data_Compd_TMC2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common TMC _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H37 N3' _chemical_formula_weight 415.60 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.6106(16) _cell_length_b 16.1279(17) _cell_length_c 19.714(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4963.2(9) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 4823 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 27.33 _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.202 _exptl_crystal_size_min 0.132 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.110 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.9779 _exptl_absorpt_correction_T_max 0.9921 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 43353 _diffrn_reflns_av_R_equivalents 0.0654 _diffrn_reflns_av_sigmaI/netI 0.0469 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.73 _reflns_number_total 6031 _reflns_number_gt 3004 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1332P)^2^+5.7257P] 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 const _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6031 _refine_ls_number_parameters 269 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1674 _refine_ls_R_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.3100 _refine_ls_wR_factor_gt 0.2419 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 N1 N -0.1239(2) 0.4498(2) 0.41434(19) 0.0698(10) Uani 1 1 d . . . N2 N -0.1355(2) 0.1923(2) 0.49152(18) 0.0630(9) Uani 1 1 d . . . N3 N 0.11646(18) 0.12531(17) 0.02510(15) 0.0458(7) Uani 1 1 d . B . C1 C -0.1192(2) 0.3790(2) 0.40445(19) 0.0536(9) Uani 1 1 d . . . C2 C -0.1093(2) 0.2936(2) 0.39330(19) 0.0487(8) Uani 1 1 d . . . C3 C -0.1237(2) 0.2394(2) 0.4477(2) 0.0508(9) Uani 1 1 d . . . C4 C -0.07492(19) 0.2629(2) 0.32901(18) 0.0448(8) Uani 1 1 d . . . C5 C -0.0522(2) 0.1793(2) 0.32107(18) 0.0455(8) Uani 1 1 d . . . H5 H -0.0627 0.1417 0.3572 0.055 Uiso 1 1 calc R . . C6 C -0.0147(2) 0.15018(19) 0.26174(17) 0.0433(8) Uani 1 1 d . . . C7 C 0.0000(2) 0.20503(19) 0.20801(17) 0.0414(7) Uani 1 1 d . . . C8 C -0.0251(2) 0.2884(2) 0.21369(18) 0.0447(8) Uani 1 1 d . . . C9 C -0.0616(2) 0.3156(2) 0.27403(18) 0.0470(8) Uani 1 1 d . . . H9 H -0.0780 0.3721 0.2779 0.056 Uiso 1 1 calc R . . C10 C 0.0108(2) 0.0602(2) 0.2567(2) 0.0530(9) Uani 1 1 d . . . H10A H -0.0027 0.0393 0.2113 0.079 Uiso 1 1 calc R . . H10B H -0.0208 0.0279 0.2907 0.079 Uiso 1 1 calc R . . H10C H 0.0724 0.0549 0.2650 0.079 Uiso 1 1 calc R . . C11 C -0.0124(3) 0.3475(2) 0.1554(2) 0.0615(10) Uani 1 1 d . . . H11A H 0.0490 0.3543 0.1467 0.092 