data_jrc1911n _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H27 Cl2 F2 N3 O' _chemical_formula_sum 'C29 H27 Cl2 F2 N3 O' _chemical_formula_weight 542.44 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' 'Cl' 'Cl' 0.1484 0.1585 '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 19.223(2) _cell_length_b 12.3110(15) _cell_length_c 22.588(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5345.6(11) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5225 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 22.56 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.348 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 0.284 _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 298(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 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54403 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.42 _reflns_number_total 5495 _reflns_number_gt 3795 _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^)+(0.0542P)^2^+1.5126P] 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 5495 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0489 _refine_ls_wR_factor_ref 0.1256 _refine_ls_wR_factor_gt 0.1120 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.95776(11) 0.35262(18) 0.41734(10) 0.0420(5) Uani 1 1 d . . . C2 C 0.89544(11) 0.37127(18) 0.45187(9) 0.0426(5) Uani 1 1 d . . . H2 H 0.8984 0.4156 0.4851 0.051 Uiso 1 1 calc R . . C3 C 0.83373(11) 0.32748(16) 0.43799(9) 0.0375(5) Uani 1 1 d . . . H3 H 0.7951 0.3434 0.4612 0.045 Uiso 1 1 calc R . . C4 C 0.82626(10) 0.25643(15) 0.38795(8) 0.0320(4) Uani 1 1 d . . . C5 C 0.76344(10) 0.20967(16) 0.36847(8) 0.0321(4) Uani 1 1 d . . . C6 C 0.81921(10) 0.10549(15) 0.29832(9) 0.0337(5) Uani 1 1 d . . . C7 C 0.88274(10) 0.14989(17) 0.31273(9) 0.0376(5) Uani 1 1 d . . . H7 H 0.9227 0.1278 0.2929 0.045 Uiso 1 1 calc R . . C8 C 0.88673(10) 0.22768(16) 0.35693(8) 0.0332(5) Uani 1 1 d . . . C9 C 1.00873(10) 0.25260(17) 0.33522(9) 0.0371(5) Uani 1 1 d . . . C10 C 1.05386(11) 0.17015(18) 0.35125(9) 0.0406(5) Uani 1 1 d . . . C11 C 1.10761(11) 0.13782(19) 0.31467(10) 0.0462(6) Uani 1 1 d . . . H11 H 1.1383 0.0836 0.3265 0.055 Uiso 1 1 calc R . . C12 C 1.11494(12) 0.1871(2) 0.26068(11) 0.0507(6) Uani 1 1 d . . . H12 H 1.1499 0.1641 0.2351 0.061 Uiso 1 1 calc R . . C13 C 1.07142(12) 0.2700(2) 0.24365(11) 0.0513(6) Uani 1 1 d . . . H13 H 1.0774 0.3035 0.2071 0.062 Uiso 1 1 calc R . . C14 C 1.01878(11) 0.30326(18) 0.28116(10) 0.0451(5) Uani 1 1 d . . . C15 C 0.69377(10) 0.23589(17) 0.39455(9) 0.0361(5) Uani 1 1 d . . . C16 C 0.66950(12) 0.33959(18) 0.40464(9) 0.0413(5) Uani 1 1 d . . . C17 C 0.60328(13) 0.3617(2) 0.42482(10) 0.0550(7) Uani 1 1 d . . . H17 H 0.5883 0.4326 0.4311 0.066 Uiso 1 1 calc R . . C18 C 0.56065(12) 0.2749(3) 0.43525(11) 0.0606(7) Uani 1 1 d . . . C19 C 0.58078(13) 0.1705(2) 0.42632(11) 0.0614(7) Uani 1 1 d . . . H19 H 0.5506 0.1131 0.4340 0.074 Uiso 1 1 calc R . . C20 C 0.64730(11) 0.1516(2) 0.40545(10) 