#------------------------------------------------------------------------------ #$Date: 2013-12-28 13:58:47 +0000 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/25/2202563.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202563 loop_ _publ_author_name '\,Samil I\,s\?ik' 'B. Can Olcay' 'Ay\,sen A\~gar' 'Selami \,Sa\,smaz' _publ_section_title 3-Phenyl-5-p-tolyl-4-(3,4,5-trimethoxybenzylamino)-4H-1,2,4-triazole _journal_issue 10 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first o1535 _journal_page_last o1537 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac 'C25 H25 N4 O3' _chemical_formula_moiety 'C25 H25 N4 O3' _chemical_formula_sum 'C25 H25 N4 O3' _chemical_formula_weight 430.51 _chemical_name_systematic ; 3-Phenyl-5-p-tolyl-4-(3,4,5-trimethoxybenzylamino)-4H-1,2,4-triazole ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 97.336(5) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 13.2141(9) _cell_length_b 9.8945(5) _cell_length_c 17.8861(12) _cell_measurement_reflns_used 22255 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.31 _cell_measurement_theta_min 1.76 _cell_volume 2319.4(3) _computing_cell_refinement X-AREA _computing_data_collection 'X-AREA (Stoe & Cie, 2002)' _computing_data_reduction 'X-RED (Stoe & Cie, 2002)' _computing_molecular_graphics 'ORTEPIII (Burnett & Johnson, 1996)' _computing_publication_material 'WinGX (Farrugia, 1997) and PARST (Nardelli, 1995)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 293 _diffrn_detector_area_resol_mean 6.67 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'Stoe IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_radiation_monochromator 'plane graphite' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 6461 _diffrn_reflns_theta_full 29.57 _diffrn_reflns_theta_max 29.57 _diffrn_reflns_theta_min 1.81 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_T_max 0.9816 _exptl_absorpt_correction_T_min 0.9282 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details '(X-RED; Stoe & Cie, 2002)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prismatic _exptl_crystal_F_000 912 _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.513 _exptl_crystal_size_min 0.230 _refine_diff_density_max 0.877 _refine_diff_density_min -0.308 _refine_ls_extinction_coef 0.013(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL97 _refine_ls_goodness_of_fit_ref 0.834 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 298 _refine_ls_number_reflns 6461 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.834 _refine_ls_R_factor_all 0.1180 _refine_ls_R_factor_gt 0.0699 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.1262P)^2^] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2076 _refine_ls_wR_factor_ref 0.2244 _reflns_number_gt 2717 _reflns_number_total 6461 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file cv6212.