Supplementary Material (ESI) for Journal of Materials Chemistry This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 1145 _publ_requested_journal 'Journal Materials Chemistry' loop_ _publ_author_name 'D'Iorio, Marie' 'Pang, Jun' 'Tao, Ye' 'Wang, Suning' 'Yang, Xiao-Ping' _publ_contact_author_name 'Prof Suning Wang' _publ_contact_author_address ; Department of Chemistry Queen's University Kingston Ontario K7L 3N6 CANADA ; _publ_contact_author_email 'WANGS@CHEM.QUEENSU.CA' _publ_section_title ; Syntheses, structrures, and electroluminescence of new blue luminescent star-shaped compounds based on 1,3 5-triazine and 1,3,5-trisubstituted benzene ; data_pang1 _database_code_CSD 166363 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H18 N6' _chemical_formula_weight 390.44 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.675(3) _cell_length_b 11.170(2) _cell_length_c 20.954(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.638(3) _cell_angle_gamma 90.00 _cell_volume 2924.7(10) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max .1 _exptl_crystal_size_mid .4 _exptl_crystal_size_min .5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 0.083 _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 293(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 20846 _diffrn_reflns_av_R_equivalents 0.0600 _diffrn_reflns_av_sigmaI/netI 0.1372 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 28.34 _reflns_number_total 6976 _reflns_number_gt 2452 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0280P)^2^+0.0000P] 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 6976 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1602 _refine_ls_R_factor_gt 0.0426 _refine_ls_wR_factor_ref 0.0872 _refine_ls_wR_factor_gt 0.0693 _refine_ls_goodness_of_fit_ref 0.772 _refine_ls_restrained_S_all 0.772 _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 0.21517(16) 0.58585(15) 0.55805(10) 0.0675(6) Uani 1 1 d . . . N2 N 0.24137(13) 0.50889(13) 0.45822(8) 0.0440(4) Uani 1 1 d . . . N3 N 0.40449(15) 0.40963(14) 0.46291(9) 0.0567(5) Uani 1 1 d . . . N4 N 0.36102(16) 0.94536(16) 0.23079(10) 0.0731(6) Uani 1 1 d . . . N5 N 0.31593(13) 0.83318(12) 0.31750(8) 0.0479(5) Uani 1 1 d . . . N6 N 0.33320(13) 1.02491(14) 0.36075(9) 0.0547(5) Uani 1 1 d . . . N7 N 0.06863(15) 0.33841(15) 0.25423(9) 0.0583(5) Uani 1 1 d . . . N8 N 0.21409(13) 0.44486(13) 0.22541(8) 0.0449(5) Uani 1 1 d . . . N9 N 0.16778(15) 0.47919(15) 0.11545(10) 0.0624(5) Uani 1 1 d . . . C1 C 0.0853(2) 0.6293(2) 0.46544(16) 0.0696(8) Uani 1 1 d . . . C2 C 0.0277(3) 0.6952(3) 0.5024(2) 0.0921(10) Uani 1 1 d . . . C3 C 0.0640(3) 0.7046(3) 0.5673(2) 0.0976(12) Uani 1 1 d . . . C4 C 0.1562(3) 0.6499(2) 0.59327(16) 0.0879(10) Uani 1 1 d . . . C5 C 0.17862(19) 0.57504(17) 0.49520(12) 0.0475(6) Uani 1 1 d . . . C6 C 0.2893(2) 0.34594(19) 0.53414(11) 0.0535(7) Uani 1 1 d . . . C7 C 0.3614(2) 0.2619(2) 0.55933(13) 0.0645(7) Uani 1 1 d . . . C8 C 0.4560(2) 0.2500(2) 0.53732(13) 0.0638(7) Uani 