -0.047(7) -0.010(6) -0.006(6) C21 0.064(8) 0.084(8) 0.072(8) -0.035(6) -0.027(6) -0.012(6) C22 0.053(6) 0.073(6) 0.044(5) -0.029(5) -0.011(5) -0.014(5) C23 0.053(5) 0.053(5) 0.028(4) -0.020(4) -0.018(4) -0.003(4) C24 0.047(5) 0.043(5) 0.035(5) -0.020(4) -0.011(4) -0.005(4) C25 0.051(6) 0.041(5) 0.043(5) -0.019(4) -0.020(4) 0.006(4) C26 0.076(7) 0.052(5) 0.055(6) -0.023(5) -0.023(5) -0.006(5) C27 0.073(7) 0.051(5) 0.057(6) -0.028(5) -0.031(6) 0.004(5) C28 0.067(7) 0.045(5) 0.075(7) -0.036(5) -0.031(6) 0.011(5) C29 0.065(7) 0.063(6) 0.077(8) -0.035(6) -0.002(6) -0.012(5) C30 0.105(10) 0.076(8) 0.071(8) -0.044(7) 0.002(7) 0.003(7) C31 0.142(12) 0.054(7) 0.078(9) -0.042(7) -0.042(9) 0.006(7) C32 0.112(10) 0.047(6) 0.073(8) -0.027(6) -0.032(8) -0.015(6) C33 0.080(7) 0.044(5) 0.057(6) -0.021(5) -0.020(6) -0.009(5) C34 0.076(8) 0.086(8) 0.090(9) -0.062(7) -0.039(7) 0.016(6) C35 0.154(15) 0.098(10) 0.143(14) -0.073(10) -0.109(13) 0.055(10) C36 0.20(2) 0.158(17) 0.27(3) -0.148(19) -0.17(2) 0.110(17) C37 0.20(3) 0.28(3) 0.42(5) -0.29(3) -0.22(3) 0.17(2) C38 0.100(13) 0.26(3) 0.31(3) -0.23(3) -0.110(17) 0.064(15) C39 0.079(9) 0.147(13) 0.178(16) -0.131(13) -0.049(10) 0.021(9) C40 0.088(9) 0.043(5) 0.055(7) -0.024(5) -0.014(6) -0.002(5) C41 0.089(9) 0.070(7) 0.079(8) -0.047(6) 0.000(7) -0.018(7) C42 0.130(14) 0.098(11) 0.134(16) -0.078(11) 0.019(12) -0.037(10) C43 0.18(2) 0.090(12) 0.091(14) -0.033(10) 0.043(14) -0.055(14) C44 0.23(3) 0.084(11) 0.087(14) -0.013(9) -0.024(18) -0.007(15) C45 0.167(16) 0.079(9) 0.045(8) -0.004(7) -0.009(9) -0.016(9) C46 0.050(5) 0.058(5) 0.020(4) -0.019(4) -0.003(4) -0.014(4) C47 0.056(6) 0.063(6) 0.032(5) -0.019(4) -0.014(5) -0.018(5) C48 0.079(7) 0.058(6) 0.029(5) -0.009(4) -0.007(5) -0.026(5) C49 0.086(8) 0.068(6) 0.050(6) -0.025(5) 0.000(6) -0.034(6) C50 0.047(6) 0.066(6) 0.062(6) -0.028(5) -0.015(5) -0.009(5) C51 0.056(6) 0.052(5) 0.059(6) -0.027(5) -0.015(5) -0.017(5) C52 0.063(7) 0.055(6) 0.093(9) -0.038(6) -0.014(6) -0.007(5) C53 0.082(9) 0.053(7) 0.107(10) -0.036(7) -0.030(8) 0.010(6) C54 0.099(10) 0.050(6) 0.086(9) -0.019(6) -0.015(8) -0.007(7) C55 0.083(9) 0.077(8) 0.080(9) -0.024(7) -0.016(7) -0.004(7) C56 0.074(8) 0.060(6) 0.063(7) -0.023(6) -0.020(6) 0.006(6) C57 0.058(7) 0.067(7) 0.049(6) -0.015(5) -0.012(5) -0.012(5) C58 0.055(7) 0.099(9) 0.065(8) -0.017(7) -0.014(6) -0.010(6) C59 0.071(10) 0.140(14) 0.054(8) -0.006(8) -0.012(7) -0.022(9) C60 0.070(10) 0.121(13) 0.060(9) -0.004(8) 0.007(7) 0.012(9) C61 0.100(13) 0.107(12) 0.110(13) -0.037(10) -0.014(10) 0.025(10) C62 0.071(9) 0.084(9) 0.100(10) -0.035(8) -0.015(7) 0.013(7) C63 0.059(7) 0.092(8) 0.061(7) -0.041(6) -0.015(5) -0.016(6) C64 0.136(13) 0.090(9) 0.082(9) -0.046(8) -0.036(9) -0.017(8) C65 0.134(14) 0.125(13) 0.105(13) -0.082(11) -0.022(11) -0.018(11) C66 0.092(11) 0.169(16) 0.066(9) -0.054(11) -0.013(8) -0.030(11) C67 0.080(9) 0.135(12) 0.062(8) -0.032(8) -0.028(7) -0.024(8) C68 0.070(7) 0.087(8) 0.045(6) -0.022(6) -0.019(5) -0.019(6) C71 0.064(6) 0.043(5) 0.039(5) -0.016(4) -0.015(5) -0.006(4) C72 0.087(8) 0.039(5) 0.046(6) -0.013(4) -0.022(5) -0.011(5) C73 0.074(7) 0.029(4) 0.060(6) -0.019(4) -0.016(5) -0.012(4) C74 0.047(5) 0.037(4) 0.042(5) -0.025(4) -0.008(4) -0.009(4) C75 0.037(5) 0.044(4) 0.031(4) -0.017(4) -0.009(4) -0.009(4) C76 0.035(4) 0.037(4) 0.030(4) -0.018(3) -0.007(3) -0.009(3) C77 0.033(4) 0.031(4) 0.042(5) -0.023(4) -0.013(4) -0.003(3) C78 0.047(5) 0.038(4) 0.022(4) -0.016(3) -0.008(4) -0.004(4) C79 0.030(4) 0.044(5) 0.034(4) -0.019(4) -0.007(4) -0.007(3) C80 0.036(4) 0.042(4) 0.024(4) -0.017(4) -0.009(3) -0.010(3) C81 0.072(6) 0.025(4) 0.031(4) -0.018(3) -0.019(5) -0.001(4) C82 0.078(7) 0.043(5) 0.047(6) -0.022(4) -0.033(5) 0.000(5) C83 0.149(13) 0.039(5) 0.058(7) -0.022(5) -0.062(8) 0.001(7) C84 0.169(15) 0.048(6) 0.029(6) -0.017(5) -0.029(8) 0.002(8) C85 0.120(11) 0.037(5) 0.047(6) -0.022(5) 0.025(7) -0.015(6) C86 0.063(7) 0.038(5) 0.044(5) -0.019(4) -0.001(5) -0.004(4) C87 0.065(6) 0.042(5) 0.039(5) -0.016(4) -0.010(5) -0.005(4) C88 0.084(8) 0.036(5) 0.068(7) -0.030(5) -0.014(6) -0.010(5) C89 0.122(10) 0.035(5) 0.064(7) -0.017(5) -0.021(7) -0.004(6) C90 0.121(11) 0.030(5) 0.104(11) -0.031(6) -0.026(8) -0.005(6) C91 0.112(10) 0.051(6) 0.075(8) -0.039(6) -0.026(7) 0.001(6) C92 0.072(7) 0.052(5) 0.054(6) -0.034(5) -0.013(5) -0.007(5) C93 0.046(5) 0.033(4) 0.032(4) -0.018(3) -0.018(4) -0.002(3) C94 0.048(5) 0.035(4) 0.024(4) -0.010(3) -0.008(4) -0.007(4) C95 0.050(6) 0.054(5) 0.035(5) -0.023(4) -0.006(4) -0.008(4) C96 0.044(5) 0.056(5) 0.038(5) -0.026(4) -0.003(4) -0.002(4) C97 0.060(6) 0.041(5) 0.044(5) -0.014(4) -0.017(5) -0.008(4) C98 0.059(7) 0.068(6) 0.037(5) -0.029(5) 0.008(5) -0.008(5) C99 0.062(7) 0.075(7) 0.063(7) -0.033(6) -0.002(5) -0.025(6) C100 0.091(10) 0.120(12) 0.089(10) -0.066(9) 0.019(8) -0.056(9) C101 0.154(16) 0.073(9) 0.079(9) -0.052(8) 0.042(10) -0.053(10) C102 0.133(14) 0.052(7) 0.095(11) -0.033(7) 0.012(10) -0.010(8) C103 0.080(8) 0.063(7) 0.082(9) -0.034(6) -0.001(7) -0.001(6) C104 0.038(5) 0.053(5) 0.051(6) -0.013(4) -0.019(5) 0.002(4) C105 0.053(7) 0.073(7) 0.078(8) -0.031(6) -0.013(6) -0.009(5) C106 0.045(7) 0.105(9) 0.085(9) -0.042(7) 0.005(6) -0.004(7) C107 0.033(6) 0.102(10) 0.098(10) -0.018(8) -0.011(6) -0.024(6) C108 0.072(9) 0.081(8) 0.090(9) -0.030(7) -0.031(8) -0.014(7) C109 0.055(7) 0.067(7) 0.057(7) -0.011(5) -0.010(6) -0.014(5) C110 0.075(7) 0.042(5) 0.060(7) -0.014(5) -0.029(6) -0.011(5) C111 0.086(9) 0.103(9) 0.075(9) -0.005(7) -0.041(7) -0.034(7) C112 0.136(14) 0.118(12) 0.092(11) -0.003(9) -0.073(11) -0.057(10) C113 0.137(14) 0.094(9) 0.057(8) -0.015(7) -0.026(9) -0.045(9) C114 0.116(11) 0.065(7) 0.041(6) -0.021(5) -0.005(6) -0.027(7) C115 0.072(7) 0.053(6) 0.047(6) -0.023(5) -0.011(5) -0.013(5) C116 0.064(6) 0.035(4) 0.036(5) -0.017(4) -0.010(4) -0.011(4) C117 0.059(6) 0.046(5) 0.028(5) -0.013(4) 0.000(4) -0.020(4) C118 0.078(8) 0.062(6) 0.058(7) -0.026(5) -0.001(6) -0.019(6) C119 0.082(9) 0.100(9) 0.075(8) -0.036(7) -0.004(7) -0.036(7) C120 0.117(12) 0.091(9) 0.093(10) -0.047(8) 0.007(9) -0.034(9) C121 0.069(8) 0.089(9) 0.112(12) -0.045(9) -0.025(8) -0.003(7) C122 0.117(14) 0.146(15) 0.074(11) -0.008(10) -0.005(10) -0.014(12) C123 0.115(14) 0.160(16) 0.074(11) -0.035(11) -0.008(10) 0.034(12) C124 0.088(11) 0.109(11) 0.076(10) -0.012(9) 0.003(8) -0.008(8) C125 0.103(11) 0.068(8) 0.126(14) -0.037(9) -0.032(10) -0.008(8) C126 0.083(9) 0.091(9) 0.076(8) -0.046(7) 0.007(7) -0.022(7) C127 0.099(11) 0.079(8) 0.090(10) -0.042(8) 0.008(9) -0.015(8) C128 0.101(12) 0.094(10) 0.175(18) -0.069(11) 0.038(11) -0.060(9) C129 0.106(13) 0.078(10) 0.166(19) -0.042(11) 0.001(14) -0.013(9) C130 0.154(19) 0.085(12) 0.139(18) -0.047(12) -0.010(16) -0.006(13) C131 0.17(2) 0.050(8) 0.141(17) -0.008(9) -0.019(15) -0.025(10) C132 0.120(13) 0.078(9) 0.128(14) -0.037(10) -0.012(12) -0.019(9) C133 0.085(10) 0.118(12) 0.135(14) -0.075(11) -0.005(10) -0.016(9) C134 0.128(13) 0.105(11) 0.116(13) -0.075(10) 0.024(10) -0.007(10) C135 0.178(19) 0.104(12) 0.130(16) -0.066(12) 0.034(14) -0.045(12) C136 0.18(2) 0.29(3) 0.26(3) -0.24(3) -0.06(2) 0.05(2) C137 0.15(2) 0.34(4) 0.40(4) -0.34(4) -0.04(2) 0.03(2) C138 0.132(16) 0.25(2) 0.18(2) -0.151(19) -0.059(15) -0.013(15) C141 0.061(6) 0.044(5) 0.037(5) -0.020(4) -0.015(4) -0.001(4) C142 0.081(8) 0.047(5) 0.054(6) -0.018(5) -0.027(6) 0.005(5) C143 0.086(8) 0.046(5) 0.065(7) -0.028(5) -0.023(6) 0.003(5) C144 0.065(6) 0.051(5) 0.054(6) -0.033(5) -0.026(5) 0.005(5) C145 0.050(5) 0.037(4) 0.041(5) -0.023(4) -0.011(4) -0.003(4) C146 0.042(5) 0.052(5) 0.038(5) -0.024(4) -0.014(4) -0.004(4) C147 0.031(4) 0.048(5) 0.031(4) -0.023(4) -0.009(3) -0.006(3) C148 0.043(5) 0.046(5) 0.025(4) -0.018(4) -0.012(4) -0.004(4) C149 0.041(5) 0.034(4) 0.030(4) -0.011(3) -0.012(4) -0.008(3) C150 0.033(4) 0.047(5) 0.028(4) -0.018(4) -0.009(3) -0.009(4) C151 0.071(6) 0.022(4) 0.034(5) -0.014(3) -0.016(5) 0.000(4) C152 0.091(8) 0.043(5) 0.055(6) -0.026(5) -0.040(6) 0.004(5) C153 0.176(15) 0.053(6) 0.052(7) -0.033(6) -0.059(9) 0.004(8) C154 0.193(18) 0.050(7) 0.041(7) -0.026(6) -0.014(10) 0.006(9) C155 0.108(10) 0.067(7) 0.053(7) -0.036(6) 0.022(7) -0.007(7) C156 0.076(8) 0.052(6) 0.041(6) -0.019(5) 0.006(5) -0.012(5) C157 0.058(6) 0.044(5) 0.050(6) -0.024(4) -0.019(5) -0.002(4) C158 0.056(6) 0.039(5) 0.050(6) -0.016(4) -0.014(5) 0.003(4) C159 0.112(10) 0.056(6) 0.052(6) -0.022(5) -0.013(6) -0.014(6) C160 0.115(11) 0.038(6) 0.079(9) -0.016(6) -0.015(8) 0.005(6) C161 0.126(11) 0.047(6) 0.064(8) -0.029(6) -0.010(7) 0.000(6) C162 0.086(8) 0.051(6) 0.051(6) -0.028(5) -0.013(6) 0.003(5) C163 0.056(6) 0.047(5) 0.030(4) -0.021(4) -0.010(4) -0.013(4) C164 0.048(6) 0.046(5) 0.031(4) -0.015(4) -0.018(4) -0.002(4) C165 0.052(6) 0.059(5) 0.044(5) -0.029(4) -0.014(4) -0.013(4) C166 0.055(6) 0.050(5) 0.067(7) -0.029(5) -0.023(5) -0.004(4) C167 0.059(6) 0.060(6) 0.056(6) -0.010(5) -0.025(5) -0.015(5) C168 0.047(6) 0.064(6) 0.055(6) -0.020(5) -0.016(5) -0.011(5) C169 0.062(7) 0.058(7) 0.090(9) -0.028(6) -0.015(6) -0.007(5) C170 0.064(8) 0.072(8) 0.118(13) -0.015(9) -0.017(8) -0.001(6) C171 0.065(8) 0.114(12) 0.068(9) 0.009(8) -0.025(7) -0.024(8) C172 0.078(9) 0.093(9) 0.075(9) -0.026(8) -0.021(7) -0.030(7) C173 0.060(7) 0.075(7) 0.056(7) -0.024(6) -0.002(5) -0.028(5) C174 0.064(8) 0.078(7) 0.051(7) -0.021(6) 0.000(6) -0.029(6) C175 0.092(10) 0.117(11) 0.056(8) -0.015(7) -0.005(7) -0.047(8) C176 0.143(16) 0.166(16) 0.040(7) -0.033(9) 0.021(9) -0.090(14) C177 0.105(13) 0.149(15) 0.105(15) -0.069(13) 0.021(11) -0.056(12) C178 0.093(11) 0.169(16) 0.081(11) -0.048(11) 0.023(9) -0.046(11) C179 0.067(9) 0.117(10) 0.064(8) -0.027(7) -0.001(7) -0.026(8) C180 0.076(8) 0.051(6) 0.070(7) -0.019(5) -0.017(6) -0.021(6) C181 0.094(9) 0.066(7) 0.090(9) -0.027(6) -0.019(7) -0.034(7) C182 0.113(14) 0.108(12) 0.22(2) -0.082(14) -0.030(14) -0.046(11) C183 0.139(16) 0.108(13) 0.19(2) -0.083(14) 0.020(14) -0.074(13) C184 0.143(15) 0.049(7) 0.113(12) -0.033(7) -0.001(10) -0.001(8) C185 0.098(10) 0.060(7) 0.101(10) -0.013(7) -0.025(8) -0.024(7) C186 0.055(6) 0.041(4) 0.032(5) -0.016(4) -0.009(4) -0.001(4) C187 0.057(6) 0.041(5) 0.036(5) -0.021(4) -0.008(5) -0.006(4) C188 0.064(7) 0.087(7) 0.048(6) -0.031(6) -0.024(5) -0.003(6) C189 0.077(8) 0.097(9) 0.053(7) -0.030(6) -0.016(6) 0.005(7) C190 0.085(10) 0.124(11) 0.092(10) -0.070(9) 0.003(8) -0.015(8) C191 0.081(9) 0.104(10) 0.090(10) -0.054(8) -0.019(8) -0.004(8) C192 0.149(16) 0.129(13) 0.109(12) -0.066(10) -0.048(11) -0.039(11) C193 0.27(3) 0.094(12) 0.20(2) -0.062(13) -0.19(2) 0.060(15) C194 0.18(2) 0.155(19) 0.144(18) -0.058(14) -0.098(17) -0.011(17) C195 0.23(3) 0.107(13) 0.127(15) -0.076(12) -0.050(17) -0.009(15) C196 0.119(13) 0.128(13) 0.120(13) -0.083(11) -0.040(10) 0.013(10) C197 0.090(9) 0.093(9) 0.074(9) -0.040(8) -0.039(8) 0.027(7) C198 0.085(10) 0.171(15) 0.080(10) -0.049(10) -0.017(8) -0.050(10) C199 0.111(13) 0.23(2) 0.093(12) -0.016(14) -0.055(11) -0.061(14) C200 0.156(15) 0.113(11) 0.087(11) -0.038(9) -0.066(11) -0.021(10) C201 0.128(12) 0.093(9) 0.062(8) -0.030(7) -0.044(8) 0.004(8) C202 0.089(10) 0.091(9) 0.095(10) -0.050(8) -0.025(8) 0.008(7) C203 0.080(10) 0.145(13) 0.076(10) -0.042(9) -0.010(8) -0.007(9) C204 0.123(14) 0.22(2) 0.084(12) -0.072(13) -0.032(11) 0.002(14) C205 0.138(18) 0.25(3) 0.076(12) -0.038(14) 0.033(13) -0.056(18) C206 0.130(19) 0.26(3) 0.115(18) -0.096(18) 0.017(14) -0.044(18) C207 0.141(18) 0.30(3) 0.090(14) -0.086(17) 0.023(13) -0.082(19) C208 0.095(13) 0.21(2) 0.111(14) -0.070(14) 0.005(11) -0.048(13) C211 0.067(8) 0.134(11) 0.075(8) -0.070(8) -0.007(7) -0.020(7) C212 0.047(8) 0.228(19) 0.120(13) -0.101(13) 0.023(8) -0.058(10) C213 0.072(10) 0.203(17) 0.104(12) -0.097(12) -0.024(9) -0.023(10) C214 0.057(7) 0.142(11) 0.083(9) -0.075(8) -0.023(7) -0.010(7) C215 0.065(7) 0.073(7) 0.067(7) -0.051(6) -0.024(6) 0.001(5) C216 0.054(6) 0.054(5) 0.042(5) -0.032(4) -0.017(5) 0.001(4) C217 0.054(6) 0.029(4) 0.036(5) -0.020(3) -0.014(4) -0.002(4) C218 0.060(6) 0.040(4) 0.026(4) -0.018(4) -0.010(4) -0.005(4) C219 0.060(6) 0.032(4) 