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'P 21/n' _cod_database_code 2202563 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' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol O2 0.25690(13) 0.16742(16) 0.48652(10) 0.0744(5) Uani d . 1 . . O N4 0.62928(15) 0.45658(17) 0.68185(11) 0.0607(5) Uani d . 1 . . N C22 0.52370(17) 0.2735(2) 0.51896(13) 0.0608(6) Uani d . 1 . . C H22 0.5864 0.2493 0.5045 0.073 Uiso calc R 1 . . H N1 0.63392(15) 0.32612(17) 0.71356(10) 0.0615(5) Uani d . 1 . . N C18 0.42537(17) 0.4140(2) 0.59168(12) 0.0591(6) Uani d . 1 . . C H18 0.4218 0.4849 0.6254 0.071 Uiso calc R 1 . . H C19 0.33795(17) 0.3437(2) 0.56356(12) 0.0595(6) Uani d . 1 . . C O1 0.24276(13) 0.3728(2) 0.58098(11) 0.0835(6) Uani d . 1 . . O C2 0.6967(2) 0.2220(2) 0.70312(14) 0.0677(7) Uani d . 1 . . C C16 0.61322(17) 0.4546(2) 0.59876(13) 0.0604(6) Uani d . 1 . . C H16A 0.6717 0.4129 0.5803 0.073 Uiso calc R 1 . . H H16B 0.6078 0.5466 0.5800 0.073 Uiso calc R 1 . . H C17 0.51815(17) 0.3777(2) 0.56914(12) 0.0551(5) Uani d . 1 . . C C20 0.34343(17) 0.2381(2) 0.51345(12) 0.0607(6) Uani d . 1 . . C O3 0.43324(16) 0.10241(19) 0.43842(12) 0.0876(6) Uani d . 1 . . O N2 0.6684(2) 0.1144(2) 0.73602(14) 0.0869(8) Uani d . 1 . . N C9 0.7788(2) 0.2302(2) 0.65563(15) 0.0733(8) Uani d . 1 . . C C21 0.43630(19) 0.2045(2) 0.48992(13) 0.0636(6) Uani d . 1 . . C C14 0.7786(2) 0.1369(3) 0.59801(17) 0.0802(8) Uani d . 1 . . C H14 0.7306 0.0677 0.5926 0.096 Uiso calc R 1 . . H C1 0.5619(2) 0.2733(2) 0.75425(13) 0.0717(7) Uani d . 1 . . C C3 0.4748(2) 0.3446(3) 0.77930(14) 0.0728(7) Uani d . 1 . . C N3 0.5824(2) 0.1469(2) 0.76896(14) 0.0860(7) Uani d . 1 . . N C10 0.8525(2) 0.3299(3) 0.66486(17) 0.0783(8) Uani d . 1 . . C H10 0.8549 0.3901 0.7050 0.094 Uiso calc R 1 . . H C24 0.2068(2) 0.2208(3) 0.41775(16) 0.0879(9) Uani d . 1 . . C H24A 0.1881 0.3131 0.4252 0.132 Uiso calc R 1 . . H H24B 0.1466 0.1687 0.4019 0.132 Uiso calc R 1 . . H H24C 0.2520 0.2166 0.3798 0.132 Uiso calc R 1 . . H C8 0.4784(2) 0.4780(3) 0.80062(16) 0.0865(8) Uani d . 1 . . C H8 0.5377 0.5276 0.7981 0.104 Uiso calc R 1 . . H C11 0.9219(3) 0.3394(3) 0.6148(2) 0.0962(10) Uani d . 1 . . C H11 0.9702 0.4083 0.6200 0.115 Uiso calc R 1 . . H C13 0.8485(3) 0.1475(3) 0.5499(2) 0.0937(10) Uani d . 1 . . C H13 0.8470 0.0846 0.5111 0.112 Uiso calc R 1 . . H C12 0.9211(2) 0.2451(4) 0.55498(19) 0.0934(9) Uani d . 1 . . C C7 0.3953(3) 0.5391(4) 0.8257(2) 0.1018(10) Uani d . 1 . . C H7 0.3993 0.6294 0.8402 0.122 Uiso calc R 1 . . H C25 0.5190(3) 0.0838(4) 0.3990(2) 0.1072(11) Uani d . 