# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Jacek Gawronski' 'Marcin Kwit' 'Urszula Rychlewska' _publ_contact_author_name 'Prof Jacek Gawronski' _publ_contact_author_address ; Department of Chemistry A.Mickiewicz University Grunwaldzka 6 60780 Poznan POLAND ; _publ_contact_author_email 'GAWRONSK@AMU.EDU.PL' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Induced Homohelicity of Diphenimide Bis-propellers ; data_dphnmeph _database_code_CSD 187215 _audit_creation_method SHELXL-97 _chemical_name_systematic ; (+-)-N-(\a-Methylbenzyl)diphenimide ; _chemical_name_common ? _chemical_melting_point 142-3\% _chemical_formula_moiety 'C22 H17 N O2' _chemical_formula_sum 'C22 H17 N O2' _chemical_formula_weight 327.37 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 9.764(2) _cell_length_b 10.273(2) _cell_length_c 17.099(3) _cell_angle_alpha 90.00 _cell_angle_beta 95.55(3) _cell_angle_gamma 90.00 _cell_volume 1707.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 6633 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description spherical _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.274 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 688 _exptl_absorpt_coefficient_mu 0.082 _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 294(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 'Kuma KM4CCD \k-geometry diffractometer' _diffrn_measurement_method \w scans\ _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8427 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0153 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.10 _diffrn_reflns_theta_max 25.03 _reflns_number_total 2981 _reflns_number_gt 2610 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Kuma KM4CCD software (Kuma Diffraction, 1999) ; _computing_cell_refinement 'Kuma KM4CCD software' _computing_data_reduction 'Kuma KM4CCD software' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Simens Analytical X-Ray Instruments (1989)' _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. The structures were phased by direct methods (SHELXS86 program) and refined by full-matrix least-squares using the SHELXL97 program. Siemens computer graphics program was used to prepare drawings. Anisotropic thermal parameters were refined for all non-hydrogen atoms. The hydrogen atoms were located on difference Fourier maps and refined isotropically. ; _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^)+(0.0557P)^2^+0.3217P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2981 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1149 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.117 _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 C1 C -0.20046(15) 0.20332(15) 0.79751(9) 0.0423(4) Uani 1 1 d . . . C2 C -0.28580(19) 0.24343(18) 0.73104(10) 0.0545(4) Uani 1 1 d . . . C3 C -0.2661(2) 0.1974(2) 0.65749(11) 0.0663(5) Uani 1 1 d . . . C4 C -0.1620(3) 0.1107(2) 0.64774(11) 0.0709(6) Uani 1 1 d . . . C5 C -0.0765(2) 0.06992(19) 0.71189(11) 0.0592(5) Uani 1 1 d . . . C6 C -0.09413(16) 0.11631(14) 0.78716(9) 0.0433(4) Uani 1 1 d . . . C7 C -0.22971(15) 0.25010(14) 0.87588(8) 0.0401(4) Uani 1 1 d . . . C8 C -0.36607(18) 0.26345(17) 0.89263(11) 0.0520(4) Uani 1 1 d . . . C9 C -0.3995(2) 0.3132(2) 0.96303(11) 0.0613(5) Uani 1 1 d . . . C10 C -0.2969(2) 0.35446(19) 1.01839(11) 0.0614(5) Uani 1 1 d . . . C11 C -0.1615(2) 0.34234(16) 1.00377(10) 0.0528(4) Uani 1 1 d . . . C12 C -0.12562(16) 0.28691(14) 0.93375(9) 0.0412(4) Uani 1 1 d . . . C13 C 0.00549(16) 0.06604(15) 0.85183(9) 0.0445(4) Uani 1 1 d . . . C14 C 0.02566(16) 0.27268(15) 0.92958(9) 0.0440(4) Uani 1 1 d . . . C15 C 0.22428(16) 0.12528(17) 0.92848(9) 0.0475(4) Uani 1 1 d . . . C16 C 0.2350(3) 0.0322(3) 0.99739(12) 0.0702(6) Uani 1 1 d . . . C17 C 0.29967(15) 0.08594(16) 0.85854(9) 0.0455(4) Uani 1 1 d . . . C18 C 0.29527(18) 0.1694(2) 0.79435(10) 0.0566(4) Uani 1 1 d . . . C19 C 0.3655(2) 0.1412(3) 0.73019(12) 0.0716(6) Uani 1 1 d . . . C20 C 0.4417(3) 0.0294(3) 0.72907(15) 0.0815(7) Uani 1 1 d . . . C21 C 0.4476(2) -0.0536(2) 0.79170(17) 0.0812(7) Uani 1 1 d . . . C22 C 0.37688(19) -0.02600(19) 0.85684(13) 0.0615(5) Uani 1 1 d . . . N1 N 0.07741(12) 0.15658(12) 0.90207(7) 0.0425(3) Uani 1 1 d . . . O1 O 0.03940(12) -0.04722(11) 0.85403(8) 0.0620(4) Uani 1 1 d . . . O2 O 0.10443(13) 0.35405(12) 0.95955(9) 0.0671(4) Uani 1 1 d . . . H2 H -0.361(2) 0.305(2) 0.7374(11) 0.068(6) Uiso 1 1 d . . . H3 H -0.328(2) 0.225(2) 0.6112(14) 0.085(7) Uiso 1 1 d . . . H4 H -0.147(2) 0.080(2) 0.5970(13) 0.077(6) Uiso 1 1 d . . . H5 H -0.002(2) 0.0102(19) 0.7090(11) 0.065(6) Uiso 1 1 d . . . H8 H -0.436(2) 0.2359(18) 0.8532(11) 0.064(5) Uiso 1 1 d . . . H9 H -0.496(2) 0.322(2) 0.9735(12) 0.083(6) Uiso 1 1 d . . . H10 H -0.320(2) 0.3919(19) 1.0702(12) 0.070(5) Uiso 1 1 d . . . H11 H -0.084(2) 0.3717(19) 1.0407(11) 0.065(5) Uiso 1 1 d . . . H15 H 0.2595(18) 0.2152(19) 0.9472(10) 0.058(5) Uiso 1 1 d . . . H161 H 0.181(2) 0.067(2) 1.0389(14) 0.085(7) Uiso 1 1 d . . . H162 H 0.197(3) -0.056(3) 0.9782(15) 0.100(8) Uiso 1 1 d . . . H163 H 0.334(3) 0.029(2) 1.0208(14) 0.093(7) Uiso 1 1 d . . . H18 H 0.243(2) 0.252(2) 0.7951(12) 0.079(6) Uiso 1 1 d . . . H19 H 0.363(2) 0.205(2) 0.6855(14) 0.082(6) Uiso 1 1 d . . . H20 H 0.494(3) 0.011(2) 0.6835(16) 0.102(8) Uiso 1 1 d . . . H21 H 0.503(3) -0.131(3) 0.7939(15) 0.106(8) Uiso 1 1 d . . . H22 H 0.380(2) -0.084(2) 0.9001(12) 0.070(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 C1 0.0434(8) 0.0425(8) 0.0408(8) -0.0007(6) 0.0027(6) -0.0092(7) C2 0.0571(11) 0.0587(11) 0.0460(9) 0.0041(8) -0.0038(8) -0.0068(9) C3 0.0815(14) 0.0704(13) 0.0444(10) 0.0035(9) -0.0063(9) -0.0159(11) C4 0.1020(17) 0.0713(13) 0.0399(10) -0.0120(9) 0.0101(10) -0.0226(12) C5 0.0724(12) 0.0518(10) 0.0552(11) -0.0137(8) 0.0156(9) -0.0100(9) C6 0.0471(9) 0.0392(8) 0.0437(8) -0.0060(6) 0.0054(7) -0.0105(7) C7 0.0438(8) 0.0351(8) 0.0411(8) 0.0024(6) 0.0032(6) -0.0009(6) C8 0.0449(9) 0.0549(10) 0.0559(10) 0.0027(8) 0.0034(8) -0.0010(8) C9 0.0541(11) 0.0666(12) 0.0660(12) 0.0035(9) 0.0189(9) 0.0077(9) C10 0.0723(13) 0.0633(11) 0.0511(10) -0.0040(9) 0.0186(9) 0.0121(9) C11 0.0647(11) 0.0491(9) 0.0439(9) -0.0062(7) 0.0026(8) 0.0034(8) C12 0.0470(9) 0.0346(7) 0.0419(8) 0.0000(6) 0.0037(7) -0.0006(6) C13 0.0413(8) 0.0385(9) 0.0549(9) -0.0058(7) 0.0120(7) -0.0048(7) C14 0.0484(9) 0.0384(8) 0.0443(8) -0.0019(6) 0.0003(7) -0.0037(7) C15 0.0429(9) 0.0499(9) 0.0488(9) 0.0010(7) 0.0003(7) 0.0005(7) C16 0.0797(15) 0.0808(15) 0.0500(11) 0.0132(10) 0.0064(10) 0.0145(12) C17 0.0354(8) 0.0506(9) 0.0501(9) -0.0013(7) 0.0012(6) -0.0033(7) C18 0.0459(9) 0.0698(12) 0.0532(10) 0.0059(9) 0.0008(8) -0.0027(9) C19 0.0660(12) 0.0965(16) 0.0529(11) -0.0007(11) 0.0080(9) -0.0210(12) C20 0.0794(15) 0.0939(17) 0.0762(15) -0.0276(14) 0.0332(12) -0.0251(13) C21 0.0715(14) 0.0633(13) 0.1135(19) -0.0243(13) 0.0334(13) -0.0011(11) C22 0.0562(11) 0.0538(10) 0.0757(13) 0.0008(10) 0.0128(9) 0.0014(8) N1 0.0388(7) 0.0400(7) 0.0484(7) -0.0044(5) 0.0019(5) -0.0028(5) O1 0.0566(7) 0.0382(7) 0.0902(9) -0.0092(6) 0.0023(6) -0.0002(5) O2 0.0556(7) 0.0482(7) 0.0943(10) -0.0205(6) -0.0087(7) -0.0097(6) _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 C6 1.394(2) . ? C1 C2 1.405(2) . ? C1 C7 1.477(2) . ? C2 C3 1.374(3) . ? C3 C4 1.374(3) . ? C4 C5 1.378(3) . ? C5 C6 1.399(2) . ? C6 C13 1.492(2) . ? C7 C8 1.395(2) . ? C7 C12 1.400(2) . ? C8 C9 1.376(3) . ? C9 C10 1.377(3) . ? C10 C11 1.375(3) . ? C11 C12 1.401(2) . ? C12 C14 1.493(2) . ? C13 O1 1.2093(18) . ? C13 N1 1.407(2) . ? C14 O2 1.2152(19) . ? C14 N1 1.395(2) . ? C15 N1 1.496(2) . ? C15 C16 1.513(3) . ? C15 C17 1.518(2) . ? C17 C22 1.377(2) . ? C17 C18 1.390(2) . ? C18 C19 1.380(3) . ? C19 C20 1.369(3) . ? C20 C21 1.366(4) . ? C21 C22 1.396(3) . ? 