0.036(5) -0.021(4) -0.011(4) -0.009(4) C220 0.049(5) 0.024(4) 0.027(4) -0.013(3) -0.011(4) -0.002(3) C221 0.042(5) 0.073(6) 0.032(5) -0.029(5) -0.010(4) -0.005(4) C222 0.049(6) 0.120(9) 0.058(6) -0.066(7) -0.002(5) -0.016(6) C223 0.059(8) 0.25(2) 0.075(10) -0.118(13) 0.013(8) -0.050(11) C224 0.076(11) 0.28(3) 0.046(9) -0.073(14) 0.002(8) -0.057(14) C225 0.057(9) 0.21(2) 0.064(10) -0.002(11) -0.025(8) -0.040(11) C226 0.063(7) 0.094(8) 0.040(6) -0.013(6) -0.011(5) -0.013(6) C227 0.050(6) 0.067(6) 0.044(5) -0.035(5) 0.012(5) -0.017(5) C228 0.050(6) 0.068(6) 0.045(6) -0.034(5) -0.001(5) -0.008(5) C229 0.050(7) 0.123(10) 0.069(8) -0.050(7) 0.003(6) -0.023(7) C230 0.044(7) 0.141(12) 0.095(10) -0.068(9) 0.000(7) -0.024(7) C231 0.063(8) 0.110(10) 0.070(8) -0.043(7) -0.009(6) -0.022(7) C232 0.063(7) 0.070(6) 0.050(6) -0.029(5) -0.009(5) -0.017(5) C233 0.061(6) 0.045(5) 0.026(4) -0.018(4) -0.013(4) -0.009(4) C234 0.060(6) 0.053(5) 0.038(5) -0.028(4) -0.008(5) -0.010(5) C235 0.072(7) 0.054(5) 0.047(5) -0.034(5) -0.007(5) -0.018(5) C236 0.083(8) 0.062(6) 0.048(6) -0.032(5) -0.017(5) -0.016(5) C237 0.087(9) 0.066(7) 0.055(7) -0.019(5) -0.014(6) -0.035(6) C238 0.082(8) 0.068(7) 0.067(7) -0.029(6) 0.003(6) -0.036(6) C239 0.090(11) 0.056(7) 0.201(18) -0.049(10) -0.039(11) -0.013(7) C240 0.122(16) 0.091(12) 0.28(3) -0.113(16) 0.031(17) -0.039(11) C241 0.16(2) 0.091(12) 0.19(2) -0.091(13) 0.049(16) -0.062(13) C242 0.156(16) 0.090(10) 0.108(12) -0.066(9) 0.009(11) -0.054(11) C243 0.128(12) 0.072(8) 0.081(9) -0.044(7) -0.004(8) -0.037(8) C244 0.073(8) 0.094(9) 0.067(8) -0.052(7) -0.005(6) -0.020(7) C245 0.110(14) 0.123(13) 0.139(15) -0.076(11) 0.022(11) -0.041(11) C246 0.069(12) 0.23(3) 0.23(3) -0.17(2) 0.011(14) -0.014(15) C247 0.100(15) 0.168(19) 0.20(2) -0.148(19) -0.040(15) 0.026(14) C248 0.121(14) 0.146(14) 0.098(11) -0.093(11) -0.034(11) 0.020(12) C249 0.076(9) 0.123(11) 0.075(8) -0.069(9) -0.024(7) 0.001(8) C250 0.108(11) 0.102(10) 0.067(8) -0.026(8) -0.007(7) -0.055(8) C251 0.30(3) 0.136(15) 0.056(9) 0.007(9) -0.043(13) -0.122(17) C252 0.33(3) 0.127(15) 0.085(13) 0.009(12) -0.028(17) -0.130(19) C253 0.39(4) 0.148(19) 0.095(14) 0.011(14) -0.10(2) -0.13(2) C254 0.155(16) 0.166(17) 0.088(12) -0.058(12) -0.004(11) -0.075(14) C255 0.128(12) 0.139(12) 0.039(7) -0.034(7) 0.004(7) -0.069(10) C256 0.053(6) 0.067(6) 0.039(5) -0.035(5) 0.005(4) -0.016(5) C257 0.048(6) 0.067(6) 0.045(6) -0.030(5) -0.013(5) -0.009(5) C258 0.067(7) 0.113(9) 0.060(7) -0.064(7) -0.024(6) 0.025(6) C259 0.076(8) 0.128(10) 0.049(7) -0.049(7) -0.014(6) 0.025(7) C260 0.091(10) 0.109(10) 0.063(8) -0.035(7) -0.026(7) 0.001(8) C261 0.060(7) 0.085(8) 0.068(8) -0.007(7) -0.023(6) -0.023(6) C262 0.048(7) 0.085(8) 0.107(11) -0.043(8) -0.004(7) 0.006(6) C263 0.071(9) 0.090(9) 0.146(14) -0.068(10) -0.016(9) 0.009(7) C264 0.107(13) 0.101(12) 0.19(2) -0.069(13) -0.079(14) 0.011(10) C265 0.138(15) 0.090(11) 0.094(12) -0.015(9) -0.023(11) -0.037(10) C266 0.139(14) 0.109(11) 0.093(11) -0.033(9) -0.033(10) -0.044(11) C267 0.061(8) 0.135(12) 0.072(9) -0.029(9) -0.022(7) -0.031(8) C268 0.085(10) 0.161(14) 0.077(9) -0.074(10) -0.022(8) -0.006(9) C269 0.109(13) 0.22(2) 0.081(12) -0.068(13) -0.020(10) -0.029(13) C270 0.17(2) 0.173(19) 0.066(11) -0.023(12) -0.043(12) -0.040(16) C271 0.167(18) 0.133(14) 0.103(14) -0.040(12) -0.067(13) -0.014(13) C272 0.136(13) 0.100(10) 0.084(10) -0.024(8) -0.059(10) -0.026(9) C273 0.078(9) 0.107(10) 0.063(8) -0.043(7) 0.004(6) -0.041(8) C274 0.077(10) 0.136(13) 0.118(12) -0.073(11) 0.000(9) -0.027(9) C275 0.105(13) 0.138(15) 0.120(14) -0.062(13) -0.004(11) -0.043(13) C276 0.121(17) 0.23(3) 0.120(17) -0.12(2) -0.003(13) -0.033(19) C277 0.20(2) 0.102(12) 0.086(11) -0.052(9) -0.002(13) -0.052(14) C278 0.142(14) 0.078(9) 0.082(10) -0.047(8) 0.016(9) -0.006(9) N1 0.040(4) 0.040(4) 0.041(4) -0.021(3) -0.021(4) -0.002(3) N2 0.048(4) 0.032(3) 0.025(3) -0.011(3) -0.014(3) -0.003(3) N3 0.056(5) 0.040(4) 0.020(3) -0.013(3) -0.015(3) -0.005(3) N4 0.037(4) 0.032(3) 0.025(3) -0.018(3) -0.010(3) 0.000(3) N5 0.048(4) 0.030(3) 0.023(3) -0.016(3) -0.011(3) -0.002(3) N6 0.056(5) 0.041(4) 0.028(4) -0.015(3) -0.015(3) -0.005(3) N7 0.038(4) 0.043(4) 0.033(4) -0.017(3) -0.005(3) -0.010(3) N8 0.048(4) 0.057(4) 0.033(4) -0.026(3) -0.001(3) -0.010(3) N9 0.061(5) 0.049(4) 0.038(4) -0.025(3) -0.025(4) -0.004(3) N10 0.070(5) 0.051(4) 0.033(4) -0.018(3) -0.003(4) -0.021(4) N11 0.045(4) 0.040(4) 0.034(4) -0.019(3) -0.015(3) -0.005(3) N12 0.030(4) 0.032(3) 0.036(4) -0.019(3) -0.011(3) -0.004(3) N13 0.050(4) 0.037(4) 0.022(3) -0.014(3) -0.010(3) -0.002(3) N14 0.045(4) 0.040(4) 0.027(3) -0.020(3) -0.013(3) -0.003(3) N15 0.041(4) 0.033(3) 0.026(3) -0.015(3) -0.010(3) -0.008(3) N16 0.052(4) 0.035(4) 0.032(4) -0.019(3) -0.011(3) -0.008(3) N17 0.061(5) 0.034(4) 0.039(4) -0.019(3) -0.011(4) -0.008(3) N18 0.057(5) 0.043(4) 0.044(5) -0.023(4) -0.009(4) -0.009(3) N19 0.040(4) 0.043(4) 0.030(4) -0.022(3) -0.005(3) -0.004(3) N20 0.060(5) 0.066(5) 0.047(5) -0.021(4) -0.003(4) -0.023(4) N21 0.044(4) 0.042(4) 0.039(4) -0.023(3) -0.011(3) -0.001(3) N22 0.036(4) 0.038(4) 0.033(4) -0.022(3) -0.009(3) -0.002(3) N23 0.048(4) 0.039(4) 0.030(4) -0.019(3) -0.016(3) -0.005(3) N24 0.036(4) 0.042(4) 0.028(3) -0.018(3) -0.012(3) -0.002(3) N25 0.043(4) 0.046(4) 0.031(4) -0.021(3) -0.011(3) -0.011(3) N26 0.041(4) 0.045(4) 0.030(4) -0.020(3) -0.011(3) 0.002(3) N27 0.042(4) 0.035(4) 0.039(4) -0.019(3) -0.011(3) 0.001(3) N28 0.058(5) 0.040(4) 0.046(5) -0.020(4) -0.011(4) 0.002(3) N29 0.044(4) 0.053(4) 0.034(4) -0.029(3) -0.011(3) -0.001(3) N30 0.067(5) 0.057(5) 0.034(4) -0.017(4) -0.013(4) -0.006(4) N31 0.054(5) 0.071(5) 0.057(5) -0.044(4) -0.008(4) -0.008(4) N32 0.052(5) 0.041(4) 0.040(4) -0.029(3) -0.013(4) -0.004(3) N33 0.060(5) 0.044(4) 0.034(4) -0.022(3) -0.016(4) -0.008(3) N34 0.045(4) 0.030(3) 0.026(3) -0.014(3) -0.007(3) -0.004(3) N35 0.047(4) 0.032(3) 0.036(4) -0.020(3) -0.009(3) -0.006(3) N36 0.052(5) 0.052(4) 0.033(4) -0.026(3) -0.007(3) -0.015(3) N37 0.048(5) 0.041(4) 0.038(4) -0.024(3) -0.006(4) -0.009(3) N38 0.045(4) 0.057(4) 0.046(5) -0.024(4) -0.013(4) -0.010(4) N39 0.068(5) 0.050(4) 0.034(4) -0.026(3) -0.008(4) -0.016(4) N40 0.065(5) 0.071(5) 0.047(5) -0.038(4) -0.009(4) 0.002(4) O1 0.079(5) 0.049(4) 0.056(4) -0.023(3) -0.029(4) -0.017(3) O2 0.072(5) 0.057(4) 0.048(4) -0.027(3) -0.005(3) -0.006(3) O3 0.052(4) 0.068(4) 0.056(4) -0.040(3) -0.010(3) -0.017(3) O4 0.054(4) 0.109(6) 0.048(4) -0.017(4) -0.009(4) -0.019(4) O5 0.046(4) 0.064(4) 0.062(4) -0.041(3) -0.016(3) 0.004(3) O6 0.061(4) 0.063(4) 0.046(4) -0.017(3) -0.016(3) -0.017(3) O7 0.085(5) 0.049(4) 0.060(4) -0.033(3) -0.030(4) 0.005(3) O8 0.071(5) 0.060(4) 0.069(5) -0.041(4) -0.009(4) -0.008(4) F1 0.083(4) 0.074(4) 0.050(3) -0.034(3) -0.010(3) -0.013(3) F2 0.089(5) 0.222(10) 0.151(8) -0.161(8) 0.003(5) -0.039(6) F3 0.090(6) 0.385(19) 0.38(2) -0.364(19) 0.053(9) -0.064(9) F4 0.297(19) 0.36(2) 0.080(8) 0.048(10) -0.043(10) -0.215(18) F5 0.108(5) 0.069(4) 0.049(3) -0.025(3) -0.026(3) -0.026(3) F6 0.408(19) 0.080(5) 0.145(8) 0.006(5) -0.205(11) -0.070(8) F7 0.164(7) 0.101(5) 0.051(4) -0.026(4) -0.043(4) -0.033(5) F8 0.193(13) 0.136(9) 0.170(12) 0.003(8) 0.042(10) 0.025(9) F9 0.40(2) 0.103(7) 0.059(6) -0.021(5) 0.014(9) -0.049(9) F10 0.47(4) 0.53(5) 0.34(3) -0.22(3) 0.06(3) -0.35(4) F11 0.59(4) 0.164(11) 0.070(7) -0.031(7) -0.064(13) 0.187(17) F12 0.192(11) 0.098(7) 0.173(10) -0.048(7) 0.065(8) -0.043(7) F13 0.176(9) 0.171(8) 0.084(6) -0.042(6) -0.043(6) -0.064(7) F14 0.185(13) 0.247(15) 0.181(13) -0.106(12) -0.064(10) 0.019(11) F15 0.101(7) 0.202(10) 0.101(7) -0.016(6) -0.032(5) -0.053(7) F16 0.188(11) 0.250(13) 0.077(6) 0.006(7) -0.045(7) -0.124(10) F17 0.077(4) 0.077(4) 0.044(3) -0.032(3) -0.023(3) 0.004(3) F18 0.151(9) 0.45(2) 0.283(16) -0.333(18) -0.130(11) 0.154(13) F19 0.095(5) 0.205(9) 0.082(5) -0.105(6) -0.021(4) 0.002(5) F20 0.30(2) 0.42(3) 0.29(2) 0.20(2) -0.243(19) -0.22(2) F21 0.362(17) 0.086(6) 0.193(10) -0.079(6) -0.215(12) 0.062(8) F22 0.099(5) 0.091(4) 0.063(4) -0.040(4) -0.039(4) 0.009(4) F23 0.54(4) 0.30(2) 0.23(2) -0.098(18) 0.23(3) 0.08(3) F24 0.64(4) 0.173(12) 0.50(3) -0.223(17) -0.52(3) 0.195(17) F25 0.64(6) 0.47(4) 0.23(2) -0.18(3) 0.17(3) -0.38(4) F26 0.252(16) 0.308(18) 0.135(10) -0.150(12) -0.033(10) 0.019(13) F27 0.245(16) 0.182(13) 0.238(16) -0.118(12) -0.033(13) 0.027(11) F28 0.50(4) 0.31(3) 0.33(3) -0.23(3) -0.19(3) 0.21(3) F29 0.26(2) 0.83(6) 0.48(4) -0.58(4) -0.24(2) 0.26(3) F30 0.53(4) 0.27(2) 0.197(18) -0.076(16) -0.06(2) -0.19(3) F31 0.30(2) 0.40(3) 0.28(2) -0.23(2) -0.205(19) 0.21(2) F32 0.275(15) 0.151(9) 0.198(12) -0.119(9) -0.145(11) 0.063(9) Cu1 0.0426(6) 0.0356(5) 0.0281(5) -0.0167(4) -0.0147(4) -0.0020(4) Cu2 0.0456(6) 0.0375(5) 0.0318(5) -0.0205(4) -0.0122(5) -0.0037(4) Cu3 0.0501(6) 0.0324(5) 0.0350(6) -0.0191(4) -0.0107(5) -0.0056(4) Cu4 0.0425(6) 0.0418(5) 0.0376(6) -0.0229(5) -0.0081(5) -0.0029(4) B1 0.069(9) 0.108(10) 0.047(7) -0.048(8) 0.008(7) -0.035(8) B2 0.105(12) 0.089(10) 0.066(9) -0.052(9) -0.001(8) -0.021(9) B3 0.18(2) 0.012(6) 0.124(17) 0.002(8) 0.029(15) -0.020(8) B4 0.105(16) 0.18(2) 0.069(12) -0.036(13) -0.035(11) -0.033(15) B5 0.111(13) 0.051(7) 0.067(9) -0.017(7) -0.037(9) 0.007(8) B6 0.118(13) 0.101(11) 0.053(8) -0.049(8) -0.043(9) 0.020(9) B7 0.92(14) 0.063(13) 0.064(15) -0.039(11) 0.06(4) 0.06(4) B8 0.18(2) 0.136(19) 0.21(3) -0.12(2) -0.13(2) 0.034(18) S1 0.0715(18) 0.0524(14) 0.0548(15) -0.0303(12) -0.0079(13) -0.0072(12) S2 0.0697(17) 0.0588(14) 0.0462(14) -0.0223(12) -0.0069(12) -0.0219(12) S3 0.0531(14) 0.0540(13) 0.0373(12) -0.0224(10) -0.0105(11) -0.0003(11) S4 0.088(2) 0.078(2) 0.098(3) -0.0412(19) -0.007(2) -0.0125(17) S5 0.0660(17) 0.0692(16) 0.0521(15) -0.0173(13) -0.0179(13) -0.0229(13) S6 0.099(3) 0.116(3) 0.063(2) -0.0360(19) -0.0169(19) 0.014(2) S7 0.0791(19) 0.0696(16) 0.0464(14) -0.0261(13) -0.0088(13) -0.0291(14) S8 0.0597(19) 0.175(4) 0.0552(19) -0.056(2) -0.0133(15) 0.006(2) C301 0.106(13) 0.088(10) 0.180(19) -0.064(11) -0.065(13) 0.008(9) C302 0.102(12) 0.105(11) 0.174(17) -0.069(11) -0.055(12) 0.006(9) N41 0.105(10) 0.093(9) 0.167(14) -0.037(9) -0.059(10) -0.016(7) C303 0.100(15) 0.078(10) 0.20(2) -0.057(13) 0.012(14) -0.018(10) C304 0.109(13) 0.083(10) 0.19(2) -0.071(12) 0.013(13) -0.025(9) N42 0.091(10) 0.102(10) 0.196(18) -0.059(11) -0.007(11) -0.028(8) C305 0.28(2) 0.195(16) 0.165(19) -0.080(18) -0.04(2) 0.019(15) C306 0.28(2) 0.21(2) 0.19(2) -0.079(18) -0.03(2) -0.017(18) N43 0.31(2) 0.162(14) 0.162(18) -0.086(15) -0.024(19) 0.014(14) C309 0.37(2) 0.155(14) 0.099(12) -0.081(12) 0.032(15) -0.127(14) C310 0.38(3) 0.183(17) 0.154(17) -0.060(15) 0.031(19) -0.120(18) N45 0.35(2) 0.188(15) 0.107(11) -0.103(12) 0.076(14) -0.119(14) C311 0.081(14) 0.39(5) 0.31(4) 0.22(3) -0.097(19) -0.14(2) C312 0.108(14) 0.25(3) 0.18(2) -0.14(2) -0.048(15) 0.035(16) N46 0.132(14) 0.080(9) 0.38(3) -0.040(14) -0.107(18) -0.006(9) C401 0.175(12) 0.221(13) 0.151(11) -0.045(10) -0.029(9) -0.058(10) C402 0.162(11) 0.200(12) 0.140(10) -0.060(9) -0.040(9) -0.071(9) C403 0.181(12) 0.212(13) 0.155(11) -0.055(10) -0.031(10) -0.060(10) C404 0.184(13) 0.217(13) 0.165(11) -0.049(10) -0.031(10) -0.051(11) C405 0.178(12) 0.222(13) 0.157(11) -0.050(10) -0.027(10) -0.049(11) C406 0.178(12) 0.229(13) 0.156(11) -0.042(10) -0.030(10) -0.050(10) C407 0.111(12) 0.163(14) 0.193(16) 0.023(12) -0.056(11) -0.078(11) C408 0.139(14) 0.061(9) 0.151(15) -0.046(9) -0.039(11) 0.012(9) C409 0.142(15) 0.062(9) 0.156(15) -0.040(10) -0.038(12) 0.014(9) C410 0.150(15) 0.067(9) 0.159(16) -0.048(10) -0.030(12) 0.005(10) C411 0.151(15) 0.073(10) 0.160(16) -0.045(10) -0.032(12) 0.001(10) C412 0.148(15) 0.079(10) 0.154(15) -0.043(10) -0.033(12) -0.001(10) C413 0.144(15) 0.073(9) 0.151(15) -0.046(10) -0.032(12) 0.007(10) C414 0.15(2) 0.068(13) 0.16(2) -0.038(14) -0.048(17) 0.007(14) C415 0.148(16) 0.170(17) 0.187(18) -0.063(15) -0.039(14) -0.040(13) C416 0.139(17) 0.169(17) 0.185(18) -0.066(15) -0.044(15) -0.048(13) C417 0.136(17) 0.166(17) 0.182(18) -0.073(16) -0.049(15) -0.043(13) C418 0.146(17) 0.169(17) 0.185(18) -0.073(16) -0.046(15) -0.035(14) C419 