0.0495(6) Uani 1 1 d . . . H20 H 0.6614 0.0804 0.3985 0.059 Uiso 1 1 calc R . . C21 C 0.82004(13) 0.08421(18) 0.18925(10) 0.0467(6) Uani 1 1 d . . . H21A H 0.7830 0.1375 0.1867 0.056 Uiso 1 1 calc R . . H21B H 0.8640 0.1227 0.1875 0.056 Uiso 1 1 calc R . . C22 C 0.81491(13) 0.0073(2) 0.13712(10) 0.0526(6) Uani 1 1 d . . . H22A H 0.8188 0.0480 0.1005 0.063 Uiso 1 1 calc R . . H22B H 0.8529 -0.0444 0.1386 0.063 Uiso 1 1 calc R . . C23 C 0.81483(10) 0.02452(16) 0.24804(9) 0.0362(5) Uani 1 1 d . . . H23 H 0.8552 -0.0238 0.2511 0.043 Uiso 1 1 calc R . . C24 C 0.74998(12) -0.04624(17) 0.24743(9) 0.0412(5) Uani 1 1 d . . . H24A H 0.7500 -0.0927 0.2821 0.049 Uiso 1 1 calc R . . H24B H 0.7091 -0.0002 0.2494 0.049 Uiso 1 1 calc R . . C25 C 0.74611(12) -0.11619(18) 0.19218(9) 0.0425(5) Uani 1 1 d . . . H25A H 0.7846 -0.1672 0.1922 0.051 Uiso 1 1 calc R . . H25B H 0.7032 -0.1576 0.1927 0.051 Uiso 1 1 calc R . . C26 C 0.73415(12) -0.11341(17) 0.08292(9) 0.0410(5) Uani 1 1 d . . . C27 C 0.78757(13) -0.2031(2) 0.07091(11) 0.0574(7) Uani 1 1 d . . . H27A H 0.8332 -0.1717 0.0682 0.086 Uiso 1 1 calc R . . H27B H 0.7765 -0.2388 0.0343 0.086 Uiso 1 1 calc R . . H27C H 0.7866 -0.2549 0.1026 0.086 Uiso 1 1 calc R . . C28 C 0.73325(15) -0.0347(2) 0.03065(11) 0.0641(7) Uani 1 1 d . . . H28A H 0.7040 0.0262 0.0399 0.096 Uiso 1 1 calc R . . H28B H 0.7155 -0.0711 -0.0038 0.096 Uiso 1 1 calc R . . H28C H 0.7797 -0.0097 0.0229 0.096 Uiso 1 1 calc R . . C29 C 0.66152(13) -0.1627(2) 0.08753(11) 0.0563(7) Uani 1 1 d . . . H29A H 0.6622 -0.2218 0.1152 0.084 Uiso 1 1 calc R . . H29B H 0.6473 -0.1890 0.0494 0.084 Uiso 1 1 calc R . . H29C H 0.6293 -0.1083 0.1008 0.084 Uiso 1 1 calc R . . Cl1 Cl 1.04083(4) 0.10439(6) 0.41801(3) 0.0660(2) Uani 1 1 d . . . Cl2 Cl 0.96443(4) 0.40818(7) 0.26025(4) 0.0829(3) Uani 1 1 d . . . F1 F 0.71049(7) 0.42549(10) 0.39251(6) 0.0570(4) Uani 1 1 d . . . F2 F 0.49555(7) 0.29565(17) 0.45463(8) 0.0936(6) Uani 1 1 d . . . N1 N 0.94945(8) 0.27790(14) 0.37115(7) 0.0372(4) Uani 1 1 d . . . N2 N 0.76001(8) 0.13652(13) 0.32476(7) 0.0348(4) Uani 1 1 d . . . N3 N 0.74882(9) -0.05055(13) 0.13829(7) 0.0356(4) Uani 1 1 d . . . O1 O 1.01355(9) 0.39576(15) 0.42575(8) 0.0620(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0404(13) 0.0446(12) 0.0411(12) -0.0083(10) -0.0019(10) -0.0013(10) C2 0.0451(13) 0.0465(13) 0.0363(12) -0.0124(10) 0.0006(10) 0.0020(10) C3 0.0397(12) 0.0435(12) 0.0292(11) -0.0037(9) 0.0045(9) 0.0043(10) C4 0.0336(11) 0.0333(10) 0.0291(10) 0.0019(9) 0.0014(8) 0.0049(9) C5 0.0335(11) 0.0340(11) 0.0288(10) 0.0040(9) 0.0008(8) 0.0057(9) C6 0.0358(11) 0.0319(10) 0.0335(11) -0.0010(9) -0.0030(9) 0.0039(9) C7 0.0314(11) 0.0452(12) 0.0362(11) -0.0091(10) 0.0009(9) 0.0048(9) C8 0.0325(11) 0.0357(11) 0.0316(11) -0.0011(9) -0.0002(9) 0.0013(9) C9 0.0278(11) 0.0426(12) 0.0408(12) -0.0096(10) 0.0026(9) -0.0040(9) C10 0.0370(12) 0.0462(13) 0.0387(12) -0.0067(10) -0.0009(9) -0.0038(10) C11 0.0337(12) 0.0523(14) 0.0526(14) -0.0113(11) 