data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'J Narasimha Moorthy' _publ_contact_author_email MOORTHY@IITK.AC.IN _publ_section_title ; Engineering of Ternary Co-Crystals Based on Differential Binding of Guest Molecules by a Tetraarylpyrene Inclusion Host ; loop_ _publ_author_name 'J Narasimha Moorthy' 'Palani Natarajan' #END data_TP-PB _database_code_depnum_ccdc_archive 'CCDC 726024' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra(2,6-dimethyl-4-methoxyphenyl)pyrene ; _chemical_name_common tetra(2,6-dimethyl-4-methoxyphenyl)pyrene _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 O4, C16 H10, C6 H6' _chemical_formula_sum 'C74 H66 O4' _chemical_formula_weight 1019.27 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 14.6772(15) _cell_length_b 14.8540(15) _cell_length_c 14.2577(14) _cell_angle_alpha 90.00 _cell_angle_beta 118.632(2) _cell_angle_gamma 90.00 _cell_volume 2728.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1895 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 22.77 _exptl_crystal_description cubes _exptl_crystal_colour 'color less' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.241 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1084 _exptl_absorpt_coefficient_mu 0.075 _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 100(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 'Bruker SMART APEX' _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 13867 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0590 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4780 _reflns_number_gt 3142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0587P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4780 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1355 _refine_ls_wR_factor_gt 0.1219 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 O1 O 0.90586(13) 1.38951(11) 0.39471(14) 0.0558(5) Uani 1 1 d . . . O2 O 0.75309(12) 0.55825(10) 0.39003(12) 0.0438(4) Uani 1 1 d . . . C1 C 0.69436(15) 1.06577(14) 0.20380(16) 0.0309(5) Uani 1 1 d . . . C2 C 0.71855(16) 0.98222(14) 0.25279(16) 0.0314(5) Uani 1 1 d . . . H2 H 0.7763 0.9774 0.3201 0.038 Uiso 1 1 calc R . . C3 C 0.66054(16) 0.90525(14) 0.20619(16) 0.0302(5) Uani 1 1 d . . . C4 C 0.57277(16) 0.91136(14) 0.10429(16) 0.0303(5) Uani 1 1 d . . . C5 C 0.54462(15) 0.99647(14) 0.05179(15) 0.0290(5) Uani 1 1 d . . . C6 C 0.60568(15) 1.07380(14) 0.10145(16) 0.0290(5) Uani 1 1 d . . . C7 C 0.57430(16) 1.15809(14) 0.04659(16) 0.0333(5) Uani 1 1 d . . . H7 H 0.6133 1.2093 0.0787 0.040 Uiso 1 1 calc R . . C8 C 0.49009(16) 1.16536(15) -0.05014(16) 0.0330(5) Uani 1 1 d . . . H8 