0.150(17) 0.167(17) 0.181(18) -0.075(15) -0.046(15) -0.033(14) C420 0.151(17) 0.173(17) 0.187(18) -0.062(16) -0.042(15) -0.036(14) C421 0.14(2) 0.15(2) 0.16(2) -0.084(19) -0.027(19) -0.026(18) C307 0.069(19) 0.18(4) 0.13(3) -0.10(3) 0.022(18) -0.05(2) C308 0.38(12) 0.06(3) 1.5(5) 0.04(9) -0.4(2) -0.13(5) N44 0.092(19) 0.099(18) 0.22(4) -0.10(2) -0.03(2) 0.004(14) C422 0.59(4) 0.187(14) 0.39(3) -0.004(17) -0.31(3) -0.180(18) C423 0.59(4) 0.194(14) 0.39(3) -0.001(17) -0.31(3) -0.180(18) C424 0.59(4) 0.191(15) 0.39(3) -0.002(17) -0.32(3) -0.182(18) C425 0.59(4) 0.193(15) 0.39(3) 0.004(17) -0.32(3) -0.172(18) C426 0.60(4) 0.181(14) 0.39(3) -0.005(17) -0.32(3) -0.169(18) C427 0.59(4) 0.172(14) 0.39(3) -0.009(17) -0.32(3) -0.178(18) C428 0.59(4) 0.221(19) 0.38(3) -0.02(2) -0.30(3) -0.18(2) C429 0.25(2) 1.12(8) 0.34(3) -0.29(4) -0.16(2) 0.22(3) C430 0.25(2) 1.12(8) 0.34(3) -0.29(4) -0.16(2) 0.22(3) C431 0.25(2) 1.12(8) 0.34(3) -0.28(4) -0.16(2) 0.22(3) C432 0.24(2) 1.12(8) 0.33(3) -0.28(4) -0.17(2) 0.22(3) C433 0.24(2) 1.12(8) 0.33(3) -0.28(4) -0.17(2) 0.22(3) C434 0.24(2) 1.12(8) 0.33(3) -0.28(4) -0.17(2) 0.22(3) C435 0.25(3) 1.10(8) 0.33(3) -0.30(4) -0.17(3) 0.20(4) C436 0.087(14) 0.124(15) 0.59(5) -0.12(2) -0.15(2) 0.041(12) C437 0.084(14) 0.122(16) 0.59(5) -0.12(2) -0.15(2) 0.036(12) C438 0.090(15) 0.127(16) 0.59(5) -0.11(2) -0.14(2) 0.039(12) C439 0.092(15) 0.126(16) 0.59(5) -0.12(2) -0.14(2) 0.042(12) C440 0.090(15) 0.125(16) 0.59(5) -0.12(2) -0.15(2) 0.045(12) C441 0.088(15) 0.122(15) 0.59(5) -0.12(2) -0.15(2) 0.044(12) C442 0.106(19) 0.14(2) 0.59(5) -0.12(3) -0.15(3) 0.048(18) N48 0.75(5) 0.22(3) 0.38(5) -0.08(2) -0.31(5) -0.18(4) C315 0.74(5) 0.22(3) 0.38(5) -0.07(2) -0.33(5) -0.19(4) C316 0.74(5) 0.24(3) 0.37(5) -0.05(2) -0.33(5) -0.16(4) N49 0.40(6) 0.28(4) 0.95(13) 0.10(6) 0.08(6) 0.12(3) C317 0.38(6) 0.27(3) 0.94(13) 0.09(6) 0.08(6) 0.16(3) C318 0.37(6) 0.26(3) 0.94(13) 0.08(6) 0.07(7) 0.18(3) N52 0.65(6) 0.67(6) 0.21(4) -0.15(3) -0.16(4) 0.49(4) C324 0.63(6) 0.66(6) 0.23(4) -0.10(4) -0.17(4) 0.51(5) C323 0.64(6) 0.67(6) 0.22(4) -0.12(4) -0.18(4) 0.50(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.334(11) . ? C1 C2 1.372(13) . ? C1 H1 0.9500 . ? C2 C3 1.409(14) . ? C2 H2 0.9500 . ? C3 C4 1.360(14) . ? C3 H3 0.9500 . ? C4 C5 1.390(12) . ? C4 H4 0.9500 . ? C5 N1 1.353(10) . ? C5 C6 1.422(12) . ? C6 N2 1.272(10) . ? C6 H6 0.9500 . ? C7 N4 1.375(9) . ? C7 C8 1.379(11) . ? C7 N3 1.389(10) . ? C8 C9 1.380(11) . ? C8 H8 0.9500 . ? C9 N5 1.344(9) . ? C9 N6 1.373(10) . ? C10 N5 1.323(10) . ? C10 N4 1.337(10) . ? C10 C11 1.490(10) . ? C11 C16 1.366(13) . ? C11 C12 1.390(12) . ? C12 C13 1.370(14) . ? C12 H12 0.9500 . ? C13 C14 1.28(2) . ? C13 H13 0.9500 . ? C14 C15 1.45(2) . ? C14 H14 0.9500 . ? C15 C16 1.454(15) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N7 1.262(11) . ? C17 C18 1.475(12) . ? C17 H17 0.9500 . ? C18 N8 1.355(11) . ? C18 C19 1.357(13) . ? C19 C20 1.396(15) . ? C19 H19 0.9500 . ? C20 C21 1.370(16) . ? C20 H20 0.9500 . ? C21 C22 1.366(14) . ? C21 H21 0.9500 . ? C22 N8 1.334(11) . ? C22 H22 0.9500 . ? C23 N3 1.452(9) . ? C23 C24 1.531(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 O1 1.210(9) . ? C24 N9 1.334(10) . ? C25 N9 1.464(10) . ? C25 C26 1.518(13) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 S1 1.820(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C40 1.500(16) . ? C27 C34 1.554(14) . ? C27 C28 1.566(13) . ? C27 S1 1.854(9) . ? C28 C29 1.380(15) . ? C28 C33 1.410(13) . ? C29 C30 1.399(16) . ? C29 H29 0.9500 . ? C30 C31 1.359(18) . ? C30 H30 0.9500 . ? C31 C32 1.376(18) . ? C31 H31 0.9500 . ? C32 C33 1.373(14) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.343(17) . ? C34 C35 1.399(17) . ? C35 C36 1.35(2) . ? C35 H35 0.9500 . ? C36 C37 1.45(4) . ? C36 H36 0.9500 . ? C37 C38 1.43(3) . ? C37 H37 0.9500 . ? C38 C39 1.41(2) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.368(16) . ? C40 C41 1.383(16) . ? C41 C42 1.438(19) . ? C41 H41 0.9500 . ? C42 C43 1.40(3) . ? C42 H42 0.9500 . ? C43 C44 1.37(3) . ? C43 H43 0.9500 . ? C44 C45 1.34(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 N6 1.460(10) . ? C46 C47 1.538(12) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 O2 1.228(11) . ? C47 N10 1.326(12) . ? C48 N10 1.452(11) . ? C48 C49 1.518(14) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 S2 1.817(10) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C63 1.525(14) . ? C50 C57 1.536(14) . ? C50 C51 1.547(14) . ? C50 S2 1.860(10) . ? C51 C56 1.357(15) . ? C51 C52 1.384(14) . ? C52 C53 1.392(16) . ? C52 H52 0.9500 . ? C53 C54 1.345(17) . ? C53 H53 0.9500 . ? C54 C55 1.383(17) . ? C54 H54 0.9500 . ? C55 C56 1.375(16) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 C62 1.372(16) . ? C57 C58 1.382(15) . ? C58 C59 1.408(18) . ? C58 H58 0.9500 . ? C59 C60 1.37(2) . ? C59 H59 0.9500 . ? C60 C61 1.37(2) . ? C60 H60 0.9500 . ? C61 C62 1.41(2) . ? C61 H61 0.9500 . ? C62 H62 0.9500 . ? C63 C68 1.401(15) . ? C63 C64 1.403(16) . ? C64 C65 1.42(2) . ? C64 H64 0.9500 . ? C65 C66 1.32(2) . ? C65 H65 0.9500 . ? C66 C67 1.40(2) . ? C66 H66 0.9500 . ? C67 C68 1.358(16) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C71 N11 1.334(11) . ? C71 C72 1.403(12) . ? C71 H71 0.9500 . ? C72 C73 1.360(13) . ? C72 H72 0.9500 . ? C73 C74 1.394(12) . ? C73 H73 0.9500 . ? C74 C75 1.395(10) . ? C74 H74 0.9500 . ? C75 N11 1.333(10) . ? C75 C76 1.459(11) . ? C76 N12 1.277(9) . ? C76 H76 0.9500 . ? C77 N14 1.358(10) . ? C77 C78 1.380(11) . ? C77 N13 1.386(9) . ? C78 C79 1.384(10) . ? C78 H78 0.9500 . ? C79 N15 1.363(9) . ? C79 N16 1.396(10) . ? C80 N14 1.329(9) . ? C80 N15 1.330(9) . ? C80 C81 1.504(10) . ? C81 C86 1.360(13) . ? C81 C82 1.393(12) . ? C82 C83 1.399(14) . ? C82 H82 0.9500 . ? C83 C84 1.325(18) . ? C83 H83 0.9500 . ? C84 C85 1.374(18) . ? C84 H84 0.9500 . ? C85 C86 1.412(14) . ? C85 H85 0.9500 . ? C86 H86 0.9500 . ? C87 N17 1.252(10) . ? C87 C88 1.482(12) . ? C87 H87 0.9500 . ? C88 N18 1.357(12) . ? C88 C89 1.401(13) . ? C89 C90 1.395(16) . ? C89 H89 0.9500 . ? C90 C91 1.350(16) . ? C90 H90 0.9500 . ? C91 C92 1.348(14) . ? C91 H91 0.9500 . ? C92 N18 1.328(11) . ? C92 H92 0.9500 . ? C93 N13 1.451(9) . ? C93 C94 1.513(12) . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? C94 O3 1.218(9) . ? C94 N19 1.337(10) . ? C95 N19 1.456(11) . ? C95 C96 1.540(12) . ? C95 H95A 0.9900 . ? C95 H95B 0.9900 . ? C96 S3 1.795(8) . ? C96 H96A 0.9900 . ? C96 H96B 0.9900 . ? C97 C110 1.520(13) . ? C97 C104 1.522(14) . ? C97 C98 1.528(13) . ? C97 S3 1.873(9) . ? C98 C99 1.378(14) . ? C98 C103 1.395(15) . ? C99 C100 1.421(16) . ? C99 H99 0.9500 . ? C100 C101 1.33(2) . ? C100 H100 0.9500 . ? C101 C102 1.38(2) . ? C101 H101 0.9500 . ? C102 C103 1.393(18) . ? C102 H102 0.9500 . ? C103 H103 0.9500 . ? C104 C109 1.375(14) . ? C104 C105 1.377(14) . ? C105 C106 1.406(16) . ? C105 H105 0.9500 . ? C106 C107 1.380(17) . ? C106 H106 0.9500 . ? C107 C108 1.358(18) . ? C107 H107 0.9500 . ? C108 C109 1.369(16) . ? C108 H108 0.9500 . ? C109 H109 0.9500 . ? C110 C115 1.399(15) . ? C110 C111 1.400(15) . ? C111 C112 1.414(19) . ? C111 H111 0.9500 . ? C112 C113 1.39(2) . ? C112 H112 0.9500 . ? C113 C114 1.347(18) . ? C113 H113 0.9500 . ? C114 C115 1.391(14) . ? C114 H114 0.9500 . ? C115 H115 0.9500 . ? C116 N16 1.454(10) . ? C116 C117 1.520(13) . ? C116 H11A 0.9900 . ? C116 H11B 0.9900 . ? C117 O4 1.236(11) . ? C117 N20 1.293(11) . ? C118 C119 1.464(15) . ? C118 N20 1.486(13) . ? C118 H11C 0.9900 . ? C118 H11D 0.9900 . ? C119 S4 1.810(13) . ? C119 H11E 0.9900 . ? C119 H11F 0.9900 . ? C120 C133 1.53(2) . ? C120 C127 1.537(19) . ? C120 C121 1.563(19) . ? C120 S4 1.875(16) . ? C121 C122 1.35(2) . ? C121 C126 1.402(18) . ? C122 C123 1.38(2) . ? C122 H122 0.9500 . ? C123 C124 1.32(2) . ? C123 H123 0.9500 . ? C124 C125 1.375(19) . ? C124 H124 0.9500 . ? C125 C126 1.373(18) . ? C125 H125 0.9500 . ? C126 H126 0.9500 . ? C127 C128 1.34(2) . ? C127 C132 1.45(2) . ? C128 C129 1.39(2) . ? C128 H128 0.9500 . ? C129 C130 1.38(2) . ? C129 H129 0.9500 . ? C130 C131 1.36(3) . ? C130 H130 0.9500 . ? C131 C132 1.41(2) . ? C131 H131 0.9500 . ? C132 H132 0.9500 . ? C133 C138 1.39(2) . ? C133 C134 1.43(2) . ? C134 C135 1.38(2) . ? C134 H134 0.9500 . ? C135 C136 1.45(3) . ? C135 H135 0.9500 . ? C136 C137 1.36(3) . ? C136 H136 0.9500 . ? C137 C138 1.38(2) . ? C137 H137 0.9500 . ? C138 H138 0.9500 . ? C141 N21 1.305(11) . ? C141 C142 1.419(12) . ? C141 H141 0.9500 . ? C142 C143 1.365(14) . ? C142 H142 0.9500 . ? C143 C144 1.374(14) . ? C143 H143 0.9500 . ? C144 C145 1.367(11) . ? C144 H144 0.9500 . ? C145 N21 1.369(10) . ? C145 C146 1.449(12) . ? C146 N22 1.289(10) . ? C146 H146 0.9500 . ? C147 N24 1.366(9) . ? C147 N23 1.381(9) . ? C147 C148 1.391(11) . ? C148 C149 1.385(10) . ? C148 H148 0.9500 . ? C149 N25 1.354(10) . ? C149 N26 1.366(10) . ? C150 N25 1.342(10) . ? C150 N24 1.357(9) . ? C150 C151 1.492(11) . ? C151 C152 1.379(12) . ? C151 C156 1.384(14) . ? C152 C153 1.407(15) . ? C152 H152 0.9500 . ? C153 C154 1.33(2) . ? C153 H153 0.9500 . ? C154 C155 1.38(2) . ? C154 H154 0.9500 . ? C155 C156 1.374(15) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? C157 N27 1.266(10) . ? C157 C158 1.475(12) . ? C157 H157 0.9500 . ? C158 N28 1.338(11) . ? C158 C159 1.387(13) . ? C159 C160 1.398(15) . ? C159 H159 0.9500 . ? C160 C161 1.364(16) . ? C160 H160 0.9500 . ? C161 C162 1.382(14) . ? C161 H161 0.9500 . ? C162 N28 1.332(11) . ? C162 H162 0.9500 . ? C163 N23 1.455(9) . ? C163 C164 1.547(12) . ? C163 H16A 0.9900 . ? C163 H16B 0.9900 . ? C164 O5 1.203(10) . ? C164 N29 1.332(10) . ? C165 N29 1.457(10) . ? C165 C166 1.503(13) . ? C165 H16C 0.9900 . ? C165 H16D 0.9900 . ? C166 S5 1.813(11) . ? C166 H16E 0.9900 . ? C166 H16F 0.9900 . ? C167 C180 1.516(14) . ? C167 C168 1.524(13) . ? C167 C174 1.550(15) . ? C167 S5 1.866(10) . ? C168 C169 1.381(14) . ? C168 C173 1.389(14) . ? C169 C170 1.403(18) . ? C169 H169 0.9500 . ? C170 C171 1.40(2) . ? C170 H170 0.9500 . ? C171 C172 1.363(19) . ? C171 H171 0.9500 . ? C172 C173 1.379(16) . ? C172 H172 0.9500 . ? C173 H173 0.9500 . ? C174 C179 1.346(16) . ? C174 C175 1.393(16) . ? C175 C176 1.38(2) . ? C175 H175 0.9500 . ? C176 C177 1.34(2) . ? C176 H176 0.9500 . ? C177 C178 1.38(2) . ? C177 H177 0.9500 . ? C178 C179 1.392(19) . ? C178 H178 0.9500 . ? C179 H179 0.9500 . ? C180 C185 1.377(16) . ? C180 C181 1.396(15) . ? C181 C182 1.349(18) . ? C181 H181 0.9500 . ? C182 C183 1.40(2) . ? C182 H182 0.9500 . ? C183 C184 1.38(2) . ? C183 H183 0.9500 . ? C184 C185 1.399(17) . ? C184 H184 0.9500 . ? C185 H185 0.9500 . ? C186 N26 1.456(10) . ? C186 C187 1.546(12) . ? C186 H18A 0.9900 . ? C186 H18B 0.9900 . ? C187 O6 1.204(10) . ? C187 N30 1.325(11) . ? C188 N30 1.453(12) . ? C188 C189 1.489(15) . ? C188 H18C 0.9900 . ? C188 H18D 0.9900 . ? C189 S6 1.811(12) . ? C189 H18E 0.9900 . ? C189 H18F 0.9900 . ? C190 C191 1.440(19) . ? C190 C197 1.477(18) . ? C190 C203 1.53(2) . ? C190 S6 1.908(15) . ? C191 C192 1.36(2) . ? C191 C196 1.422(19) . ? C192 C193 1.35(2) . ? C192 H192 0.9500 . ? C193 C194 1.42(3) . ? C193 H193 0.9500 . ? C194 C195 1.37(3) . ? C194 H194 0.9500 . ? C195 C196 1.34(2) . ? C195 H195 0.9500 . ? C196 H196 0.9500 . ? C197 C198 1.360(18) . ? C197 C202 1.461(19) . ? C198 C199 1.36(2) . ? C198 H198 0.9500 . ? C199 C200 1.37(2) . ? C199 H199 0.9500 . ? C200 C201 1.343(18) . ? C200 H200 0.9500 . ? C201 C202 1.431(17) . ? C201 H201 0.9500 . ? C202 H202 0.9500 . ? C203 C204 1.39(2) . ? C203 C208 1.42(2) . ? C204 C205 1.51(2) . ? C204 H204 0.9500 . ? C205 C206 1.35(3) . ? C205 H205 0.9500 . ? C206 C207 1.38(3) . ? C206 H206 0.9500 . ? C207 C208 1.41(2) . ? C207 H207 0.9500 . ? C208 H208 0.9500 . ? C211 N31 1.324(14) . ? C211 C212 1.411(17) . ? C211 H211 0.9500 . ? C212 C213 1.40(2) . ? C212 H212 0.9500 . ? C213 C214 1.343(18) . ? C213 H213 0.9500 . ? C214 C215 1.410(14) . ? C214 H214 0.9500 . ? C215 N31 1.362(12) . ? C215 C216 1.416(14) . ? C216 N32 1.278(10) . ? C216 H216 0.9500 . ? C217 N34 1.341(10) . ? C217 C218 1.373(12) . ? C217 N33 1.399(10) . ? C218 C219 1.393(11) . ? C218 H218 0.9500 . ? C219 N35 1.366(10) . ? C219 N36 1.380(11) . ? C220 N35 1.329(10) . ? C220 N34 1.334(10) . ? C220 C221 1.499(11) . ? C221 C226 1.364(14) . ? C221 C222 1.403(13) . ? C222 C223 1.394(17) . ? C222 H222 0.9500 . ? C223 C224 1.31(3) . ? C223 H223 0.9500 . ? C224 C225 1.38(3) . ? C224 H224 0.9500 . ? C225 C226 1.441(19) . ? C225 H225 0.9500 . ? C226 H226 0.9500 . ? C227 N37 1.259(11) . ? C227 C228 1.475(13) . ? C227 H227 0.9500 . ? C228 N38 1.345(11) . ? C228 C229 1.360(14) . ? C229 C230 1.389(16) . ? C229 H229 0.9500 . ? C230 C231 1.343(16) . ? C230 H230 0.9500 . ? C231 C232 1.398(15) . ? C231 H231 0.9500 . ? C232 N38 1.323(11) . ? C232 H232 0.9500 . ? C233 N33 1.463(9) . ? C233 C234 1.542(11) . ? C233 H23C 0.9900 . ? C233 H23D 0.9900 . ? C234 O7 1.212(11) . ? C234 N39 1.328(11) . ? C235 N39 1.463(10) . ? C235 C236 1.508(14) . ? C235 H23E 0.9900 . ? C235 H23F 0.9900 . ? C236 S7 1.807(9) . ? C236 H23G 0.9900 . ? C236 H23H 0.9900 . ? C237 C244 1.457(17) . ? C237 C238 1.543(15) . ? C237 C250 1.565(16) . ? C237 S7 1.871(11) . ? C238 C239 1.381(18) . ? C238 C243 1.396(17) . ? C239 C240 1.35(2) . ? C239 H239 0.9500 . ? C240 C241 1.32(3) . ? C240 H240 0.9500 . ? C241 C242 1.36(3) . ? C241 H241 0.9500 . ? C242 C243 1.375(17) . ? C242 H242 0.9500 . ? C243 H243 0.9500 . ? C244 C249 1.398(18) . ? C244 C245 1.420(19) . ? C245 C246 1.42(3) . ? C245 H245 0.9500 . ? C246 C247 1.30(3) . ? C246 H246 0.9500 . ? C247 C248 1.41(3) . ? C247 H247 0.9500 . ? C248 C249 1.397(19) . ? C248 H248 0.9500 . ? C249 H249 0.9500 . ? C250 C251 1.38(2) . ? C250 C255 1.394(18) . ? C251 C252 1.39(2) . ? C251 H251 0.9500 . ? C252 C253 1.39(3) . ? C252 H252 0.9500 . ? C253 C254 1.37(3) . ? C253 H253 0.9500 . ? C254 C255 1.382(19) . ? C254 H254 0.9500 . ? C255 H255 0.9500 . ? C256 N36 1.463(10) . ? C256 C257 1.503(13) . ? C256 H25C 0.9900 . ? C256 H25D 0.9900 . ? C257 O8 1.220(11) . ? C257 N40 1.335(12) . ? C258 N40 1.448(13) . ? C258 C259 1.531(15) . ? C258 H25E 0.9900 . ? C258 H25F 0.9900 . ? C259 S8 1.804(11) . ? C259 H25G 0.9900 . ? C259 H25H 0.9900 . ? C260 C261 1.517(18) . ? C260 C267 1.522(17) . ? C260 C273 1.525(18) . ? C260 S8 1.876(14) . ? C261 C266 1.321(18) . ? C261 C262 1.430(17) . ? C262 C263 1.351(17) . ? C262 H262 0.9500 . ? C263 C264 1.47(2) . ? C263 H263 0.9500 . ? C264 C265 1.40(2) . ? C264 H264 0.9500 . ? C265 C266 1.40(2) . ? C265 H265 0.9500 . ? C266 H266 0.9500 . ? C267 C272 1.375(19) . ? C267 C268 1.384(19) . ? C268 C269 1.364(19) . ? C268 H268 0.9500 . ? C269 C270 1.36(3) . ? C269 H269 0.9500 . ? C270 C271 1.36(3) . ? C270 H270 0.9500 . ? C271 C272 1.39(2) . ? C271 H271 0.9500 . ? C272 H272 0.9500 . ? C273 C278 1.301(18) . ? C273 C274 1.465(19) . ? C274 C275 1.33(2) . ? C274 H274 0.9500 . ? C275 C276 1.30(3) . ? C275 H275 0.9500 . ? C276 C277 1.37(3) . ? C276 H276 0.9500 . ? C277 C278 1.43(2) . ? C277 H277 0.9500 . ? C278 H278 0.9500 . ? N1 Cu1 2.062(7) . ? N2 N3 1.354(9) . ? N2 Cu1 1.968(6) . ? N4 Cu1 2.123(6) . ? N5 Cu2 2.331(6) . ? N6 N7 1.378(9) . ? N7 Cu2 2.032(7) . ? N8 Cu2 2.247(7) . ? N9 H9 0.8800 . ? N10 H10 0.8800 . ? N11 Cu1 2.265(6) . ? N12 N13 1.361(9) . ? N12 Cu1 2.050(6) . ? N14 Cu1 2.311(6) . ? N15 Cu3 2.127(6) . ? N16 N17 1.353(9) . ? N17 Cu3 1.972(7) . ? N18 Cu3 2.048(7) . ? N19 H19A 0.8800 . ? N20 H20A 0.8800 . ? N21 Cu2 2.083(6) . ? N22 N23 1.357(9) . ? N22 Cu2 1.959(6) . ? N24 Cu2 2.116(6) . ? N25 Cu4 2.289(6) . ? N26 N27 1.372(9) . ? N27 Cu4 2.047(7) . ? N28 Cu4 2.280(7) . ? N29 H29A 0.8800 . ? N30 H30X 0.8800 . ? N31 Cu3 2.272(8) . ? N32 N33 1.374(10) . ? N32 Cu3 2.051(7) . ? N34 Cu3 2.330(7) . ? N35 Cu4 2.102(7) . ? N36 N37 1.359(9) . ? N37 Cu4 1.975(7) . ? N38 Cu4 2.064(7) . ? N39 H39A 0.8800 . ? N40 H40 0.8800 . ? F1 B1 1.377(14) . ? F2 B1 1.331(13) . ? F3 B1 1.324(17) . ? F4 B1 1.327(18) . ? F5 B2 1.408(17) . ? F6 B2 1.279(16) . ? F7 B2 1.313(15) . ? F8 B2 1.404(19) . ? F9 B3 1.26(2) . ? F10 B3 1.36(3) . ? F10 F11 1.75(4) . ? F11 B3 1.22(2) . ? F12 B3 1.301(18) . ? F13 B4 1.364(18) . ? F14 B4 1.47(3) . ? F15 B4 1.34(2) . ? F16 B4 1.28(2) . ? F17 B5 1.408(17) . ? F18 B5 1.280(17) . ? F19 B5 1.319(16) . ? F20 B5 1.27(2) . ? F21 B6 1.296(16) . ? F22 B6 1.353(15) . ? F23 B6 1.29(2) . ? F24 B6 1.218(18) . ? F25 B7 1.336(18) . ? F26 B7 1.334(18) . ? F27 B7 1.334(18) . ? F28 B7 1.335(18) . ? F29 B8 1.37(4) . ? F30 B8 1.31(3) . ? F31 B8 1.23(3) . ? F32 B8 1.35(2) . ? C301 N41 1.13(2) . ? C301 C302 1.47(2) . ? C302 H30A 0.9800 . ? C302 H30B 0.9800 . ? C302 H30C 0.9800 . ? C303 N42 1.16(2) . ? C303 C304 1.33(3) . ? C304 H30D 0.9800 . ? C304 H30E 0.9800 . ? C304 H30F 0.9800 . ? C305 N43 1.15(5) . ? C305 C306 1.53(5) . ? C309 N45 1.14(5) . ? C309 C310 1.52(5) . ? C311 N46 1.15(5) . ? C311 C312 1.53(5) . ? C313 N47 1.15(5) . ? C313 C314 1.52(5) . ? N50 C319 1.15(5) . ? C319 C320 1.53(5) . ? C401 C402 1.3900 . ? C401 C406 1.3900 . ? C401 H401 0.9500 . ? C402 C403 1.3900 . ? C402 C407 1.53(3) . ? C403 C404 1.3900 . ? C403 H403 0.9500 . ? C404 C405 1.3900 . ? C404 H404 0.9500 . ? C405 C406 1.3900 . ? C405 H405 0.9500 . ? C406 H406 0.9500 . ? C407 H40A 0.9800 . ? C407 H40B 0.9800 . ? C407 H40C 0.9800 . ? C408 C409 1.3900 . ? C408 C413 1.3900 . ? C408 C414 1.54(4) . ? C409 C410 1.3900 . ? C410 C411 1.3900 . ? C411 C412 1.3900 . ? C411 C412 1.59(3) 2_775 ? C411 C411 1.67(4) 2_775 ? C412 C413 1.3900 . ? C412 C411 1.59(4) 2_775 ? C415 C416 1.3900 . ? C415 C420 1.3900 . ? C415 C421 1.54(3) . ? C416 C417 1.3900 . ? C416 H416 0.9500 . ? C417 C418 1.3900 . ? C417 H417 0.9500 . ? C418 C419 1.3900 . ? C418 H418 0.9500 . ? C419 C420 1.3900 . ? C419 H419 0.9500 . ? C420 H420 0.9500 . ? C421 H42A 0.9800 . ? C421 H42B 0.9800 . ? C421 H42C 0.9800 . ? C307 N44 1.14(5) . ? C307 C308 1.53(5) . ? C422 C423 1.3900 . ? C422 C427 1.3900 . ? C422 C428 1.53(3) . ? C423 C424 1.3900 . ? C423 H423 0.9500 . ? C424 C425 1.3900 . ? C424 H424 0.9500 . ? C425 C426 1.3900 . ? C425 H425 0.9500 . ? C426 C427 1.3900 . ? C426 H426 0.9500 . ? C427 H427 0.9500 . ? C428 H42D 0.9800 . ? C428 H42E 0.9800 . ? C428 H42F 0.9800 . ? C429 C430 1.3900 . ? C429 C434 1.3900 . ? C429 C435 1.54(3) . ? C430 C431 1.3900 . ? C430 H430 0.9500 . ? C431 C432 1.3900 . ? C431 H431 0.9500 . ? C432 C433 1.3900 . ? C432 H432 0.9500 . ? C433 C434 1.3900 . ? C433 H433 0.9500 . ? C434 H434 0.9500 . ? C435 H43A 0.9800 . ? C435 H43B 0.9800 . ? C435 H43C 0.9800 . ? C436 C437 1.3900 . ? C436 C441 1.3900 . ? C436 C442 1.54(3) . ? C437 C438 1.3900 . ? C437 H437 0.9500 . ? C438 C439 1.3900 . ? C438 H438 0.9500 . ? C439 C440 1.3900 . ? C439 H439 0.9500 . ? C440 C441 1.3900 . ? C440 H440 0.9500 . ? C441 H441 0.9500 . ? C442 H44A 0.9800 . ? C442 H44B 0.9800 . ? C442 H44C 0.9800 . ? N48 C315 1.14(5) . ? C315 C316 1.52(5) . ? N49 C317 1.14(5) . ? C317 C318 1.52(5) . ? N52 C323 1.15(5) . ? C324 C323 1.52(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 123.2(8) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 118.2(10) . . ? C1 C2 H2 120.9 . . ? C3 C2 H2 120.9 . . ? C4 C3 C2 119.2(9) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 119.0(8) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 122.2(9) . . ? N1 C5 C6 114.9(7) . . ? C4 C5 C6 122.8(7) . . ? N2 C6 C5 117.0(7) . . ? N2 C6 H6 121.5 . . ? C5 C6 H6 121.5 . . ? N4 C7 C8 122.4(7) . . ? N4 C7 N3 115.0(7) . . ? C8 C7 N3 122.6(7) . . ? C7 C8 C9 116.4(7) . . ? C7 C8 H8 121.8 . . ? C9 C8 H8 121.8 . . ? N5 C9 N6 117.1(7) . . ? N5 C9 C8 121.7(7) . . ? N6 C9 C8 121.3(7) . . ? N5 C10 N4 125.0(7) . . ? N5 C10 C11 115.6(7) . . ? N4 C10 C11 119.4(7) . . ? C16 C11 C12 121.1(9) . . ? C16 C11 C10 120.3(8) . . ? C12 C11 C10 118.5(8) . . ? C13 C12 C11 121.1(12) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C14 C13 C12 120.1(13) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 123.7(12) . . ? C13 C14 H14 118.1 . . ? C15 C14 H14 118.1 . . ? C14 C15 C16 115.6(11) . . ? C14 C15 H15 122.2 . . ? C16 C15 H15 122.2 . . ? C11 C16 C15 118.4(11) . . ? C11 C16 H16 120.8 . . ? C15 C16 H16 120.8 . . ? N7 C17 C18 120.0(7) . . ? N7 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? N8 C18 C19 123.9(8) . . ? N8 C18 C17 114.8(7) . . ? C19 C18 C17 121.4(9) . . ? C18 C19 C20 118.3(10) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.9 . . ? C21 C20 C19 117.8(10) . . ? C21 C20 H20 121.1 . . ? C19 C20 H20 121.1 . . ? C22 C21 C20 120.6(10) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? N8 C22 C21 122.2(9) . . ? N8 C22 H22 118.9 . . ? C21 C22 H22 118.9 . . ? N3 C23 C24 109.7(6) . . ? N3 C23 H23A 109.7 . . ? C24 C23 H23A 109.7 . . ? N3 C23 H23B 109.7 . . ? C24 C23 H23B 109.7 . . ? H23A C23 H23B 108.2 . . ? O1 C24 N9 125.7(8) . . ? O1 C24 C23 119.3(7) . . ? N9 C24 C23 115.0(7) . . ? N9 C25 C26 112.6(8) . . ? N9 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? N9 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? C25 C26 S1 114.9(7) . . ? C25 C26 H26A 108.5 . . ? S1 C26 H26A 108.5 . . ? C25 C26 H26B 108.5 . . ? S1 C26 H26B 108.5 . . ? H26A C26 H26B 107.5 . . ? C40 C27 C34 113.0(9) . . ? C40 C27 C28 114.5(8) . . ? C34 C27 C28 105.1(8) . . ? C40 C27 S1 107.8(7) . . ? C34 C27 S1 112.8(7) . . ? C28 C27 S1 103.3(6) . . ? C29 C28 C33 118.3(9) . . ? C29 C28 C27 119.6(9) . . ? C33 C28 C27 122.0(10) . . ? C28 C29 C30 120.9(11) . . ? C28 C29 H29 119.6 . . ? C30 C29 H29 119.6 . . ? C31 C30 C29 119.8(13) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 120.2(11) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 121.0(10) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 C28 119.8(11) . . ? C32 C33 H33 120.1 . . ? C28 C33 H33 120.1 . . ? C39 C34 C35 120.2(12) . . ? C39 C34 C27 123.6(11) . . ? C35 C34 C27 116.3(11) . . ? C36 C35 C34 123.2(17) . . ? C36 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? C35 C36 C37 116.8(19) . . ? C35 C36 H36 121.6 . . ? C37 C36 H36 121.6 . . ? C38 C37 C36 120.4(17) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C39 C38 C37 117.8(19) . . ? C39 C38 H38 121.1 . . ? C37 C38 H38 121.1 . . ? C34 C39 C38 121.4(16) . . ? C34 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C45 C40 C41 116.9(13) . . ? C45 C40 C27 122.5(13) . . ? C41 C40 C27 120.0(10) . . ? C40 C41 C42 122.1(14) . . ? C40 C41 H41 118.9 . . ? C42 C41 H41 118.9 . . ? C43 C42 C41 115.1(18) . . ? C43 C42 H42 122.5 . . ? C41 C42 H42 122.5 . . ? C44 C43 C42 122.6(19) . . ? C44 C43 H43 118.7 . . ? C42 C43 H43 118.7 . . ? C45 C44 C43 119(2) . . ? C45 C44 H44 120.7 . . ? C43 C44 H44 120.7 . . ? C44 C45 C40 124.6(19) . . ? C44 C45 H45 117.7 . . ? C40 C45 H45 117.7 . . ? N6 C46 C47 109.5(6) . . ? N6 C46 H46A 109.8 . . ? C47 C46 H46A 109.8 . . ? N6 C46 H46B 109.8 . . ? C47 C46 H46B 109.8 . . ? H46A C46 H46B 108.2 . . ? O2 C47 N10 125.4(9) . . ? O2 C47 C46 119.9(8) . . ? N10 C47 C46 114.7(8) . . ? N10 C48 C49 112.9(8) . . ? N10 C48 H48A 109.0 . . ? C49 C48 H48A 109.0 . . ? N10 C48 H48B 109.0 . . ? C49 C48 H48B 109.0 . . ? H48A C48 H48B 107.8 . . ? C48 C49 S2 109.8(7) . . ? C48 C49 H49A 109.7 . . ? S2 C49 H49A 109.7 . . ? C48 C49 H49B 109.7 . . ? S2 C49 H49B 109.7 . . ? H49A C49 H49B 108.2 . . ? C63 C50 C57 108.5(8) . . ? C63 C50 C51 114.3(9) . . ? C57 C50 C51 112.4(8) . . ? C63 C50 S2 102.4(7) . . ? C57 C50 S2 113.2(7) . . ? C51 C50 S2 105.7(6) . . ? C56 C51 C52 116.9(10) . . ? C56 C51 C50 122.5(9) . . ? C52 C51 C50 120.5(9) . . ? C51 C52 C53 120.3(11) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C54 C53 C52 121.4(12) . . ? C54 C53 H53 119.3 . . ? C52 C53 H53 119.3 . . ? C53 C54 C55 119.1(12) . . ? C53 C54 H54 120.5 . . ? C55 C54 H54 120.5 . . ? C56 C55 C54 118.8(13) . . ? C56 C55 H55 120.6 . . ? C54 C55 H55 120.6 . . ? C51 C56 C55 123.4(11) . . ? C51 C56 H56 118.3 . . ? C55 C56 H56 118.3 . . ? C62 C57 C58 119.2(11) . . ? C62 C57 C50 122.9(10) . . ? C58 C57 C50 117.8(10) . . ? C57 C58 C59 120.9(14) . . ? C57 C58 H58 119.5 . . ? C59 C58 H58 119.5 . . ? C60 C59 C58 119.1(15) . . ? C60 C59 H59 120.4 . . ? C58 C59 H59 120.4 . . ? C59 C60 C61 120.6(15) . . ? C59 C60 H60 119.7 . . ? C61 C60 H60 119.7 . . ? C60 C61 C62 120.1(16) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C57 C62 C61 120.0(15) . . ? C57 C62 H62 120.0 . . ? C61 C62 H62 120.0 . . ? C68 