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 C6 C1 C2 118.44(15) . . ? C6 C1 C7 122.37(14) . . ? C2 C1 C7 119.14(15) . . ? C3 C2 C1 121.01(19) . . ? C4 C3 C2 120.30(19) . . ? C3 C4 C5 119.93(18) . . ? C4 C5 C6 120.7(2) . . ? C1 C6 C5 119.64(16) . . ? C1 C6 C13 124.60(13) . . ? C5 C6 C13 115.76(16) . . ? C8 C7 C12 118.04(14) . . ? C8 C7 C1 119.35(14) . . ? C12 C7 C1 122.56(14) . . ? C9 C8 C7 121.86(17) . . ? C8 C9 C10 119.84(18) . . ? C11 C10 C9 119.71(17) . . ? C10 C11 C12 121.12(17) . . ? C7 C12 C11 119.30(15) . . ? C7 C12 C14 126.42(13) . . ? C11 C12 C14 114.28(14) . . ? O1 C13 N1 119.87(15) . . ? O1 C13 C6 120.85(14) . . ? N1 C13 C6 118.34(13) . . ? O2 C14 N1 119.69(15) . . ? O2 C14 C12 120.08(14) . . ? N1 C14 C12 119.49(13) . . ? N1 C15 C16 111.29(15) . . ? N1 C15 C17 110.06(13) . . ? C16 C15 C17 116.29(16) . . ? C22 C17 C18 118.28(17) . . ? C22 C17 C15 123.16(16) . . ? C18 C17 C15 118.52(15) . . ? C19 C18 C17 121.2(2) . . ? C20 C19 C18 120.0(2) . . ? C21 C20 C19 119.7(2) . . ? C20 C21 C22 120.8(2) . . ? C17 C22 C21 120.1(2) . . ? C14 N1 C13 126.55(13) . . ? C14 N1 C15 116.74(13) . . ? C13 N1 C15 116.71(12) . . ? 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 C6 C1 C2 C3 0.5(2) . . . . ? C7 C1 C2 C3 -176.93(16) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C2 C1 C6 C5 -1.0(2) . . . . ? C7 C1 C6 C5 176.38(14) . . . . ? C2 C1 C6 C13 179.38(14) . . . . ? C7 C1 C6 C13 -3.2(2) . . . . ? C4 C5 C6 C1 0.9(3) . . . . ? C4 C5 C6 C13 -179.44(16) . . . . ? C6 C1 C7 C8 -139.96(16) . . . . ? C2 C1 C7 C8 37.4(2) . . . . ? C6 C1 C7 C12 42.6(2) . . . . ? C2 C1 C7 C12 -139.99(15) . . . . ? C12 C7 C8 C9 1.1(2) . . . . ? C1 C7 C8 C9 -176.40(16) . . . . ? C7 C8 C9 C10 1.6(3) . . . . ? C8 C9 C10 C11 -1.7(3) . . . . ? C9 C10 C11 C12 -0.9(3) . . . . ? C8 C7 C12 C11 -3.7(2) . . . . ? C1 C7 C12 C11 173.74(14) . . . . ? C8 C7 C12 C14 175.90(14) . . . . ? C1 C7 C12 C14 -6.7(2) . . . . ? C10 C11 C12 C7 3.7(2) . . . . ? C10 C11 C12 C14 -175.97(15) . . . . ? C1 C6 C13 O1 138.20(16) . . . . ? C5 C6 C13 O1 -41.4(2) . . . . ? C1 C6 C13 N1 -52.9(2) . . . . ? C5 C6 C13 N1 127.48(15) . . . . ? C7 C12 C14 O2 145.34(16) . . . . ? C11 C12 C14 O2 -35.0(2) . . . . ? C7 C12 C14 N1 -44.5(2) . . . . ? C11 C12 C14 N1 135.13(15) . . . . ? N1 C15 C17 C22 -129.13(17) . . . . ? C16 C15 C17 C22 -1.4(2) . . . . ? N1 C15 C17 C18 53.57(19) . . . . ? C16 C15 C17 C18 -178.74(17) . . . . ? C22 C17 C18 C19 0.3(3) . . . . ? C15 C17 C18 C19 177.78(16) . . . . ? C17 C18 C19 C20 -0.2(3) . . . . ? C18 C19 C20 C21 -0.1(3) . . . . ? C19 C20 C21 C22 0.1(4) . . . . ? C18 C17 C22 C21 -0.3(3) . . . . ? C15 C17 C22 C21 -177.61(17) . . . . ? C20 C21 C22 C17 0.1(3) . . . . ? O2 C14 N1 C13 -165.43(15) . . . . ? C12 C14 N1 C13 24.4(2) . . . . ? O2 C14 N1 C15 14.4(2) . . . . ? C12 C14 N1 C15 -155.80(13) . . . . ? O1 C13 N1 C14 -153.38(15) . . . . ? C6 C13 N1 C14 37.6(2) . . . . ? O1 C13 N1 C15 26.8(2) . . . . ? C6 C13 N1 C15 -142.24(14) . . . . ? C16 C15 N1 C14 97.90(18) . . . . ? C17 C15 N1 C14 -131.69(14) . . . . ? C16 C15 N1 C13 -82.23(19) . . . . ? C17 C15 N1 C13 48.17(18) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.125 _refine_diff_density_min -0.189 _refine_diff_density_rms 0.031 data_dfic _database_code_CSD 187216 _audit_creation_method SHELXL-97 _chemical_name_systematic ; trans-(1R,2R)-N,N'-Bis(diphenoyl)-1,2-diaminocyclohexane ; _chemical_name_common ? _chemical_melting_point 264-6\% _chemical_formula_moiety 'C34 H26 N2 O4' _chemical_formula_sum 'C34 H26 N2 O4' _chemical_formula_weight 526.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.907(2) _cell_length_b 12.579(3) _cell_length_c 21.288(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.90(3) _cell_angle_gamma 90.00 _cell_volume 2621.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 70 _cell_measurement_theta_min 12.7 _cell_measurement_theta_max 23.9 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.707 _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 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM-4 four circle diffractometer' _diffrn_measurement_method '\Q--2\Q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.58 _diffrn_reflns_number 9356 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 65.09 _reflns_number_total 8760 _reflns_number_gt 7379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_cell_refinement 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_data_reduction 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Simens Analytical X-Ray Instruments (1989)' _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. The structures were phased by direct methods (SHELXS86 program) and refined by full-matrix least-squares using the SHELXL97 program. Siemens computer graphics program was used to prepare drawings. Anisotropic thermal parameters were refined for all non-hydrogen atoms. The hydrogen atoms were placed at calculated positions (C-H = 0.96 A) and refined in a riding model with their Uiso increased by 1.2 compared to Ueq of atoms to which they were bonded. ; _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^)+(0.0584P)^2^+0.2031P] 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 SHELXL _refine_ls_extinction_coef 0.00215(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(15) _refine_ls_number_reflns 8760 _refine_ls_number_parameters 722 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0494 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.0955 _refine_ls_wR_factor_gt 0.0872 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 -0.2819(2) -1.07760(15) -0.67724(9) 0.0448(4) Uani 1 1 d . . . H1 H -0.3158 -1.0616 -0.7209 0.058 Uiso 1 1 d R . . C2 C -0.17602(19) -0.99207(14) -0.65353(9) 0.0422(4) Uani 1 1 d . . . H2 H -0.1267 -1.0165 -0.6138 0.055 Uiso 1 1 d R . . C3 C -0.0744(2) -0.98533(18) -0.70120(10) 0.0534(5) Uani 1 1 d . . . H3A H -0.1219 -0.9653 -0.7423 0.069 Uiso 1 1 d R . . H3B H -0.0075 -0.9316 -0.6875 0.069 Uiso 1 1 d R . . C4 C -0.0030(2) -1.09126(19) -0.70615(12) 0.0647(6) Uani 1 1 d . . . H4A H 0.0539 -1.0867 -0.7387 0.084 Uiso 1 1 d R . . H4B H 0.0548 -1.1059 -0.6666 0.084 Uiso 1 1 d R . . C5 C -0.1037(2) -1.18250(19) -0.72126(12) 0.0649(6) Uani 1 1 d . . . H5A H -0.1497 -1.1750 -0.7642 0.084 Uiso 1 1 d R . . H5B H -0.0547 -1.2486 -0.7184 0.084 Uiso 1 1 d R . . C6 C -0.2086(2) -1.18442(17) -0.67628(11) 0.0590(5) Uani 1 1 d . . . H6A H -0.1643 -1.1996 -0.6339 0.077 Uiso 1 1 d R . . H6B H -0.2743 -1.2394 -0.6890 0.077 Uiso 1 1 d R . . C7 C -0.3836(2) -1.06353(16) -0.57688(8) 0.0467(4) Uani 1 1 d . . . C8 C -0.5233(2) -1.11812(17) -0.67866(9) 0.0521(5) Uani 1 1 d . . . C9 C -0.15516(19) -0.82724(15) -0.59307(9) 0.0436(4) Uani 1 1 d . . . C10 C -0.34044(19) -0.84463(15) -0.68624(9) 0.0426(4) Uani 1 1 d . . . C11 C -0.6298(2) -1.02552(17) -0.56215(9) 0.0494(5) Uani 1 1 d . . . C12 C -0.7208(2) -0.9563(2) -0.53939(10) 0.0642(6) Uani 1 1 d . . . H12 H -0.8165 -0.9729 -0.5465 0.083 Uiso 1 1 d R . . C13 C -0.6747(3) -0.8644(2) -0.50723(12) 0.0720(7) Uani 1 1 d . . . H13 H -0.7387 -0.8165 -0.4927 0.094 Uiso 1 1 d R . . C14 C -0.5377(3) -0.8419(2) -0.49585(12) 0.0717(7) Uani 1 1 d . . . H14 H -0.5047 -0.7791 -0.4728 0.093 Uiso 1 1 d R . . C15 C -0.4459(3) -0.90906(18) -0.51775(10) 0.0595(6) Uani 1 1 d . . . H15 H -0.3498 -0.8942 -0.5093 0.077 Uiso 1 1 d R . . C16 C -0.4910(2) -0.99985(16) -0.55196(8) 0.0477(4) Uani 1 1 d . . . C17 C -0.6771(2) -1.12798(17) -0.59184(9) 0.0495(5) Uani 1 1 d . . . C18 C -0.7750(2) -1.1865(2) -0.56550(10) 0.0624(6) Uani 1 1 d . . . H18 H -0.8090 -1.1597 -0.5287 0.081 Uiso 1 1 d R . . C19 C -0.8232(3) -1.2819(2) -0.59127(13) 0.0724(7) Uani 1 1 d . . . H19 H -0.8891 -1.3216 -0.5722 0.094 Uiso 1 1 d R . . C20 C -0.7768(3) -1.3213(2) -0.64426(13) 0.0737(7) Uani 1 1 d . . . H20 H -0.8113 -1.3878 -0.6622 0.096 Uiso 1 1 d R . . C21 C -0.6816(2) -1.26492(19) -0.67170(12) 0.0629(6) Uani 1 1 d . . . H21 H -0.6508 -1.2920 -0.7092 0.082 Uiso 1 1 d R . . C22 C -0.6288(2) -1.16858(16) -0.64510(9) 0.0490(5) Uani 1 1 d . . . C31 C -0.2639(2) -0.64074(16) -0.61345(9) 0.0459(4) Uani 1 1 d . . . C32 C -0.2389(2) -0.53117(18) -0.61371(12) 0.0603(5) Uani 1 1 d . . . H32 H -0.3142 -0.4839 -0.6267 0.078 Uiso 1 1 d R . . C33 C -0.1101(3) -0.4903(2) -0.59582(14) 0.0740(7) Uani 1 1 d . . . H33 H -0.0956 -0.4149 -0.5974 0.096 Uiso 1 1 d R . . C34 C -0.0011(2) -0.5563(2) -0.57599(13) 0.0702(7) Uani 1 1 d . . . H34 H 0.0883 -0.5276 -0.5620 0.091 Uiso 1 1 d R . . C35 C -0.0231(2) -0.66489(18) -0.57606(11) 0.0565(5) Uani 1 1 d . . . H35 H 0.0523 -0.7116 -0.5623 0.073 Uiso 1 1 d R . . C36 C -0.15244(19) -0.70840(15) -0.59555(8) 0.0430(4) Uani 1 1 d . . . C37 C -0.40606(19) -0.67880(16) -0.62815(9) 0.0454(4) Uani 1 1 d . . . C38 C -0.5118(2) -0.6189(2) -0.60919(11) 0.0609(6) Uani 1 1 d . . . H38 H -0.4890 -0.5545 -0.5857 0.079 Uiso 1 1 d R . . C39 C -0.6457(2) -0.6498(2) -0.62379(13) 0.0718(7) Uani 1 1 d . . . H39 H -0.7167 -0.6077 -0.6102 0.093 Uiso 1 1 d R . . C40 C -0.6785(2) -0.7422(2) -0.65815(12) 0.0686(6) Uani 1 1 d . . . H40 H -0.7721 -0.7644 -0.6682 0.089 Uiso 1 1 d R . . C41 C -0.5770(2) -0.80230(19) -0.67808(10) 0.0555(5) Uani 1 1 d . . . H41 H -0.5997 -0.8656 -0.7026 0.072 Uiso 1 1 d R . . C42 C -0.44044(19) -0.77205(16) -0.66235(9) 0.0449(4) Uani 1 1 d . . . N1 N -0.40229(16) -1.08121(13) -0.64321(7) 0.0445(4) Uani 1 1 d . . . N2 N -0.23287(15) -0.88535(12) -0.64219(7) 0.0406(3) Uani 1 1 d . . . O1 O -0.27615(15) -1.08581(14) -0.54403(7) 0.0609(4) Uani 1 1 d . . . O2 O -0.53603(18) -1.12163(17) -0.73627(7) 0.0789(5) Uani 1 1 d . . . O3 O -0.07761(15) -0.87316(12) -0.55196(7) 0.0619(4) Uani 1 1 d . . . O4 O -0.36188(16) -0.87885(12) -0.74013(6) 0.0569(4) Uani 1 1 d . . . C1' C -0.2683(2) 0.42242(18) -0.81466(10) 0.0587(5) Uani 1 1 d . . . H1' H -0.2113 0.4388 -0.7752 0.076 Uiso 1 1 d R . . C2' C -0.2407(3) 0.50841(17) -0.86309(11) 0.0622(6) Uani 1 1 d . . . H2' H -0.3066 0.4972 -0.9006 0.081 Uiso 1 1 d R . . C3' C -0.2695(3) 0.6177(2) -0.83727(15) 0.0910(10) Uani 1 1 d . . . H3'A H -0.2083 0.6300 -0.7984 0.118 Uiso 1 1 d R . . H3'B H -0.2536 0.6715 -0.8673 0.118 Uiso 1 1 d R . . C4' C -0.4155(4) 0.6240(3) -0.82461(18) 0.1132(14) Uani 1 1 d . . . H4'A H -0.4323 0.6930 -0.8082 0.147 Uiso 1 1 d R . . H4'B H -0.4759 0.6148 -0.8641 0.147 Uiso 1 1 d R . . C5' C -0.4473(4) 0.5391(3) -0.77863(18) 0.1127(13) Uani 1 1 d . . . H5'A H -0.3917 0.5509 -0.7381 0.147 Uiso 1 1 d R . . H5'B H -0.5414 0.5435 -0.7730 0.147 Uiso 1 1 d R . . C6' C -0.4161(3) 0.4280(3) -0.80255(14) 0.0834(8) Uani 1 1 d . . . H6'A H -0.4756 0.4141 -0.8417 0.108 Uiso 1 1 d R . . H6'B H -0.4323 0.3749 -0.7722 0.108 Uiso 1 1 d R . . C7' C -0.3079(2) 0.26400(16) -0.88536(10) 0.0491(5) Uani 1 1 d . . . C8' C -0.1171(2) 0.26767(16) -0.79482(9) 0.0493(5) Uani 1 1 d . . . C9' C -0.0953(3) 0.46375(18) -0.94378(10) 0.0600(6) Uani 1 1 d . . . C10' C 0.0098(3) 0.53846(18) -0.83953(10) 0.0634(6) Uani 1 1 d . . . C11' C -0.2049(2) 0.07461(16) -0.87613(9) 0.0507(5) Uani 1 1 d . . . C12' C -0.2324(3) -0.03472(18) -0.87947(12) 0.0672(6) Uani 1 1 d . . . H12' H -0.1582 -0.0844 -0.8712 0.087 Uiso 1 1 d R . . C13' C -0.3636(3) -0.0719(2) -0.89328(16) 0.0870(9) Uani 1 1 d . . . H13' H -0.3799 -0.1472 -0.8953 0.113 Uiso 1 1 d R . . C14' C -0.4703(3) -0.0033(2) -0.90607(18) 0.0928(10) Uani 1 1 d . . . H14' H -0.5616 -0.0307 -0.9156 0.121 Uiso 1 1 d R . . C15' C -0.4470(2) 0.1049(2) -0.90340(13) 0.0703(7) Uani 1 1 d . . . H15' H -0.5222 0.1534 -0.9130 0.091 Uiso 1 1 d R . . C16' C -0.3148(2) 0.14466(17) -0.88740(10) 0.0509(5) Uani 1 1 d . . . C17' C -0.0615(2) 0.11030(17) -0.86324(9) 0.0502(5) Uani 1 1 d . . . C18' C 0.0408(3) 0.0520(2) -0.88590(11) 0.0650(6) Uani 1 1 d . . . H18' H 0.0158 -0.0095 -0.9119 0.084 Uiso 1 1 d R . . C19' C 0.1759(3) 0.0812(2) -0.87198(13) 0.0755(7) Uani 1 1 d . . . H19' H 0.2443 0.0403 -0.8885 0.098 Uiso 1 1 d R . . C20' C 0.2138(3) 0.1681(3) -0.83452(12) 0.0750(7) Uani 1 1 d . . . H20' H 0.3084 0.1876 -0.8248 0.098 Uiso 1 1 d R . . C21' C 0.1153(2) 0.2271(2) -0.81101(11) 0.0630(6) Uani 1 1 d . . . H21' H 0.1417 0.2882 -0.7850 0.082 Uiso 1 1 d R . . C22' C -0.0220(2) 0.19910(16) -0.82520(9) 0.0487(4) Uani 1 1 d . . . C31' C 0.1624(3) 0.45623(19) -0.94290(10) 0.0618(6) Uani 1 1 d . . . C32' C 0.2737(3) 0.3983(2) -0.95782(12) 0.0804(8) Uani 1 1 d . . . H32' H 0.3628 0.4299 -0.9490 0.105 Uiso 1 1 d R . . C33' C 0.2578(4) 0.2987(3) -0.98391(13) 0.0922(9) Uani 1 1 d . . . H33' H 0.3359 0.2600 -0.9932 0.120 Uiso 1 1 d R . . C34' C 0.1302(4) 0.2545(2) -0.99696(13) 0.0936(10) Uani 1 1 d . . . H34' H 0.1180 0.1851 -1.0157 0.122 Uiso 1 1 d R . . C35' C 0.0170(4) 0.3093(2) -0.98336(11) 0.0785(8) Uani 1 1 d . . . H35' H -0.0726 0.2786 -0.9929 0.102 Uiso 1 1 d R . . C36' C 0.0329(3) 0.41086(17) -0.95514(9) 0.0606(6) Uani 1 1 d . . . C37' C 0.1816(2) 0.56516(19) -0.91707(11) 0.0625(6) Uani 1 1 d . . . C38' C 0.2720(3) 0.6339(2) -0.94065(13) 0.0729(7) Uani 1 1 d . . . H38' H 0.3175 0.6109 -0.9749 0.095 Uiso 1 1 d R . . C39' C 0.2962(3) 0.7348(2) -0.91507(16) 0.0853(9) Uani 1 1 d . . . H39' H 0.3553 0.7824 -0.9332 0.111 Uiso 1 1 d R . . C40' C 0.2373(3) 0.7662(2) -0.86408(16) 0.0858(9) Uani 1 1 d . . . H40' H 0.2598 0.8348 -0.8456 0.112 Uiso 1 1 d R . . C41' C 0.1474(3) 0.6995(2) -0.83977(13) 0.0746(7) Uani 1 1 d . . . H41' H 0.1049 0.7224 -0.8045 0.097 Uiso 1 1 d R . . C42' C 0.1160(2) 0.59887(18) -0.86701(11) 0.0611(6) Uani 1 1 d . . . N1' N -0.22906(17) 0.31404(13) -0.83406(7) 0.0493(4) Uani 1 1 d . . . N2' N -0.1038(2) 0.50085(14) -0.88186(8) 0.0577(4) Uani 1 1 d . . . O1' O -0.38526(16) 0.31575(12) -0.92376(7) 0.0624(4) Uani 1 1 d . . . O2' O -0.08780(18) 0.29378(12) -0.73976(7) 0.0655(4) Uani 1 1 d . . . O3' O -0.19569(19) 0.46442(16) -0.98422(7) 0.0787(5) Uani 1 1 d . . . O4' O 0.0087(2) 0.53509(16) -0.78254(8) 0.0833(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 0.0519(11) 0.0383(10) 0.0443(9) -0.0020(8) 0.0078(8) -0.0054(8) C2 0.0472(10) 0.0351(9) 0.0446(9) -0.0025(7) 0.0076(8) 0.0009(8) C3 0.0541(11) 0.0488(12) 0.0604(12) -0.0020(9) 0.0186(9) -0.0028(9) C4 0.0589(13) 0.0603(14) 0.0775(15) -0.0104(12) 0.0185(11) 0.0097(11) C5 0.0719(14) 0.0500(12) 0.0731(14) -0.0112(11) 0.0123(11) 0.0117(11) C6 0.0697(14) 0.0374(11) 0.0683(13) -0.0042(9) 0.0061(10) 0.0022(10) C7 0.0512(11) 0.0473(11) 0.0397(9) 0.0032(8) 0.0016(8) -0.0155(9) C8 0.0575(12) 0.0552(12) 0.0415(10) -0.0028(9) 0.0006(9) -0.0120(9) C9 0.0446(10) 0.0416(11) 0.0444(10) -0.0049(8) 0.0062(8) -0.0014(8) C10 0.0485(10) 0.0372(10) 0.0416(9) -0.0005(7) 0.0053(8) -0.0042(8) C11 0.0559(11) 0.0511(12) 0.0408(10) 0.0025(8) 0.0063(8) -0.0117(9) C12 0.0647(14) 0.0727(16) 0.0555(12) 0.0000(11) 0.0108(10) -0.0055(12) C13 0.0904(18) 0.0645(16) 0.0652(14) -0.0071(12) 0.0251(13) -0.0003(14) C14 0.0980(19) 0.0599(15) 0.0617(13) -0.0154(11) 0.0265(13) -0.0182(14) C15 0.0748(14) 0.0604(14) 0.0445(10) -0.0064(9) 0.0132(10) -0.0248(11) C16 0.0582(11) 0.0479(11) 0.0373(9) 0.0001(8) 0.0080(8) -0.0138(9) C17 0.0483(10) 0.0520(12) 0.0450(10) 0.0077(8) -0.0025(8) -0.0121(9) C18 0.0571(13) 0.0727(15) 0.0545(12) 0.0125(11) 0.0000(9) -0.0230(11) C19 0.0652(14) 0.0715(16) 0.0748(16) 0.0228(13) -0.0069(12) -0.0285(12) C20 0.0742(15) 0.0531(14) 0.0859(18) 0.0080(12) -0.0128(13) -0.0269(12) C21 0.0652(13) 0.0505(13) 0.0674(14) -0.0040(10) -0.0075(11) -0.0125(11) C22 0.0491(11) 0.0458(11) 0.0483(10) 0.0014(8) -0.0044(8) -0.0126(9) C31 0.0493(11) 0.0432(11) 0.0462(10) -0.0080(8) 0.0108(8) -0.0030(8) C32 0.0602(13) 0.0424(11) 0.0786(15) -0.0076(10) 0.0117(11) 0.0008(10) C33 0.0697(15) 0.0444(12) 0.110(2) -0.0148(13) 0.0194(14) -0.0133(12) C34 0.0549(13) 0.0533(14) 0.1041(19) -0.0178(13) 0.0177(12) -0.0144(11) C35 0.0470(11) 0.0506(12) 0.0725(13) -0.0117(10) 0.0115(10) -0.0051(9) C36 0.0444(10) 0.0424(10) 0.0434(9) -0.0061(8) 0.0106(7) -0.0053(8) C37 0.0457(10) 0.0451(10) 0.0455(10) -0.0021(8) 0.0077(8) 0.0023(8) C38 0.0556(12) 0.0616(14) 0.0670(13) -0.0095(11) 0.0139(10) 0.0078(11) C39 0.0530(13) 0.0836(19) 0.0806(16) -0.0037(14) 0.0162(11) 0.0115(12) C40 0.0419(11) 0.0875(19) 0.0744(15) 0.0059(13) 0.0024(10) -0.0007(12) C41 0.0466(11) 0.0591(13) 0.0573(12) 0.0034(10) -0.0028(9) -0.0054(10) C42 0.0453(10) 0.0455(11) 0.0423(9) 0.0025(8) 0.0022(7) -0.0024(8) N1 0.0471(8) 0.0456(9) 0.0397(8) -0.0015(6) 0.0033(6) -0.0109(7) N2 0.0468(8) 0.0348(8) 0.0400(8) -0.0024(6) 0.0057(6) -0.0021(7) O1 0.0562(9) 0.0767(10) 0.0468(7) 0.0082(7) -0.0014(6) -0.0069(8) O2 