H 0.4721 1.2215 -0.0828 0.040 Uiso 1 1 calc R . . C9 C 0.68758(15) 0.81614(14) 0.26151(15) 0.0290(5) Uani 1 1 d . . . C10 C 0.76161(15) 0.76084(15) 0.25366(15) 0.0311(5) Uani 1 1 d . . . C11 C 0.78169(16) 0.67618(15) 0.29921(16) 0.0334(5) Uani 1 1 d . . . H11 H 0.8313 0.6400 0.2951 0.040 Uiso 1 1 calc R . . C12 C 0.72874(16) 0.64455(14) 0.35098(16) 0.0340(5) Uani 1 1 d . . . C13 C 0.65786(16) 0.69921(14) 0.36131(16) 0.0318(5) Uani 1 1 d . . . H13 H 0.6242 0.6787 0.3983 0.038 Uiso 1 1 calc R . . C14 C 0.63675(16) 0.78522(14) 0.31630(16) 0.0304(5) Uani 1 1 d . . . C15 C 0.55882(17) 0.84446(15) 0.32830(18) 0.0386(6) Uani 1 1 d . . . H15A H 0.5917 0.8998 0.3628 0.058 Uiso 1 1 calc R . . H15B H 0.5338 0.8138 0.3707 0.058 Uiso 1 1 calc R . . H15C H 0.5017 0.8573 0.2590 0.058 Uiso 1 1 calc R . . C16 C 0.81757(17) 0.79360(15) 0.19539(17) 0.0396(6) Uani 1 1 d . . . H16A H 0.8706 0.7512 0.2047 0.059 Uiso 1 1 calc R . . H16B H 0.8487 0.8510 0.2235 0.059 Uiso 1 1 calc R . . H16C H 0.7692 0.7995 0.1207 0.059 Uiso 1 1 calc R . . C17 C 0.6936(2) 0.52132(16) 0.4351(2) 0.0510(7) Uani 1 1 d . . . H17A H 0.7027 0.5573 0.4949 0.076 Uiso 1 1 calc R . . H17B H 0.7163 0.4609 0.4585 0.076 Uiso 1 1 calc R . . H17C H 0.6216 0.5208 0.3823 0.076 Uiso 1 1 calc R . . C18 C 0.75682(15) 1.14880(14) 0.25678(15) 0.0303(5) Uani 1 1 d . . . C19 C 0.84205(16) 1.17425(14) 0.24563(16) 0.0312(5) Uani 1 1 d . . . C20 C 0.89232(17) 1.25557(15) 0.28930(17) 0.0360(5) Uani 1 1 d . . . H20 H 0.9487 1.2729 0.2806 0.043 Uiso 1 1 calc R . . C21 C 0.85949(17) 1.31026(15) 0.34507(18) 0.0384(6) Uani 1 1 d . . . C22 C 0.77536(17) 1.28385(16) 0.35784(18) 0.0408(6) Uani 1 1 d . . . H22 H 0.7531 1.3206 0.3957 0.049 Uiso 1 1 calc R . . C23 C 0.72404(16) 1.20368(15) 0.31526(16) 0.0348(5) Uani 1 1 d . . . C24 C 0.63598(17) 1.17482(16) 0.33383(19) 0.0457(6) Uani 1 1 d . . . H24A H 0.6245 1.2196 0.3756 0.069 Uiso 1 1 calc R . . H24B H 0.6529 1.1185 0.3714 0.069 Uiso 1 1 calc R . . H24C H 0.5742 1.1679 0.2664 0.069 Uiso 1 1 calc R . . C25 C 0.88408(18) 1.11567(16) 0.18895(18) 0.0459(6) Uani 1 1 d . . . H25A H 0.9532 1.0968 0.2386 0.069 Uiso 1 1 calc R . . H25B H 0.8853 1.1491 0.1320 0.069 Uiso 1 1 calc R . . H25C H 0.8405 1.0637 0.1601 0.069 Uiso 1 1 calc R . . C26 C 0.9917(2) 1.42026(18) 0.3829(2) 0.0615(8) Uani 1 1 d . . . H26A H 1.0470 1.3770 0.4137 0.092 Uiso 1 1 calc R . . H26B H 1.0153 1.4770 0.4187 0.092 Uiso 1 1 calc R . . H26C H 0.9707 1.4275 0.3084 0.092 Uiso 1 1 calc R . . C27 C 0.83270(17) 0.00450(18) 0.57003(18) 0.0444(6) Uani 1 1 d . . . H27 H 0.7971 0.0419 0.5937 0.053 Uiso 1 1 calc R . . C28 C 0.81021(18) -0.08688(18) 