C63 C64 118.8(11) . . ? C68 C63 C50 118.1(10) . . ? C64 C63 C50 123.1(11) . . ? C63 C64 C65 116.8(13) . . ? C63 C64 H64 121.6 . . ? C65 C64 H64 121.6 . . ? C66 C65 C64 123.9(14) . . ? C66 C65 H65 118.1 . . ? C64 C65 H65 118.1 . . ? C65 C66 C67 119.1(14) . . ? C65 C66 H66 120.5 . . ? C67 C66 H66 120.5 . . ? C68 C67 C66 119.7(14) . . ? C68 C67 H67 120.1 . . ? C66 C67 H67 120.1 . . ? C67 C68 C63 121.7(12) . . ? C67 C68 H68 119.2 . . ? C63 C68 H68 119.2 . . ? N11 C71 C72 121.8(8) . . ? N11 C71 H71 119.1 . . ? C72 C71 H71 119.1 . . ? C73 C72 C71 119.1(8) . . ? C73 C72 H72 120.4 . . ? C71 C72 H72 120.4 . . ? C72 C73 C74 119.9(8) . . ? C72 C73 H73 120.1 . . ? C74 C73 H73 120.1 . . ? C73 C74 C75 117.3(8) . . ? C73 C74 H74 121.4 . . ? C75 C74 H74 121.4 . . ? N11 C75 C74 123.3(7) . . ? N11 C75 C76 116.5(7) . . ? C74 C75 C76 120.2(7) . . ? N12 C76 C75 119.2(7) . . ? N12 C76 H76 120.4 . . ? C75 C76 H76 120.4 . . ? N14 C77 C78 121.9(6) . . ? N14 C77 N13 116.3(6) . . ? C78 C77 N13 121.8(7) . . ? C77 C78 C79 116.1(7) . . ? C77 C78 H78 121.9 . . ? C79 C78 H78 121.9 . . ? N15 C79 C78 123.0(7) . . ? N15 C79 N16 115.7(6) . . ? C78 C79 N16 121.3(7) . . ? N14 C80 N15 126.4(7) . . ? N14 C80 C81 114.7(6) . . ? N15 C80 C81 118.8(6) . . ? C86 C81 C82 121.2(8) . . ? C86 C81 C80 120.7(8) . . ? C82 C81 C80 118.0(8) . . ? C81 C82 C83 118.0(11) . . ? C81 C82 H82 121.0 . . ? C83 C82 H82 121.0 . . ? C84 C83 C82 122.0(11) . . ? C84 C83 H83 119.0 . . ? C82 C83 H83 119.0 . . ? C83 C84 C85 119.9(10) . . ? C83 C84 H84 120.0 . . ? C85 C84 H84 120.0 . . ? C84 C85 C86 120.7(11) . . ? C84 C85 H85 119.7 . . ? C86 C85 H85 119.7 . . ? C81 C86 C85 118.2(10) . . ? C81 C86 H86 120.9 . . ? C85 C86 H86 120.9 . . ? N17 C87 C88 115.5(8) . . ? N17 C87 H87 122.3 . . ? C88 C87 H87 122.3 . . ? N18 C88 C89 123.4(9) . . ? N18 C88 C87 114.7(7) . . ? C89 C88 C87 121.8(10) . . ? C90 C89 C88 116.3(10) . . ? C90 C89 H89 121.8 . . ? C88 C89 H89 121.8 . . ? C91 C90 C89 119.5(9) . . ? C91 C90 H90 120.3 . . ? C89 C90 H90 120.3 . . ? C92 C91 C90 120.6(10) . . ? C92 C91 H91 119.7 . . ? C90 C91 H91 119.7 . . ? N18 C92 C91 123.5(10) . . ? N18 C92 H92 118.2 . . ? C91 C92 H92 118.2 . . ? N13 C93 C94 109.1(6) . . ? N13 C93 H93A 109.9 . . ? C94 C93 H93A 109.9 . . ? N13 C93 H93B 109.9 . . ? C94 C93 H93B 109.9 . . ? H93A C93 H93B 108.3 . . ? O3 C94 N19 124.1(8) . . ? O3 C94 C93 120.5(7) . . ? N19 C94 C93 115.3(7) . . ? N19 C95 C96 112.4(7) . . ? N19 C95 H95A 109.1 . . ? C96 C95 H95A 109.1 . . ? N19 C95 H95B 109.1 . . ? C96 C95 H95B 109.1 . . ? H95A C95 H95B 107.9 . . ? C95 C96 S3 110.1(6) . . ? C95 C96 H96A 109.6 . . ? S3 C96 H96A 109.6 . . ? C95 C96 H96B 109.6 . . ? S3 C96 H96B 109.6 . . ? H96A C96 H96B 108.2 . . ? C110 C97 C104 115.6(8) . . ? C110 C97 C98 107.6(7) . . ? C104 C97 C98 113.3(8) . . ? C110 C97 S3 102.7(6) . . ? C104 C97 S3 105.1(6) . . ? C98 C97 S3 112.0(7) . . ? C99 C98 C103 117.1(10) . . ? C99 C98 C97 124.0(9) . . ? C103 C98 C97 118.7(10) . . ? C98 C99 C100 120.6(12) . . ? C98 C99 H99 119.7 . . ? C100 C99 H99 119.7 . . ? C101 C100 C99 121.5(14) . . ? C101 C100 H100 119.2 . . ? C99 C100 H100 119.2 . . ? C100 C101 C102 119.0(13) . . ? C100 C101 H101 120.5 . . ? C102 C101 H101 120.5 . . ? C101 C102 C103 120.7(13) . . ? C101 C102 H102 119.6 . . ? C103 C102 H102 119.6 . . ? C102 C103 C98 121.0(13) . . ? C102 C103 H103 119.5 . . ? C98 C103 H103 119.5 . . ? C109 C104 C105 118.1(10) . . ? C109 C104 C97 119.4(9) . . ? C105 C104 C97 122.2(9) . . ? C104 C105 C106 119.8(11) . . ? C104 C105 H105 120.1 . . ? C106 C105 H105 120.1 . . ? C107 C106 C105 119.1(12) . . ? C107 C106 H106 120.4 . . ? C105 C106 H106 120.4 . . ? C108 C107 C106 121.6(12) . . ? C108 C107 H107 119.2 . . ? C106 C107 H107 119.2 . . ? C107 C108 C109 117.9(12) . . ? C107 C108 H108 121.0 . . ? C109 C108 H108 121.0 . . ? C108 C109 C104 123.4(11) . . ? C108 C109 H109 118.3 . . ? C104 C109 H109 118.3 . . ? C115 C110 C111 117.4(10) . . ? C115 C110 C97 119.0(9) . . ? C111 C110 C97 123.3(11) . . ? C110 C111 C112 121.1(14) . . ? C110 C111 H111 119.5 . . ? C112 C111 H111 119.5 . . ? C113 C112 C111 118.1(12) . . ? C113 C112 H112 121.0 . . ? C111 C112 H112 121.0 . . ? C114 C113 C112 122.2(12) . . ? C114 C113 H113 118.9 . . ? C112 C113 H113 118.9 . . ? C113 C114 C115 119.6(13) . . ? C113 C114 H114 120.2 . . ? C115 C114 H114 120.2 . . ? C114 C115 C110 121.6(11) . . ? C114 C115 H115 119.2 . . ? C110 C115 H115 119.2 . . ? N16 C116 C117 110.2(7) . . ? N16 C116 H11A 109.6 . . ? C117 C116 H11A 109.6 . . ? N16 C116 H11B 109.6 . . ? C117 C116 H11B 109.6 . . ? H11A C116 H11B 108.1 . . ? O4 C117 N20 125.9(9) . . ? O4 C117 C116 120.1(8) . . ? N20 C117 C116 113.9(8) . . ? C119 C118 N20 112.9(10) . . ? C119 C118 H11C 109.0 . . ? N20 C118 H11C 109.0 . . ? C119 C118 H11D 109.0 . . ? N20 C118 H11D 109.0 . . ? H11C C118 H11D 107.8 . . ? C118 C119 S4 115.0(9) . . ? C118 C119 H11E 108.5 . . ? S4 C119 H11E 108.5 . . ? C118 C119 H11F 108.5 . . ? S4 C119 H11F 108.5 . . ? H11E C119 H11F 107.5 . . ? C133 C120 C127 106.2(11) . . ? C133 C120 C121 112.0(13) . . ? C127 C120 C121 111.3(12) . . ? C133 C120 S4 106.7(10) . . ? C127 C120 S4 114.5(11) . . ? C121 C120 S4 106.1(9) . . ? C122 C121 C126 118.6(14) . . ? C122 C121 C120 119.3(15) . . ? C126 C121 C120 121.8(14) . . ? C121 C122 C123 120.0(17) . . ? C121 C122 H122 120.0 . . ? C123 C122 H122 120.0 . . ? C124 C123 C122 121.9(17) . . ? C124 C123 H123 119.1 . . ? C122 C123 H123 119.1 . . ? C123 C124 C125 119.6(16) . . ? C123 C124 H124 120.2 . . ? C125 C124 H124 120.2 . . ? C126 C125 C124 120.0(15) . . ? C126 C125 H125 120.0 . . ? C124 C125 H125 120.0 . . ? C125 C126 C121 119.7(14) . . ? C125 C126 H126 120.1 . . ? C121 C126 H126 120.1 . . ? C128 C127 C132 119.4(16) . . ? C128 C127 C120 120.5(16) . . ? C132 C127 C120 119.7(14) . . ? C127 C128 C129 122(2) . . ? C127 C128 H128 119.0 . . ? C129 C128 H128 119.0 . . ? C130 C129 C128 122(2) . . ? C130 C129 H129 119.0 . . ? C128 C129 H129 119.0 . . ? C131 C130 C129 115(2) . . ? C131 C130 H130 122.4 . . ? C129 C130 H130 122.4 . . ? C130 C131 C132 127(2) . . ? C130 C131 H131 116.6 . . ? C132 C131 H131 116.6 . . ? C131 C132 C127 114.3(17) . . ? C131 C132 H132 122.8 . . ? C127 C132 H132 122.8 . . ? C138 C133 C134 119.2(16) . . ? C138 C133 C120 124.3(16) . . ? C134 C133 C120 116.2(15) . . ? C135 C134 C133 119.7(19) . . ? C135 C134 H134 120.2 . . ? C133 C134 H134 120.2 . . ? C134 C135 C136 119(2) . . ? C134 C135 H135 120.4 . . ? C136 C135 H135 120.4 . . ? C137 C136 C135 120.0(19) . . ? C137 C136 H136 120.0 . . ? C135 C136 H136 120.0 . . ? C136 C137 C138 121(3) . . ? C136 C137 H137 119.6 . . ? C138 C137 H137 119.6 . . ? C137 C138 C133 121(2) . . ? C137 C138 H138 119.4 . . ? C133 C138 H138 119.4 . . ? N21 C141 C142 122.6(8) . . ? N21 C141 H141 118.7 . . ? C142 C141 H141 118.7 . . ? C143 C142 C141 117.8(9) . . ? C143 C142 H142 121.1 . . ? C141 C142 H142 121.1 . . ? C142 C143 C144 120.0(9) . . ? C142 C143 H143 120.0 . . ? C144 C143 H143 120.0 . . ? C145 C144 C143 119.1(9) . . ? C145 C144 H144 120.4 . . ? C143 C144 H144 120.4 . . ? C144 C145 N21 122.0(8) . . ? C144 C145 C146 123.1(8) . . ? N21 C145 C146 114.9(7) . . ? N22 C146 C145 116.7(7) . . ? N22 C146 H146 121.6 . . ? C145 C146 H146 121.6 . . ? N24 C147 N23 115.1(7) . . ? N24 C147 C148 122.3(7) . . ? N23 C147 C148 122.5(7) . . ? C149 C148 C147 116.9(7) . . ? C149 C148 H148 121.5 . . ? C147 C148 H148 121.5 . . ? N25 C149 N26 115.6(6) . . ? N25 C149 C148 122.5(7) . . ? N26 C149 C148 121.9(7) . . ? N25 C150 N24 126.3(7) . . ? N25 C150 C151 115.1(6) . . ? N24 C150 C151 118.6(7) . . ? C152 C151 C156 119.6(9) . . ? C152 C151 C150 120.9(9) . . ? C156 C151 C150 119.4(8) . . ? C151 C152 C153 119.2(12) . . ? C151 C152 H152 120.4 . . ? C153 C152 H152 120.4 . . ? C154 C153 C152 120.1(13) . . ? C154 C153 H153 120.0 . . ? C152 C153 H153 120.0 . . ? C153 C154 C155 121.5(12) . . ? C153 C154 H154 119.2 . . ? C155 C154 H154 119.2 . . ? C156 C155 C154 119.3(13) . . ? C156 C155 H155 120.4 . . ? C154 C155 H155 120.4 . . ? C155 C156 C151 120.4(11) . . ? C155 C156 H156 119.8 . . ? C151 C156 H156 119.8 . . ? N27 C157 C158 117.9(8) . . ? N27 C157 H157 121.1 . . ? C158 C157 H157 121.1 . . ? N28 C158 C159 122.4(9) . . ? N28 C158 C157 117.3(7) . . ? C159 C158 C157 120.3(9) . . ? C158 C159 C160 118.1(10) . . ? C158 C159 H159 120.9 . . ? C160 C159 H159 120.9 . . ? C161 C160 C159 119.1(10) . . ? C161 C160 H160 120.4 . . ? C159 C160 H160 120.4 . . ? C160 C161 C162 119.0(10) . . ? C160 C161 H161 120.5 . . ? C162 C161 H161 120.5 . . ? N28 C162 C161 122.7(10) . . ? N28 C162 H162 118.6 . . ? C161 C162 H162 118.6 . . ? N23 C163 C164 109.5(7) . . ? N23 C163 H16A 109.8 . . ? C164 C163 H16A 109.8 . . ? N23 C163 H16B 109.8 . . ? C164 C163 H16B 109.8 . . ? H16A C163 H16B 108.2 . . ? O5 C164 N29 125.7(8) . . ? O5 C164 C163 119.5(7) . . ? N29 C164 C163 114.7(8) . . ? N29 C165 C166 111.9(7) . . ? N29 C165 H16C 109.2 . . ? C166 C165 H16C 109.2 . . ? N29 C165 H16D 109.2 . . ? C166 C165 H16D 109.2 . . ? H16C C165 H16D 107.9 . . ? C165 C166 S5 114.9(7) . . ? C165 C166 H16E 108.6 . . ? S5 C166 H16E 108.6 . . ? C165 C166 H16F 108.6 . . ? S5 C166 H16F 108.6 . . ? H16E C166 H16F 107.5 . . ? C180 C167 C168 113.8(8) . . ? C180 C167 C174 104.9(8) . . ? C168 C167 C174 114.9(9) . . ? C180 C167 S5 113.1(7) . . ? C168 C167 S5 105.2(6) . . ? C174 C167 S5 104.6(7) . . ? C169 C168 C173 119.3(10) . . ? C169 C168 C167 119.9(10) . . ? C173 C168 C167 120.6(9) . . ? C168 C169 C170 119.8(12) . . ? C168 C169 H169 120.1 . . ? C170 C169 H169 120.1 . . ? C171 C170 C169 119.0(13) . . ? C171 C170 H170 120.5 . . ? C169 C170 H170 120.5 . . ? C172 C171 C170 121.0(12) . . ? C172 C171 H171 119.5 . . ? C170 C171 H171 119.5 . . ? C171 C172 C173 119.4(13) . . ? C171 C172 H172 120.3 . . ? C173 C172 H172 120.3 . . ? C172 C173 C168 121.3(11) . . ? C172 C173 H173 119.4 . . ? C168 C173 H173 119.4 . . ? C179 C174 C175 115.5(12) . . ? C179 C174 C167 124.5(10) . . ? C175 C174 C167 119.8(11) . . ? C176 C175 C174 120.5(15) . . ? C176 C175 H175 119.7 . . ? C174 C175 H175 119.7 . . ? C177 C176 C175 123.2(17) . . ? C177 C176 H176 118.4 . . ? C175 C176 H176 118.4 . . ? C176 C177 C178 117.2(17) . . ? C176 C177 H177 121.4 . . ? C178 C177 H177 121.4 . . ? C177 C178 C179 119.4(17) . . ? C177 C178 H178 120.3 . . ? C179 C178 H178 120.3 . . ? C174 C179 C178 124.1(14) . . ? C174 C179 H179 118.0 . . ? C178 C179 H179 118.0 . . ? C185 C180 C181 116.8(10) . . ? C185 C180 C167 123.7(10) . . ? C181 C180 C167 119.3(10) . . ? C182 C181 C180 123.9(14) . . ? C182 C181 H181 118.1 . . ? C180 C181 H181 118.1 . . ? C181 C182 C183 118.2(15) . . ? C181 C182 H182 120.9 . . ? C183 C182 H182 120.9 . . ? C184 C183 C182 120.4(14) . . ? C184 C183 H183 119.8 . . ? C182 C183 H183 119.8 . . ? C183 C184 C185 119.0(15) . . ? C183 C184 H184 120.5 . . ? C185 C184 H184 120.5 . . ? C180 C185 C184 121.5(13) . . ? C180 C185 H185 119.2 . . ? C184 C185 H185 119.2 . . ? N26 C186 C187 109.6(7) . . ? N26 C186 H18A 109.8 . . ? C187 C186 H18A 109.8 . . ? N26 C186 H18B 109.8 . . ? C187 C186 H18B 109.8 . . ? H18A C186 H18B 108.2 . . ? O6 C187 N30 125.7(9) . . ? O6 C187 C186 120.3(8) . . ? N30 C187 C186 113.9(8) . . ? N30 C188 C189 114.6(9) . . ? N30 C188 H18C 108.6 . . ? C189 C188 H18C 108.6 . . ? N30 C188 H18D 108.6 . . ? C189 C188 H18D 108.6 . . ? H18C C188 H18D 107.6 . . ? C188 C189 S6 110.4(8) . . ? C188 C189 H18E 109.6 . . ? S6 C189 H18E 109.6 . . ? C188 C189 H18F 109.6 . . ? S6 C189 H18F 109.6 . . ? H18E C189 H18F 108.1 . . ? C191 C190 C197 116.6(13) . . ? C191 C190 C203 110.1(12) . . ? C197 C190 C203 114.3(13) . . ? C191 C190 S6 106.9(10) . . ? C197 C190 S6 106.8(9) . . ? C203 C190 S6 100.5(10) . . ? C192 C191 C196 110.5(15) . . ? C192 C191 C190 131.0(14) . . ? C196 C191 C190 117.6(14) . . ? C193 C192 C191 132.1(19) . . ? C193 C192 H192 113.9 . . ? C191 C192 H192 113.9 . . ? C192 C193 C194 114(2) . . ? C192 C193 H193 123.0 . . ? C194 C193 H193 123.0 . . ? C195 C194 C193 117(2) . . ? C195 C194 H194 121.3 . . ? C193 C194 H194 121.3 . . ? C196 C195 C194 125(2) . . ? C196 C195 H195 117.7 . . ? C194 C195 H195 117.7 . . ? C195 C196 C191 121.2(18) . . ? C195 C196 H196 119.4 . . ? C191 