0.0774(11) 0.1146(15) 0.0423(8) -0.0088(8) 0.0021(7) -0.0313(10) O3 0.0690(9) 0.0514(9) 0.0577(8) -0.0019(7) -0.0143(7) -0.0012(7) O4 0.0740(9) 0.0513(8) 0.0423(7) -0.0053(6) -0.0008(6) 0.0034(7) C1' 0.0754(14) 0.0457(12) 0.0537(11) -0.0077(9) 0.0057(10) 0.0146(11) C2' 0.0797(15) 0.0383(11) 0.0613(13) -0.0043(9) -0.0124(11) 0.0098(10) C3' 0.118(2) 0.0484(15) 0.0946(19) -0.0158(13) -0.0227(17) 0.0286(16) C4' 0.134(3) 0.084(2) 0.109(3) -0.033(2) -0.021(2) 0.063(2) C5' 0.113(3) 0.121(3) 0.103(2) -0.037(2) 0.016(2) 0.052(2) C6' 0.0876(18) 0.087(2) 0.0801(17) -0.0098(15) 0.0258(14) 0.0241(16) C7' 0.0534(11) 0.0432(11) 0.0520(11) -0.0005(9) 0.0127(9) 0.0001(9) C8' 0.0632(12) 0.0393(10) 0.0456(11) 0.0031(8) 0.0084(9) 0.0014(9) C9' 0.0865(16) 0.0447(11) 0.0424(10) 0.0062(9) -0.0102(11) -0.0238(11) C10' 0.0853(16) 0.0476(12) 0.0498(12) -0.0046(9) -0.0131(11) -0.0052(11) C11' 0.0661(13) 0.0394(11) 0.0499(11) -0.0016(8) 0.0192(9) 0.0020(9) C12' 0.0856(17) 0.0411(12) 0.0796(15) -0.0027(11) 0.0279(13) 0.0044(12) C13' 0.0896(19) 0.0469(14) 0.133(3) -0.0134(15) 0.0432(18) -0.0122(14) C14' 0.0750(17) 0.0551(17) 0.158(3) -0.0183(17) 0.0485(19) -0.0200(14) C15' 0.0596(13) 0.0535(14) 0.1029(19) -0.0119(13) 0.0287(13) -0.0059(11) C16' 0.0607(12) 0.0431(11) 0.0527(11) -0.0038(8) 0.0201(9) -0.0051(9) C17' 0.0610(12) 0.0461(11) 0.0458(10) 0.0039(8) 0.0151(9) 0.0060(9) C18' 0.0712(15) 0.0641(15) 0.0625(13) -0.0041(11) 0.0194(11) 0.0165(12) C19' 0.0674(16) 0.0885(19) 0.0737(16) 0.0036(14) 0.0202(13) 0.0234(14) C20' 0.0544(13) 0.102(2) 0.0685(15) 0.0082(15) 0.0089(11) 0.0083(14) C21' 0.0647(14) 0.0665(15) 0.0559(12) 0.0044(11) 0.0030(10) 0.0018(11) C22' 0.0573(12) 0.0459(11) 0.0431(10) 0.0064(8) 0.0084(8) 0.0047(9) C31' 0.0825(15) 0.0514(13) 0.0460(11) 0.0011(9) -0.0076(10) -0.0027(12) C32' 0.102(2) 0.0739(18) 0.0609(14) -0.0027(12) 0.0001(13) 0.0167(15) C33' 0.133(3) 0.075(2) 0.0659(16) -0.0020(14) 0.0070(17) 0.025(2) C34' 0.167(3) 0.0521(16) 0.0610(16) -0.0062(12) 0.0144(18) 0.017(2) C35' 0.125(2) 0.0527(15) 0.0524(13) -0.0019(11) -0.0044(13) -0.0179(15) C36' 0.0948(17) 0.0387(11) 0.0438(10) 0.0019(8) -0.0033(10) -0.0067(11) C37' 0.0707(14) 0.0507(13) 0.0584(12) 0.0013(10) -0.0136(11) -0.0016(11) C38' 0.0681(15) 0.0658(16) 0.0783(16) 0.0058(12) -0.0091(12) -0.0097(13) C39' 0.0737(17) 0.0646(17) 0.108(2) 0.0073(16) -0.0172(16) -0.0181(14) C40' 0.0866(19) 0.0483(14) 0.110(2) -0.0087(14) -0.0245(17) -0.0141(14) C41' 0.0828(17) 0.0496(14) 0.0820(17) -0.0135(12) -0.0165(13) -0.0064(12) C42' 0.0704(14) 0.0464(12) 0.0583(12) -0.0026(10) -0.0156(11) -0.0049(10) N1' 0.0613(10) 0.0382(9) 0.0483(9) -0.0028(7) 0.0083(7) 0.0055(7) N2' 0.0728(11) 0.0429(9) 0.0514(10) 0.0005(7) -0.0089(8) -0.0078(8) O1' 0.0662(9) 0.0529(9) 0.0641(9) 0.0014(7) -0.0021(7) -0.0003(8) O2' 0.0910(11) 0.0584(9) 0.0452(8) -0.0042(7) 0.0047(7) 0.0131(8) O3' 0.0847(12) 0.0930(13) 0.0513(9) 0.0053(8) -0.0115(8) -0.0253(10) O4' 0.1035(13) 0.0884(13) 0.0504(9) -0.0050(9) -0.0117(9) -0.0153(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 C1 N1 1.488(2) . ? C1 C6 1.526(3) . ? C1 C2 1.533(3) . ? C2 N2 1.490(2) . ? C2 C3 1.538(3) . ? C3 C4 1.520(3) . ? C4 C5 1.522(4) . ? C5 C6 1.518(3) . ? C7 O1 1.212(2) . ? C7 N1 1.413(2) . ? C7 C16 1.493(3) . ? C8 O2 1.214(2) . ? C8 N1 1.394(2) . ? C8 C22 1.496(3) . ? C9 O3 1.217(2) . ? C9 N2 1.404(2) . ? C9 C36 1.496(3) . ? C10 O4 1.213(2) . ? C10 N2 1.403(2) . ? C10 C42 1.493(3) . ? C11 C12 1.393(3) . ? C11 C16 1.397(3) . ? C11 C17 1.479(3) . ? C12 C13 1.385(4) . ? C13 C14 1.371(4) . ? C14 C15 1.374(4) . ? C15 C16 1.391(3) . ? C17 C22 1.394(3) . ? C17 C18 1.402(3) . ? C18 C19 1.374(4) . ? C19 C20 1.375(4) . ? C20 C21 1.380(4) . ? C21 C22 1.404(3) . ? C31 C36 1.399(3) . ? C31 C32 1.400(3) . ? C31 C37 1.475(3) . ? C32 C33 1.375(3) . ? C33 C34 1.376(4) . ? C34 C35 1.383(3) . ? C35 C36 1.396(3) . ? C37 C42 1.395(3) . ? C37 C38 1.400(3) . ? C38 C39 1.370(3) . ? C39 C40 1.384(4) . ? C40 C41 1.377(3) . ? C41 C42 1.395(3) . ? C1' N1' 1.493(3) . ? C1' C6' 1.527(4) . ? C1' C2' 1.548(3) . ? C2' N2' 1.476(3) . ? C2' C3' 1.524(3) . ? C3' C4' 1.513(5) . ? C4' C5' 1.515(6) . ? C5' C6' 1.535(4) . ? C7' O1' 1.219(2) . ? C7' N1' 1.391(3) . ? C7' C16' 1.503(3) . ? C8' O2' 1.209(2) . ? C8' N1' 1.408(3) . ? C8' C22' 1.496(3) . ? C9' O3' 1.211(3) . ? C9' N2' 1.413(3) . ? C9' C36' 1.486(4) . ? C10' O4' 1.216(3) . ? C10' N2' 1.410(3) . ? C10' C42' 1.489(4) . ? C11' C16' 1.393(3) . ? C11' C12' 1.402(3) . ? C11' C17' 1.474(3) . ? C12' C13' 1.370(4) . ? C13' C14' 1.359(4) . ? C14' C15' 1.381(4) . ? C15' C16' 1.394(3) . ? C17' C18' 1.397(3) . ? C17' C22' 1.399(3) . ? C18' C19' 1.375(4) . ? C19' C20' 1.371(4) . ? C20' C21' 1.380(4) . ? C21' C22' 1.392(3) . ? C31' C36' 1.392(4) . ? C31' C32' 1.399(4) . ? C31' C37' 1.478(3) . ? C32' C33' 1.370(4) . ? C33' C34' 1.369(5) . ? C34' C35' 1.384(5) . ? C35' C36' 1.410(3) . ? C37' C38' 1.393(4) . ? C37' C42' 1.397(4) . ? C38' C39' 1.387(4) . ? C39' C40' 1.368(5) . ? C40' C41' 1.382(4) . ? C41' C42' 1.407(3) . ? 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 C6 112.48(16) . . ? N1 C1 C2 114.85(15) . . ? C6 C1 C2 108.25(16) . . ? N2 C2 C1 115.41(15) . . ? N2 C2 C3 111.08(16) . . ? C1 C2 C3 107.82(15) . . ? C4 C3 C2 110.89(18) . . ? C3 C4 C5 112.25(18) . . ? C6 C5 C4 111.64(19) . . ? C5 C6 C1 110.41(18) . . ? O1 C7 N1 120.52(19) . . ? O1 C7 C16 121.95(17) . . ? N1 C7 C16 116.67(17) . . ? O2 C8 N1 120.34(19) . . ? O2 C8 C22 119.74(18) . . ? N1 C8 C22 119.29(16) . . ? O3 C9 N2 120.05(18) . . ? O3 C9 C36 119.12(17) . . ? N2 C9 C36 120.31(16) . . ? O4 C10 N2 120.43(18) . . ? O4 C10 C42 120.72(18) . . ? N2 C10 C42 118.10(16) . . ? C12 C11 C16 118.42(19) . . ? C12 C11 C17 120.93(19) . . ? C16 C11 C17 120.47(19) . . ? C13 C12 C11 120.8(2) . . ? C14 C13 C12 120.1(2) . . ? C13 C14 C15 120.1(2) . . ? C14 C15 C16 120.5(2) . . ? C15 C16 C11 120.0(2) . . ? C15 C16 C7 115.97(18) . . ? C11 C16 C7 124.02(17) . . ? C22 C17 C18 118.6(2) . . ? C22 C17 C11 122.74(17) . . ? C18 C17 C11 118.7(2) . . ? C19 C18 C17 121.2(2) . . ? C18 C19 C20 120.2(2) . . ? C19 C20 C21 119.9(2) . . ? C20 C21 C22 120.6(2) . . ? C17 C22 C21 119.4(2) . . ? C17 C22 C8 125.88(18) . . ? C21 C22 C8 114.7(2) . . ? C36 C31 C32 117.88(18) . . ? C36 C31 C37 123.21(18) . . ? C32 C31 C37 118.80(19) . . ? C33 C32 C31 121.6(2) . . ? C32 C33 C34 120.7(2) . . ? C33 C34 C35 118.7(2) . . ? C34 C35 C36 121.6(2) . . ? C35 C36 C31 119.45(18) . . ? C35 C36 C9 113.69(18) . . ? C31 C36 C9 126.84(17) . . ? C42 C37 C38 118.02(19) . . ? C42 C37 C31 122.13(18) . . ? C38 C37 C31 119.82(19) . . ? C39 C38 C37 121.5(2) . . ? C38 C39 C40 119.9(2) . . ? C41 C40 C39 120.0(2) . . ? C40 C41 C42 120.2(2) . . ? C37 C42 C41 120.27(19) . . ? C37 C42 C10 124.80(17) . . ? C41 C42 C10 114.91(18) . . ? C8 N1 C7 124.21(16) . . ? C8 N1 C1 115.69(15) . . ? C7 N1 C1 119.37(16) . . ? C10 N2 C9 125.45(16) . . ? C10 N2 C2 119.19(15) . . ? C9 N2 C2 114.36(15) . . ? N1' C1' C6' 112.7(2) . . ? N1' C1' C2' 111.92(17) . . ? C6' C1' C2' 110.7(2) . . ? N2' C2' C3' 112.8(2) . . ? N2' C2' C1' 113.58(17) . . ? C3' C2' C1' 109.1(2) . . ? C4' C3' C2' 110.4(3) . . ? C3' C4' C5' 112.2(3) . . ? C4' C5' C6' 110.8(3) . . ? C1' C6' C5' 110.2(3) . . ? O1' C7' N1' 120.22(19) . . ? O1' C7' C16' 119.55(19) . . ? N1' C7' C16' 119.47(18) . . ? O2' C8' N1' 120.79(19) . . ? O2' C8' C22' 120.21(19) . . ? N1' C8' C22' 118.25(16) . . ? O3' C9' N2' 120.0(2) . . ? O3' C9' C36' 121.1(2) . . ? N2' C9' C36' 118.38(18) . . ? O4' C10' N2' 119.8(2) . . ? O4' C10' C42' 121.7(2) . . ? N2' C10' C42' 117.56(19) . . ? C16' C11' C12' 118.1(2) . . ? C16' C11' C17' 123.00(18) . . ? C12' C11' C17' 118.9(2) . . ? C13' C12' C11' 121.1(2) . . ? C14' C13' C12' 120.6(3) . . ? C13' C14' C15' 119.9(3) . . ? C14' C15' C16' 120.6(3) . . ? C11' C16' C15' 119.7(2) . . ? C11' C16' C7' 126.61(19) . . ? C15' C16' C7' 113.7(2) . . ? C18' C17' C22' 117.8(2) . . ? C18' C17' C11' 120.4(2) . . ? C22' C17' C11' 121.72(18) . . ? C19' C18' C17' 121.3(2) . . ? C20' C19' C18' 120.6(2) . . ? C19' C20' C21' 119.6(2) . . ? C20' C21' C22' 120.5(2) . . ? C21' C22' C17' 120.2(2) . . ? C21' C22' C8' 114.83(19) . . ? C17' C22' C8' 124.90(19) . . ? C36' C31' C32' 118.7(2) . . ? C36' C31' C37' 120.8(2) . . ? C32' C31' C37' 120.5(2) . . ? C33' C32' C31' 121.6(3) . . ? C32' C33' C34' 119.9(3) . . ? C33' C34' C35' 120.5(3) . . ? C34' C35' C36' 119.9(3) . . ? C31' C36' C35' 119.4(3) . . ? C31' C36' C9' 124.9(2) . . ? C35' C36' C9' 115.6(2) . . ? C38' C37' C42' 119.2(2) . . ? C38' C37' C31' 119.6(2) . . ? C42' C37' C31' 121.1(2) . . ? C39' C38' C37' 120.5(3) . . ? C40' C39' C38' 120.5(3) . . ? C39' C40' C41' 120.0(3) . . ? C40' C41' C42' 120.4(3) . . ? C37' C42' C41' 119.2(2) . . ? C37' C42' C10' 125.8(2) . . ? C41' C42' C10' 114.9(2) . . ? C7' N1' C8' 125.00(17) . . ? C7' N1' C1' 119.44(17) . . ? C8' N1' C1' 115.42(16) . . ? C10' N2' C9' 123.4(2) . . ? C10' N2' C2' 118.78(19) . . ? C9' N2' C2' 117.64(18) . . ? 