1 1 d . . . C9 C 0.4752(2) 0.3236(2) 0.48913(13) 0.0627(7) Uani 1 1 d . . . C10 C 0.31361(17) 0.41968(16) 0.48682(10) 0.0409(5) Uani 1 1 d . . . C11 C 0.4664(2) 0.7770(3) 0.26966(15) 0.0522(7) Uani 1 1 d . . . C12 C 0.5275(2) 0.7916(3) 0.22321(18) 0.0840(10) Uani 1 1 d . . . C13 C 0.5094(3) 0.8817(4) 0.18067(17) 0.0918(12) Uani 1 1 d . . . C14 C 0.4274(3) 0.9580(3) 0.18537(14) 0.0847(10) Uani 1 1 d . . . C15 C 0.38425(18) 0.85265(17) 0.27191(10) 0.0453(6) Uani 1 1 d . . . C16 C 0.16665(19) 0.9245(2) 0.35788(11) 0.0490(6) Uani 1 1 d . . . C17 C 0.2892(2) 1.1185(2) 0.38625(12) 0.0624(7) Uani 1 1 d . . . C18 C 0.1885(2) 1.1217(2) 0.39896(12) 0.0624(7) Uani 1 1 d . . . C19 C 0.1249(2) 1.0225(2) 0.38474(11) 0.0564(7) Uani 1 1 d . . . C20 C 0.26985(17) 0.92977(16) 0.34655(9) 0.0411(5) Uani 1 1 d . . . C21 C 0.1858(2) 0.2395(2) 0.19427(13) 0.0647(8) Uani 1 1 d . . . C22 C 0.1267(3) 0.1366(2) 0.19410(17) 0.0907(11) Uani 1 1 d . . . C23 C 0.0396(3) 0.1345(3) 0.22421(16) 0.0840(10) Uani 1 1 d . . . C24 C 0.0142(2) 0.2350(3) 0.25337(14) 0.0736(8) Uani 1 1 d . . . C25 C 0.15405(17) 0.33781(16) 0.22454(10) 0.0421(5) Uani 1 1 d . . . C26A C 0.3475(2) 0.51790(18) 0.16363(13) 0.0502(6) Uani 1 1 d . . . C27 C 0.1947(3) 0.5134(2) 0.05897(14) 0.0782(9) Uani 1 1 d . . . C28 C 0.2944(3) 0.5528(2) 0.05206(15) 0.0742(8) Uani 1 1 d . . . C29 C 0.3729(3) 0.5539(2) 0.10514(14) 0.0607(7) Uani 1 1 d . . . C30 C 0.24460(19) 0.48201(16) 0.16651(11) 0.0439(5) Uani 1 1 d . . . C31 C 0.24901(15) 0.55208(16) 0.39499(10) 0.0389(5) Uani 1 1 d . . . C32 C 0.27765(16) 0.67067(17) 0.38767(11) 0.0424(6) Uani 1 1 d . . . C33 C 0.28275(15) 0.71295(15) 0.32681(11) 0.0393(5) Uani 1 1 d . . . C34 C 0.25793(16) 0.63956(17) 0.27316(11) 0.0401(5) Uani 1 1 d . . . C35 C 0.23332(15) 0.51902(15) 0.28050(10) 0.0378(5) Uani 1 1 d . . . C36 C 0.22923(16) 0.47620(17) 0.34253(10) 0.0400(5) Uani 1 1 d . . . H1 H 0.0673(17) 0.6202(17) 0.4228(10) 0.069(8) Uiso 1 1 d . . . H2 H -0.0307(19) 0.737(2) 0.4801(12) 0.101(10) Uiso 1 1 d . . . H3 H 0.028(2) 0.747(2) 0.5900(12) 0.112(11) Uiso 1 1 d . . . H4 H 0.187(2) 0.651(2) 0.6401(13) 0.110(10) Uiso 1 1 d . . . H6 H 0.2317(16) 0.3562(17) 0.5476(10) 0.060(8) Uiso 1 1 d . . . H7 H 0.3375(17) 0.2122(17) 0.5890(10) 0.084(8) Uiso 1 1 d . . . H8 H 0.5058(16) 0.1873(16) 0.5507(10) 0.073(7) Uiso 1 1 d . . . H9 H 0.5382(17) 0.3174(18) 0.4694(10) 0.090(9) Uiso 1 1 d . . . H11 H 0.4760(17) 0.7291(15) 0.2896(10) 0.038(8) Uiso 1 1 d . . . H12 H 0.5799(17) 0.7371(17) 0.2209(11) 0.079(9) Uiso 1 1 d . . . H13 H 0.549(2) 0.895(2) 0.1432(14) 0.143(12) Uiso 1 1 d . . . H14 H 0.4049(18) 1.0204(19) 0.1580(11) 0.089(9) Uiso 1 1 d . . . H16 H 0.1255(14) 0.8600(14) 0.3485(9) 0.048(6) Uiso 1 1 d . . . H17 H 0.3369(14) 1.1872(15) 0.3957(8) 0.057(6) Uiso 1 1 d . . . H18 H 0.1601(16) 1.1924(17) 0.4177(10) 0.086(8) Uiso 1 1 d . . . H19 H 0.0521(15) 1.0206(15) 0.3916(9) 0.058(7) Uiso 1 1 d . . . H21 H 0.2392(16) 0.2409(18) 0.1756(10) 0.069(9) Uiso 1 1 d . . . H24 H 