1 . . C H25A 0.5337 0.1668 0.3747 0.161 Uiso calc R 1 . . H H25B 0.5044 0.0143 0.3618 0.161 Uiso calc R 1 . . H H25C 0.5770 0.0579 0.4340 0.161 Uiso calc R 1 . . H C23 0.2293(2) 0.4968(4) 0.6155(2) 0.1058(11) Uani d . 1 . . C H23A 0.2643 0.4957 0.6660 0.159 Uiso calc R 1 . . H H23B 0.1579 0.5123 0.6170 0.159 Uiso calc R 1 . . H H23C 0.2566 0.5677 0.5874 0.159 Uiso calc R 1 . . H C15 0.9943(3) 0.2586(6) 0.5039(3) 0.1458(17) Uani d . 1 . . C H15A 0.9710 0.2111 0.4581 0.219 Uiso calc R 1 . . H H15B 1.0582 0.2213 0.5260 0.219 Uiso calc R 1 . . H H15C 1.0031 0.3525 0.4929 0.219 Uiso calc R 1 . . H C6 0.3059(3) 0.4683(5) 0.8297(2) 0.1191(13) Uani d . 1 . . C H6 0.2496 0.5098 0.8462 0.143 Uiso calc R 1 . . H C4 0.3851(3) 0.2734(4) 0.7833(2) 0.1094(12) Uani d . 1 . . C H4 0.3804 0.1831 0.7687 0.131 Uiso calc R 1 . . H C5 0.3031(3) 0.3367(6) 0.8089(3) 0.1358(17) Uani d . 1 . . C H5 0.2439 0.2874 0.8119 0.163 Uiso calc R 1 . . H H4N 0.6789(18) 0.498(2) 0.7003(13) 0.058(7) Uiso d . 1 . . H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O2 0.0726(10) 0.0734(10) 0.0704(10) -0.0228(8) -0.0170(8) 0.0003(8) N4 0.0663(12) 0.0408(8) 0.0680(12) -0.0070(8) -0.0189(9) 0.0044(8) C22 0.0616(13) 0.0562(12) 0.0609(13) 0.0027(10) -0.0071(10) 0.0054(10) N1 0.0741(12) 0.0462(9) 0.0559(10) -0.0023(9) -0.0232(9) 0.0039(8) C18 0.0633(14) 0.0561(12) 0.0531(12) -0.0043(10) -0.0106(10) 0.0006(9) C19 0.0571(13) 0.0660(13) 0.0519(12) -0.0062(10) -0.0062(10) 0.0035(10) O1 0.0602(11) 0.1040(14) 0.0845(12) -0.0097(9) 0.0027(9) -0.0231(11) C2 0.0825(16) 0.0505(12) 0.0620(14) 0.0007(11) -0.0217(12) -0.0002(10) C16 0.0605(12) 0.0536(11) 0.0622(13) -0.0038(9) -0.0114(10) 0.0132(10) C17 0.0611(13) 0.0494(10) 0.0499(11) -0.0035(9) -0.0115(9) 0.0122(9) C20 0.0676(14) 0.0544(12) 0.0544(12) -0.0112(10) -0.0141(10) 0.0055(10) O3 0.0951(14) 0.0739(11) 0.0887(13) -0.0013(10) -0.0074(11) -0.0266(10) N2 0.122(2) 0.0501(11) 0.0776(14) -0.0038(12) -0.0274(14) 0.0154(10) C9 0.0883(17) 0.0445(11) 0.0757(16) 0.0110(11) -0.0331(14) -0.0088(11) C21 0.0740(15) 0.0516(12) 0.0601(13) 0.0000(10) -0.0113(11) 0.0003(10) C14 0.0867(19) 0.0688(15) 0.0784(18) 0.0085(14) -0.0154(15) -0.0112(13) C1 0.0953(18) 0.0580(13) 0.0538(13) -0.0216(13) -0.0209(12) 0.0162(10) C3 0.0805(17) 0.0750(16) 0.0576(13) -0.0075(13) -0.0120(12) 0.0160(12) N3 0.1095(19) 0.0677(14) 0.0755(15) -0.0045(13) -0.0083(14) 0.0185(11) C10 0.0756(17) 0.0673(15) 0.0882(19) 0.0058(12) -0.0036(15) -0.0190(13) C24 0.0788(17) 0.102(2) 0.0744(17) -0.0102(15) -0.0242(14) -0.0024(15) C8 0.0842(19) 0.096(2) 0.0724(17) -0.0120(16) -0.0156(14) 0.0001(15) C11 0.085(2) 0.0848(19) 0.114(3) 0.0015(15) -0.0061(19) -0.0155(18) C13 0.096(2) 0.0820(19) 0.094(2) 0.0068(16) -0.0239(18) -0.0206(16) C12 0.0733(18) 0.122(3) 0.085(2) 0.0187(18) 0.0107(15) 0.0006(18) C7 0.086(2) 0.117(3) 0.098(2) 