Uiso 1 1 calc R . . H11B H -0.0377 0.4013 0.1668 0.092 Uiso 1 1 calc R . . H11C H -0.0403 0.3252 0.1147 0.092 Uiso 1 1 calc R . . C12 C 0.0411(2) 0.17545(19) 0.14434(17) 0.0421(7) Uani 1 1 d . . . C13 C 0.1310(2) 0.1785(2) 0.13666(18) 0.0472(8) Uani 1 1 d . . . C14 C 0.1658(2) 0.1528(2) 0.07625(19) 0.0503(9) Uani 1 1 d . . . H14 H 0.2262 0.1545 0.0705 0.060 Uiso 1 1 calc R . . C15 C 0.0311(2) 0.1198(2) 0.03258(17) 0.0447(8) Uani 1 1 d . . . H15 H -0.0025 0.0982 -0.0035 0.054 Uiso 1 1 calc R . . C16 C -0.0086(2) 0.14479(19) 0.09103(17) 0.0413(7) Uani 1 1 d . . . C17 C 0.1889(2) 0.2089(3) 0.1922(2) 0.0658(11) Uani 1 1 d . . . H17A H 0.2487 0.2044 0.1775 0.099 Uiso 1 1 calc R . . H17B H 0.1802 0.1752 0.2330 0.099 Uiso 1 1 calc R . . H17C H 0.1756 0.2670 0.2023 0.099 Uiso 1 1 calc R . . C18 C -0.1047(2) 0.1397(2) 0.09720(19) 0.0488(8) Uani 1 1 d . . . H18A H -0.1286 0.1958 0.1000 0.073 Uiso 1 1 calc R . . H18B H -0.1198 0.1087 0.1382 0.073 Uiso 1 1 calc R . . H18C H -0.1283 0.1114 0.0574 0.073 Uiso 1 1 calc R . . C19 C 0.1560(3) 0.0990(2) -0.03961(18) 0.0550(9) Uani 1 1 d . . . H19A H 0.1403 0.0406 -0.0489 0.066 Uiso 1 1 calc R A 1 H19B H 0.2191 0.1018 -0.0353 0.066 Uiso 1 1 calc R A 1 C20 C 0.1286(5) 0.1515(4) -0.0977(3) 0.0673(6) Uani 0.693(3) 1 d P B 1 H20 H 0.0647 0.1513 -0.0934 0.081 Uiso 0.693(3) 1 calc PR B 1 C21 C 0.1435(4) 0.1005(4) -0.1630(3) 0.0673(6) Uani 0.693(3) 1 d P B 1 H21A H 0.1128 0.0472 -0.1584 0.081 Uiso 0.693(3) 1 calc PR B 1 H21B H 0.1173 0.1308 -0.2014 0.081 Uiso 0.693(3) 1 calc PR B 1 C22 C 0.2334(5) 0.0826(4) -0.1804(3) 0.0673(6) Uani 0.693(3) 1 d P B 1 H22A H 0.2584 0.0444 -0.1465 0.081 Uiso 0.693(3) 1 calc PR B 1 H22B H 0.2672 0.1346 -0.1803 0.081 Uiso 0.693(3) 1 calc PR B 1 C23 C 0.2363(5) 0.0408(5) -0.2548(3) 0.0673(6) Uani 0.693(3) 1 d P B 1 H23A H 0.1998 -0.0086 -0.2554 0.081 Uiso 0.693(3) 1 calc PR B 1 H23B H 0.2954 0.0250 -0.2656 0.081 Uiso 0.693(3) 1 calc PR B 1 H23C H 0.2156 0.0807 -0.2885 0.081 Uiso 0.693(3) 1 calc PR B 1 C24 C 0.1472(4) 0.2350(5) -0.1048(4) 0.0673(6) Uani 0.693(3) 1 d P B 1 H24A H 0.1159 0.2539 -0.1456 0.081 Uiso 0.693(3) 1 calc PR B 1 H24B H 0.2089 0.2381 -0.1162 0.081 Uiso 0.693(3) 1 calc PR B 1 C25 C 0.1323(4) 0.2985(4) -0.0525(3) 0.0673(6) Uani 0.693(3) 1 d P B 1 H25A H 0.1687 0.2847 -0.0129 0.081 Uiso 0.693(3) 1 calc PR B 1 H25B H 0.0720 0.2938 -0.0376 0.081 Uiso 0.693(3) 1 calc PR B 1 C26 C 0.1492(4) 0.3905(4) -0.0713(3) 0.0673(6) Uani 0.693(3) 1 d P B 1 H26A H 0.2120 0.3985 -0.0732 0.081 Uiso 0.693(3) 1 calc PR B 1 H26B H 0.1269 0.3995 -0.1177 0.081 Uiso 0.693(3) 1 calc PR B 1 C27 C 0.1165(5) 