0.0016(10) 0.0029(10) C12 0.0385(12) 0.0611(15) 0.0525(15) -0.0144(12) 0.0126(11) -0.0043(11) C13 0.0505(14) 0.0613(15) 0.0421(13) 0.0004(12) 0.0079(11) -0.0088(13) C14 0.0404(13) 0.0480(13) 0.0469(13) -0.0018(11) 0.0000(10) -0.0011(10) C15 0.0326(11) 0.0478(12) 0.0280(10) 0.0025(9) -0.0002(8) 0.0047(9) C16 0.0423(13) 0.0486(13) 0.0331(11) 0.0003(10) 0.0009(10) 0.0062(11) C17 0.0525(15) 0.0720(17) 0.0407(13) -0.0071(12) 0.0003(11) 0.0263(14) C18 0.0326(13) 0.102(2) 0.0473(15) -0.0045(15) 0.0047(11) 0.0094(15) C19 0.0404(14) 0.085(2) 0.0588(16) 0.0043(15) 0.0077(12) -0.0067(14) C20 0.0383(13) 0.0633(16) 0.0467(14) 0.0009(12) 0.0027(10) -0.0024(11) C21 0.0536(14) 0.0457(13) 0.0409(13) -0.0066(10) 0.0043(10) -0.0153(11) C22 0.0576(16) 0.0582(15) 0.0420(13) -0.0094(11) 0.0081(11) -0.0135(12) C23 0.0354(11) 0.0357(11) 0.0375(12) -0.0049(9) -0.0040(9) 0.0064(9) C24 0.0531(13) 0.0380(12) 0.0324(11) 0.0029(9) -0.0034(10) -0.0064(10) C25 0.0541(14) 0.0364(12) 0.0371(12) 0.0017(9) -0.0082(10) -0.0032(10) C26 0.0508(14) 0.0395(12) 0.0328(11) -0.0040(9) -0.0062(10) 0.0025(10) C27 0.0671(17) 0.0555(15) 0.0495(14) -0.0172(12) -0.0052(12) 0.0105(13) C28 0.095(2) 0.0600(16) 0.0373(13) 0.0035(12) -0.0114(13) -0.0029(15) C29 0.0583(16) 0.0622(16) 0.0483(14) -0.0090(12) -0.0150(12) -0.0053(13) Cl1 0.0683(5) 0.0792(5) 0.0506(4) 0.0137(3) 0.0075(3) 0.0169(4) Cl2 0.0812(5) 0.0849(5) 0.0825(6) 0.0284(4) 0.0095(4) 0.0296(4) F1 0.0657(9) 0.0470(8) 0.0582(9) 0.0047(7) 0.0085(7) 0.0081(7) F2 0.0380(8) 0.1555(17) 0.0873(12) -0.0112(12) 0.0166(8) 0.0196(10) N1 0.0292(9) 0.0453(10) 0.0371(10) -0.0114(8) 0.0019(7) 0.0001(8) N2 0.0326(9) 0.0372(9) 0.0345(9) -0.0002(8) -0.0012(7) 0.0036(7) N3 0.0428(10) 0.0332(9) 0.0309(9) -0.0002(7) -0.0012(7) -0.0034(8) O1 0.0429(10) 0.0744(12) 0.0686(12) -0.0318(10) 0.0037(8) -0.0144(9) _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 O1 1.212(2) . ? C1 N1 1.400(3) . ? C1 C2 1.448(3) . ? C2 C3 1.340(3) . ? C2 H2 0.9300 . ? C3 C4 1.436(3) . ? C3 H3 0.9300 . ? C4 C8 1.403(3) . ? C4 C5 1.408(3) . ? C5 N2 1.338(2) . ? C5 C15 1.498(3) . ? C6 N2 1.341(2) . ? C6 C7 1.377(3) . ? C6 C23 1.513(3) . ? C7 C8 1.386(3) . ? C7 H7 0.9300 . ? C8 N1 1.392(2) . ? C9 C10 1.384(3) . ? C9 C14 1.385(3) . ? C9 N1 1.433(2) . ? C10 C11 1.382(3) . ? C10 Cl1 1.730(2) . ? C11 C12 1.369(3) . ? C11 H11 0.9300 . ? C12 C13 1.375(3) . ? C12 H12 0.9300 . ? C13 C14 1.382(3) . ? C13 H13 0.9300 . ? C14 Cl2 1.727(2) . ? C15 C16 1.378(3) . ? C15 C20 1.392(3) . ? C16 F1 1.347(2) . ? C16 C17 1.379(3) . ? C17 C18 1.367(4) . ? C17 H17 0.9300 . ? C18 F2 1.350(3) . ? C18 C19 1.358(4) . ? C19 C20 1.383(3) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.514(3) . ? C21 C23 1.521(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N3 1.457(3) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.521(3) . ? C23 H23 0.9800 . ? C24 C25 1.518(3) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N3 1.462(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N3 