0.55680(18) 0.0466(7) Uani 1 1 d . . . H28 H 0.7594 -0.1100 0.5713 0.056 Uiso 1 1 calc R . . C29 C 0.86240(17) -0.14381(17) 0.52239(17) 0.0433(6) Uani 1 1 d . . . H29 H 0.8464 -0.2049 0.5141 0.052 Uiso 1 1 calc R . . C30 C 0.93872(16) -0.11126(16) 0.49984(16) 0.0375(6) Uani 1 1 d . . . C31 C 0.96223(15) -0.01808(16) 0.51262(15) 0.0346(5) Uani 1 1 d . . . C32 C 0.90819(17) 0.04071(17) 0.54810(17) 0.0383(6) Uani 1 1 d . . . C33 C 0.93357(18) 0.13445(17) 0.55970(17) 0.0424(6) Uani 1 1 d . . . H33 H 0.8992 0.1732 0.5835 0.051 Uiso 1 1 calc R . . C34 C 1.00554(17) 0.16753(17) 0.53715(16) 0.0410(6) Uani 1 1 d . . . H34 H 1.0199 0.2289 0.5457 0.049 Uiso 1 1 calc R . . C35 C 0.56308(19) 0.07320(16) 0.5203(2) 0.0472(6) Uani 1 1 d . . . H35 H 0.6060 0.1230 0.5339 0.057 Uiso 1 1 calc R . . C36 C 0.58924(19) 0.00794(17) 0.5980(2) 0.0465(6) Uani 1 1 d . . . H36 H 0.6490 0.0137 0.6636 0.056 Uiso 1 1 calc R . . C37 C 0.52556(19) -0.06576(17) 0.5771(2) 0.0476(7) Uani 1 1 d . . . H37 H 0.5423 -0.1104 0.6285 0.057 Uiso 1 1 calc R . . 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 O1 0.0537(11) 0.0379(11) 0.0693(12) -0.0167(9) 0.0243(10) -0.0090(9) O2 0.0549(10) 0.0309(10) 0.0435(9) 0.0077(8) 0.0219(8) 0.0090(8) C1 0.0285(12) 0.0348(14) 0.0239(11) -0.0022(10) 0.0080(9) 0.0002(10) C2 0.0297(12) 0.0340(13) 0.0223(10) 0.0021(10) 0.0060(9) 0.0018(10) C3 0.0304(12) 0.0325(13) 0.0249(11) 0.0019(10) 0.0110(9) 0.0049(10) C4 0.0332(12) 0.0295(13) 0.0260(11) 0.0024(10) 0.0125(10) 0.0028(10) C5 0.0320(12) 0.0279(13) 0.0241(11) 0.0026(10) 0.0109(9) 0.0021(10) C6 0.0279(11) 0.0311(13) 0.0251(11) 0.0013(10) 0.0104(9) 0.0006(10) C7 0.0344(12) 0.0285(13) 0.0317(12) 0.0005(10) 0.0116(10) -0.0008(10) C8 0.0367(13) 0.0301(13) 0.0271(11) 0.0011(10) 0.0112(10) 0.0000(10) C9 0.0274(11) 0.0293(12) 0.0206(10) 0.0004(9) 0.0037(9) 0.0019(9) C10 0.0312(12) 0.0325(13) 0.0226(11) -0.0003(10) 0.0072(9) 0.0003(10) C11 0.0315(12) 0.0350(14) 0.0284(11) -0.0020(10) 0.0101(10) 0.0070(10) C12 0.0370(13) 0.0283(13) 0.0260(11) 0.0039(10) 0.0065(10) 0.0045(10) C13 0.0335(12) 0.0317(13) 0.0264(11) 0.0042(10) 0.0114(10) 0.0013(10) C14 0.0294(12) 0.0320(13) 0.0238(11) 0.0013(10) 0.0080(9) 0.0039(10) C15 0.0417(13) 0.0347(14) 0.0396(13) 0.0037(11) 0.0199(11) 0.0070(11) C16 0.0387(13) 0.0436(15) 0.0354(13) 0.0027(11) 0.0169(11) 0.0067(11) C17 0.0761(19) 0.0317(14) 0.0494(15) 0.0087(12) 0.0336(14) 0.0050(13) C18 0.0283(12) 0.0308(13) 0.0234(11) 0.0044(10) 0.0056(9) 0.0021(10) C19 0.0312(12) 0.0317(13) 0.0251(11) 0.0018(10) 0.0089(10) 0.0038(10) C20 0.0330(12) 0.0377(14) 0.0324(12) 0.0034(11) 0.0118(10) -0.0004(11) C21 0.0347(13) 0.0285(13) 