0.005(2) -0.0085(18) -0.003(2) C25 0.123(3) 0.102(2) 0.099(2) 0.006(2) 0.020(2) -0.0332(19) C23 0.0744(19) 0.126(3) 0.115(3) 0.0066(18) 0.0064(17) -0.032(2) C15 0.100(3) 0.203(5) 0.135(3) -0.007(3) 0.016(3) -0.004(4) C6 0.122(3) 0.126(3) 0.104(3) -0.008(3) -0.003(2) 0.035(2) C4 0.124(3) 0.092(2) 0.110(3) -0.034(2) 0.005(2) 0.0335(19) C5 0.093(3) 0.162(4) 0.158(4) -0.013(3) 0.037(3) 0.056(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O2 C20 . 1.374(2) ? O2 C24 . 1.422(3) ? N4 N1 . 1.408(2) yes N4 C16 . 1.474(3) yes N4 H4N . 0.81(2) ? C22 C17 . 1.375(3) ? C22 C21 . 1.384(3) ? C22 H22 . 0.9300 ? N1 C2 . 1.351(3) yes N1 C1 . 1.373(3) yes C18 C17 . 1.386(3) ? C18 C19 . 1.387(3) ? C18 H18 . 0.9300 ? C19 O1 . 1.365(3) ? C19 C20 . 1.385(3) ? O1 C23 . 1.395(4) ? C2 N2 . 1.295(3) yes C2 C9 . 1.462(4) ? C16 C17 . 1.506(3) ? C16 H16A . 0.9700 ? C16 H16B . 0.9700 ? C20 C21 . 1.388(4) ? O3 C21 . 1.365(3) ? O3 C25 . 1.421(4) ? N2 N3 . 1.382(4) yes C9 C10 . 1.382(4) ? C9 C14 . 1.383(4) ? C14 C13 . 1.346(5) ? C14 H14 . 0.9300 ? C1 N3 . 1.300(3) yes C1 C3 . 1.468(4) ? C3 C8 . 1.372(4) ? C3 C4 . 1.388(4) ? C10 C11 . 1.364(5) ? C10 H10 . 0.9300 ? C24 H24A . 0.9600 ? C24 H24B . 0.9600 ? C24 H24C . 0.9600 ? C8 C7 . 1.379(5) ? C8 H8 . 0.9300 ? C11 C12 . 1.419(5) ? C11 H11 . 0.9300 ? C13 C12 . 1.356(5) ? C13 H13 . 0.9300 ? C12 C15 . 1.419(5) ? C7 C6 . 1.382(5) ? C7 H7 . 0.9300 ? C25 H25A . 0.9600 ? C25 H25B . 0.9600 ? C25 H25C . 0.9600 ? C23 H23A . 0.9600 ? C23 H23B . 0.9600 ? C23 H23C . 0.9600 ? C15 H15A . 0.9600 ? C15 H15B . 0.9600 ? C15 H15C . 0.9600 ? C6 C5 . 1.353(6) ? C6 H6 . 0.9300 ? C4 C5 . 1.380(6) ? C4 H4 . 0.9300 ? C5 H5 . 0.9300 ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C20 O2 C24 112.87(19) N1 N4 C16 112.76(16) N1 N4 H4N 108.0(16) C16 N4 H4N 115.1(17) C17 C22 C21 120.2(2) C17 C22 H22 119.9 C21 C22 H22 119.9 C2 N1 C1 105.2(2) C2 N1 N4 129.7(2) C1 N1 N4 124.4(2) C17 C18 C19 119.4(2) C17 C18 H18 120.3 C19 C18 H18 120.3 O1 C19 C20 115.64(19) O1 C19 C18 124.1(2) C20 C19 C18 120.2(2) C19 O1 C23 117.4(2) N2 C2 N1 110.2(3) N2 C2 C9 126.0(2) N1 C2 C9 123.5(2) N4 C16 C17 111.57(19) N4 C16 H16A 109.3 C17 C16 H16A 109.3 N4 C16 H16B 109.3 C17 C16 H16B 109.3 H16A C16 H16B 108.0 C22 C17 C18 120.5(2) C22 C17 C16 119.8(2) C18 C17 C16 119.7(2) O2 C20 C19 120.1(2) O2 C20 C21 120.0(2) C19 C20 C21 119.9(2) C21 O3 C25 118.3(2) C2 N2 N3 107.7(2) C10 C9 C14 120.0(3) C10 C9 C2 122.3(2) C14 C9 C2 117.7(3) O3 C21 C22 124.7(2) O3 C21 C20 115.5(2) C22 C21 C20 119.7(2) C13 C14 C9 119.3(3) C13 C14 H14 120.4 C9 C14 H14 120.4 N3 C1 N1 109.4(3) N3 C1 C3 123.5(3) N1 C1 C3 127.0(2) C8 C3 C4 118.3(3) C8 C3 C1 123.1(3) C4 C3 C1 118.6(3) C1 N3 N2 107.4(2) C11 C10 C9 119.6(3) C11 C10 H10 120.2 C9 C10 H10 120.2 O2 C24 H24A 109.5 O2 