C196 H196 119.4 . . ? C198 C197 C202 117.5(12) . . ? C198 C197 C190 124.8(14) . . ? C202 C197 C190 117.5(13) . . ? C197 C198 C199 121.7(16) . . ? C197 C198 H198 119.2 . . ? C199 C198 H198 119.2 . . ? C198 C199 C200 123.3(17) . . ? C198 C199 H199 118.4 . . ? C200 C199 H199 118.4 . . ? C201 C200 C199 117.7(14) . . ? C201 C200 H200 121.2 . . ? C199 C200 H200 121.2 . . ? C200 C201 C202 122.8(14) . . ? C200 C201 H201 118.6 . . ? C202 C201 H201 118.6 . . ? C201 C202 C197 117.0(13) . . ? C201 C202 H202 121.5 . . ? C197 C202 H202 121.5 . . ? C204 C203 C208 118.1(16) . . ? C204 C203 C190 118.2(15) . . ? C208 C203 C190 123.0(14) . . ? C203 C204 C205 119.3(18) . . ? C203 C204 H204 120.4 . . ? C205 C204 H204 120.4 . . ? C206 C205 C204 118(2) . . ? C206 C205 H205 121.0 . . ? C204 C205 H205 121.0 . . ? C205 C206 C207 124(2) . . ? C205 C206 H206 118.2 . . ? C207 C206 H206 118.2 . . ? C206 C207 C208 118(2) . . ? C206 C207 H207 120.8 . . ? C208 C207 H207 120.8 . . ? C207 C208 C203 122.1(19) . . ? C207 C208 H208 118.9 . . ? C203 C208 H208 118.9 . . ? N31 C211 C212 121.9(12) . . ? N31 C211 H211 119.1 . . ? C212 C211 H211 119.1 . . ? C213 C212 C211 118.7(12) . . ? C213 C212 H212 120.7 . . ? C211 C212 H212 120.7 . . ? C214 C213 C212 119.7(12) . . ? C214 C213 H213 120.1 . . ? C212 C213 H213 120.1 . . ? C213 C214 C215 119.2(12) . . ? C213 C214 H214 120.4 . . ? C215 C214 H214 120.4 . . ? N31 C215 C214 121.7(10) . . ? N31 C215 C216 117.5(8) . . ? C214 C215 C216 120.8(10) . . ? N32 C216 C215 118.9(8) . . ? N32 C216 H216 120.5 . . ? C215 C216 H216 120.5 . . ? N34 C217 C218 123.6(7) . . ? N34 C217 N33 115.3(8) . . ? C218 C217 N33 121.0(7) . . ? C217 C218 C219 115.5(7) . . ? C217 C218 H218 122.3 . . ? C219 C218 H218 122.3 . . ? N35 C219 N36 116.7(7) . . ? N35 C219 C218 122.9(8) . . ? N36 C219 C218 120.5(7) . . ? N35 C220 N34 127.2(7) . . ? N35 C220 C221 117.5(7) . . ? N34 C220 C221 115.3(7) . . ? C226 C221 C222 120.7(9) . . ? C226 C221 C220 118.7(8) . . ? C222 C221 C220 120.5(9) . . ? C223 C222 C221 118.8(13) . . ? C223 C222 H222 120.6 . . ? C221 C222 H222 120.6 . . ? C224 C223 C222 123.1(17) . . ? C224 C223 H223 118.5 . . ? C222 C223 H223 118.5 . . ? C223 C224 C225 118.8(15) . . ? C223 C224 H224 120.6 . . ? C225 C224 H224 120.6 . . ? C224 C225 C226 121.6(17) . . ? C224 C225 H225 119.2 . . ? C226 C225 H225 119.2 . . ? C221 C226 C225 117.0(14) . . ? C221 C226 H226 121.5 . . ? C225 C226 H226 121.5 . . ? N37 C227 C228 115.6(8) . . ? N37 C227 H227 122.2 . . ? C228 C227 H227 122.2 . . ? N38 C228 C229 123.1(9) . . ? N38 C228 C227 114.2(8) . . ? C229 C228 C227 122.6(9) . . ? C228 C229 C230 118.1(11) . . ? C228 C229 H229 120.9 . . ? C230 C229 H229 120.9 . . ? C231 C230 C229 119.5(11) . . ? C231 C230 H230 120.3 . . ? C229 C230 H230 120.3 . . ? C230 C231 C232 119.5(11) . . ? C230 C231 H231 120.3 . . ? C232 C231 H231 120.3 . . ? N38 C232 C231 121.5(10) . . ? N38 C232 H232 119.2 . . ? C231 C232 H232 119.2 . . ? N33 C233 C234 109.0(7) . . ? N33 C233 H23C 109.9 . . ? C234 C233 H23C 109.9 . . ? N33 C233 H23D 109.9 . . ? C234 C233 H23D 109.9 . . ? H23C C233 H23D 108.3 . . ? O7 C234 N39 125.6(8) . . ? O7 C234 C233 119.5(7) . . ? N39 C234 C233 114.8(8) . . ? N39 C235 C236 112.2(8) . . ? N39 C235 H23E 109.2 . . ? C236 C235 H23E 109.2 . . ? N39 C235 H23F 109.2 . . ? C236 C235 H23F 109.2 . . ? H23E C235 H23F 107.9 . . ? C235 C236 S7 111.0(6) . . ? C235 C236 H23G 109.4 . . ? S7 C236 H23G 109.4 . . ? C235 C236 H23H 109.4 . . ? S7 C236 H23H 109.4 . . ? H23G C236 H23H 108.0 . . ? C244 C237 C238 115.4(9) . . ? C244 C237 C250 106.0(11) . . ? C238 C237 C250 113.6(10) . . ? C244 C237 S7 113.9(8) . . ? C238 C237 S7 106.0(8) . . ? C250 C237 S7 101.2(7) . . ? C239 C238 C243 117.5(12) . . ? C239 C238 C237 122.0(12) . . ? C243 C238 C237 120.3(12) . . ? C240 C239 C238 119.2(17) . . ? C240 C239 H239 120.4 . . ? C238 C239 H239 120.4 . . ? C241 C240 C239 124(2) . . ? C241 C240 H240 118.2 . . ? C239 C240 H240 118.2 . . ? C240 C241 C242 119.7(17) . . ? C240 C241 H241 120.2 . . ? C242 C241 H241 120.2 . . ? C241 C242 C243 119.2(17) . . ? C241 C242 H242 120.4 . . ? C243 C242 H242 120.4 . . ? C242 C243 C238 120.9(15) . . ? C242 C243 H243 119.6 . . ? C238 C243 H243 119.6 . . ? C249 C244 C245 116.4(14) . . ? C249 C244 C237 125.0(11) . . ? C245 C244 C237 118.6(13) . . ? C244 C245 C246 116.4(18) . . ? C244 C245 H245 121.8 . . ? C246 C245 H245 121.8 . . ? C247 C246 C245 126(2) . . ? C247 C246 H246 117.0 . . ? C245 C246 H246 117.0 . . ? C246 C247 C248 119(2) . . ? C246 C247 H247 120.3 . . ? C248 C247 H247 120.3 . . ? C249 C248 C247 116.6(18) . . ? C249 C248 H248 121.7 . . ? C247 C248 H248 121.7 . . ? C248 C249 C244 124.9(15) . . ? C248 C249 H249 117.5 . . ? C244 C249 H249 117.5 . . ? C251 C250 C255 118.8(14) . . ? C251 C250 C237 122.4(13) . . ? C255 C250 C237 118.7(12) . . ? C250 C251 C252 119.2(18) . . ? C250 C251 H251 120.4 . . ? C252 C251 H251 120.4 . . ? C251 C252 C253 121.0(18) . . ? C251 C252 H252 119.5 . . ? C253 C252 H252 119.5 . . ? C254 C253 C252 120.3(18) . . ? C254 C253 H253 119.8 . . ? C252 C253 H253 119.8 . . ? C253 C254 C255 118.2(18) . . ? C253 C254 H254 120.9 . . ? C255 C254 H254 120.9 . . ? C254 C255 C250 122.4(15) . . ? C254 C255 H255 118.8 . . ? C250 C255 H255 118.8 . . ? N36 C256 C257 110.2(8) . . ? N36 C256 H25C 109.6 . . ? C257 C256 H25C 109.6 . . ? N36 C256 H25D 109.6 . . ? C257 C256 H25D 109.6 . . ? H25C C256 H25D 108.1 . . ? O8 C257 N40 123.8(9) . . ? O8 C257 C256 120.5(9) . . ? N40 C257 C256 115.7(9) . . ? N40 C258 C259 113.7(9) . . ? N40 C258 H25E 108.8 . . ? C259 C258 H25E 108.8 . . ? N40 C258 H25F 108.8 . . ? C259 C258 H25F 108.8 . . ? H25E C258 H25F 107.7 . . ? C258 C259 S8 109.3(8) . . ? C258 C259 H25G 109.8 . . ? S8 C259 H25G 109.8 . . ? C258 C259 H25H 109.8 . . ? S8 C259 H25H 109.8 . . ? H25G C259 H25H 108.3 . . ? C261 C260 C267 115.0(12) . . ? C261 C260 C273 116.5(11) . . ? C267 C260 C273 106.9(10) . . ? C261 C260 S8 102.9(8) . . ? C267 C260 S8 102.2(9) . . ? C273 C260 S8 112.5(10) . . ? C266 C261 C262 115.4(14) . . ? C266 C261 C260 123.0(14) . . ? C262 C261 C260 121.4(11) . . ? C263 C262 C261 126.4(14) . . ? C263 C262 H262 116.8 . . ? C261 C262 H262 116.8 . . ? C262 C263 C264 117.4(16) . . ? C262 C263 H263 121.3 . . ? C264 C263 H263 121.3 . . ? C265 C264 C263 114.8(15) . . ? C265 C264 H264 122.6 . . ? C263 C264 H264 122.6 . . ? C266 C265 C264 123.9(15) . . ? C266 C265 H265 118.0 . . ? C264 C265 H265 118.0 . . ? C261 C266 C265 121.8(17) . . ? C261 C266 H266 119.1 . . ? C265 C266 H266 119.1 . . ? C272 C267 C268 118.1(14) . . ? C272 C267 C260 120.7(14) . . ? C268 C267 C260 121.0(14) . . ? C269 C268 C267 122.0(17) . . ? C269 C268 H268 119.0 . . ? C267 C268 H268 119.0 . . ? C270 C269 C268 120.5(19) . . ? C270 C269 H269 119.8 . . ? C268 C269 H269 119.8 . . ? C269 C270 C271 118.0(17) . . ? C269 C270 H270 121.0 . . ? C271 C270 H270 121.0 . . ? C270 C271 C272 122.9(18) . . ? C270 C271 H271 118.6 . . ? C272 C271 H271 118.6 . . ? C267 C272 C271 118.4(16) . . ? C267 C272 H272 120.8 . . ? C271 C272 H272 120.8 . . ? C278 C273 C274 114.7(13) . . ? C278 C273 C260 131.9(14) . . ? C274 C273 C260 113.0(13) . . ? C275 C274 C273 122.5(17) . . ? C275 C274 H274 118.8 . . ? C273 C274 H274 118.8 . . ? C276 C275 C274 119(2) . . ? C276 C275 H275 120.5 . . ? C274 C275 H275 120.5 . . ? C275 C276 C277 124(2) . . ? C275 C276 H276 117.8 . . ? C277 C276 H276 117.8 . . ? C276 C277 C278 115.4(19) . . ? C276 C277 H277 122.3 . . ? C278 C277 H277 122.3 . . ? C273 C278 C277 124.0(17) . . ? C273 C278 H278 118.0 . . ? C277 C278 H278 118.0 . . ? C1 N1 C5 118.1(7) . . ? C1 N1 Cu1 130.1(5) . . ? C5 N1 Cu1 111.7(6) . . ? C6 N2 N3 124.7(7) . . ? C6 N2 Cu1 116.9(6) . . ? N3 N2 Cu1 118.3(5) . . ? N2 N3 C7 116.2(6) . . ? N2 N3 C23 119.3(6) . . ? C7 N3 C23 124.3(7) . . ? C10 N4 C7 115.9(7) . . ? C10 N4 Cu1 131.3(5) . . ? C7 N4 Cu1 112.7(5) . . ? C10 N5 C9 118.5(6) . . ? C10 N5 Cu2 129.7(5) . . ? C9 N5 Cu2 111.5(5) . . ? C9 N6 N7 117.0(6) . . ? C9 N6 C46 123.8(7) . . ? N7 N6 C46 118.7(7) . . ? C17 N7 N6 121.2(7) . . ? C17 N7 Cu2 117.7(5) . . ? N6 N7 Cu2 120.8(5) . . ? C22 N8 C18 117.0(8) . . ? C22 N8 Cu2 133.0(6) . . ? C18 N8 Cu2 110.0(5) . . ? C24 N9 C25 124.2(7) . . ? C24 N9 H9 117.9 . . ? C25 N9 H9 117.9 . . ? C47 N10 C48 121.5(8) . . ? C47 N10 H10 119.3 . . ? C48 N10 H10 119.3 . . ? C75 N11 C71 118.6(7) . . ? C75 N11 Cu1 109.8(5) . . ? C71 N11 Cu1 131.6(5) . . ? C76 N12 N13 121.2(6) . . ? C76 N12 Cu1 117.6(5) . . ? N13 N12 Cu1 121.1(4) . . ? N12 N13 C77 116.8(6) . . ? N12 N13 C93 120.1(6) . . ? C77 N13 C93 122.9(6) . . ? C80 N14 C77 116.9(6) . . ? C80 N14 Cu1 130.6(5) . . ? C77 N14 Cu1 112.3(4) . . ? C80 N15 C79 115.5(6) . . ? C80 N15 Cu3 131.9(5) . . ? C79 N15 Cu3 112.4(5) . . ? N17 N16 C79 115.6(6) . . ? N17 N16 C116 119.6(6) . . ? C79 N16 C116 123.7(6) . . ? C87 N17 N16 123.8(7) . . ? C87 N17 Cu3 117.8(6) . . ? N16 N17 Cu3 118.3(5) . . ? C92 N18 C88 116.6(8) . . ? C92 N18 Cu3 131.7(7) . . ? C88 N18 Cu3 111.5(5) . . ? C94 N19 C95 122.9(7) . . ? C94 N19 H19A 118.5 . . ? C95 N19 H19A 118.5 . . ? C117 N20 C118 122.8(9) . . ? C117 N20 H20A 118.6 . . ? C118 N20 H20A 118.6 . . ? C141 N21 C145 118.5(7) . . ? C141 N21 Cu2 130.6(6) . . ? C145 N21 Cu2 110.9(5) . . ? C146 N22 N23 123.4(6) . . ? C146 N22 Cu2 117.2(6) . . ? N23 N22 Cu2 119.4(4) . . ? N22 N23 C147 115.1(6) . . ? N22 N23 C163 119.1(6) . . ? C147 N23 C163 125.3(7) . . ? C150 N24 C147 115.4(6) . . ? C150 N24 Cu2 131.0(5) . . ? C147 N24 Cu2 113.4(5) . . ? C150 N25 C149 116.3(6) . . ? C150 N25 Cu4 130.2(5) . . ? C149 N25 Cu4 113.1(5) . . ? C149 N26 N27 117.6(6) . . ? C149 N26 C186 122.0(6) . . ? N27 N26 C186 119.9(6) . . ? C157 N27 N26 120.6(7) . . ? C157 N27 Cu4 118.9(6) . . ? N26 N27 Cu4 120.1(5) . . ? C162 N28 C158 118.5(8) . . ? C162 N28 Cu4 132.5(7) . . ? C158 N28 Cu4 108.9(5) . . ? C164 N29 C165 124.3(8) . . ? C164 N29 H29A 117.9 . . ? C165 N29 H29A 117.9 . . ? C187 N30 C188 122.0(9) . . ? C187 N30 H30X 119.0 . . ? C188 N30 H30X 119.0 . . ? C211 N31 C215 118.7(9) . . ? C211 N31 Cu3 132.5(7) . . ? C215 N31 Cu3 108.8(7) . . ? C216 N32 N33 120.8(7) . . ? C216 N32 Cu3 118.7(6) . . ? N33 N32 Cu3 120.4(5) . . ? N32 N33 C217 117.7(6) . . ? N32 N33 C233 119.3(7) . . ? C217 N33 C233 122.7(7) . . ? C220 N34 C217 115.8(7) . . ? C220 N34 Cu3 130.8(5) . . ? C217 N34 Cu3 113.0(5) . . ? C220 N35 C219 114.9(7) . . ? C220 N35 Cu4 132.6(5) . . ? C219 N35 Cu4 112.4(6) . . ? N37 N36 C219 114.7(6) . . ? N37 N36 C256 120.7(7) . . ? C219 N36 C256 123.9(7) . . ? C227 N37 N36 123.4(7) . . ? C227 N37 Cu4 118.2(6) . . ? N36 N37 Cu4 118.3(5) . . ? C232 N38 C228 118.2(8) . . ? C232 N38 Cu4 129.2(7) . . ? C228 N38 Cu4 112.5(6) . . ? C234 N39 C235 122.7(8) . . ? C234 N39 H39A 118.6 . . ? C235 N39 H39A 118.6 . . ? C257 N40 C258 122.3(9) . . ? C257 N40 H40 118.9 . . ? C258 N40 H40 118.9 . . ? B3 F10 F11 43.8(14) . . ? B3 F11 F10 50.7(14) . . ? N2 Cu1 N12 170.3(3) . . ? N2 Cu1 N1 79.3(3) . . ? N12 Cu1 N1 94.7(3) . . ? N2 Cu1 N4 77.7(3) . . ? N12 Cu1 N4 108.4(2) . . ? N1 Cu1 N4 156.8(2) . . ? N2 Cu1 N11 95.8(2) . . ? N12 Cu1 N11 76.7(2) . . ? N1 Cu1 N11 92.3(2) . . ? N4 Cu1 N11 92.3(2) . . ? N2 Cu1 N14 114.6(2) . . ? N12 Cu1 N14 73.0(2) . . ? N1 Cu1 N14 93.1(2) . . ? N4 Cu1 N14 94.4(2) . . ? N11 Cu1 N14 149.5(2) . . ? N22 Cu2 N7 170.4(3) . . ? N22 Cu2 N21 80.2(3) . . ? N7 Cu2 N21 93.7(3) . . ? N22 Cu2 N24 76.8(2) . . ? N7 Cu2 N24 109.4(3) . . ? N21 Cu2 N24 156.9(3) . . ? N22 Cu2 N8 95.5(3) . . ? N7 Cu2 N8 77.3(3) . . ? N21 Cu2 N8 92.8(3) . . ? N24 Cu2 N8 92.4(3) . . ? N22 Cu2 N5 113.9(2) . . ? N7 Cu2 N5 73.2(3) . . ? N21 Cu2 N5 90.4(2) . . ? N24 Cu2 N5 96.0(2) . . ? N8 Cu2 N5 150.5(2) . . ? N17 Cu3 N18 80.2(3) . . ? N17 Cu3 N32 171.0(3) . . ? N18 Cu3 N32 93.5(3) . . ? N17 Cu3 N15 77.7(2) . . ? N18 Cu3 N15 157.9(3) . . ? N32 Cu3 N15 108.6(2) . . ? N17 Cu3 N31 97.7(3) . . ? N18 Cu3 N31 92.3(3) . . ? N32 Cu3 N31 76.0(3) . . ? N15 Cu3 N31 91.4(3) . . ? N17 Cu3 N34 113.6(3) . . ? N18 Cu3 N34 93.1(3) . . ? N32 Cu3 N34 72.9(3) . . ? N15 Cu3 N34 95.0(2) . . ? N31 Cu3 N34 148.7(3) . . ? N37 Cu4 N27 168.0(3) . . ? N37 Cu4 N38 79.1(3) . . ? N27 Cu4 N38 93.0(3) . . ? N37 Cu4 N35 77.8(3) . . ? N27 