0.1485(19) 0.080(2) 0.1733(12) 0.095(10) Uiso 1 1 d . . . H23 H 0.0027(17) 0.0634(19) 0.2247(10) 0.092(8) Uiso 1 1 d . . . H22 H -0.0447(19) 0.2386(19) 0.2792(11) 0.107(10) Uiso 1 1 d . . . H30 H 0.3972(14) 0.5155(15) 0.2016(9) 0.046(7) Uiso 1 1 d . . . H27 H 0.1358(18) 0.5098(19) 0.0221(11) 0.099(9) Uiso 1 1 d . . . H28 H 0.3129(15) 0.5759(15) 0.0105(10) 0.070(7) Uiso 1 1 d . . . H29 H 0.4450(18) 0.5767(17) 0.1027(10) 0.084(8) Uiso 1 1 d . . . H32 H 0.2897(12) 0.7183(13) 0.4244(8) 0.035(5) Uiso 1 1 d . . . H34 H 0.2603(12) 0.6703(13) 0.2291(8) 0.039(5) Uiso 1 1 d . . . H36 H 0.2096(13) 0.3929(14) 0.3477(8) 0.053(6) 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 N1 0.0951(16) 0.0644(12) 0.0422(14) -0.0031(11) 0.0094(13) 0.0245(12) N2 0.0505(12) 0.0468(9) 0.0361(11) 0.0024(9) 0.0112(10) 0.0064(9) N3 0.0553(13) 0.0596(12) 0.0543(14) 0.0036(10) 0.0069(11) 0.0013(10) N4 0.0864(16) 0.0697(13) 0.0635(16) 0.0058(12) 0.0132(13) -0.0109(12) N5 0.0592(12) 0.0336(9) 0.0568(13) -0.0031(9) 0.0270(10) -0.0038(9) N6 0.0570(12) 0.0414(10) 0.0660(14) -0.0121(9) 0.0115(11) -0.0089(10) N7 0.0511(13) 0.0676(12) 0.0547(14) 0.0000(10) 0.0039(11) -0.0132(11) N8 0.0597(12) 0.0423(9) 0.0342(12) -0.0065(9) 0.0121(10) -0.0116(9) N9 0.0620(14) 0.0846(13) 0.0389(14) 0.0018(12) 0.0036(12) -0.0015(11) C1 0.056(2) 0.0936(19) 0.059(2) -0.0017(18) 0.0098(18) 0.0132(15) C2 0.068(2) 0.114(2) 0.095(3) 0.002(2) 0.017(2) 0.034(2) C3 0.109(3) 0.098(2) 0.097(3) -0.001(2) 0.050(3) 0.040(2) C4 0.131(3) 0.0799(18) 0.057(2) -0.0037(17) 0.028(2) 0.0420(19) C5 0.0554(16) 0.0467(12) 0.0422(16) 0.0038(12) 0.0135(14) 0.0037(12) C6 0.0640(19) 0.0432(13) 0.0583(19) 0.0097(12) 0.0253(16) 0.0053(14) C7 0.085(2) 0.0519(15) 0.0594(19) 0.0093(14) 0.0199(17) -0.0030(16) C8 0.066(2) 0.0541(15) 0.066(2) 0.0113(14) -0.0050(16) 0.0075(15) C9 0.0525(19) 0.0671(16) 0.066(2) 0.0061(15) 0.0043(16) 0.0096(14) C10 0.0475(15) 0.0378(11) 0.0375(14) -0.0041(10) 0.0067(12) -0.0032(11) C11 0.0504(18) 0.0480(16) 0.060(2) -0.0052(16) 0.0127(16) 0.0031(15) C12 0.057(2) 0.110(3) 0.090(3) -0.042(2) 0.027(2) -0.010(2) C13 0.088(3) 0.137(3) 0.058(2) -0.032(2) 0.035(2) -0.057(3) C14 0.115(3) 0.085(2) 0.053(2) 0.0100(18) 0.010(2) -0.034(2) C15 0.0526(15) 0.0384(11) 0.0465(16) -0.0031(11) 0.0133(13) -0.0070(11) C16 0.0449(16) 0.0467(13) 0.0550(16) -0.0076(12) 0.0073(13) -0.0068(13) C17 0.073(2) 0.0425(13) 0.072(2) -0.0174(13) 0.0130(16) -0.0103(14) C18 0.074(2) 0.0504(15) 0.0639(19) -0.0107(13) 0.0135(16) 0.0114(15) C19 0.0502(17) 0.0632(16) 0.0570(17) -0.0015(13) 0.0127(14) 0.0108(14) C20 0.0486(15) 0.0359(11) 0.0388(14) -0.0009(10) 0.0069(12) 0.0007(11) C21 0.063(2) 0.0480(15) 0.086(2) -0.0234(14) 0.0213(17) -0.0054(14) C22 0.091(3) 0.0520(18) 0.123(3) -0.0278(18) 0.000(2) 0.0005(19) C23 0.088(3) 0.0585(19) 0.093(3) 0.0191(18) -0.022(2) -0.033(2) C24 0.059(2) 0.091(2) 0.067(2) 0.0071(17) -0.0001(16) -0.0292(18) C25 0.0414(14) 0.0431(12) 0.0402(15) 0.0007(11) 0.0020(12) -0.0042(11) C26A 0.0549(18) 0.0479(13) 