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 N2 -44.6(2) . . . . ? C6 C1 C2 N2 -171.26(16) . . . . ? N1 C1 C2 C3 -169.46(16) . . . . ? C6 C1 C2 C3 63.9(2) . . . . ? N2 C2 C3 C4 172.64(17) . . . . ? C1 C2 C3 C4 -60.0(2) . . . . ? C2 C3 C4 C5 53.7(3) . . . . ? C3 C4 C5 C6 -51.1(3) . . . . ? C4 C5 C6 C1 55.4(3) . . . . ? N1 C1 C6 C5 169.67(17) . . . . ? C2 C1 C6 C5 -62.4(2) . . . . ? C16 C11 C12 C13 -0.2(3) . . . . ? C17 C11 C12 C13 174.9(2) . . . . ? C11 C12 C13 C14 -1.8(4) . . . . ? C12 C13 C14 C15 1.7(4) . . . . ? C13 C14 C15 C16 0.5(4) . . . . ? C14 C15 C16 C11 -2.5(3) . . . . ? C14 C15 C16 C7 176.4(2) . . . . ? C12 C11 C16 C15 2.4(3) . . . . ? C17 C11 C16 C15 -172.84(18) . . . . ? C12 C11 C16 C7 -176.42(18) . . . . ? C17 C11 C16 C7 8.4(3) . . . . ? O1 C7 C16 C15 46.4(3) . . . . ? N1 C7 C16 C15 -123.04(19) . . . . ? O1 C7 C16 C11 -134.8(2) . . . . ? N1 C7 C16 C11 55.8(3) . . . . ? C12 C11 C17 C22 140.4(2) . . . . ? C16 C11 C17 C22 -44.5(3) . . . . ? C12 C11 C17 C18 -39.3(3) . . . . ? C16 C11 C17 C18 135.7(2) . . . . ? C22 C17 C18 C19 0.0(3) . . . . ? C11 C17 C18 C19 179.7(2) . . . . ? C17 C18 C19 C20 -0.7(4) . . . . ? C18 C19 C20 C21 -0.1(4) . . . . ? C19 C20 C21 C22 1.6(4) . . . . ? C18 C17 C22 C21 1.6(3) . . . . ? C11 C17 C22 C21 -178.14(19) . . . . ? C18 C17 C22 C8 -178.9(2) . . . . ? C11 C17 C22 C8 1.3(3) . . . . ? C20 C21 C22 C17 -2.4(3) . . . . ? C20 C21 C22 C8 178.1(2) . . . . ? O2 C8 C22 C17 -141.3(2) . . . . ? N1 C8 C22 C17 47.8(3) . . . . ? O2 C8 C22 C21 38.2(3) . . . . ? N1 C8 C22 C21 -132.7(2) . . . . ? C36 C31 C32 C33 -1.3(3) . . . . ? C37 C31 C32 C33 175.1(2) . . . . ? C31 C32 C33 C34 -1.0(4) . . . . ? C32 C33 C34 C35 1.7(4) . . . . ? C33 C34 C35 C36 -0.1(4) . . . . ? C34 C35 C36 C31 -2.2(3) . . . . ? C34 C35 C36 C9 179.2(2) . . . . ? C32 C31 C36 C35 2.9(3) . . . . ? C37 C31 C36 C35 -173.35(19) . . . . ? C32 C31 C36 C9 -178.79(19) . . . . ? C37 C31 C36 C9 5.0(3) . . . . ? O3 C9 C36 C35 32.9(3) . . . . ? N2 C9 C36 C35 -138.81(18) . . . . ? O3 C9 C36 C31 -145.5(2) . . . . ? N2 C9 C36 C31 42.8(3) . . . . ? C36 C31 C37 C42 -40.1(3) . . . . ? C32 C31 C37 C42 143.8(2) . . . . ? C36 C31 C37 C38 141.8(2) . . . . ? C32 C31 C37 C38 -34.3(3) . . . . ? C42 C37 C38 C39 -0.4(3) . . . . ? C31 C37 C38 C39 177.8(2) . . . . ? C37 C38 C39 C40 -0.1(4) . . . . ? C38 C39 C40 C41 -0.6(4) . . . . ? C39 C40 C41 C42 1.7(4) . . . . ? C38 C37 C42 C41 1.5(3) . . . . ? C31 C37 C42 C41 -176.65(18) . . . . ? C38 C37 C42 C10 179.80(19) . . . . ? C31 C37 C42 C10 1.7(3) . . . . ? C40 C41 C42 C37 -2.2(3) . . . . ? C40 C41 C42 C10 179.35(19) . . . . ? O4 C10 C42 C37 -134.4(2) . . . . ? N2 C10 C42 C37 55.6(3) . . . . ? O4 C10 C42 C41 44.0(3) . . . . ? N2 C10 C42 C41 -126.02(19) . . . . ? O2 C8 N1 C7 172.9(2) . . . . ? C22 C8 N1 C7 -16.3(3) . . . . ? O2 C8 N1 C1 -17.0(3) . . . . ? C22 C8 N1 C1 153.76(18) . . . . ? O1 C7 N1 C8 141.1(2) . . . . ? C16 C7 N1 C8 -49.3(3) . . . . ? O1 C7 N1 C1 -28.6(3) . . . . ? C16 C7 N1 C1 140.95(17) . . . . ? C6 C1 N1 C8 -84.2(2) . . . . ? C2 C1 N1 C8 151.36(17) . . . . ? C6 C1 N1 C7 86.4(2) . . . . ? C2 C1 N1 C7 -38.0(2) . . . . ? O4 C10 N2 C9 147.30(19) . . . . ? C42 C10 N2 C9 -42.6(3) . . . . ? O4 C10 N2 C2 -20.6(3) . . . . ? C42 C10 N2 C2 149.54(16) . . . . ? O3 C9 N2 C10 169.38(18) . . . . ? C36 C9 N2 C10 -19.0(3) . . . . ? O3 C9 N2 C2 -22.3(3) . . . . ? C36 C9 N2 C2 149.41(16) . . . . ? C1 C2 N2 C10 -42.3(2) . . . . ? C3 C2 N2 C10 80.8(2) . . . . ? C1 C2 N2 C9 148.58(16) . . . . ? C3 C2 N2 C9 -88.31(19) . . . . ? N1' C1' C2' N2' -47.6(2) . . . . ? C6' C1' C2' N2' -174.29(19) . . . . ? N1' C1' C2' C3' -174.4(2) . . . . ? C6' C1' C2' C3' 58.9(3) . . . . ? N2' C2' C3' C4' 174.7(2) . . . . ? C1' C2' C3' C4' -58.0(3) . . . . ? C2' C3' C4' C5' 57.5(3) . . . . ? C3' C4' C5' C6' -55.7(4) . . . . ? N1' C1' C6' C5' 176.3(2) . . . . ? C2' C1' C6' C5' -57.5(3) . . . . ? C4' C5' C6' C1' 55.2(4) . . . . ? C16' C11' C12' C13' -0.1(4) . . . . ? C17' C11' C12' C13' -178.0(2) . . . . ? C11' C12' C13' C14' 2.1(5) . . . . ? C12' C13' C14' C15' -1.8(5) . . . . ? C13' C14' C15' C16' -0.3(5) . . . . ? C12' C11' C16' C15' -2.0(3) . . . . ? C17' C11' C16' C15' 175.8(2) . . . . ? C12' C11' C16' C7' 179.2(2) . . . . ? C17' C11' C16' C7' -3.1(3) . . . . ? C14' C15' C16' C11' 2.2(4) . . . . ? C14' C15' C16' C7' -178.8(3) . . . . ? O1' C7' C16' C11' 142.4(2) . . . . ? N1' C7' C16' C11' -47.6(3) . . . . ? O1' C7' C16' C15' -36.5(3) . . . . ? N1' C7' C16' C15' 133.5(2) . . . . ? C16' C11' C17' C18' -144.3(2) . . . . ? C12' C11' C17' C18' 33.4(3) . . . . ? C16' C11' C17' C22' 39.5(3) . . . . ? C12' C11' C17' C22' -142.8(2) . . . . ? C22' C17' C18' C19' -0.7(3) . . . . ? C11' C17' C18' C19' -177.0(2) . . . . ? C17' C18' C19' C20' 0.9(4) . . . . ? C18' C19' C20' C21' -0.4(4) . . . . ? C19' C20' C21' C22' -0.2(4) . . . . ? C20' C21' C22' C17' 0.4(3) . . . . ? C20' C21' C22' C8' 178.0(2) . . . . ? C18' C17' C22' C21' 0.0(3) . . . . ? C11' C17' C22' C21' 176.33(19) . . . . ? C18' C17' C22' C8' -177.35(19) . . . . ? C11' C17' C22' C8' -1.1(3) . . . . ? O2' C8' C22' C21' -43.3(3) . . . . ? N1' C8' C22' C21' 126.8(2) . . . . ? O2' C8' C22' C17' 134.2(2) . . . . ? N1' C8' C22' C17' -55.7(3) . . . . ? C36' C31' C32' C33' -0.1(4) . . . . ? C37' C31' C32' C33' -177.6(2) . . . . ? C31' C32' C33' C34' 1.1(4) . . . . ? C32' C33' C34' C35' -0.7(4) . . . . ? C33' C34' C35' C36' -0.7(4) . . . . ? C32' C31' C36' C35' -1.4(3) . . . . ? C37' C31' C36' C35' 176.2(2) . . . . ? C32' C31' C36' C9' -178.0(2) . . . . ? C37' C31' C36' C9' -0.5(3) . . . . ? C34' C35' C36' C31' 1.8(3) . . . . ? C34' C35' C36' C9' 178.7(2) . . . . ? O3' C9' C36' C31' 131.7(2) . . . . ? N2' C9' C36' C31' -56.7(3) . . . . ? O3' C9' C36' C35' -45.1(3) . . . . ? N2' C9' C36' C35' 126.5(2) . . . . ? C36' C31' C37' C38' -138.5(2) . . . . ? C32' C31' C37' C38' 39.0(3) . . . . ? C36' C31' C37' C42' 44.9(3) . . . . ? C32' C31' C37' C42' -137.6(2) . . . . ? C42' C37' C38' C39' -0.4(3) . . . . ? C31' C37' C38' C39' -177.0(2) . . . . ? C37' C38' C39' C40' 3.5(4) . . . . ? C38' C39' C40' C41' -3.5(4) . . . . ? C39' C40' C41' C42' 0.2(4) . . . . ? C38' C37' C42' C41' -2.8(3) . . . . ? C31' C37' C42' C41' 173.8(2) . . . . ? C38' C37' C42' C10' 175.4(2) . . . . ? C31' C37' C42' C10' -8.0(3) . . . . ? C40' C41' C42' C37' 2.9(3) . . . . ? C40' C41' C42' C10' -175.5(2) . . . . ? O4' C10' C42' C37' 138.9(3) . . . . ? N2' C10' C42' C37' -52.2(3) . . . . ? O4' C10' C42' C41' -42.8(3) . . . . ? N2' C10' C42' C41' 126.1(2) . . . . ? O1' C7' N1' C8' -165.91(19) . . . . ? C16' C7' N1' C8' 24.1(3) . . . . ? O1' C7' N1' C1' 18.6(3) . . . . ? C16' C7' N1' C1' -151.35(19) . . . . ? O2' C8' N1' C7' -150.4(2) . . . . ? C22' C8' N1' C7' 39.5(3) . . . . ? O2' C8' N1' C1' 25.2(3) . . . . ? C22' C8' N1' C1' -144.93(18) . . . . ? C6' C1' N1' C7' 53.9(3) . . . . ? C2' C1' N1' C7' -71.6(2) . . . . ? C6' C1' N1' C8' -122.0(2) . . . . ? C2' C1' N1' C8' 112.5(2) . . . . ? O4' C10' N2' C9' -155.1(2) . . . . ? C42' C10' N2' C9' 35.8(3) . . . . ? O4' C10' N2' C2' 30.2(3) . . . . ? C42' C10' N2' C2' -139.0(2) . . . . ? O3' C9' N2' C10' -156.6(2) . . . . ? C36' C9' N2' C10' 31.8(3) . . . . ? O3' C9' N2' C2' 18.2(3) . . . . ? C36' C9' N2' C2' -153.42(19) . . . . ? C3' C2' N2' C10' 47.7(3) . . . . ? C1' C2' N2' C10' -77.2(2) . . . . ? C3' C2' N2' C9' -127.4(2) . . . . ? C1' C2' N2' C9' 107.