0.0402(13) -0.0043(11) 0.0084(11) -0.0001(10) C22 0.0371(13) 0.0394(15) 0.0404(13) -0.0119(11) 0.0142(11) 0.0046(11) C23 0.0304(12) 0.0371(14) 0.0302(12) 0.0004(11) 0.0091(10) 0.0042(10) C24 0.0375(14) 0.0532(16) 0.0453(14) -0.0099(13) 0.0189(12) -0.0018(12) C25 0.0449(15) 0.0491(16) 0.0431(14) -0.0110(12) 0.0206(12) -0.0064(12) C26 0.0643(18) 0.0491(18) 0.0671(19) -0.0120(15) 0.0281(16) -0.0207(14) C27 0.0352(14) 0.0582(18) 0.0348(13) 0.0044(12) 0.0129(11) 0.0066(12) C28 0.0385(14) 0.0608(19) 0.0350(13) 0.0091(13) 0.0133(11) -0.0021(13) C29 0.0387(14) 0.0484(16) 0.0326(12) 0.0056(12) 0.0089(11) 0.0013(12) C30 0.0317(13) 0.0442(15) 0.0245(11) 0.0023(11) 0.0036(10) 0.0009(11) C31 0.0255(12) 0.0440(15) 0.0233(11) 0.0028(10) 0.0026(9) 0.0047(10) C32 0.0313(13) 0.0464(15) 0.0260(11) 0.0035(11) 0.0047(10) 0.0035(11) C33 0.0398(14) 0.0463(16) 0.0326(12) -0.0024(12) 0.0104(11) 0.0051(12) C34 0.0393(14) 0.0401(15) 0.0307(12) 0.0009(11) 0.0065(11) 0.0020(11) C35 0.0525(16) 0.0341(15) 0.0629(17) 0.0007(13) 0.0340(15) 0.0014(12) C36 0.0463(15) 0.0468(17) 0.0522(15) 0.0031(13) 0.0283(13) 0.0053(13) C37 0.0525(16) 0.0429(16) 0.0551(16) 0.0132(13) 0.0321(14) 0.0098(13) _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 O1 C21 1.374(3) . ? O1 C26 1.424(3) . ? O2 C12 1.375(2) . ? O2 C17 1.418(3) . ? C1 C2 1.384(3) . ? C1 C6 1.420(3) . ? C1 C18 1.506(3) . ? C2 C3 1.390(3) . ? C2 H2 0.9300 . ? C3 C4 1.409(3) . ? C3 C9 1.494(3) . ? C4 C5 1.426(3) . ? C4 C8 1.436(3) 3_675 ? C5 C6 1.420(3) . ? C5 C5 1.433(4) 3_675 ? C6 C7 1.430(3) . ? C7 C8 1.345(3) . ? C7 H7 0.9300 . ? C8 C4 1.436(3) 3_675 ? C8 H8 0.9300 . ? C9 C14 1.391(3) . ? C9 C10 1.409(3) . ? C10 C11 1.381(3) . ? C10 C16 1.502(3) . ? C11 C12 1.386(3) . ? C11 H11 0.9300 . ? C12 C13 1.382(3) . ? C13 C14 1.396(3) . ? C13 H13 0.9300 . ? C14 C15 1.516(3) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.387(3) . ? C18 C23 1.406(3) . ? C19 C20 1.397(3) . ? C19 C25 1.506(3) . ? C20 C21 1.375(3) . ? C20 H20 0.9300 . ? C21 C22 1.388(3) . ? C22 C23 1.384(3) . ? C22 H22 0.9300 . ? C23 C24 1.501(3) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.388(3) . ? C27 C32 1.395(3) . ? C27 H27 0.9300 . ? C28 C29 1.379(3) . ? C28 H28 0.9300 . ? C29 C30 1.392(3) . ? C29 H29 0.9300 . ? C30 C31 1.417(3) . ? C30 C34 1.435(3) 3_756 ? C31 C31 1.425(4) 3_756 ? C31 C32 1.425(3) . ? C32 C33 1.430(3) . ? C33 C34 1.336(3) . ? C33 H33 0.9300 . ? C34 C30 1.435(3) 3_756 ? C34 H34 0.9300 . ? C35 C37 1.379(3) 3_656 ? C35 C36 1.381(3) . ? C35 H35 0.9300 . ? C36 C37 1.376(3) . ? C36 H36 0.9300 . ? C37 C35 1.379(3) 3_656 ? C37 H37 0.9300 . ? 