0.0485(19) -0.0037(13) 0.0111(15) -0.0034(12) C27 0.083(2) 0.107(2) 0.041(2) 0.0039(17) 0.0010(19) 0.0032(19) C28 0.099(3) 0.0791(17) 0.050(2) 0.0122(16) 0.028(2) -0.0028(18) C29 0.067(2) 0.0585(14) 0.062(2) -0.0022(14) 0.0277(18) -0.0058(15) C30 0.0528(16) 0.0387(11) 0.0396(16) -0.0038(11) 0.0061(13) 0.0005(11) C31 0.0419(13) 0.0414(11) 0.0330(14) 0.0030(11) 0.0048(11) 0.0023(10) C32 0.0498(15) 0.0414(12) 0.0362(16) -0.0081(12) 0.0081(12) -0.0005(11) C33 0.0409(13) 0.0347(10) 0.0435(15) -0.0030(11) 0.0110(11) -0.0017(10) C34 0.0469(14) 0.0401(12) 0.0346(15) 0.0020(11) 0.0107(12) 0.0006(10) C35 0.0393(13) 0.0391(11) 0.0351(14) -0.0017(10) 0.0069(11) -0.0008(10) C36 0.0448(14) 0.0332(11) 0.0418(15) 0.0016(11) 0.0066(12) -0.0019(10) _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 C5 1.326(2) . ? N1 C4 1.342(3) . ? N2 C5 1.409(2) . ? N2 C10 1.417(2) . ? N2 C31 1.429(2) . ? N3 C10 1.335(2) . ? N3 C9 1.365(3) . ? N4 C15 1.348(2) . ? N4 C14 1.379(3) . ? N5 C15 1.409(2) . ? N5 C20 1.412(2) . ? N5 C33 1.430(2) . ? N6 C20 1.335(2) . ? N6 C17 1.338(2) . ? N7 C25 1.336(2) . ? N7 C24 1.344(3) . ? N8 C35 1.409(2) . ? N8 C30 1.416(2) . ? N8 C25 1.416(2) . ? N9 C30 1.321(2) . ? N9 C27 1.341(3) . ? C1 C2 1.366(4) . ? C1 C5 1.381(3) . ? C2 C3 1.364(4) . ? C3 C4 1.351(4) . ? C6 C7 1.354(3) . ? C6 C10 1.363(3) . ? C7 C8 1.361(3) . ? C8 C9 1.355(3) . ? C11 C15 1.349(3) . ? C11 C12 1.351(4) . ? C12 C13 1.338(4) . ? C13 C14 1.361(4) . ? C16 C20 1.369(3) . ? C16 C19 1.376(3) . ? C17 C18 1.348(3) . ? C18 C19 1.373(3) . ? C21 C25 1.362(3) . ? C21 C22 1.372(3) . ? C22 C23 1.359(4) . ? C23 C24 1.343(4) . ? C26A C30 1.376(3) . ? C26A C29 1.378(3) . ? C27 C28 1.369(4) . ? C28 C29 1.362(3) . ? C31 C36 1.377(2) . ? C31 C32 1.389(2) . ? C32 C33 1.372(2) . ? C33 C34 1.384(2) . ? C34 C35 1.396(2) . ? C35 C36 1.394(2) . ? 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 C5 N1 C4 117.4(2) . . ? C5 N2 C10 121.38(17) . . ? C5 N2 C31 117.72(16) . . ? C10 N2 C31 119.37(16) . . ? C10 N3 C9 117.2(2) . . ? C15 N4 C14 115.3(2) . . ? C15 N5 C20 121.30(15) . . ? C15 N5 C33 117.73(15) . . ? C20 N5 C33 120.42(16) . . ? C20 N6 C17 115.83(19) . . ? C25 N7 C24 116.3(2) . . ? C35 N8 C30 120.46(16) . . ? C35 N8 C25 121.74(16) . . ? C30 N8 C25 117.45(16) . . ? C30 N9 C27 116.5(2) . . ? C2 C1 C5 118.6(3) . . ? C3 C2 C1 119.0(3) . . ? C4 C3 C2 119.4(3) . . ? N1 C4 C3 123.0(3) . . ? N1 C5 C1 122.6(2) . . ? N1 C5 N2 117.3(2) . . ? C1 C5 N2 120.1(2) . . ? C7 C6 C10 118.8(3) . . ? C6 C7 C8 120.7(3) . . ? C9 C8 C7 118.1(3) . . ? C8 C9 N3 122.7(3) . . ? N3 C10 C6 122.4(2) . . ? N3 C10 N2 115.95(18) . . ? C6 C10 N2 121.6(2) . . ? C15 C11 C12 119.2(3) . . ? C13 C12 C11 121.1(3) . . ? C12 C13 C14 118.1(3) . . ? C13 C14 N4 123.2(3) . . ? N4 C15 C11 123.1(2) . . ? N4 C15 N5 117.3(2) . . ? C11 C15 N5 119.5(2) . . ? C20 C16 C19 118.7(2) . . ? N6 C17 C18 124.9(2) . . ? C17 C18 C19 118.5(2) . . ? C18 C19 C16 118.6(2) . . ? N6 C20 C16 123.48(19) . . ? N6 C20 N5 115.31(18) . . ? C16 C20 N5 