0.4506(4) -0.0313(3) 0.0673(6) Uani 0.693(3) 1 d P B 1 H27A H 0.0538 0.4418 -0.0288 0.081 Uiso 0.693(3) 1 calc PR B 1 H27B H 0.1257 0.5041 -0.0548 0.081 Uiso 0.693(3) 1 calc PR B 1 C20A C 0.1880(11) 0.1634(9) -0.0864(7) 0.0673(6) Uani 0.307(3) 1 d P B 2 H20A H 0.2412 0.1741 -0.0595 0.081 Uiso 0.307(3) 1 calc PR B 2 C21A C 0.2355(9) 0.1299(10) -0.1465(7) 0.0673(6) Uani 0.307(3) 1 d P B 2 H21C H 0.2843 0.0967 -0.1296 0.081 Uiso 0.307(3) 1 calc PR B 2 H21D H 0.2596 0.1775 -0.1719 0.081 Uiso 0.307(3) 1 calc PR B 2 C22A C 0.1824(11) 0.0734(9) -0.1993(8) 0.0673(6) Uani 0.307(3) 1 d P B 2 H22C H 0.1415 0.0376 -0.1745 0.081 Uiso 0.307(3) 1 calc PR B 2 H22D H 0.1495 0.1091 -0.2308 0.081 Uiso 0.307(3) 1 calc PR B 2 C23A C 0.2444(12) 0.0213(10) -0.2382(8) 0.0673(6) Uani 0.307(3) 1 d P B 2 H2ED H 0.2268 0.0188 -0.2859 0.081 Uiso 0.307(3) 1 calc PR B 2 H23E H 0.2454 -0.0348 -0.2192 0.081 Uiso 0.307(3) 1 calc PR B 2 H23F H 0.3018 0.0458 -0.2350 0.081 Uiso 0.307(3) 1 calc PR B 2 C24A C 0.1764(10) 0.2414(12) -0.1019(10) 0.0673(6) Uani 0.307(3) 1 d P B 2 H24C H 0.1683 0.2308 -0.1509 0.081 Uiso 0.307(3) 1 calc PR B 2 H24D H 0.2379 0.2559 -0.0987 0.081 Uiso 0.307(3) 1 calc PR B 2 C25A C 0.1502(10) 0.3194(9) -0.1051(7) 0.0673(6) Uani 0.307(3) 1 d P B 2 H25C H 0.0947 0.3230 -0.1293 0.081 Uiso 0.307(3) 1 calc PR B 2 H25D H 0.1927 0.3538 -0.1295 0.081 Uiso 0.307(3) 1 calc PR B 2 C26A C 0.1403(10) 0.3497(10) -0.0308(7) 0.0673(6) Uani 0.307(3) 1 d P B 2 H26C H 0.1980 0.3465 -0.0103 0.081 Uiso 0.307(3) 1 calc PR B 2 H26D H 0.1049 0.3075 -0.0074 0.081 Uiso 0.307(3) 1 calc PR B 2 C27A C 0.0960(11) 0.4515(10) -0.0056(8) 0.0673(6) Uani 0.307(3) 1 d P B 2 H27C H 0.1017 0.4941 -0.0414 0.081 Uiso 0.307(3) 1 calc PR B 2 H27D H 0.0359 0.4481 0.0102 0.081 Uiso 0.307(3) 1 calc PR B 2 C28 C 0.1497(4) 0.4612(4) 0.0432(3) 0.1060(19) Uani 1 1 d . . . H28A H 0.1797 0.4106 0.0573 0.127 Uiso 0.693(3) 1 calc PR B 1 H28B H 0.1010 0.4711 0.0735 0.127 Uiso 0.693(3) 1 calc PR B 1 H28C H 0.1892 0.5084 0.0454 0.127 Uiso 0.693(3) 1 calc PR B 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 N1 0.081(2) 0.056(2) 0.073(2) -0.0205(18) -0.0144(18) 0.0153(18) N2 0.0557(19) 0.069(2) 0.064(2) -0.0093(18) 0.0072(16) -0.0125(16) N3 0.0448(16) 0.0399(15) 0.0526(17) 0.0088(13) 0.0085(13) 0.0038(12) C1 0.047(2) 0.059(2) 0.055(2) -0.0124(18) -0.0076(16) 0.0068(17) C2 0.0402(18) 0.0476(19) 0.058(2) -0.0125(17) 0.0014(15) -0.0018(14) C3 0.0386(18) 0.054(2) 0.059(2) -0.0188(19) 0.0029(16) -0.0057(16) C4 0.0352(16) 0.0418(17) 0.057(2) -0.0084(15) -0.0011(14) -0.0026(13) C5 0.0453(18) 0.0382(17) 0.053(2) -0.0009(15) 0.0021(15) -0.0052(14) C6 