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 65.09 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.138 _refine_diff_density_min -0.128 _refine_diff_density_rms 0.030 data_mk11 _database_code_CSD 187217 _audit_creation_method SHELXL-97 _chemical_name_systematic ; N,N'-Bis(diphenoyl)-1,2-diaminobenzene ; _chemical_name_common ? _chemical_melting_point 289-92\% _chemical_formula_moiety 'C34 H20 N2 O4' _chemical_formula_sum 'C34 H20 N2 O4' _chemical_formula_weight 520.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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/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 9.855(2) _cell_length_b 12.280(2) _cell_length_c 20.602(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.97(3) _cell_angle_gamma 90.00 _cell_volume 2469.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 6.6 _cell_measurement_theta_max 12.7 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.400 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.750 _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 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM-4 four circle diffractometer' _diffrn_measurement_method '\Q--2\Q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.35 _diffrn_reflns_number 4039 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0238 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.20 _diffrn_reflns_theta_max 65.10 _reflns_number_total 3920 _reflns_number_gt 2961 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_cell_refinement 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_data_reduction 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Simens Analytical X-Ray Instruments (1989)' _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. The structures were phased by direct methods (SHELXS86 program) and refined by full-matrix least-squares using the SHELXL97 program. Siemens computer graphics program was used to prepare drawings. Anisotropic thermal parameters were refined for all non-hydrogen atoms. The hydrogen atoms were placed at calculated positions (C-H = 0.96 A) and refined in a riding model with their Uiso increased by 1.2 compared to Ueq of atoms to which they were bonded. ; _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^)+(0.0893P)^2^+0.7619P] 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 SHELXL _refine_ls_extinction_coef 0.0019(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3920 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1435 _refine_ls_wR_factor_gt 0.1285 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _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 C1 C -0.0173(2) 0.21436(17) 0.08563(11) 0.0443(5) Uani 1 1 d . . . C2 C 0.0566(2) 0.30898(17) 0.07947(11) 0.0426(5) Uani 1 1 d . . . C3 C 0.1812(3) 0.3032(2) 0.05588(12) 0.0525(6) Uani 1 1 d . . . H3 H 0.2344 0.3680 0.0530 0.063 Uiso 1 1 d R . . C4 C 0.2293(3) 0.2037(2) 0.03727(13) 0.0623(7) Uani 1 1 d . . . H4 H 0.3146 0.1998 0.0199 0.075 Uiso 1 1 d R . . C5 C 0.1550(3) 0.1104(2) 0.04308(14) 0.0652(7) Uani 1 1 d . . . H5 H 0.1897 0.0414 0.0309 0.078 Uiso 1 1 d R . . C6 C 0.0316(3) 0.11571(19) 0.06673(13) 0.0580(7) Uani 1 1 d . . . H6 H -0.0216 0.0509 0.0698 0.070 Uiso 1 1 d R . . C7 C -0.1356(2) 0.24904(18) 0.17919(11) 0.0441(5) Uani 1 1 d . . . C8 C -0.2629(3) 0.17852(18) 0.07319(12) 0.0476(6) Uani 1 1 d . . . C9 C -0.1090(2) 0.45256(17) 0.05485(11) 0.0413(5) Uani 1 1 d . . . C10 C 0.0866(2) 0.47036(18) 0.14815(11) 0.0423(5) Uani 1 1 d . . . C11 C -0.3875(2) 0.29044(18) 0.18657(11) 0.0455(5) Uani 1 1 d . . . C12 C -0.2486(2) 0.31573(17) 0.19962(11) 0.0447(5) Uani 1 1 d . . . C13 C -0.2065(3) 0.4102(2) 0.23415(12) 0.0557(6) Uani 1 1 d . . . H13 H -0.1104 0.4257 0.2443 0.067 Uiso 1 1 d R . . C14 C -0.3009(3) 0.4806(2) 0.25388(13) 0.0674(8) Uani 1 1 d . . . H14 H -0.2708 0.5461 0.2770 0.081 Uiso 1 1 d R . . C15 C -0.4381(3) 0.4572(2) 0.24038(13) 0.0676(8) Uani 1 1 d . . . H15 H -0.5041 0.5070 0.2536 0.081 Uiso 1 1 d R . . C16 C -0.4815(3) 0.3625(2) 0.20791(13) 0.0593(7) Uani 1 1 d . . . H16 H -0.5775 0.3459 0.1995 0.071 Uiso 1 1 d R . . C21 C -0.4341(2) 0.18456(18) 0.15744(11) 0.0452(5) Uani 1 1 d . . . C22 C -0.3775(2) 0.13553(17) 0.10614(11) 0.0458(5) Uani 1 1 d . . . C23 C -0.4285(3) 0.03466(19) 0.08187(13) 0.0561(6) Uani 1 1 d . . . H23 H -0.3919 0.0022 0.0456 0.067 Uiso 1 1 d R . . C24 C -0.5309(3) -0.0182(2) 0.10923(14) 0.0640(7) Uani 1 1 d . . . H24 H -0.5646 -0.0876 0.0927 0.077 Uiso 1 1 d R . . C25 C -0.5845(3) 0.0298(2) 0.16023(14) 0.0652(7) Uani 1 1 d . . . H25 H -0.6541 -0.0070 0.1801 0.078 Uiso 1 1 d R . . C26 C -0.5388(3) 0.1297(2) 0.18354(12) 0.0561(6) Uani 1 1 d . . . H26 H -0.5796 0.1631 0.2183 0.067 Uiso 1 1 d R . . C31 C -0.1626(2) 0.62712(17) 0.11459(11) 0.0428(5) Uani 1 1 d . . . C32 C -0.2038(2) 0.53162(17) 0.08054(10) 0.0417(5) Uani 1 1 d . . . C33 C -0.3421(2) 0.5060(2) 0.06630(12) 0.0529(6) Uani 1 1 d . . . H33 H -0.3695 0.4411 0.0421 0.063 Uiso 1 1 d R . . C34 C -0.4402(3) 0.5731(2) 0.08633(14) 0.0650(7) Uani 1 1 d . . . H34 H -0.5354 0.5544 0.0768 0.078 Uiso 1 1 d R . . C35 C -0.4013(3) 0.6671(2) 0.12073(15) 0.0649(7) Uani 1 1 d . . . H35 H -0.4694 0.7138 0.1351 0.078 Uiso 1 1 d R . . C36 C -0.2651(3) 0.6938(2) 0.13409(13) 0.0555(6) Uani 1 1 d . . . H36 H -0.2393 0.7600 0.1574 0.067 Uiso 1 1 d R . . C41 C -0.0190(2) 0.66236(17) 0.12854(11) 0.0431(5) Uani 1 1 d . . . C42 C 0.0909(2) 0.59183(18) 0.14808(10) 0.0426(5) Uani 1 1 d . . . C43 C 0.2207(2) 0.6348(2) 0.16917(12) 0.0533(6) Uani 1 1 d . . . H43 H 0.2951 0.5862 0.1837 0.064 Uiso 1 1 d R . . C44 C 0.2439(3) 0.7454(2) 0.16902(15) 0.0644(7) Uani 1 1 d . . . H44 H 0.3328 0.7740 0.1853 0.077 Uiso 1 1 d R . . C45 C 0.1386(3) 0.8140(2) 0.14609(16) 0.0708(8) Uani 1 1 d . . . H45 H 0.1553 0.8908 0.1434 0.085 Uiso 1 1 d R . . C46 C 0.0094(3) 0.77382(19) 0.12691(14) 0.0572(6) Uani 1 1 d . . . H46 H -0.0635 0.8234 0.1117 0.069 Uiso 1 1 d R . . N1 N -0.14591(18) 0.21917(14) 0.11219(9) 0.0430(4) Uani 1 1 d . . . N2 N 0.00523(18) 0.41368(13) 0.09727(8) 0.0397(4) Uani 1 1 d . . . O7 O -0.03026(18) 0.23291(15) 0.21519(8) 0.0615(5) Uani 1 1 d . . . O8 O -0.2621(2) 0.16579(17) 0.01513(9) 0.0691(5) Uani 1 1 d . . . O9 O -0.13816(19) 0.41256(14) 0.00142(8) 0.0569(5) Uani 1 1 d . . . O10 O 0.16520(19) 0.41878(14) 0.18699(9) 0.0594(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 0.0513(13) 0.0373(11) 0.0460(13) -0.0020(9) 0.0122(10) 0.0018(9) C2 0.0496(12) 0.0371(11) 0.0434(12) 0.0011(9) 0.0152(10) 0.0042(9) C3 0.0529(14) 0.0555(14) 0.0523(14) 0.0015(11) 0.0185(11) 0.0017(11) C4 0.0575(15) 0.0738(18) 0.0587(16) -0.0037(13) 0.0186(13) 0.0181(13) C5 0.0682(17) 0.0567(16) 0.0711(18) -0.0145(13) 0.0112(14) 0.0203(13) C6 0.0675(16) 0.0392(12) 0.0677(17) -0.0084(11) 0.0104(13) 0.0043(11) C7 0.0501(13) 0.0403(11) 0.0425(13) 0.0032(10) 0.0089(11) -0.0131(10) C8 0.0583(14) 0.0400(11) 0.0451(14) -0.0032(10) 0.0100(11) -0.0075(10) C9 0.0508(13) 0.0362(10) 0.0385(12) 0.0016(9) 0.0113(10) -0.0045(10) C10 0.0428(12) 0.0427(11) 0.0431(13) 0.0034(10) 0.0124(10) 0.0009(10) C11 0.0576(14) 0.0407(11) 0.0400(12) 0.0024(9) 0.0135(10) -0.0052(10) C12 0.0615(14) 0.0381(11) 0.0368(12) 0.0018(9) 0.0147(10) -0.0089(10) C13 0.0731(16) 0.0498(13) 0.0460(14) -0.0073(11) 0.0149(12) -0.0177(12) C14 0.098(2) 0.0478(14) 0.0596(17) -0.0145(12) 0.0223(15) -0.0081(14) C15 0.090(2) 0.0546(15) 0.0620(17) -0.0077(13) 0.0229(15) 0.0098(14) C16 0.0651(16) 0.0579(15) 0.0574(16) -0.0019(12) 0.0177(13) 0.0023(12) C21 0.0495(13) 0.0427(12) 0.0437(13) 0.0031(10) 0.0070(10) -0.0079(10) C22 0.0517(13) 0.0394(11) 0.0457(13) -0.0004(10) 0.0051(10) -0.0077(10) C23 0.0656(16) 0.0451(13) 0.0564(15) -0.0032(11) 0.0041(12) -0.0099(12) C24 0.0713(17) 0.0468(14) 0.0698(18) 0.0016(13) -0.0053(14) -0.0236(13) C25 0.0660(16) 0.0647(16) 0.0638(17) 0.0135(14) 0.0051(13) -0.0246(14) C26 0.0590(15) 0.0605(15) 0.0498(15) 