121.21(18) . . ? C25 C21 C22 118.3(3) . . ? C23 C22 C21 119.9(3) . . ? C24 C23 C22 118.2(3) . . ? C23 C24 N7 124.2(3) . . ? N7 C25 C21 123.1(2) . . ? N7 C25 N8 117.74(18) . . ? C21 C25 N8 119.1(2) . . ? C30 C26A C29 119.2(3) . . ? N9 C27 C28 124.1(3) . . ? C29 C28 C27 118.5(3) . . ? C28 C29 C26A 118.4(3) . . ? N9 C30 C26A 123.2(2) . . ? N9 C30 N8 115.3(2) . . ? C26A C30 N8 121.5(2) . . ? C36 C31 C32 121.0(2) . . ? C36 C31 N2 120.06(17) . . ? C32 C31 N2 118.95(18) . . ? C33 C32 C31 119.0(2) . . ? C32 C33 C34 120.76(18) . . ? C32 C33 N5 120.71(19) . . ? C34 C33 N5 118.51(18) . . ? C33 C34 C35 120.4(2) . . ? C36 C35 C34 118.52(19) . . ? C36 C35 N8 122.28(17) . . ? C34 C35 N8 119.21(18) . . ? C31 C36 C35 120.18(18) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 28.34 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.130 _refine_diff_density_min -0.140 _refine_diff_density_rms 0.032 data_pang2a _database_code_CSD 166364 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26.40 H18.40 N9.60' _chemical_formula_weight 470.11 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.890(4) _cell_length_b 19.438(6) _cell_length_c 12.707(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.380(6) _cell_angle_gamma 90.00 _cell_volume 2852.3(15) _cell_formula_units_Z 5 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max .05 _exptl_crystal_size_mid .05 _exptl_crystal_size_min .5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 0.088 _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 296(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 20657 _diffrn_reflns_av_R_equivalents 0.2496 _diffrn_reflns_av_sigmaI/netI 0.8612 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 28.43 _reflns_number_total 6762 _reflns_number_gt 1019 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0504P)^2^+0.0000P] 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 6762 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.4086 _refine_ls_R_factor_gt 0.0723 _refine_ls_wR_factor_ref 0.1696 _refine_ls_wR_factor_gt 0.1211 _refine_ls_goodness_of_fit_ref 0.644 _refine_ls_restrained_S_all 0.644 _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 0.0606(6) 0.7105(4) 0.3949(5) 0.085(2) Uani 1 1 d . . . C1 C 0.0471(7) 0.5967(4) 0.3403(7) 0.079(3) Uani 1 1 d . . . H1 H 0.0819 0.5539 0.3478 0.094 Uiso 1 1 calc R . . N2 N 0.2244(5) 0.6454(3) 0.4880(4) 0.0521(17) Uani 1 1 d . . . C2 C -0.0663(8) 0.6057(6) 0.2638(8) 0.127(5) Uani 1 1 d . . . H2 H -0.1075 0.5682 0.2193 0.152 Uiso 1 1 calc R . . C3 C -0.1204(7) 0.6645(6) 0.2499(6) 0.093(4) Uani 1 1 d . . . H3 H -0.1984 0.6695 0.1983 0.112 Uiso 1 1 calc R . . N3 N 0.1816(4) 0.6289(3) 0.6460(4) 0.0612(19) Uani 1 1 d . . . C4 C -0.0551(8) 0.7180(5) 0.3157(7) 0.103(3) Uani 1 1 d . . . H4 H -0.0894 0.7610 0.3072 0.123 Uiso 1 1 calc R . . N4 N 0.6897(5) 0.6161(3) 0.7909(6) 0.073(2) Uani 1 1 d . . . N5 N 0.6115(5) 0.6271(3) 0.5858(4) 0.0501(17) Uani 1 1 d . . . C5 C 0.1076(7) 0.6497(5) 0.4041(6) 0.049(2) Uani 1 1 d . . . C6 C 0.3332(6) 0.7083(4) 0.6739(6) 0.068(2) Uani 1 1 d . . . H6 H 0.3756 0.7318 0.6423 0.081 Uiso 1 1 calc R . . N6 N 0.7953(6) 0.6550(3) 0.6103(4) 0.0576(18) Uani 1 1 d . . . N7 N 0.4491(5) 0.6183(3) 0.1045(4) 0.0577(18) Uani 1 1 d . . . C7 C 0.3519(6) 0.7191(4) 0.7891(6) 0.077(3) Uani 1 1 d . . . H7 H 0.4107 0.7484 0.8378 0.093 Uiso 1 1 calc R . . C8 C 0.2829(8) 0.6862(5) 0.8311(7) 0.083(3) Uani 1 1 d . . . H8 H 0.2933 0.6931 0.9076 0.100 Uiso 1 1 calc R . . N8 N 0.3373(4) 0.5903(3) 0.2022(4) 0.0437(15) Uani 1 1 d . . . C9 C 0.1979(7) 0.6426(5) 0.7557(6) 0.090(3) Uani 1 1 d . . . H9 H 0.1493 0.6215 0.7824 0.108 Uiso 1 1 calc R . . N9 N 0.2013(6) 0.5410(4) 0.0332(6) 0.073(2) Uani 1 1 d . . . N10 N 0.2746(4) 0.6165(3) 0.3433(4) 0.0436(16) Uani 1 1 d . . . C10 C 0.2494(7) 0.6615(4) 0.6090(6) 0.050(2) Uani 1 1 d . . . N11 N 0.4793(4) 0.6105(3) 0.3916(4) 0.0454(16) Uani 1 1 d . . . C11 C 0.7084(6) 0.5543(4) 0.4985(6) 0.056(2) Uani 1 1 d . . . H11 H 0.6443 0.5254 0.4658 0.068 Uiso 1 1 calc R . . N12 N 0.4193(5) 0.6308(3) 0.5433(4) 0.0499(17) Uani 1 1 d . . . C12 C 0.8045(8) 0.5409(4) 0.4836(6) 0.085(3) Uani 1 1 d . . . H12 H 0.8083 0.5024 0.4420 0.102 Uiso 1 1 calc R . . C13 C 0.8971(7) 0.5864(5) 0.5321(7) 0.081(3) Uani 1 1 d . . . H13 H 0.9640 0.5793 0.5231 0.098 Uiso 1 1 calc R . . C14 C 0.8875(7) 0.6413(5) 0.5926(6) 0.080(3) Uani 1 1 d . . . H14 H 0.9497 0.6715 0.6241 0.096 Uiso 1 1 calc R . . C15 C 0.7073(7) 0.6105(5) 0.5622(5) 0.047(2) Uani 1 1 d . . . C16 C 0.7164(6) 0.6469(5) 0.8975(6) 0.067(3) Uani 1 1 d . . . H16 H 0.7533 0.6205 0.9652 0.081 Uiso 1 1 calc R . . C17 C 0.6922(7) 0.7125(6) 0.9090(8) 0.088(3) Uani 1 1 d . . . H17 H 0.7096 0.7322 0.9816 0.106 Uiso 1 1 calc R . . C18 C 0.6384(6) 0.7494(4) 0.8029(8) 0.077(3) Uani 1 1 d . . . H18 H 0.6217 0.7954 0.8087 0.093 Uiso 1 1 calc R . . C19 C 0.6089(6) 0.7255(4) 0.6951(6) 0.047(2) Uani 1 1 d . . . C20 C 0.6374(5) 0.6602(5) 0.6956(5) 0.047(2) Uani 1 1 d . . . C21 C 0.1429(7) 0.6420(4) 0.0994(6) 0.068(2) Uani 1 1 d . . . H21 H 0.1619 0.6779 0.1533 0.082 Uiso 1 1 calc R . . C22 C 0.0356(6) 0.6374(5) 0.0076(6) 0.085(3) Uani 1 1 d . . . H22 H -0.0207 0.6695 0.0003 0.102 Uiso 1 1 calc R . . C23 C 0.0097(8) 0.5871(5) -0.0729(7) 0.092(3) Uani 1 1 d . . . H23 H -0.0629 0.5839 -0.1370 0.110 Uiso 1 1 calc R . . C24 C 0.0953(8) 0.5415(5) -0.0556(7) 0.083(3) Uani 1 1 d . . . H24 H 0.0781 0.5069 -0.1114 0.099 Uiso 1 1 calc R . . C25 C 0.2218(6) 0.5922(5) 0.1101(6) 0.049(2) Uani 1 1 d . . . C26 C 0.4926(7) 0.5149(4) 0.2127(6) 0.065(2) Uani 1 1 d . . . H26 H 0.4774 0.4855 0.2620 0.077 Uiso 1 1 calc R . . C27 C 0.5791(7) 0.4987(5) 0.1821(7) 0.084(3) Uani 1 1 d . . . H27 H 0.6213 0.4582 0.2075 0.101 Uiso 1 1 calc R . . C28 C 0.6013(7) 0.5450(5) 0.1123(7) 0.076(3) Uani 1 1 d . . . H28 H 0.6601 0.5371 0.0902 0.091 Uiso 1 1 calc R . . C29 C 0.5361(7) 0.6011(5) 0.0775(6) 0.073(3) Uani 1 1 d . . . H29 H 0.5517 0.6316 0.0301 0.087 Uiso 1 1 calc R . . C30 C 0.4298(6) 0.5720(5) 0.1729(6) 0.050(2) Uani 