C24 H24B 109.5 H24A C24 H24B 109.5 O2 C24 H24C 109.5 H24A C24 H24C 109.5 H24B C24 H24C 109.5 C3 C8 C7 120.7(3) C3 C8 H8 119.6 C7 C8 H8 119.6 C10 C11 C12 120.6(3) C10 C11 H11 119.7 C12 C11 H11 119.7 C14 C13 C12 123.4(3) C14 C13 H13 118.3 C12 C13 H13 118.3 C13 C12 C15 123.9(4) C13 C12 C11 117.1(3) C15 C12 C11 118.9(4) C8 C7 C6 121.1(4) C8 C7 H7 119.5 C6 C7 H7 119.5 O3 C25 H25A 109.5 O3 C25 H25B 109.5 H25A C25 H25B 109.5 O3 C25 H25C 109.5 H25A C25 H25C 109.5 H25B C25 H25C 109.5 O1 C23 H23A 109.5 O1 C23 H23B 109.5 H23A C23 H23B 109.5 O1 C23 H23C 109.5 H23A C23 H23C 109.5 H23B C23 H23C 109.5 C12 C15 H15A 109.5 C12 C15 H15B 109.5 H15A C15 H15B 109.5 C12 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C5 C6 C7 117.9(4) C5 C6 H6 121.1 C7 C6 H6 121.1 C5 C4 C3 119.8(4) C5 C4 H4 120.1 C3 C4 H4 120.1 C6 C5 C4 122.2(4) C6 C5 H5 118.9 C4 C5 H5 118.9 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA N4 H4N N2 2_656 0.81(2) 2.47(2) 3.277(3) 176.0(10) C10 H10 N2 2_656 0.93 2.49 3.357(4) 155 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_publ_flag C16 N4 N1 C2 57.1(3) ? C16 N4 N1 C1 -112.4(2) ? C17 C18 C19 O1 -178.7(2) ? C17 C18 C19 C20 0.0(3) ? C20 C19 O1 C23 -164.5(2) ? C18 C19 O1 C23 14.3(4) ? C1 N1 C2 N2 -1.6(2) ? N4 N1 C2 N2 -172.65(19) ? C1 N1 C2 C9 173.51(19) ? N4 N1 C2 C9 2.5(3) ? N1 N4 C16 C17 56.6(3) yes C21 C22 C17 C18 0.6(3) ? C21 C22 C17 C16 -178.32(19) ? C19 C18 C17 C22 0.4(3) ? C19 C18 C17 C16 179.33(19) ? N4 C16 C17 C22 -125.8(2) ? N4 C16 C17 C18 55.3(2) ? C24 O2 C20 C19 92.0(3) ? C24 O2 C20 C21 -87.4(3) ? O1 C19 C20 O2 -2.0(3) ? C18 C19 C20 O2 179.09(19) ? O1 C19 C20 C21 177.4(2) ? C18 C19 C20 C21 -1.5(3) ? N1 C2 N2 N3 0.8(3) ? C9 C2 N2 N3 -174.1(2) ? N2 C2 C9 C10 -132.2(3) ? N1 C2 C9 C10 53.5(3) ? N2 C2 C9 C14 50.4(3) ? N1 C2 C9 C14 -124.0(2) ? C25 O3 C21 C22 -14.6(4) ? C25 O3 C21 C20 165.6(3) ? C17 C22 C21 O3 178.1(2) ? C17 C22 C21 C20 -2.0(3) ? O2 C20 C21 O3 1.7(3) ? C19 C20 C21 O3 -177.7(2) ? O2 C20 C21 C22 -178.10(19) ? C19 C20 C21 C22 2.5(3) ? C10 C9 C14 C13 -2.3(4) ? C2 C9 C14 C13 175.2(2) ? C2 N1 C1 N3 1.8(2) ? N4 N1 C1 N3 173.45(19) ? C2 N1 C1 C3 -178.9(2) ? N4 N1 C1 C3 -7.2(3) ? N3 C1 C3 C8 144.5(3) ? N1 C1 C3 C8 -34.8(3) ? N3 C1 C3 C4 -34.1(4) ? N1 C1 C3 C4 146.7(3) ? N1 C1 N3 N2 -1.3(3) ? C3 C1 N3 N2 179.3(2) ? C2 N2 N3 C1 0.3(3) ? C14 C9 C10 C11 3.1(4) ? C2 C9 C10 C11 -174.4(2) ? C4 C3 C8 C7 0.4(4) ? C1 C3 C8 C7 -178.2(3) ? C9 C10 C11 C12 -2.2(4) ? C9 C14 C13 C12 0.7(4) ? C14 C13 C12 C15 -178.9(4) ? C14 C13 C12 C11 0.2(5) ? C10 C11 C12 C13 0.6(5) ? C10 C11 C12 C15 179.7(4) ? C3 C8 C7 C6 -0.4(5) ? C8 C7 C6 C5 0.6(6) ? C8 C3 C4 C5 -0.6(5) ? C1 C3 C4 C5 178.0(3) ? C7 C6 C5 C4 -0.9(6) ? C3 C4 C5 C6 0.9(6) ? _cod_database_fobs_code 2202563 _journal_paper_doi 10.1107/S1600536803017148