Cu4 N35 110.2(3) . . ? N38 Cu4 N35 156.8(3) . . ? N37 Cu4 N28 94.8(3) . . ? N27 Cu4 N28 76.3(3) . . ? N38 Cu4 N28 92.0(3) . . ? N35 Cu4 N28 92.2(3) . . ? N37 Cu4 N25 115.9(3) . . ? N27 Cu4 N25 73.1(2) . . ? N38 Cu4 N25 92.7(3) . . ? N35 Cu4 N25 95.2(2) . . ? N28 Cu4 N25 149.3(3) . . ? F3 B1 F4 100.9(14) . . ? F3 B1 F2 112.8(12) . . ? F4 B1 F2 114.0(13) . . ? F3 B1 F1 107.7(11) . . ? F4 B1 F1 109.1(13) . . ? F2 B1 F1 111.7(9) . . ? F6 B2 F7 115.6(14) . . ? F6 B2 F8 108.9(14) . . ? F7 B2 F8 102.2(14) . . ? F6 B2 F5 110.9(13) . . ? F7 B2 F5 111.2(10) . . ? F8 B2 F5 107.2(12) . . ? F11 B3 F9 121.3(17) . . ? F11 B3 F12 116(2) . . ? F9 B3 F12 117.3(13) . . ? F11 B3 F10 85(2) . . ? F9 B3 F10 109(3) . . ? F12 B3 F10 99(2) . . ? F16 B4 F15 114.4(16) . . ? F16 B4 F13 114.0(19) . . ? F15 B4 F13 115.3(17) . . ? F16 B4 F14 109.6(19) . . ? F15 B4 F14 101.9(19) . . ? F13 B4 F14 99.7(16) . . ? F20 B5 F18 108(2) . . ? F20 B5 F19 106.4(17) . . ? F18 B5 F19 111.6(12) . . ? F20 B5 F17 107.7(11) . . ? F18 B5 F17 112.5(12) . . ? F19 B5 F17 110.5(13) . . ? F24 B6 F23 97(2) . . ? F24 B6 F21 117.2(16) . . ? F23 B6 F21 109.7(19) . . ? F24 B6 F22 109.8(14) . . ? F23 B6 F22 106.6(17) . . ? F21 B6 F22 114.4(10) . . ? F27 B7 F26 114.2(14) . . ? F27 B7 F28 120.4(15) . . ? F26 B7 F28 112.9(16) . . ? F27 B7 F25 101(2) . . ? F26 B7 F25 105.2(17) . . ? F28 B7 F25 100(2) . . ? F31 B8 F30 110(3) . . ? F31 B8 F32 114.1(19) . . ? F30 B8 F32 111(3) . . ? F31 B8 F29 113(3) . . ? F30 B8 F29 105(2) . . ? F32 B8 F29 104(2) . . ? C26 S1 C27 101.5(4) . . ? C49 S2 C50 104.5(5) . . ? C96 S3 C97 102.6(4) . . ? C119 S4 C120 100.1(6) . . ? C166 S5 C167 102.2(5) . . ? C189 S6 C190 102.0(6) . . ? C236 S7 C237 103.6(5) . . ? C259 S8 C260 103.6(6) . . ? N41 C301 C302 178(2) . . ? C301 C302 H30A 109.5 . . ? C301 C302 H30B 109.5 . . ? H30A C302 H30B 109.5 . . ? C301 C302 H30C 109.5 . . ? H30A C302 H30C 109.5 . . ? H30B C302 H30C 109.5 . . ? N42 C303 C304 172(3) . . ? C303 C304 H30D 109.5 . . ? C303 C304 H30E 109.5 . . ? H30D C304 H30E 109.5 . . ? C303 C304 H30F 109.5 . . ? H30D C304 H30F 109.5 . . ? H30E C304 H30F 109.5 . . ? N43 C305 C306 159.0(19) . . ? N45 C309 C310 170(3) . . ? N46 C311 C312 161(2) . . ? N47 C313 C314 168(3) . . ? N50 C319 C320 165(3) . . ? C402 C401 C406 120.0 . . ? C402 C401 H401 120.0 . . ? C406 C401 H401 120.0 . . ? C401 C402 C403 120.0 . . ? C401 C402 C407 120.2(3) . . ? C403 C402 C407 119.8(3) . . ? C404 C403 C402 120.0 . . ? C404 C403 H403 120.0 . . ? C402 C403 H403 120.0 . . ? C405 C404 C403 120.0 . . ? C405 C404 H404 120.0 . . ? C403 C404 H404 120.0 . . ? C406 C405 C404 120.0 . . ? C406 C405 H405 120.0 . . ? C404 C405 H405 120.0 . . ? C405 C406 C401 120.0 . . ? C405 C406 H406 120.0 . . ? C401 C406 H406 120.0 . . ? C402 C407 H40A 109.5 . . ? C402 C407 H40B 109.5 . . ? H40A C407 H40B 109.5 . . ? C402 C407 H40C 109.5 . . ? H40A C407 H40C 109.5 . . ? H40B C407 H40C 109.5 . . ? C409 C408 C413 120.0 . . ? C409 C408 C414 119.7(3) . . ? C413 C408 C414 119.7(3) . . ? C408 C409 C410 120.0 . . ? C411 C410 C409 120.0 . . ? C410 C411 C412 120.0 . . ? C410 C411 C412 125(3) . 2_775 ? C412 C411 C412 112(3) . 2_775 ? C410 C411 C411 166(3) . 2_775 ? C412 C411 C411 62(2) . 2_775 ? C412 C411 C411 50.3(11) 2_775 2_775 ? C413 C412 C411 120.0 . . ? C413 C412 C411 163(2) . 2_775 ? C411 C412 C411 68(2) . 2_775 ? C412 C413 C408 120.0 . . ? C416 C415 C420 120.0 . . ? C416 C415 C421 120.0 . . ? C420 C415 C421 120.0 . . ? C415 C416 C417 120.0 . . ? C415 C416 H416 120.0 . . ? C417 C416 H416 120.0 . . ? C416 C417 C418 120.0 . . ? C416 C417 H417 120.0 . . ? C418 C417 H417 120.0 . . ? C419 C418 C417 120.0 . . ? C419 C418 H418 120.0 . . ? C417 C418 H418 120.0 . . ? C418 C419 C420 120.0 . . ? C418 C419 H419 120.0 . . ? C420 C419 H419 120.0 . . ? C419 C420 C415 120.0 . . ? C419 C420 H420 120.0 . . ? C415 C420 H420 120.0 . . ? C415 C421 H42A 109.5 . . ? C415 C421 H42B 109.5 . . ? H42A C421 H42B 109.5 . . ? C415 C421 H42C 109.5 . . ? H42A C421 H42C 109.5 . . ? H42B C421 H42C 109.5 . . ? N44 C307 C308 169(3) . . ? C423 C422 C427 120.0 . . ? C423 C422 C428 120.0 . . ? C427 C422 C428 120.0 . . ? C424 C423 C422 120.0 . . ? C424 C423 H423 120.0 . . ? C422 C423 H423 120.0 . . ? C423 C424 C425 120.0 . . ? C423 C424 H424 120.0 . . ? C425 C424 H424 120.0 . . ? C426 C425 C424 120.0 . . ? C426 C425 H425 120.0 . . ? C424 C425 H425 120.0 . . ? C425 C426 C427 120.0 . . ? C425 C426 H426 120.0 . . ? C427 C426 H426 120.0 . . ? C426 C427 C422 120.0 . . ? C426 C427 H427 120.0 . . ? C422 C427 H427 120.0 . . ? C422 C428 H42D 109.5 . . ? C422 C428 H42E 109.5 . . ? H42D C428 H42E 109.5 . . ? C422 C428 H42F 109.5 . . ? H42D C428 H42F 109.5 . . ? H42E C428 H42F 109.5 . . ? C430 C429 C434 120.0 . . ? C430 C429 C435 120.0 . . ? C434 C429 C435 120.0 . . ? C429 C430 C431 120.0 . . ? C429 C430 H430 120.0 . . ? C431 C430 H430 120.0 . . ? C432 C431 C430 120.0 . . ? C432 C431 H431 120.0 . . ? C430 C431 H431 120.0 . . ? C431 C432 C433 120.0 . . ? C431 C432 H432 120.0 . . ? C433 C432 H432 120.0 . . ? C434 C433 C432 120.0 . . ? C434 C433 H433 120.0 . . ? C432 C433 H433 120.0 . . ? C433 C434 C429 120.0 . . ? C433 C434 H434 120.0 . . ? C429 C434 H434 120.0 . . ? C429 C435 H43A 109.5 . . ? C429 C435 H43B 109.5 . . ? H43A C435 H43B 109.5 . . ? C429 C435 H43C 109.5 . . ? H43A C435 H43C 109.5 . . ? H43B C435 H43C 109.5 . . ? C437 C436 C441 120.0 . . ? C437 C436 C442 120.0 . . ? C441 C436 C442 120.0 . . ? C436 C437 C438 120.0 . . ? C436 C437 H437 120.0 . . ? C438 C437 H437 120.0 . . ? C439 C438 C437 120.0 . . ? C439 C438 H438 120.0 . . ? C437 C438 H438 120.0 . . ? C438 C439 C440 120.0 . . ? C438 C439 H439 120.0 . . ? C440 C439 H439 120.0 . . ? C441 C440 C439 120.0 . . ? C441 C440 H440 120.0 . . ? C439 C440 H440 120.0 . . ? C440 C441 C436 120.0 . . ? C440 C441 H441 120.0 . . ? C436 C441 H441 120.0 . . ? C436 C442 H44A 109.5 . . ? C436 C442 H44B 109.5 . . ? H44A C442 H44B 109.5 . . ? C436 C442 H44C 109.5 . . ? H44A C442 H44C 109.5 . . ? H44B C442 H44C 109.5 . . ? N48 C315 C316 168(3) . . ? N49 C317 C318 170(4) . . ? N52 C323 C324 167(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.171 _refine_diff_density_min -1.142 _refine_diff_density_rms 0.142 # Attachment 'CIF_for_6.cif' data_ext061 _database_code_depnum_ccdc_archive 'CCDC 711188' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H22 Br N O S' _chemical_formula_sum 'C23 H22 Br N O S' _chemical_formula_weight 440.39 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' S S 0.1246 0.1234 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 2(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 7.1365(14) _cell_length_b 33.713(7) _cell_length_c 9.1192(18) _cell_angle_alpha 90.00 _cell_angle_beta 112.68(3) _cell_angle_gamma 90.00 _cell_volume 2024.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 14699 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.5 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 2.146 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.4806 _exptl_absorpt_correction_T_max 0.8140 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3523 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 40 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 5.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3523 _reflns_number_gt 2964 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+5.0541P] 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 3523 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0655 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.087 _refine_ls_restrained_S_all 1.087 _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 Br1 Br 0.24413(8) 0.236438(14) 0.14880(7) 0.0649(2) Uani 1 1 d . . . C2 C 0.0004(6) 0.22133(12) 0.1804(6) 0.0449(10) Uani 1 1 d . . . H2A H -0.1128 0.2173 0.0764 0.054 Uiso 1 1 calc R . . H2B H 0.0236 0.1962 0.2410 0.054 Uiso 1 1 calc R . . C3 C -0.0525(6) 0.25394(11) 0.2709(5) 0.0344(9) Uani 1 1 d . . . O3 O 0.0378(4) 0.25728(8) 0.4161(3) 0.0434(7) Uani 1 1 d . . . N4 N -0.1969(4) 0.27870(9) 0.1841(4) 0.0316(7) Uani 1 1 d . . . H4A H -0.2533 0.2749 0.0808 0.038 Uiso 1 1 calc R . . C5 C -0.2665(5) 0.31187(10) 0.2513(5) 0.0312(8) Uani 1 1 d . . . H5A H -0.2346 0.3065 0.3652 0.037 Uiso 1 1 calc R . . H5B H -0.4159 0.3140 0.1972 0.037 Uiso 1 1 calc R . . C6 C -0.1715(5) 0.35121(11) 0.2363(5) 0.0316(8) Uani 1 1 d . . . H6A H -0.2424 0.3732 0.2653 0.038 Uiso 1 1 calc R . . H6B H -0.1854 0.3552 0.1250 0.038 Uiso 1 1 calc R . . S7 S 0.09628(13) 0.35123(3) 0.36760(11) 0.0283(2) Uani 1 1 d . . . C8 C 0.1977(5) 0.39527(10) 0.3002(4) 0.0252(7) Uani 1 1 d . . . C9 C 0.2455(5) 0.38619(10) 0.1518(4) 0.0271(8) Uani 1 1 d . . . C10 C 0.3664(5) 0.41283(11) 0.1108(4) 0.0314(8) Uani 1 1 d . . . H10A H 0.4190 0.4355 0.1753 0.038 Uiso 1 1 calc R . . C11 C 0.4115(6) 0.40680(12) -0.0233(5) 0.0383(9) Uani 1 1 d . . . H11A H 0.4939 0.4254 -0.0494 0.046 Uiso 1 1 calc R . . C12 C 0.3367(6) 0.37396(13) -0.1179(5) 0.0423(10) Uani 1 1 d . . . H12A H 0.3651 0.3701 -0.2105 0.051 Uiso 1 1 calc R . . C13 C 0.2200(6) 0.34674(13) -0.0774(5) 0.0416(10) Uani 1 1 d . . . H13A H 0.1697 0.3239 -0.1414 0.050 Uiso 1 1 calc R . . C14 C 0.1757(5) 0.35271(11) 0.0577(4) 0.0321(8) Uani 1 1 d . . . H14A H 0.0970 0.3336 0.0854 0.039 Uiso 1 1 calc R . . C15 C 0.3987(5) 0.40326(10) 0.4420(4) 0.0273(7) Uani 1 1 d . . . C16 C 0.4458(6) 0.43879(11) 0.5237(4) 0.0333(8) Uani 1 1 d . . . H16A H 0.3510 0.4600 0.4926 0.040 Uiso 1 1 calc R . . C17 C 0.6311(6) 0.44382(12) 0.6514(5) 0.0404(9) Uani 1 1 d . . . H17A H 0.6608 0.4683 0.7071 0.049 Uiso 1 1 calc R . . C18 C 0.7717(6) 0.41346(13) 0.6973(5) 0.0407(10) Uani 1 1 d . . . H18A H 0.8981 0.4170 0.7840 0.049 Uiso 1 1 calc R . . C19 C 0.7273(6) 0.37776(12) 0.6162(4) 0.0371(9) Uani 1 1 d . . . H19A H 0.8229 0.3567 0.6471 0.045 Uiso 1 1 calc R . . C20 C 0.5432(5) 0.37294(11) 0.4898(4) 0.0314(8) Uani 1 1 d . . . H20A H 0.5144 0.3484 0.4341 0.038 Uiso 1 1 calc R . . C21 C 0.0446(5) 0.42949(10) 0.2701(4) 0.0273(8) Uani 1 1 d . . . C22 C -0.0268(5) 0.45106(11) 0.1299(4) 0.0332(8) Uani 1 1 d . . . H22A H 0.0176 0.4444 0.0473 0.040 Uiso 1 1 calc R . . C23 C -0.1624(6) 0.48229(12) 0.1079(5) 0.0390(9) Uani 1 1 d . . . H23A H -0.2085 0.4968 0.0111 0.047 Uiso 1 1 calc R . . C24 C -0.2303(6) 0.49236(11) 0.2256(5) 0.0395(9) Uani 1 1 d . . . H24A H -0.3218 0.5139 0.2113 0.047 Uiso 1 1 calc R . . C25 C -0.1627(6) 0.47056(11) 0.3650(5) 0.0358(9) Uani 1 1 d . . . H25A H -0.2099 0.4769 0.4463 0.043 Uiso 1 1 calc R . . C26 C -0.0277(5) 0.43974(10) 0.3870(5) 0.0321(8) Uani 1 1 d . . . H26A H 0.0170 0.4252 0.4837 0.039 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 0.0683(4) 0.0440(3) 0.1023(5) -0.0124(3) 0.0550(3) -0.0032(2) C2 0.042(2) 0.030(2) 0.060(3) -0.0066(19) 0.017(2) -0.0027(18) C3 0.0309(19) 0.0272(19) 0.040(2) -0.0023(17) 0.0087(17) -0.0041(16) O3 0.0443(16) 0.0429(16) 0.0345(16) 0.0046(13) 0.0056(13) 0.0092(13) N4 0.0295(16) 0.0309(16) 0.0270(16) -0.0028(13) 0.0026(13) 0.0015(13) C5 0.0228(17) 0.033(2) 0.036(2) 0.0015(16) 0.0103(16) -0.0008(15) C6 0.0225(17) 0.0311(19) 0.039(2) 0.0030(16) 0.0090(16) 0.0014(15) S7 0.0232(4) 0.0256(4) 0.0341(5) 0.0031(4) 0.0088(4) 0.0003(3) C8 0.0244(17) 0.0234(17) 0.0284(18) -0.0011(14) 0.0108(15) -0.0016(14) C9 0.0232(17) 0.0269(18) 0.0284(18) 0.0035(15) 0.0067(15) 0.0078(14) C10 0.0269(18) 0.034(2) 0.033(2) 0.0013(16) 0.0105(16) 0.0043(15) C11 0.031(2) 0.047(2) 0.039(2) 0.0107(19) 0.0159(18) 0.0111(17) C12 0.042(2) 0.053(3) 0.033(2) 0.0020(19) 0.0169(19) 0.017(2) C13 0.039(2) 0.045(2) 0.035(2) -0.0099(18) 0.0072(18) 0.0100(19) C14 0.0321(19) 0.0273(19) 0.036(2) -0.0010(16) 0.0114(17) 0.0043(15) C15 0.0254(17) 0.0292(18) 0.0277(18) 0.0009(15) 0.0107(15) -0.0004(14) C16 0.0318(19) 0.033(2) 0.034(2) -0.0018(16) 0.0112(17) 0.0002(16) C17 0.043(2) 0.042(2) 0.036(2) -0.0143(18) 0.0159(19) -0.0071(18) C18 0.030(2) 0.055(3) 0.033(2) -0.0019(19) 0.0076(17) -0.0040(18) C19 0.0290(19) 0.043(2) 0.036(2) 0.0037(18) 0.0089(17) 0.0031(17) C20 0.0301(19) 0.0299(19) 0.034(2) -0.0014(16) 0.0118(16) 0.0006(15) C21 0.0225(17) 0.0256(18) 0.033(2) -0.0019(15) 0.0095(15) -0.0016(14) C22 