1 1 d . . . C31 C 0.3122(6) 0.6301(4) 0.4589(6) 0.051(2) Uani 1 1 d . . . C32 C 0.4976(7) 0.6207(3) 0.5039(5) 0.046(2) Uani 1 1 d . . . C33 C 0.3651(7) 0.6049(3) 0.3188(5) 0.045(2) 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 N1 0.050(5) 0.097(7) 0.075(5) 0.004(5) -0.004(4) 0.003(5) C1 0.051(6) 0.053(7) 0.115(7) -0.032(6) 0.022(6) 0.004(6) N2 0.034(4) 0.085(5) 0.029(3) 0.008(3) 0.006(3) 0.013(4) C2 0.033(7) 0.184(14) 0.137(9) -0.079(8) 0.015(7) 0.016(7) C3 0.033(6) 0.183(12) 0.041(5) -0.045(6) -0.004(4) 0.011(7) N3 0.059(5) 0.086(6) 0.046(3) 0.002(4) 0.030(3) 0.001(4) C4 0.080(8) 0.099(9) 0.082(6) 0.017(6) -0.007(6) 0.039(7) N4 0.065(5) 0.096(6) 0.062(4) -0.004(5) 0.031(4) -0.011(4) N5 0.032(4) 0.075(5) 0.034(3) -0.008(3) 0.007(3) 0.003(4) C5 0.055(6) 0.059(7) 0.042(5) -0.004(5) 0.029(5) 0.002(6) C6 0.075(7) 0.060(7) 0.062(5) 0.006(5) 0.025(5) 0.016(5) N6 0.046(4) 0.067(5) 0.056(4) -0.010(3) 0.019(4) -0.020(4) N7 0.045(4) 0.063(5) 0.061(4) 0.017(4) 0.020(3) 0.006(4) C7 0.053(6) 0.090(8) 0.067(6) -0.030(5) 0.007(5) 0.012(5) C8 0.075(8) 0.103(9) 0.062(6) -0.003(6) 0.022(6) 0.028(6) N8 0.024(4) 0.067(5) 0.043(3) -0.001(3) 0.018(3) 0.008(3) C9 0.083(8) 0.152(10) 0.052(5) 0.018(6) 0.045(5) 0.019(6) N9 0.068(6) 0.102(7) 0.048(4) -0.017(4) 0.024(4) -0.004(5) N10 0.027(3) 0.064(5) 0.044(3) 0.004(3) 0.019(3) 0.002(3) C10 0.050(6) 0.052(7) 0.047(5) 0.011(4) 0.022(5) 0.011(5) N11 0.026(4) 0.061(5) 0.049(3) -0.005(3) 0.016(3) -0.010(3) C11 0.022(5) 0.075(7) 0.063(5) 0.000(5) 0.011(4) 0.005(5) N12 0.025(4) 0.072(5) 0.049(3) 0.003(3) 0.013(3) 0.003(3) C12 0.056(6) 0.108(9) 0.078(6) -0.028(5) 0.017(6) 0.010(6) C13 0.043(6) 0.119(10) 0.081(6) 0.005(6) 0.027(6) 0.010(7) C14 0.051(6) 0.105(9) 0.092(6) -0.007(6) 0.040(5) -0.003(6) C15 0.045(6) 0.054(7) 0.026(4) 0.008(4) 0.003(4) 0.005(5) C16 0.032(5) 0.126(9) 0.031(5) 0.000(6) 0.002(4) -0.009(6) C17 0.061(7) 0.134(11) 0.077(7) -0.044(8) 0.037(5) -0.007(7) C18 0.054(6) 0.063(7) 0.095(6) 0.002(6) 0.014(5) -0.002(5) C19 0.052(6) 0.032(6) 0.045(5) -0.014(5) 0.012(4) -0.012(5) C20 0.037(5) 0.070(7) 0.025(4) 0.003(5) 0.005(4) -0.006(5) C21 0.055(6) 0.071(7) 0.062(5) 0.001(5) 0.011(5) 0.025(5) C22 0.036(6) 0.131(10) 0.062(5) 0.029(6) -0.002(5) 0.019(6) C23 0.048(7) 0.149(11) 0.057(6) -0.014(6) 0.004(5) 0.000(7) C24 0.057(7) 0.116(10) 0.064(6) -0.014(6) 0.017(6) -0.004(7) C25 0.031(5) 0.066(7) 0.048(5) 0.013(5) 0.015(5) -0.003(5) C26 0.061(6) 0.060(7) 0.063(5) -0.013(5) 0.019(5) 0.006(5) C27 0.063(7) 0.085(9) 0.084(6) -0.023(6) 0.014(5) 0.035(6) C28 0.040(6) 0.109(10) 0.076(6) -0.031(6) 0.025(5) 0.002(6) C29 0.058(6) 0.089(9) 0.094(6) -0.012(6) 0.055(6) -0.008(6) C30 0.030(5) 0.068(7) 0.039(4) 0.002(4) 0.004(4) 0.009(5) C31 0.035(5) 0.077(7) 0.041(4) 0.005(4) 0.018(4) 0.000(5) C32 0.046(6) 0.050(6) 0.031(4) 0.004(4) 0.009(4) 0.003(4) C33 0.041(5) 0.055(6) 0.041(4) 0.005(4) 0.020(4) 0.011(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 N1 C5 1.309(8) . ? N1 C4 1.387(8) . ? C1 C5 1.329(9) . ? C1 