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 C21 O1 C26 117.50(19) . . ? C12 O2 C17 116.56(17) . . ? C2 C1 C6 118.74(19) . . ? C2 C1 C18 122.26(18) . . ? C6 C1 C18 118.97(18) . . ? C1 C2 C3 123.09(19) . . ? C1 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? C2 C3 C4 119.21(19) . . ? C2 C3 C9 121.98(18) . . ? C4 C3 C9 118.81(19) . . ? C3 C4 C5 119.36(19) . . ? C3 C4 C8 122.52(19) . 3_675 ? C5 C4 C8 118.12(18) . 3_675 ? C6 C5 C4 120.04(18) . . ? C6 C5 C5 120.1(2) . 3_675 ? C4 C5 C5 119.8(2) . 3_675 ? C5 C6 C1 119.54(19) . . ? C5 C6 C7 118.33(18) . . ? C1 C6 C7 122.1(2) . . ? C8 C7 C6 121.9(2) . . ? C8 C7 H7 119.1 . . ? C6 C7 H7 119.1 . . ? C7 C8 C4 121.7(2) . 3_675 ? C7 C8 H8 119.1 . . ? C4 C8 H8 119.1 3_675 . ? C14 C9 C10 119.58(19) . . ? C14 C9 C3 120.70(18) . . ? C10 C9 C3 119.64(19) . . ? C11 C10 C9 119.51(19) . . ? C11 C10 C16 120.35(19) . . ? C9 C10 C16 120.14(19) . . ? C10 C11 C12 120.8(2) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? O2 C12 C13 124.6(2) . . ? O2 C12 C11 115.39(19) . . ? C13 C12 C11 120.0(2) . . ? C12 C13 C14 120.1(2) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C9 C14 C13 119.96(19) . . ? C9 C14 C15 120.54(19) . . ? C13 C14 C15 119.49(19) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C17 H17A 109.5 . . ? O2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 119.6(2) . . ? C19 C18 C1 122.10(18) . . ? C23 C18 C1 118.25(18) . . ? C18 C19 C20 119.83(19) . . ? C18 C19 C25 121.9(2) . . ? C20 C19 C25 118.31(19) . . ? C21 C20 C19 120.8(2) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? O1 C21 C20 125.4(2) . . ? O1 C21 C22 115.2(2) . . ? C20 C21 C22 119.3(2) . . ? C23 C22 C21 121.1(2) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C18 119.3(2) . . ? C22 C23 C24 120.1(2) . . ? C18 C23 C24 120.5(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C25 H25A 109.5 . . ? C19 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C19 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O1 C26 H26A 109.5 . . ? O1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 120.6(2) . . ? C28 C27 H27 119.7 . . ? C32 C27 H27 119.7 . . ? C29 C28 C27 120.7(2) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 121.0(2) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C29 C30 C31 118.9(2) . . ? C29 C30 C34 123.1(2) . 3_756 ? C31 C30 C34 118.0(2) . 3_756 ? C30 C31 C31 120.5(3) . 3_756 ? C30 C31 C32 120.1(2) . . ? C31 C31 C32 119.4(3) 3_756 . ? C27 C32 C31 118.7(2) . . ? C27 C32 C33 122.7(2) . . ? C31 C32 C33 118.6(2) . . ? C34 C33 C32 121.5(2) . . ? C34 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? C33 C34 C30 122.0(2) . 