0.0428(17) 0.0345(16) 0.053(2) -0.0024(14) 0.0013(15) -0.0019(13) C7 0.0357(16) 0.0368(17) 0.0517(19) -0.0029(14) 0.0015(14) -0.0046(12) C8 0.0435(18) 0.0352(16) 0.056(2) -0.0012(14) -0.0011(15) -0.0039(13) C9 0.0464(19) 0.0355(16) 0.059(2) -0.0072(15) -0.0046(16) 0.0004(14) C10 0.063(2) 0.0384(18) 0.058(2) -0.0023(16) 0.0046(17) 0.0012(16) C11 0.075(3) 0.0376(19) 0.072(3) 0.0034(18) 0.003(2) -0.0045(17) C12 0.0372(16) 0.0341(16) 0.055(2) 0.0042(14) 0.0047(14) -0.0021(12) C13 0.0389(17) 0.0445(18) 0.058(2) 0.0040(16) 0.0032(15) -0.0030(14) C14 0.0363(17) 0.052(2) 0.063(2) 0.0091(17) 0.0044(16) 0.0027(15) C15 0.0444(18) 0.0379(17) 0.052(2) 0.0034(14) 0.0036(15) -0.0001(14) C16 0.0394(17) 0.0336(16) 0.0509(19) 0.0026(14) 0.0013(14) -0.0017(13) C17 0.045(2) 0.081(3) 0.071(3) -0.003(2) -0.0015(19) -0.0126(19) C18 0.0391(18) 0.052(2) 0.055(2) 0.0030(16) 0.0018(15) -0.0060(15) C19 0.054(2) 0.056(2) 0.055(2) 0.0060(17) 0.0147(17) 0.0109(17) C20 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C21 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C22 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C23 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C24 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C25 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C26 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C27 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C20A 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C21A 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C22A 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C23A 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C24A 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C25A 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C26A 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C27A 0.0704(14) 0.0664(13) 0.0651(14) 0.0073(10) 0.0102(11) 0.0038(12) C28 0.109(4) 0.084(4) 0.125(5) 0.007(3) -0.004(4) -0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.160(5) . ? N2 C3 1.165(5) . ? N3 C15 1.344(4) . ? N3 C14 1.344(5) . ? N3 C19 1.479(4) . ? C1 C2 1.402(5) . ? C2 C3 1.402(6) . ? C2 C4 1.463(5) . ? C4 C9 1.393(5) . ? C4 C5 1.402(5) . ? C5 C6 1.390(5) . ? C5 H5 0.9500 . ? C6 C7 1.399(5) . ? C6 C10 1.508(4) . ? C7 C8 1.405(5) . ? C7 C12 1.488(5) . ? C8 C9 1.390(5) . ? C8 C11 1.507(5) . ? C9 H9 0.9500 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C16 1.397(5) . ? C12 C13 1.413(5) . ? C13 C14 1.373(5) . ? C13 C17 1.502(5) . ? C14 H14 0.9500 . ? C15 C16 1.369(5) . ? C15 H15 0.9500 . ? C16 C18 1.508(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20A 