C2 1.360(9) . ? N2 C31 1.370(6) . ? N2 C5 1.409(8) . ? N2 C10 1.458(7) . ? C2 C3 1.309(11) . ? C3 C4 1.366(10) . ? N3 C10 1.325(7) . ? N3 C9 1.340(6) . ? N4 C16 1.377(7) . ? N4 C20 1.390(7) . ? N5 C32 1.377(7) . ? N5 C15 1.432(7) . ? N5 C20 1.434(7) . ? C6 C10 1.372(8) . ? C6 C7 1.389(7) . ? N6 C14 1.331(7) . ? N6 C15 1.338(7) . ? N7 C30 1.348(7) . ? N7 C29 1.351(7) . ? C7 C8 1.381(9) . ? C8 C9 1.380(9) . ? N8 C33 1.390(6) . ? N8 C25 1.429(7) . ? N8 C30 1.442(7) . ? N9 C24 1.330(8) . ? N9 C25 1.337(8) . ? N10 C33 1.352(7) . ? N10 C31 1.354(6) . ? N11 C33 1.351(7) . ? N11 C32 1.353(6) . ? C11 C12 1.359(8) . ? C11 C15 1.364(8) . ? N12 C31 1.320(6) . ? N12 C32 1.325(7) . ? C12 C13 1.390(9) . ? C13 C14 1.352(9) . ? C16 C17 1.335(9) . ? C17 C18 1.409(9) . ? C18 C19 1.333(8) . ? C19 C20 1.320(8) . ? C21 C22 1.359(8) . ? C21 C25 1.366(8) . ? C22 C23 1.345(9) . ? C23 C24 1.355(9) . ? C26 C30 1.334(8) . ? C26 C27 1.371(8) . ? C27 C28 1.379(9) . ? C28 C29 1.328(9) . ? 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 C5 N1 C4 117.7(8) . . ? C5 C1 C2 119.3(9) . . ? C31 N2 C5 122.8(6) . . ? C31 N2 C10 120.6(6) . . ? C5 N2 C10 116.5(6) . . ? C3 C2 C1 123.2(10) . . ? C2 C3 C4 115.8(9) . . ? C10 N3 C9 116.8(7) . . ? C3 C4 N1 122.4(9) . . ? C16 N4 C20 113.7(7) . . ? C32 N5 C15 123.4(6) . . ? C32 N5 C20 119.0(6) . . ? C15 N5 C20 117.0(6) . . ? N1 C5 C1 121.6(8) . . ? N1 C5 N2 114.7(8) . . ? C1 C5 N2 123.8(9) . . ? C10 C6 C7 117.1(8) . . ? C14 N6 C15 115.6(7) . . ? C30 N7 C29 114.2(7) . . ? C8 C7 C6 119.8(8) . . ? C9 C8 C7 117.7(8) . . ? C33 N8 C25 123.3(6) . . ? C33 N8 C30 118.3(6) . . ? C25 N8 C30 118.4(5) . . ? N3 C9 C8 123.6(8) . . ? C24 N9 C25 114.1(7) . . ? C33 N10 C31 110.7(6) . . ? N3 C10 C6 124.8(7) . . ? N3 C10 N2 113.6(7) . . ? C6 C10 N2 121.6(7) . . ? C33 N11 C32 111.1(6) . . ? C12 C11 C15 119.1(8) . . ? C31 N12 C32 112.9(6) . . ? C11 C12 C13 118.2(8) . . ? C14 C13 C12 118.5(9) . . ? N6 C14 C13 124.6(9) . . ? N6 C15 C11 124.0(7) . . ? N6 C15 N5 113.2(8) . . ? C11 C15 N5 122.8(8) . . ? C17 C16 N4 123.6(8) . . ? C16 C17 C18 114.9(8) . . ? C19 C18 C17 126.9(8) . . ? C20 C19 C18 112.2(7) . . ? C19 C20 N4 128.5(6) . . ? C19 C20 N5 118.9(7) . . ? N4 C20 N5 112.6(7) . . ? C22 C21 C25 117.8(8) . . ? C23 C22 C21 121.0(9) . . ? C22 C23 C24 116.3(9) . . ? N9 C24 C23 126.7(9) . . ? N9 C25 C21 124.0(7) . . ? N9 C25 N8 112.0(8) . . ? C21 C25 N8 124.0(8) . . ? C30 C26 C27 121.1(8) . . ? C26 C27 C28 117.4(9) . . ? C29 C28 C27 117.9(9) . . ? C28 C29 N7 126.3(9) . . ? C26 C30 N7 123.0(7) . . ? C26 C30 N8 122.6(8) . . ? N7 C30 N8 114.3(8) . . ? N12 C31 N10 128.6(6) . . ? N12 C31 N2 118.0(6) . . ? N10 C31 N2 113.3(6) . . ? N12 C32 N11 127.9(6) . . ? N12 C32 N5 115.8(6) . . ? N11 C32 N5 116.0(7) . . ? N11 C33 N10 128.1(6) . . ? N11 C33 N8 115.6(6) . . ? N10 C33 N8 116.0(6) . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 28.43 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 0.189 _refine_diff_density_min -0.209 _refine_diff_density_rms 0.049