3_756 ? C33 C34 H34 119.0 . . ? C30 C34 H34 119.0 3_756 . ? C37 C35 C36 121.1(2) 3_656 . ? C37 C35 H35 119.4 3_656 . ? C36 C35 H35 119.4 . . ? C37 C36 C35 119.0(2) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? C36 C37 C35 119.8(2) . 3_656 ? C36 C37 H37 120.1 . . ? C35 C37 H37 120.1 3_656 . ? 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(3) . . . . ? C18 C1 C2 C3 178.55(19) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? C1 C2 C3 C9 -179.15(19) . . . . ? C2 C3 C4 C5 -0.8(3) . . . . ? C9 C3 C4 C5 178.44(18) . . . . ? C2 C3 C4 C8 178.96(19) . . . 3_675 ? C9 C3 C4 C8 -1.8(3) . . . 3_675 ? C3 C4 C5 C6 0.9(3) . . . . ? C8 C4 C5 C6 -178.79(18) 3_675 . . . ? C3 C4 C5 C5 -179.9(2) . . . 3_675 ? C8 C4 C5 C5 0.4(3) 3_675 . . 3_675 ? C4 C5 C6 C1 -0.4(3) . . . . ? C5 C5 C6 C1 -179.6(2) 3_675 . . . ? C4 C5 C6 C7 -179.44(18) . . . . ? C5 C5 C6 C7 1.4(3) 3_675 . . . ? C2 C1 C6 C5 -0.3(3) . . . . ? C18 C1 C6 C5 -178.43(18) . . . . ? C2 C1 C6 C7 178.67(18) . . . . ? C18 C1 C6 C7 0.6(3) . . . . ? C5 C6 C7 C8 -0.8(3) . . . . ? C1 C6 C7 C8 -179.78(19) . . . . ? C6 C7 C8 C4 -0.5(3) . . . 3_675 ? C2 C3 C9 C14 98.1(2) . . . . ? C4 C3 C9 C14 -81.1(2) . . . . ? C2 C3 C9 C10 -85.1(3) . . . . ? C4 C3 C9 C10 95.7(2) . . . . ? C14 C9 C10 C11 0.9(3) . . . . ? C3 C9 C10 C11 -175.95(18) . . . . ? C14 C9 C10 C16 -179.59(18) . . . . ? C3 C9 C10 C16 3.6(3) . . . . ? C9 C10 C11 C12 1.0(3) . . . . ? C16 C10 C11 C12 -178.49(19) . . . . ? C17 O2 C12 C13 6.0(3) . . . . ? C17 O2 C12 C11 -174.65(18) . . . . ? C10 C11 C12 O2 177.98(18) . . . . ? C10 C11 C12 C13 -2.6(3) . . . . ? O2 C12 C13 C14 -178.38(19) . . . . ? C11 C12 C13 C14 2.3(3) . . . . ? C10 C9 C14 C13 -1.2(3) . . . . ? C3 C9 C14 C13 175.60(18) . . . . ? C10 C9 C14 C15 178.40(18) . . . . ? C3 C9 C14 C15 -4.8(3) . . . . ? C12 C13 C14 C9 -0.4(3) . . . . ? C12 C13 C14 C15 -179.99(19) . . . . ? C2 C1 C18 C19 89.3(3) . . . . ? C6 C1 C18 C19 -92.7(2) . . . . ? C2 C1 C18 C23 -93.5(2) . . . . ? C6 C1 C18 C23 84.5(2) . . . . ? C23 C18 C19 C20 -2.2(3) . . . . ? C1 C18 C19 C20 174.90(19) . . . . ? C23 C18 C19 C25 176.65(19) . . . . ? C1 C18 C19 C25 -6.2(3) . . . . ? C18 C19 C20 C21 1.2(3) . . . . ? C25 C19 C20 C21 -177.77(19) . . . . ? C26 O1 C21 C20 3.5(3) . . . . ? C26 O1 C21 C22 -179.2(2) . . . . ? C19 C20 C21 O1 177.2(2) . . . . ? C19 C20 C21 C22 0.0(3) . . . . ? O1 C21 C22 C23 -177.6(2) . . . . ? C20 C21 C22 C23 -0.1(3) . . . . ? C21 C22 C23 C18 -0.9(3) . . . . ? C21 C22 C23 C24 177.6(2) . . . . ? C19 C18 C23 C22 2.1(3) . . . . ? C1 C18 C23 C22 -175.12(19) . . . . ? C19 C18 C23 C24 -176.38(19) . . . . ? C1 C18 C23 C24 6.4(3) . . . . ? C32 C27 C28 C29 0.4(3) . . . . ? C27 C28 C29 C30 -0.1(3) . . . . ? C28 C29 C30 C31 -0.1(3) . . . . ? C28 C29 C30 C34 -179.4(2) . . . 