0.0061(12) 0.0108(12) -0.0146(12) C31 0.0467(12) 0.0417(11) 0.0428(12) 0.0036(9) 0.0160(10) 0.0015(9) C32 0.0461(12) 0.0414(11) 0.0388(12) 0.0051(9) 0.0105(9) -0.0023(9) C33 0.0487(13) 0.0573(14) 0.0528(14) 0.0045(11) 0.0076(11) -0.0087(11) C34 0.0429(13) 0.0817(19) 0.0723(18) 0.0047(15) 0.0150(13) 0.0007(13) C35 0.0511(15) 0.0757(18) 0.0718(18) 0.0000(14) 0.0218(13) 0.0150(13) C36 0.0560(15) 0.0521(14) 0.0621(16) -0.0055(12) 0.0208(12) 0.0067(11) C41 0.0507(13) 0.0382(11) 0.0430(12) -0.0027(9) 0.0151(10) -0.0010(9) C42 0.0458(12) 0.0437(11) 0.0414(12) -0.0031(9) 0.0170(10) -0.0047(10) C43 0.0464(13) 0.0539(14) 0.0625(16) -0.0056(12) 0.0177(11) -0.0038(11) C44 0.0525(15) 0.0563(15) 0.087(2) -0.0102(14) 0.0200(14) -0.0162(12) C45 0.0683(18) 0.0435(14) 0.104(2) -0.0075(14) 0.0228(17) -0.0151(13) C46 0.0588(15) 0.0416(13) 0.0721(17) -0.0013(12) 0.0123(13) -0.0024(11) N1 0.0469(10) 0.0392(9) 0.0442(11) -0.0044(8) 0.0116(8) -0.0069(8) N2 0.0453(10) 0.0335(9) 0.0420(10) -0.0016(7) 0.0120(8) -0.0014(7) O7 0.0580(11) 0.0752(12) 0.0510(11) 0.0060(9) 0.0069(9) -0.0078(9) O8 0.0764(13) 0.0887(14) 0.0440(10) -0.0113(9) 0.0151(9) -0.0206(10) O9 0.0740(12) 0.0544(10) 0.0418(10) -0.0076(8) 0.0063(8) 0.0047(8) O10 0.0651(11) 0.0527(10) 0.0584(11) 0.0048(8) 0.0015(9) 0.0012(8) _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 C6 1.380(3) . ? C1 C2 1.387(3) . ? C1 N1 1.450(3) . ? C2 C3 1.383(3) . ? C2 N2 1.448(3) . ? C3 C4 1.383(3) . ? C4 C5 1.374(4) . ? C5 C6 1.373(4) . ? C7 O7 1.206(3) . ? C7 N1 1.418(3) . ? C7 C12 1.489(3) . ? C8 O8 1.207(3) . ? C8 N1 1.403(3) . ? C8 C22 1.492(3) . ? C9 O9 1.203(3) . ? C9 N2 1.409(3) . ? C9 C32 1.494(3) . ? C10 O10 1.212(3) . ? C10 N2 1.412(3) . ? C10 C42 1.492(3) . ? C11 C12 1.393(3) . ? C11 C16 1.395(3) . ? C11 C21 1.478(3) . ? C12 C13 1.394(3) . ? C13 C14 1.372(4) . ? C14 C15 1.373(4) . ? C15 C16 1.380(4) . ? C21 C22 1.398(3) . ? C21 C26 1.400(3) . ? C22 C23 1.403(3) . ? C23 C24 1.384(4) . ? C24 C25 1.373(4) . ? C25 C26 1.370(4) . ? C31 C32 1.398(3) . ? C31 C36 1.402(3) . ? C31 C41 1.470(3) . ? C32 C33 1.391(3) . ? C33 C34 1.376(4) . ? C34 C35 1.381(4) . ? C35 C36 1.371(4) . ? C41 C46 1.398(3) . ? C41 C42 1.401(3) . ? C42 C43 1.397(3) . ? C43 C44 1.377(4) . ? C44 C45 1.369(4) . ? C45 C46 1.371(4) . ? 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 C6 C1 C2 120.1(2) . . ? C6 C1 N1 120.0(2) . . ? C2 C1 N1 119.90(18) . . ? C3 C2 C1 119.5(2) . . ? C3 C2 N2 119.57(19) . . ? C1 C2 N2 120.94(18) . . ? C2 C3 C4 119.8(2) . . ? C5 C4 C3 120.4(2) . . ? C6 C5 C4 120.0(2) . . ? C5 C6 C1 120.2(2) . . ? O7 C7 N1 119.7(2) . . ? O7 C7 C12 122.0(2) . . ? N1 C7 C12 117.5(2) . . ? O8 C8 N1 119.7(2) . . ? O8 C8 C22 120.9(2) . . ? N1 C8 C22 118.6(2) . . ? O9 C9 N2 119.9(2) . . ? O9 C9 C32 120.5(2) . . ? N2 C9 C32 119.03(18) . . ? O10 C10 N2 118.5(2) . . ? O10 C10 C42 120.5(2) . . ? N2 C10 C42 120.4(2) . . ? C12 C11 C16 118.4(2) . . ? C12 C11 C21 121.1(2) . . ? C16 C11 C21 120.2(2) . . ? C11 C12 C13 119.9(2) . . ? C11 C12 C7 125.2(2) . . ? C13 C12 C7 114.9(2) . . ? C14 C13 C12 120.6(3) . . ? C13 C14 C15 119.8(2) . . ? C14 C15 C16 120.3(3) . . ? C15 C16 C11 120.8(3) . . ? C22 C21 C26 118.4(2) . . ? C22 C21 C11 123.5(2) . . ? C26 C21 C11 118.1(2) . . ? C21 C22 C23 119.2(2) . . ? C21 C22 C8 126.7(2) . . ? C23 C22 C8 114.0(2) . . ? C24 C23 C22 121.0(2) . . ? C25 C24 C23 119.3(2) . . ? C26 C25 C24 120.7(2) . . ? C25 C26 C21 121.3(2) . . ? C32 C31 C36 117.6(2) . . ? C32 C31 C41 123.36(19) . . ? C36 C31 C41 119.0(2) . . ? C33 C32 C31 120.2(2) . . ? C33 C32 C9 114.9(2) . . ? C31 C32 C9 124.8(2) . . ? C34 C33 C32 120.7(2) . . ? C33 C34 C35 119.9(2) . . ? C36 C35 C34 119.8(2) . . ? C35 C36 C31 121.8(2) . . ? C46 C41 C42 117.6(2) . . ? C46 C41 C31 118.3(2) . . ? C42 C41 C31 123.97(19) . . ? C43 C42 C41 119.6(2) . . ? C43 C42 C10 113.7(2) . . ? C41 C42 C10 126.7(2) . . ? C44 C43 C42 121.1(2) . . ? C45 C44 C43 119.3(2) . . ? C44 C45 C46 120.5(2) . . ? C45 C46 C41 121.7(2) . . ? C8 N1 C7 126.27(18) . . ? C8 N1 C1 117.49(18) . . ? C7 N1 C1 115.45(19) . . ? C9 N2 C10 128.02(18) . . ? C9 N2 C2 114.92(17) . . ? C10 N2 C2 116.31(18) . . ? 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 C6 C1 C2 C3 -1.7(4) . . . . ? N1 C1 C2 C3 178.1(2) . . . . ? C6 C1 C2 N2 178.2(2) . . . . ? N1 C1 C2 N2 -2.0(3) . . . . ? C1 C2 C3 C4 1.5(4) . . . . ? N2 C2 C3 C4 -178.4(2) . . . . ? C2 C3 C4 C5 -1.0(4) . . . . ? C3 C4 C5 C6 0.8(4) . . . . ? C4 C5 C6 C1 -0.9(4) . . . . ? C2 C1 C6 C5 1.4(4) . . . . ? N1 C1 C6 C5 -178.4(2) . . . . ? C16 C11 C12 C13 1.0(3) . . . . ? C21 C11 C12 C13 -172.3(2) . . . . ? C16 C11 C12 C7 -178.7(2) . . . . ? C21 C11 C12 C7 7.9(3) . . . . ? O7 C7 C12 C11 -138.1(2) . . . . ? N1 C7 C12 C11 51.9(3) . . . . ? O7 C7 C12 C13 42.1(3) . . . . ? N1 C7 C12 C13 -127.8(2) . . . . ? C11 C12 C13 C14 -1.9(4) . . . . ? C7 C12 C13 C14 177.9(2) . . . . ? C12 C13 C14 C15 0.9(4) . . . . ? C13 C14 C15 C16 1.0(4) . . . . ? C14 C15 C16 C11 -1.9(4) . . . . ? C12 C11 C16 C15 0.9(4) . . . . ? C21 C11 C16 C15 174.3(2) . . . . ? C12 C11 C21 C22 -42.4(3) . . . . ? C16 C11 C21 C22 144.4(2) . . . . ? C12 C11 C21 C26 136.3(2) . . . . ? C16 C11 C21 C26 -36.9(3) . . . . ? C26 C21 C22 C23 1.1(3) . . . . ? C11 C21 C22 C23 179.9(2) . . . . ? C26 C21 C22 C8 -177.9(2) . . . . ? C11 C21 C22 C8 0.8(4) . . . . ? O8 C8 C22 C21 -143.9(3) . . . . ? N1 C8 C22 C21 45.9(3) . . . . ? O8 C8 C22 C23 37.0(3) . . . . ? N1 C8 C22 C23 -133.2(2) . . . . ? C21 C22 C23 C24 -2.0(4) . . . . ? C8 C22 C23 C24 177.2(2) . . . . ? C22 C23 C24 C25 1.0(4) . . . . ? C23 C24 C25 C26 0.8(4) . . . . ? C24 C25 C26 C21 -1.6(4) . . . . ? C22 C21 C26 C25 0.6(4) . . . . ? C11 C21 C26 C25 -178.2(2) . . . . ? C36 C31 C32 C33 0.8(3) . . . . ? C41 C31 C32 C33 -176.8(2) . . . . ? C36 C31 C32 C9 178.6(2) . . . . ? C41 C31 C32 C9 0.9(3) . . . . ? O9 C9 C32 C33 39.6(3) . . . . ? N2 C9 C32 C33 -131.5(2) . . . . ? O9 C9 C32 C31 -138.3(2) . . . . ? N2 C9 C32 C31 50.6(3) . . . . ? C31 C32 C33 C34 -1.0(3) . . . . ? C9 C32 C33 C34 -179.0(2) . . . . ? C32 C33 C34 C35 0.2(4) . . . . ? C33 C34 C35 C36 0.8(4) . . . . ? C34 C35 C36 C31 -1.0(4) . . . . ? C32 C31 C36 C35 0.2(4) . . . . ? C41 C31 C36 C35 178.0(2) . . . . ? C32 C31 C41 C46 143.8(2) . . . . ? C36 C31 C41 C46 -33.8(3) . . . . ? C32 C31 C41 C42 -41.0(3) . . . . ? C36 C31 C41 C42 141.4(2) . . . . ? C46 C41 C42 C43 4.3(3) . . . . ? C31 C41 C42 C43 -170.9(2) . . . . ? C46 C41 C42 C10 -174.6(2) . . . . ? C31 C41 C42 C10 10.2(3) . . . . ? O10 C10 C42 C43 29.6(3) . . . . ? N2 C10 C42 C43 -141.2(2) . . . . ? O10 C10 C42 C41 -151.5(2) . . . . ? N2 C10 C42 C41 37.8(3) . . . . ? C41 C42 C43 C44 -2.2(3) . . . . ? C10 C42 C43 C44 176.8(2) . . . . ? C42 C43 C44 C45 -1.8(4) . . . . ? C43 C44 C45 C46 3.7(5) . . . . ? C44 C45 C46 C41 -1.5(5) . . . . ? C42 C41 C46 C45 -2.5(4) . . . . ? C31 C41 C46 C45 173.0(3) . . . . ? O8 C8 N1 C7 173.0(2) . . . . ? C22 C8 N1 C7 -16.6(3) . . . . ? O8 C8 N1 C1 -17.6(3) . . . . ? C22 C8 N1 C1 152.8(2) . . . . ? O7 C7 N1 C8 144.5(2) . . . . ? C12 C7 N1 C8 -45.3(3) . . . . ? O7 C7 N1 C1 -25.0(3) . . . . ? C12 C7 N1 C1 145.21(19) . . . . ? C6 C1 N1 C8 -57.4(3) . . . . ? C2 C1 N1 C8 122.8(2) . . . . ? C6 C1 N1 C7 113.1(2) . . . . ? C2 C1 N1 C7 -66.7(3) . . . . ? O9 C9 N2 C10 153.8(2) . . . . ? C32 C9 N2 C10 -35.1(3) . . . . ? O9 C9 N2 C2 -15.9(3) . . . . ? C32 C9 N2 C2 155.28(18) . . . . ? O10 C10 N2 C9 167.1(2) . . . . ? C42 C10 N2 C9 -22.0(3) . . . . ? O10 C10 N2 C2 -23.4(3) . . . . ? C42 C10 N2 C2 147.53(18) . . . . ? C3 C2 N2 C9 109.5(2) . . . . ? C1 C2 N2 C9 -70.4(3) . . . . ? C3 C2 N2 C10 -61.4(3) . . . . ? C1 C2 N2 C10 118.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 65.10 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.269 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.050 data_dphi _database_code_CSD 187218 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(diphenimide)methane ; _chemical_name_common ? _chemical_melting_point 340-3\% _chemical_formula_moiety 'C29 H18 N2 O4' _chemical_formula_sum 'C29 H18 N2 O4' _chemical_formula_weight 458.