0.0309(19) 0.033(2) 0.035(2) -0.0006(16) 0.0125(17) 0.0018(16) C23 0.036(2) 0.036(2) 0.043(2) 0.0085(18) 0.0133(18) 0.0084(17) C24 0.035(2) 0.029(2) 0.056(3) -0.0007(18) 0.020(2) 0.0074(16) C25 0.033(2) 0.032(2) 0.049(2) -0.0049(18) 0.0219(18) -0.0003(16) C26 0.0328(19) 0.0279(19) 0.038(2) -0.0001(16) 0.0157(17) 0.0000(15) _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 Br1 C2 1.937(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C2 C3 1.508(6) . ? C3 O3 1.234(5) . ? C3 N4 1.325(5) . ? N4 H4A 0.8800 . ? N4 C5 1.452(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C5 C6 1.520(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 S7 1.822(3) . ? S7 C8 1.857(3) . ? C8 C9 1.548(5) . ? C8 C15 1.540(5) . ? C8 C21 1.539(5) . ? C9 C10 1.393(5) . ? C9 C14 1.389(5) . ? C10 H10A 0.9500 . ? C10 C11 1.394(5) . ? C11 H11A 0.9500 . ? C11 C12 1.379(6) . ? C12 H12A 0.9500 . ? C12 C13 1.382(6) . ? C13 H13A 0.9500 . ? C13 C14 1.399(5) . ? C14 H14A 0.9500 . ? C15 C16 1.382(5) . ? C15 C20 1.397(5) . ? C16 H16A 0.9500 . ? C16 C17 1.395(5) . ? C17 H17A 0.9500 . ? C17 C18 1.381(6) . ? C18 H18A 0.9500 . ? C18 C19 1.384(6) . ? C19 H19A 0.9500 . ? C19 C20 1.383(5) . ? C20 H20A 0.9500 . ? C21 C22 1.386(5) . ? C21 C26 1.395(5) . ? C22 H22A 0.9500 . ? C22 C23 1.391(5) . ? C23 H23A 0.9500 . ? C23 C24 1.380(6) . ? C24 H24A 0.9500 . ? C24 C25 1.384(6) . ? C25 H25A 0.9500 . ? C25 C26 1.378(5) . ? C26 H26A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br1 C2 H2A 110.0 . . ? Br1 C2 H2B 110.0 . . ? Br1 C2 C3 108.6(3) . . ? H2A C2 H2B 108.4 . . ? H2A C2 C3 110.0 . . ? H2B C2 C3 110.0 . . ? C2 C3 O3 121.1(4) . . ? C2 C3 N4 115.7(3) . . ? O3 C3 N4 123.2(4) . . ? C3 N4 H4A 118.4 . . ? C3 N4 C5 123.2(3) . . ? H4A N4 C5 118.4 . . ? N4 C5 H5A 108.9 . . ? N4 C5 H5B 108.9 . . ? N4 C5 C6 113.4(3) . . ? H5A C5 H5B 107.7 . . ? H5A C5 C6 108.9 . . ? H5B C5 C6 108.9 . . ? C5 C6 H6A 109.8 . . ? C5 C6 H6B 109.8 . . ? C5 C6 S7 109.4(2) . . ? H6A C6 H6B 108.2 . . ? H6A C6 S7 109.8 . . ? H6B C6 S7 109.8 . . ? C6 S7 C8 103.08(16) . . ? S7 C8 C9 112.1(2) . . ? S7 C8 C15 102.6(2) . . ? S7 C8 C21 108.5(2) . . ? C9 C8 C15 108.7(3) . . ? C9 C8 C21 111.9(3) . . ? C15 C8 C21 112.7(3) . . ? C8 C9 C10 118.4(3) . . ? C8 C9 C14 123.6(3) . . ? C10 C9 C14 118.0(3) . . ? C9 C10 H10A 119.4 . . ? C9 C10 C11 121.2(4) . . ? H10A C10 C11 119.4 . . ? C10 C11 H11A 119.9 . . ? C10 C11 C12 120.1(4) . . ? H11A C11 C12 119.9 . . ? C11 C12 H12A 120.2 . . ? C11 C12 C13 119.6(4) . . ? H12A C12 C13 120.2 . . ? C12 C13 H13A 119.9 . . ? C12 C13 C14 120.3(4) . . ? H13A C13 C14 119.9 . . ? C9 C14 C13 120.8(4) . . ? C9 C14 H14A 119.6 . . ? C13 C14 H14A 119.6 . . ? C8 C15 C16 124.0(3) . . ? C8 C15 C20 118.1(3) . . ? C16 C15 C20 118.0(3) . . ? C15 C16 H16A 119.7 . . ? C15 C16 C17 120.7(3) . . ? H16A C16 C17 119.7 . . ? C16 C17 H17A 119.8 . . ? C16 C17 C18 120.5(4) . . ? H17A C17 C18 119.8 . . ? C17 C18 H18A 120.2 . . ? C17 C18 C19 119.5(4) . . ? H18A C18 C19 120.2 . . ? C18 C19 H19A 120.1 . . ? C18 C19 C20 119.7(4) . . ? H19A C19 C20 120.1 . . ? C15 C20 C19 121.6(3) . . ? C15 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C8 C21 C22 122.8(3) . . ? C8 C21 C26 119.7(3) . . ? C22 C21 C26 117.5(3) . . ? C21 C22 H22A 119.4 . . ? C21 C22 C23 121.2(4) . . ? H22A C22 C23 119.4 . . ? C22 C23 H23A 119.8 . . ? C22 C23 C24 120.5(4) . . ? H23A C23 C24 119.8 . . ? C23 C24 H24A 120.6 . . ? C23 C24 C25 118.7(3) . . ? H24A C24 C25 120.6 . . ? C24 C25 H25A 119.6 . . ? C24 C25 C26 120.8(4) . . ? H25A C25 C26 119.6 . . ? C21 C26 C25 121.3(4) . . ? C21 C26 H26A 119.4 . . ? C25 C26 H26A 119.4 . . ? 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 Br1 C2 C3 O3 -78.9(4) . . . . ? Br1 C2 C3 N4 99.7(3) . . . . ? C2 C3 N4 C5 -179.7(3) . . . . ? O3 C3 N4 C5 -1.2(6) . . . . ? C3 N4 C5 C6 98.6(4) . . . . ? N4 C5 C6 S7 -69.9(3) . . . . ? C5 C6 S7 C8 167.4(2) . . . . ? C6 S7 C8 C9 -81.7(3) . . . . ? C6 S7 C8 C15 161.9(2) . . . . ? C6 S7 C8 C21 42.5(3) . . . . ? S7 C8 C9 C10 -164.7(2) . . . . ? S7 C8 C9 C14 14.7(4) . . . . ? C15 C8 C9 C10 -52.1(4) . . . . ? C15 C8 C9 C14 127.4(3) . . . . ? C21 C8 C9 C10 73.0(4) . . . . ? C21 C8 C9 C14 -107.5(4) . . . . ? C8 C9 C10 C11 -178.6(3) . . . . ? C14 C9 C10 C11 1.8(5) . . . . ? C9 C10 C11 C12 -0.2(5) . . . . ? C10 C11 C12 C13 -1.2(6) . . . . ? C11 C12 C13 C14 0.9(6) . . . . ? C8 C9 C14 C13 178.3(3) . . . . ? C10 C9 C14 C13 -2.2(5) . . . . ? C12 C13 C14 C9 0.9(6) . . . . ? S7 C8 C15 C16 -122.8(3) . . . . ? S7 C8 C15 C20 58.1(3) . . . . ? C9 C8 C15 C16 118.4(4) . . . . ? C9 C8 C15 C20 -60.8(4) . . . . ? C21 C8 C15 C16 -6.2(5) . . . . ? C21 C8 C15 C20 174.6(3) . . . . ? C8 C15 C16 C17 179.9(3) . . . . ? C20 C15 C16 C17 -0.9(5) . . . . ? C15 C16 C17 C18 0.7(6) . . . . ? C16 C17 C18 C19 -0.3(6) . . . . ? C17 C18 C19 C20 0.2(6) . . . . ? C18 C19 C20 C15 -0.5(6) . . . . ? C8 C15 C20 C19 -179.9(3) . . . . ? C16 C15 C20 C19 0.9(5) . . . . ? S7 C8 C21 C22 -128.9(3) . . . . ? S7 C8 C21 C26 50.9(4) . . . . ? C9 C8 C21 C22 -4.7(5) . . . . ? C9 C8 C21 C26 175.2(3) . . . . ? C15 C8 C21 C22 118.2(4) . . . . ? C15 C8 C21 C26 -61.9(4) . . . . ? C8 C21 C22 C23 -178.8(3) . . . . ? C26 C21 C22 C23 1.3(5) . . . . ? C21 C22 C23 C24 -0.5(6) . . . . ? C22 C23 C24 C25 -0.7(6) . . . . ? C23 C24 C25 C26 1.0(6) . . . . ? C24 C25 C26 C21 -0.1(6) . . . . ? C8 C21 C26 C25 179.1(3) . . . . ? C22 C21 C26 C25 -1.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.822 _refine_diff_density_min -0.894 _refine_diff_density_rms 0.068 # Attachment 'CIF_for_7.cif' data_as1 _database_code_depnum_ccdc_archive 'CCDC 711189' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H10 Br N O' _chemical_formula_weight 264.12 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 P21/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 20.9960(17) _cell_length_b 5.8370(16) _cell_length_c 8.616(6) _cell_angle_alpha 90.00 _cell_angle_beta 100.784(8) _cell_angle_gamma 90.00 _cell_volume 1037.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 2229 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.691 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 528 _exptl_absorpt_coefficient_mu 3.932 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6498 _exptl_absorpt_correction_T_max 0.6945 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '/p scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3892 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0516 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 27.56 _reflns_number_total 2394 _reflns_number_gt 1921 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo (Nonius B.V., 1998)' _computing_data_reduction 'Denzo (Nonius B.V., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON 98 (Spek, 1998)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0284P)^2^+0.6098P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2394 _refine_ls_number_parameters 140 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0506 _refine_ls_R_factor_gt 0.0340 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.581717(11) -0.14000(5) 0.47641(3) 0.02570(11) Uani 1 1 d . . . O O 0.63085(8) 0.0747(4) 0.1474(2) 0.0272(4) Uani 1 1 d . . . N N 0.66417(10) 0.3293(4) 0.3464(3) 0.0218(5) Uani 1 1 d . . . C1 C 0.56461(12) 0.1271(5) 0.3396(3) 0.0232(6) Uani 1 1 d . . . H1A H 0.5266 0.0981 0.2549 0.028 Uiso 1 1 calc . . . H1B H 0.5550 0.2614 0.4015 0.028 Uiso 1 1 calc . . . C2 C 0.62376(12) 0.1749(5) 0.2678(3) 0.0207(6) Uani 1 1 d . . . C3 C 0.72299(11) 0.4150(5) 0.3101(3) 0.0198(6) Uani 1 1 d . . . C4 C 0.74394(12) 0.6304(5) 0.3736(3) 0.0226(6) Uani 1 1 d . . . H4 H 0.7175 0.7147 0.4315 0.027 Uiso 1 1 calc . . . C5 C 0.80167(12) 0.7191(5) 0.3527(3) 0.0234(6) Uani 1 1 d . . . H5 H 0.8152 0.8647 0.3959 0.028 Uiso 1 1 calc . . . C6 C 0.84166(12) 0.5961(5) 0.2671(3) 0.0207(6) Uani 1 1 d . . . C7 C 0.90285(13) 0.6800(5) 0.2466(3) 0.0266(6) Uani 1 1 d . . . H7 H 0.9179 0.8240 0.2901 0.032 Uiso 1 1 calc . . . C8 C 0.94013(12) 0.5552(6) 0.1648(3) 0.0298(7) Uani 1 1 d . . . H8 H 0.9812 0.6126 0.1522 0.036 Uiso 1 1 calc . . . C9 C 0.91877(13) 0.3432(5) 0.0989(3) 0.0280(7) Uani 1 1 d . . . H9 H 0.9453 0.2584 0.0416 0.034 Uiso 1 1 calc . . . C10 C 0.86007(12) 0.2575(5) 0.1164(3) 0.0237(6) Uani 1 1 d . . . H10 H 0.8460 0.1134 0.0714 0.028 Uiso 1 1 calc . . . C11 C 0.82011(12) 0.3819(4) 0.2010(3) 0.0189(6) Uani 1 1 d . . . C12 C 0.75965(12) 0.2927(5) 0.2242(3) 0.0199(6) Uani 1 1 d . . . H12 H 0.7448 0.1488 0.1802 0.024 Uiso 1 1 calc . . . H1N H 0.6543(13) 0.383(5) 0.416(4) 0.019(8) Uiso 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 0.02229(16) 0.02939(19) 0.02771(17) 0.00584(13) 0.01060(11) 0.00036(12) O 0.0296(10) 0.0327(11) 0.0217(10) -0.0051(9) 0.0109(8) -0.0079(9) N 0.0217(11) 0.0309(14) 0.0153(11) -0.0042(11) 0.0099(9) 0.0002(10) C1 0.0182(13) 0.0292(16) 0.0223(13) 0.0056(12) 0.0043(10) 0.0022(11) C2 0.0199(13) 0.0248(15) 0.0176(13) 0.0040(12) 0.0045(10) 0.0020(11) C3 0.0158(12) 0.0286(15) 0.0152(12) 0.0014(11) 0.0033(9) -0.0017(11) C4 0.0232(13) 0.0238(15) 0.0219(13) -0.0029(12) 0.0074(10) 0.0052(12) C5 0.0263(14) 0.0219(15) 0.0207(14) 0.0001(12) 0.0012(10) 0.0013(12) C6 0.0195(13) 0.0261(16) 0.0162(12) 0.0045(11) 0.0024(9) 0.0012(11) C7 0.0217(13) 0.0284(17) 0.0292(15) 0.0026(13) 0.0033(11) -0.0045(12) C8 0.0173(13) 0.0385(18) 0.0339(16) 0.0057(15) 0.0058(11) -0.0038(13) C9 0.0208(14) 0.0390(19) 0.0261(15) 0.0020(14) 0.0094(11) 0.0045(13) C10 0.0209(13) 0.0274(16) 0.0231(14) -0.0019(13) 0.0049(10) 0.0022(12) C11 0.0189(12) 0.0221(15) 0.0155(12) 0.0037(11) 0.0025(9) 0.0036(11) C12 0.0209(13) 0.0223(14) 0.0165(12) -0.0010(11) 0.0036(10) -0.0010(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 Br1 C1 1.947(3) . ? O C2 1.224(3) . ? N C2 1.333(3) . ? N C3 1.420(3) . ? N H1N 0.74(3) . ? C1 C2 1.513(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C3 C12 1.365(4) . ? C3 C4 1.409(4) . ? C4 C5 1.361(4) . ? C4 H4 0.9500 . ? C5 C6 1.412(4) . ? C5 H5 0.9500 . ? C6 C11 1.413(4) . ? C6 C7 1.416(4) . ? C7 C8 1.358(4) . ? C7 H7 0.9500 . ? C8 C9 1.400(4) . ? C8 H8 0.9500 . ? C9 C10 1.364(4) . ? C9 H9 0.9500 . ? C10 C11 1.411(4) . ? C10 H10 0.9500 . ? C11 C12 1.420(4) . ? C12 H12 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 N C3 128.6(2) . . ? C2 N H1N 117(2) . . ? C3 N H1N 115(2) . . ? C2 C1 Br1 108.81(17) . . ? C2 C1 H1A 109.9 . . ? Br1 C1 H1A 109.9 . . ? C2 C1 H1B 109.9 . . ? Br1 C1 H1B 109.9 . . ? H1A C1 H1B 108.3 . . ? O C2 N 125.9(2) . . ? O C2 C1 119.9(2) . . ? N C2 C1 114.2(2) . . ? C12 C3 C4 120.7(2) . . ? C12 C3 N 122.5(3) . . ? C4 C3 N 116.8(2) . . ? C5 C4 C3 120.6(2) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C11 118.9(2) . . ? C5 C6 C7 122.1(3) . . ? C11 C6 C7 119.0(2) . . ? C8 C7 C6 120.3(3) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 120.8(3) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C10 C9 C8 120.4(3) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C11 120.4(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C10 C11 C6 119.1(2) . . ? C10 C11 C12 121.2(2) . . ? C6 C11 C12 119.7(2) . . ? C3 C12 C11 119.6(2) . . ? C3 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? 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 C3 N C2 O 0.8(5) . . . . ? C3 N C2 C1 -179.0(2) . . . . ? Br1 C1 C2 O 85.3(3) . . . . ? Br1 C1 C2 N -94.9(2) . . . . ? C2 N C3 C12 -25.8(4) . . . . ? C2 N C3 C4 157.2(3) . . . . ? C12 C3 C4 C5 -1.1(4) . . . . ? N C3 C4 C5 176.0(2) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C4 C5 C6 C11 1.3(4) . . . . ? C4 C5 C6 C7 -178.2(3) . . . . ? C5 C6 C7 C8 179.3(3) . . . . ? C11 C6 C7 C8 -0.2(4) . . . . ? C6 C7 C8 C9 0.3(4) . . . . ? C7 C8 C9 C10 -0.3(4) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C9 C10 C11 C6 0.1(4) . . . . ? C9 C10 C11 C12 -178.3(3) . . . . ? C5 C6 C11 C10 -179.5(2) . . . . ? C7 C6 C11 C10 0.0(4) . . . . ? C5 C6 C11 C12 -1.2(4) . . . . ? C7 C6 C11 C12 178.3(2) . . . . ? C4 C3 C12 C11 1.1(4) . . . . ? N C3 C12 C11 -175.8(2) . . . . ? C10 C11 C12 C3 178.3(2) . . . . ? C6 C11 C12 C3 0.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.458 _refine_diff_density_min -0.872 _refine_diff_density_rms 0.092