1.475(14) . ? C19 C20 1.487(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C24 1.385(10) . ? C20 C21 1.545(9) . ? C20 H20 1.0000 . ? C21 C22 1.472(9) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.614(10) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.472(11) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.551(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.351(9) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.566(9) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C20A C24A 1.31(2) . ? C20A C21A 1.499(19) . ? C20A H20A 1.0000 . ? C21A C22A 1.61(2) . ? C21A H21C 0.9900 . ? C21A H21D 0.9900 . ? C22A C23A 1.49(2) . ? C22A H22C 0.9900 . ? C22A H22D 0.9900 . ? C23A H2ED 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A C25A 1.32(2) . ? C24A H24C 0.9900 . ? C24A H24D 0.9900 . ? C25A C26A 1.55(2) . ? C25A H25C 0.9900 . ? C25A H25D 0.9900 . ? C26A C27A 1.85(2) . ? C26A H26C 0.9900 . ? C26A H26D 0.9900 . ? C27A C28 1.285(17) . ? C27A H27C 0.9900 . ? C27A H27D 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 C15 N3 C14 120.5(3) . . ? C15 N3 C19 119.3(3) . . ? C14 N3 C19 120.1(3) . . ? N1 C1 C2 177.2(4) . . ? C3 C2 C1 118.3(3) . . ? C3 C2 C4 120.7(3) . . ? C1 C2 C4 120.6(3) . . ? N2 C3 C2 177.8(4) . . ? C9 C4 C5 117.5(3) . . ? C9 C4 C2 121.5(3) . . ? C5 C4 C2 121.0(3) . . ? C6 C5 C4 121.7(3) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 119.5(3) . . ? C5 C6 C10 119.5(3) . . ? C7 C6 C10 121.0(3) . . ? C6 C7 C8 119.9(3) . . ? C6 C7 C12 120.4(3) . . ? C8 C7 C12 119.6(3) . . ? C9 C8 C7 119.0(3) . . ? C9 C8 C11 120.4(3) . . ? C7 C8 C11 120.5(3) . . ? C8 C9 C4 122.3(3) . . ? C8 C9 H9 118.9 . . ? C4 C9 H9 118.9 . . ? C6 C10 H10A 109.5 . . ? C6 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C6 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C16 C12 C13 118.9(3) . . ? C16 C12 C7 120.6(3) . . ? C13 C12 C7 120.5(3) . . ? C14 C13 C12 118.4(3) . . ? C14 C13 C17 119.6(3) . . ? C12 C13 C17 122.1(3) . . ? N3 C14 C13 121.6(3) . . ? N3 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? N3 C15 C16 121.5(3) . . ? N3 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C15 C16 C12 119.1(3) . . ? C15 C16 C18 120.2(3) . . ? C12 C16 C18 120.8(3) . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20A C19 N3 118.6(6) . . ? C20A C19 C20 38.4(6) . . ? N3 C19 C20 112.4(3) . . ? C20A C19 H19A 129.6 . . ? N3 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? C20A C19 H19B 71.6 . . ? N3 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? C24 C20 C19 124.7(6) . . ? C24 C20 C21 113.7(6) . . ? C19 C20 C21 107.2(5) . . ? C24 C20 H20 102.7 . . ? C19 C20 H20 102.7 . . ? C21 C20 H20 102.7 . . ? C22 C21 C20 116.3(6) . . ? C22 C21 H21A 108.2 . . ? C20 C21 H21A 108.2 . . ? C22 C21 H21B 108.2 . . ? C20 C21 H21B 108.2 . . ? H21A C21 H21B 107.4 . . ? C21 C22 C23 108.7(6) . . ? C21 C22 H22A 109.9 . . ? C23 C22 H22A 109.9 . . ? C21 C22 H22B 109.9 . . ? C23 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C20 C24 C25 125.0(7) . . ? C20 C24 H24A 106.1 . . ? C25 C24 H24A 106.1 . . ? C20 C24 H24B 106.1 . . ? C25 C24 H24B 106.1 . . ? H24A C24 H24B 106.3 . . ? C24 C25 C26 118.1(6) . . ? C24 C25 H25A 107.8 . . ? C26 C25 H25A 107.8 . . ? C24 C25 H25B 107.8 . . ? C26 C25 H25B 107.8 . . ? H25A C25 H25B 107.1 . . ? C27 C26 C25 118.9(6) . . ? C27 C26 H26A 107.6 . . ? C25 C26 H26A 107.6 . . ? C27 C26 H26B 107.6 . . ? C25 C26 H26B 107.6 . . ? H26A C26 H26B 107.0 . . ? C26 C27 C28 120.1(6) . . ? C26 C27 H27A 107.3 . . ? C28 C27 H27A 107.3 . . ? C26 C27 H27B 107.3 . . ? C28 C27 H27B 107.3 . . ? H27A C27 H27B 106.9 . . ? C24A C20A C19 140.9(13) . . ? C24A C20A C21A 103.3(13) . . ? C19 C20A C21A 114.1(11) . . ? C24A C20A H20A 94.1 . . ? C19 C20A H20A 94.1 . . ? C21A C20A H20A 94.1 . . ? C20A C21A C22A 117.4(12) . . ? C20A C21A H21C 108.0 . . ? C22A C21A H21C 108.0 . . ? C20A C21A H21D 108.0 . . ? C22A C21A H21D 108.0 . . ? H21C C21A H21D 107.2 . . ? C23A C22A C21A 108.4(14) . . ? C23A C22A H22C 110.0 . . ? C21A C22A H22C 110.0 . . ? C23A C22A H22D 110.0 . . ? C21A C22A H22D 110.0 . . ? H22C C22A H22D 108.4 . . ? C22A C23A H2ED 109.5 . . ? C22A C23A H23E 109.5 . . ? H2ED C23A H23E 109.5 . . ? C22A C23A H23F 109.5 . . ? H2ED C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C20A C24A C25A 165.5(17) . . ? C20A C24A H24C 94.5 . . ? C25A C24A H24C 94.5 . . ? C20A C24A H24D 94.5 . . ? C25A C24A H24D 94.5 . . ? H24C C24A H24D 103.2 . . ? C24A C25A C26A 106.6(14) . . ? C24A C25A H25C 110.4 . . ? C26A C25A H25C 110.4 . . ? C24A C25A H25D 110.4 . . ? C26A C25A H25D 110.4 . . ? H25C C25A H25D 108.6 . . ? C25A C26A C27A 124.8(12) . . ? C25A C26A H26C 106.1 . . ? C27A C26A H26C 106.1 . . ? C25A C26A H26D 106.1 . . ? C27A C26A H26D 106.1 . . ? H26C C26A H26D 106.3 . . ? C28 C27A C26A 93.8(11) . . ? C28 C27A H27C 113.0 . . ? C26A C27A H27C 113.0 . . ? C28 C27A H27D 113.0 . . ? C26A C27A H27D 113.0 . . ? H27C C27A H27D 110.4 . . ? C27A C28 C27 21.5(7) . . ? C27A C28 H28A 115.0 . . ? C27 C28 H28A 109.5 . . ? C27A C28 H28B 88.3 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27A C28 H28C 122.