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.325(3) _cell_length_b 8.587(2) _cell_length_c 14.868(3) _cell_angle_alpha 90.00 _cell_angle_beta 106.36(3) _cell_angle_gamma 90.00 _cell_volume 2122.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 60 _cell_measurement_theta_min 6.21 _cell_measurement_theta_max 18.91 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 952 _exptl_absorpt_coefficient_mu 0.788 _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 295(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'KM-4 four circle diffractometer' _diffrn_measurement_method '\Q--2\Q' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count 100 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.93 _diffrn_reflns_number 1844 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0960 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.32 _diffrn_reflns_theta_max 65.09 _reflns_number_total 1792 _reflns_number_gt 1054 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_cell_refinement 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_data_reduction 'Kuma KM-4 software (Kuma Diffraction, 1991)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Simens Analytical X-Ray Instruments (1989)' _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. The structures were phased by direct methods (SHELXS86 program) and refined by full-matrix least-squares using the SHELXL97 program. Siemens computer graphics program was used to prepare drawings. Anisotropic thermal parameters were refined for all non-hydrogen atoms. The hydrogen atoms were placed at calculated positions (C-H = 0.96 A) and refined in a riding model with their Uiso increased by 1.2 compared to Ueq of atoms to which they were bonded. ; _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^)+(0.0510P)^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 'riding model' _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0029(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 1792 _refine_ls_number_parameters 160 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.0415 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _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 C1 C 0.35011(15) 0.3871(3) 0.55837(18) 0.0352(6) Uani 1 1 d . . . C2 C 0.30930(16) 0.5298(3) 0.5496(2) 0.0464(8) Uani 1 1 d . . . H2 H 0.3200 0.6073 0.5081 0.056 Uiso 1 1 d R . . C3 C 0.25472(17) 0.5620(4) 0.5995(2) 0.0540(9) Uani 1 1 d . . . H3 H 0.2285 0.6615 0.5928 0.065 Uiso 1 1 d R . . C4 C 0.23779(17) 0.4521(4) 0.6582(2) 0.0512(9) Uani 1 1 d . . . H4 H 0.1992 0.4737 0.6919 0.061 Uiso 1 1 d R . . C5 C 0.27680(16) 0.3112(4) 0.6680(2) 0.0439(7) Uani 1 1 d . . . H5 H 0.2649 0.2330 0.7082 0.053 Uiso 1 1 d R . . C6 C 0.33352(15) 0.2782(3) 0.61987(18) 0.0338(6) Uani 1 1 d . . . C11 C 0.40289(15) 0.3538(3) 0.49841(18) 0.0348(6) Uani 1 1 d . . . C12 C 0.38371(17) 0.4179(3) 0.40816(18) 0.0441(7) Uani 1 1 d . . . H12 H 0.3363 0.4811 0.3876 0.053 Uiso 1 1 d R . . C13 C 0.43045(19) 0.3937(4) 0.3487(2) 0.0501(8) Uani 1 1 d . . . H13 H 0.4155 0.4402 0.2875 0.060 Uiso 1 1 d R . . C14 C 0.49912(19) 0.3032(4) 0.3768(2) 0.0478(8) Uani 1 1 d . . . H14 H 0.5319 0.2857 0.3353 0.057 Uiso 1 1 d R . . C15 C 0.51958(17) 0.2386(3) 0.46527(19) 0.0414(7) Uani 1 1 d . . . H15 H 0.5669 0.1749 0.4851 0.050 Uiso 1 1 d R . . C16 C 0.47288(15) 0.2624(3) 0.52664(17) 0.0327(6) Uani 1 1 d . . . C17 C 0.50782(15) 0.1940(3) 0.62165(18) 0.0331(6) Uani 1 1 d . . . C18 C 0.37380(15) 0.1250(3) 0.64300(17) 0.0346(6) Uani 1 1 d . . . C19 C 0.5000 0.0270(4) 0.7500 0.0346(9) Uani 1 2 d S . . H19 H 0.5388 -0.0386 0.7336 0.042 Uiso 1 1 d R . . N1 N 0.45920(12) 0.1234(2) 0.66888(14) 0.0314(5) Uani 1 1 d . . . O1 O 0.58129(11) 0.1862(2) 0.65482(13) 0.0456(6) Uani 1 1 d . . . O2 O 0.33835(11) 0.0075(2) 0.65347(13) 0.0471(6) 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 0.0283(14) 0.0386(16) 0.0359(15) -0.0012(13) 0.0043(11) -0.0017(13) C2 0.0395(17) 0.0429(19) 0.0528(19) 0.0041(15) 0.0064(14) 0.0052(14) C3 0.0430(19) 0.052(2) 0.064(2) -0.0001(17) 0.0094(16) 0.0146(15) C4 0.0412(18) 0.060(2) 0.055(2) -0.0056(16) 0.0175(15) 0.0103(15) C5 0.0353(16) 0.0527(19) 0.0449(17) -0.0011(15) 0.0134(13) -0.0035(14) C6 0.0273(13) 0.0364(16) 0.0345(15) -0.0021(12) 0.0035(11) -0.0020(12) C11 0.0342(14) 0.0356(16) 0.0322(14) -0.0047(12) 0.0052(11) -0.0077(12) C12 0.0448(17) 0.0483(19) 0.0350(16) 0.0043(14) 0.0043(13) -0.0025(15) C13 0.0609(19) 0.054(2) 0.0339(16) 0.0016(16) 0.0102(15) -0.0120(17) C14 0.060(2) 0.0527(19) 0.0347(17) -0.0086(15) 0.0199(15) -0.0156(16) C15 0.0423(16) 0.0422(17) 0.0405(17) -0.0071(14) 0.0130(14) -0.0054(14) C16 0.0313(15) 0.0343(15) 0.0320(15) -0.0059(12) 0.0082(12) -0.0065(12) C17 0.0328(15) 0.0307(15) 0.0361(15) -0.0065(12) 0.0102(12) -0.0002(12) C18 0.0335(14) 0.0414(16) 0.0295(14) -0.0030(13) 0.0098(11) -0.0054(13) C19 0.037(2) 0.028(2) 0.037(2) 0.000 0.0081(17) 0.000 N1 0.0309(11) 0.0315(12) 0.0308(12) 0.0022(10) 0.0070(9) -0.0003(10) O1 0.0304(11) 0.0580(14) 0.0465(12) 0.0058(10) 0.0079(9) 0.0026(9) O2 0.0434(11) 0.0438(12) 0.0514(13) 0.0021(10) 0.0092(9) -0.0149(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 C1 C6 1.393(4) . ? C1 C2 1.403(4) . ? C1 C11 1.474(4) . ? C2 C3 1.383(4) . ? C3 C4 1.373(4) . ? C4 C5 1.374(4) . ? C5 C6 1.397(4) . ? C6 C18 1.484(4) . ? C11 C12 1.401(3) . ? C11 C16 1.406(4) . ? C12 C13 1.372(4) . ? C13 C14 1.383(4) . ? C14 C15 1.379(4) . ? C15 C16 1.395(3) . ? C16 C17 1.491(4) . ? C17 O1 1.231(3) . ? C17 N1 1.380(3) . ? C18 O2 1.213(3) . ? C18 N1 1.420(3) . ? C19 N1 1.470(3) 2_656 ? C19 N1 1.470(3) . ? 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 C6 C1 C2 117.1(2) . . ? C6 C1 C11 123.0(2) . . ? C2 C1 C11 119.7(3) . . ? C3 C2 C1 121.9(3) . . ? C4 C3 C2 120.3(3) . . ? C3 C4 C5 119.0(3) . . ? C4 C5 C6 121.4(3) . . ? C1 C6 C5 120.3(3) . . ? C1 C6 C18 125.2(2) . . ? C5 C6 C18 114.4(2) . . ? C12 C11 C16 117.2(2) . . ? C12 C11 C1 118.9(2) . . ? C16 C11 C1 123.9(2) . . ? C13 C12 C11 122.2(3) . . ? C12 C13 C14 120.3(3) . . ? C15 C14 C13 118.8(3) . . ? C14 C15 C16 121.7(3) . . ? C15 C16 C11 119.8(2) . . ? C15 C16 C17 114.0(2) . . ? C11 C16 C17 126.0(2) . . ? O1 C17 N1 118.9(2) . . ? O1 C17 C16 119.9(2) . . ? N1 C17 C16 120.8(2) . . ? O2 C18 N1 118.9(3) . . ? O2 C18 C6 123.0(2) . . ? N1 C18 C6 117.2(2) . . ? N1 C19 N1 111.4(3) 2_656 . ? C17 N1 C18 126.6(2) . . ? C17 N1 C19 116.36(18) . . ? C18 N1 C19 116.82(18) . . ? 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 C6 C1 C2 C3 -0.1(4) . . . . ? C11 C1 C2 C3 175.3(3) . . . . ? C1 C2 C3 C4 -1.3(5) . . . . ? C2 C3 C4 C5 1.1(5) . . . . ? C3 C4 C5 C6 0.5(4) . . . . ? C2 C1 C6 C5 1.7(4) . . . . ? C11 C1 C6 C5 -173.6(3) . . . . ? C2 C1 C6 C18 -176.2(2) . . . . ? C11 C1 C6 C18 8.5(4) . . . . ? C4 C5 C6 C1 -1.9(4) . . . . ? C4 C5 C6 C18 176.2(2) . . . . ? C6 C1 C11 C12 143.7(3) . . . . ? C2 C1 C11 C12 -31.4(4) . . . . ? C6 C1 C11 C16 -37.2(4) . . . . ? C2 C1 C11 C16 147.7(3) . . . . ? C16 C11 C12 C13 0.1(4) . . . . ? C1 C11 C12 C13 179.2(3) . . . . ? C11 C12 C13 C14 0.1(5) . . . . ? C12 C13 C14 C15 -0.1(4) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C11 0.2(4) . . . . ? C14 C15 C16 C17 -175.4(3) . . . . ? C12 C11 C16 C15 -0.3(4) . . . . ? C1 C11 C16 C15 -179.3(3) . . . . ? C12 C11 C16 C17 174.8(2) . . . . ? C1 C11 C16 C17 -4.3(4) . . . . ? C15 C16 C17 O1 31.7(4) . . . . ? C11 C16 C17 O1 -143.7(3) . . . . ? C15 C16 C17 N1 -141.0(2) . . . . ? C11 C16 C17 N1 43.6(4) . . . . ? C1 C6 C18 O2 -141.1(3) . . . . ? C5 C6 C18 O2 40.9(4) . . . . ? C1 C6 C18 N1 49.5(3) . . . . ? C5 C6 C18 N1 -128.4(3) . . . . ? O1 C17 N1 C18 177.7(3) . . . . ? C16 C17 N1 C18 -9.5(4) . . . . ? O1 C17 N1 C19 -7.4(4) . . . . ? C16 C17 N1 C19 165.4(2) . . . . ? O2 C18 N1 C17 141.0(3) . . . . ? C6 C18 N1 C17 -49.2(3) . . . . ? O2 C18 N1 C19 -33.9(3) . . . . ? C6 C18 N1 C19 135.9(2) . . . . ? N1 C19 N1 C17 75.17(19) 2_656 . . . ? N1 C19 N1 C18 -109.4(2) 2_656 . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 65.09 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.178 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.047