1.498(3) . ? C26 C29 1.526(3) . ? C26 C28 1.528(3) . ? C26 C27 1.532(3) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 N1 120.38(19) . . ? O1 C1 C2 125.3(2) . . ? N1 C1 C2 114.27(18) . . ? C3 C2 C1 122.87(19) . . ? C3 C2 H2 118.6 . . ? C1 C2 H2 118.6 . . ? C2 C3 C4 121.17(19) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C8 C4 C5 116.83(17) . . ? C8 C4 C3 117.64(18) . . ? C5 C4 C3 125.49(18) . . ? N2 C5 C4 123.23(17) . . ? N2 C5 C15 113.03(17) . . ? C4 C5 C15 123.74(18) . . ? N2 C6 C7 122.30(18) . . ? N2 C6 C23 118.34(17) . . ? C7 C6 C23 119.22(18) . . ? C6 C7 C8 119.59(18) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? C7 C8 N1 121.39(17) . . ? C7 C8 C4 119.25(18) . . ? N1 C8 C4 119.36(17) . . ? C10 C9 C14 118.28(19) . . ? C10 C9 N1 120.65(19) . . ? C14 C9 N1 120.83(19) . . ? C11 C10 C9 121.6(2) . . ? C11 C10 Cl1 119.66(18) . . ? C9 C10 Cl1 118.73(16) . . ? C12 C11 C10 118.8(2) . . ? C12 C11 H11 120.6 . . ? C10 C11 H11 120.6 . . ? C11 C12 C13 121.0(2) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C14 119.6(2) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C9 120.6(2) . . ? C13 C14 Cl2 119.79(19) . . ? C9 C14 Cl2 119.58(17) . . ? C16 C15 C20 116.39(19) . . ? C16 C15 C5 124.55(19) . . ? C20 C15 C5 118.86(19) . . ? F1 C16 C15 119.72(19) . . ? F1 C16 C17 116.9(2) . . ? C15 C16 C17 123.3(2) . . ? C18 C17 C16 117.1(2) . . ? C18 C17 H17 121.4 . . ? C16 C17 H17 121.4 . . ? F2 C18 C19 119.4(3) . . ? F2 C18 C17 117.6(3) . . ? C19 C18 C17 122.9(2) . . ? C18 C19 C20 118.3(3) . . ? C18 C19 H19 120.9 . . ? C20 C19 H19 120.9 . . ? C19 C20 C15 121.9(2) . . ? C19 C20 H20 119.1 . . ? C15 C20 H20 119.1 . . ? C22 C21 C23 111.88(18) . . ? C22 C21 H21A 109.2 . . ? C23 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C23 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N3 C22 C21 110.39(18) . . ? N3 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? N3 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C6 C23 C21 109.47(16) . . ? C6 C23 C24 115.45(17) . . ? C21 C23 C24 108.82(17) . . ? C6 C23 H23 107.6 . . ? C21 C23 H23 107.6 . . ? C24 C23 H23 107.6 . . ? C25 C24 C23 111.88(18) . . ? C25 C24 H24A 109.2 . . ? C23 C24 H24A 109.2 . . ? C25 C24 H24B 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? N3 C25 C24 111.66(17) . . ? N3 C25 H25A 109.3 . . ? C24 C25 H25A 109.3 . . ? N3 C25 H25B 109.3 . . ? C24 C25 H25B 109.3 . . ? H25A C25 H25B 107.9 . . ? N3 C26 C29 108.72(17) . . ? N3 C26 C28 108.64(17) . . ? C29 C26 C28 107.14(19) . . ? N3 C26 C27 113.20(17) . . ? C29 C26 C27 109.80(19) . . ? C28 C26 C27 109.1(2) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C8 N1 C1 124.23(17) . . ? C8 N1 C9 117.48(16) . . ? C1 N1 C9 118.29(16) . . ? C5 N2 C6 118.60(17) . . ? C22 N3 C25 108.46(17) . . ? C22 N3 C26 113.69(16) . . ? C25 N3 C26 113.77(16) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.42 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.345 _refine_diff_density_min -0.230 _refine_diff_density_rms 0.042