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 91(9) . . . . ? N1 C1 C2 C4 -81(9) . . . . ? C1 C2 C3 N2 172(100) . . . . ? C4 C2 C3 N2 -15(10) . . . . ? C3 C2 C4 C9 178.9(3) . . . . ? C1 C2 C4 C9 -8.6(5) . . . . ? C3 C2 C4 C5 -2.7(5) . . . . ? C1 C2 C4 C5 169.9(3) . . . . ? C9 C4 C5 C6 2.4(5) . . . . ? C2 C4 C5 C6 -176.1(3) . . . . ? C4 C5 C6 C7 -0.8(5) . . . . ? C4 C5 C6 C10 178.2(3) . . . . ? C5 C6 C7 C8 -1.7(5) . . . . ? C10 C6 C7 C8 179.4(3) . . . . ? C5 C6 C7 C12 179.2(3) . . . . ? C10 C6 C7 C12 0.2(5) . . . . ? C6 C7 C8 C9 2.4(5) . . . . ? C12 C7 C8 C9 -178.5(3) . . . . ? C6 C7 C8 C11 -177.9(3) . . . . ? C12 C7 C8 C11 1.2(5) . . . . ? C7 C8 C9 C4 -0.6(5) . . . . ? C11 C8 C9 C4 179.6(3) . . . . ? C5 C4 C9 C8 -1.7(5) . . . . ? C2 C4 C9 C8 176.8(3) . . . . ? C6 C7 C12 C16 89.8(4) . . . . ? C8 C7 C12 C16 -89.4(4) . . . . ? C6 C7 C12 C13 -90.7(4) . . . . ? C8 C7 C12 C13 90.1(4) . . . . ? C16 C12 C13 C14 1.4(5) . . . . ? C7 C12 C13 C14 -178.1(3) . . . . ? C16 C12 C13 C17 -178.7(3) . . . . ? C7 C12 C13 C17 1.8(5) . . . . ? C15 N3 C14 C13 -2.1(5) . . . . ? C19 N3 C14 C13 179.3(3) . . . . ? C12 C13 C14 N3 0.1(5) . . . . ? C17 C13 C14 N3 -179.8(3) . . . . ? C14 N3 C15 C16 2.5(5) . . . . ? C19 N3 C15 C16 -178.8(3) . . . . ? N3 C15 C16 C12 -0.9(5) . . . . ? N3 C15 C16 C18 178.6(3) . . . . ? C13 C12 C16 C15 -1.0(5) . . . . ? C7 C12 C16 C15 178.5(3) . . . . ? C13 C12 C16 C18 179.5(3) . . . . ? C7 C12 C16 C18 -1.0(5) . . . . ? C15 N3 C19 C20A 106.4(8) . . . . ? C14 N3 C19 C20A -74.9(9) . . . . ? C15 N3 C19 C20 64.2(5) . . . . ? C14 N3 C19 C20 -117.1(4) . . . . ? C20A C19 C20 C24 -43.3(10) . . . . ? N3 C19 C20 C24 65.0(8) . . . . ? C20A C19 C20 C21 93.3(11) . . . . ? N3 C19 C20 C21 -158.5(4) . . . . ? C24 C20 C21 C22 75.1(8) . . . . ? C19 C20 C21 C22 -66.8(7) . . . . ? C20 C21 C22 C23 -172.1(5) . . . . ? C19 C20 C24 C25 -50.9(10) . . . . ? C21 C20 C24 C25 174.9(6) . . . . ? C20 C24 C25 C26 -174.4(7) . . . . ? C24 C25 C26 C27 163.7(7) . . . . ? C25 C26 C27 C28 66.1(9) . . . . ? N3 C19 C20A C24A -24(3) . . . . ? C20 C19 C20A C24A 66(2) . . . . ? N3 C19 C20A C21A 173.5(9) . . . . ? C20 C19 C20A C21A -95.9(16) . . . . ? C24A C20A C21A C22A -104.5(16) . . . . ? C19 C20A C21A C22A 63.9(17) . . . . ? C20A C21A C22A C23A -158.5(12) . . . . ? C19 C20A C24A C25A 1(9) . . . . ? C21A C20A C24A C25A 164(7) . . . . ? C20A C24A C25A C26A 42(8) . . . . ? C24A C25A C26A C27A -174.3(13) . . . . ? C25A C26A C27A C28 -141.6(14) . . . . ? C26A C27A C28 C27 63(2) . . . . ? C26 C27 C28 C27A -126(3) . . . . ? _diffrn_measured_fraction_theta_max 0.937 _diffrn_reflns_theta_full 28.73 _diffrn_measured_fraction_theta_full 0.937 _refine_diff_density_max 0.789 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.061 #===END