3_756 ? C29 C30 C31 C31 -178.2(2) . . . 3_756 ? C34 C30 C31 C31 1.1(3) 3_756 . . 3_756 ? C29 C30 C31 C32 0.0(3) . . . . ? C34 C30 C31 C32 179.35(18) 3_756 . . . ? C28 C27 C32 C31 -0.4(3) . . . . ? C28 C27 C32 C33 179.5(2) . . . . ? C30 C31 C32 C27 0.2(3) . . . . ? C31 C31 C32 C27 178.5(2) 3_756 . . . ? C30 C31 C32 C33 -179.74(19) . . . . ? C31 C31 C32 C33 -1.5(3) 3_756 . . . ? C27 C32 C33 C34 -179.3(2) . . . . ? C31 C32 C33 C34 0.6(3) . . . . ? C32 C33 C34 C30 0.0(3) . . . 3_756 ? C37 C35 C36 C37 0.3(4) 3_656 . . . ? C35 C36 C37 C35 -0.3(4) . . . 3_656 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.244 _refine_diff_density_min -0.180 _refine_diff_density_rms 0.048 # Attachment 'Ternary_Meopyrenes_revf2 .cif' data_TP-PO _database_code_depnum_ccdc_archive 'CCDC 726025' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra(2,6-dimethyl-4-methoxyphenyl)pyrene ; _chemical_name_common tetra(2,6-dimethyl-4-methoxyphenyl)pyrene _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 O4, 0.5(C16 H10), C8 H16' _chemical_formula_sum 'C68 H71 O4' _chemical_formula_weight 952.25 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 18.140(3) _cell_length_b 15.209(2) _cell_length_c 19.375(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.403(3) _cell_angle_gamma 90.00 _cell_volume 5312.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3447 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.63 _exptl_crystal_description blacks _exptl_crystal_colour 'color less' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2044 _exptl_absorpt_coefficient_mu 0.072 _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 100(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 'Bruker SMART APEX' _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 27714 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9811 _reflns_number_gt 5817 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0808P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9811 _refine_ls_number_parameters 695 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1182 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1787 _refine_ls_wR_factor_gt 0.1571 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.057 _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 O1 O 0.71075(10) 0.89899(12) 0.26253(10) 0.0556(5) Uani 1 1 d . . . O2 O 0.70212(12) 0.11864(14) 0.11413(12) 0.0746(6) Uani 1 1 d . . . O3 O 0.09377(12) 0.11714(13) 0.04536(12) 0.0736(6) Uani 1 1 d . . . O4 O 0.09708(10) 0.93313(12) 0.11789(9) 0.0510(5) Uani 1 1 d . . . C1 C 0.54953(12) 0.58778(16) 0.18922(11) 0.0344(6) Uani 1 1 d . . . C2 C 0.58467(12) 0.50746(16) 0.18424(12) 0.0367(6) Uani 1 1 d . . . H2 H 0.6369 0.5048 0.1960 0.044 Uiso 1 1 calc R . . C3 C 0.54745(12) 0.43096(16) 0.16295(11) 0.0344(6) Uani 1 1 d . . . C4 C 0.42712(12) 0.35681(16) 0.12543(11) 0.0366(6) Uani 1 1 d . . . H4 H 0.4519 0.3022 0.1222 0.044 Uiso 1 1 calc R . . C5 C 0.35354(12) 0.35995(16) 0.11038(11) 0.0366(6) Uani 1 1 d . . . H5 H 0.3274 0.3074 0.0973 0.044 Uiso 1 1 calc R . . C6 C 0.23509(12) 0.44465(16) 0.09789(12) 0.0346(6) Uani 1 1 d . . . C7 C 0.19959(12) 0.52511(16) 0.10217(12) 0.0357(6) Uani 1 1 d . . . H7 H 0.1472 0.5275 0.0913 0.043 Uiso 1 1 calc R . . C8 C 0.23724(12) 0.60207(15) 0.12157(12) 0.0332(5) Uani 1 1 d . . . C9 C 0.35729(12) 0.67595(16) 0.15875(11) 0.0350(6) Uani 1 1 d . . . H9 H 0.3325 0.7307 0.1610 0.042 Uiso 1 1 calc R . . C10 C 0.43134(12) 0.67284(16) 0.17511(11) 0.0350(6) Uani 1 1 d . . . H10 H 0.4573 0.7253 0.1891 0.042 Uiso 1 1 calc R . . C11 C 0.47209(12) 0.59258(15) 0.17199(11) 0.0327(5) Uani 1 1 d . . . C12 C 0.46970(12) 0.43351(16) 0.14627(11) 0.0331(5) Uani 1 1 d . . . C13 C 0.31286(12) 0.44049(15) 0.11341(11) 0.0325(5) Uani 1 1 d . . . C14 C 0.31478(12) 0.59912(15) 0.13806(11) 0.0322(5) Uani 1 1 d . . . C15 C 0.35287(11) 0.51798(15) 0.13397(11) 0.0303(5) Uani 1 1 d . . . C16 C 0.43195(12) 0.51467(15) 0.15093(11) 0.0310(5) Uani 1 1 d . . . C17 C 0.59314(12) 0.66865(16) 0.21035(12) 0.0346(6) Uani 1 1 d . . . C18 C 0.60584(12) 0.69299(17) 0.28020(12) 0.0411(6) Uani 1 1 d . . . C19 C 0.64551(13) 0.76982(18) 0.29858(13) 0.0438(7) Uani 1 1 d . . . H19 H 0.6543 0.7864 0.3461 0.053 Uiso 1 1 calc R . . C20 C 0.67186(13) 0.82137(17) 0.24907(14) 0.0428(6) Uani 1 1 d . . . C21 C 0.62136(13) 0.72152(17) 0.15986(13) 0.0417(6) Uani 1 1 d . . . C22 C 0.60646(16) 0.6977(2) 0.08394(13) 0.0589(8) Uani 1 1 d . . . H22A H 0.5548 0.7116 0.0671 0.088 Uiso 1 1 calc R . . H22B H 0.6152 0.6347 0.0781 0.088 Uiso 1 1 calc R . . H22C H 0.6397 0.7313 0.0573 0.088 Uiso 1 1 calc R . . C23 C 0.57703(16) 0.6380(2) 0.33539(14) 0.0599(8) Uani 1 1 d . . . H23A H 0.5237 0.6485 0.3355 0.090 Uiso 1 1 calc R . . H23B H 0.6030 0.6538 0.3808 0.090 Uiso 1 1 calc R . . H23C H 0.5855 0.5757 0.3260 0.090 Uiso 1 1 calc R . . C24 C 0.71760(16) 0.9294(2) 0.33137(16) 0.0633(9) Uani 1 1 d . . . H24A H 0.6683 0.9340 0.3472 0.095 Uiso 1 1 calc R . . H24B H 0.7414 0.9873 0.3338 0.095 Uiso 1 1 calc R . . H24C H 0.7479 0.8881 0.3612 0.095 Uiso 1 1 calc R . . C25 C 0.58897(12) 0.34778(16) 0.15379(13) 0.0362(6) Uani 1 1 d . . . C26 C 0.61585(13) 0.29601(17) 0.21041(13) 0.0434(6) Uani 1 1 d . . . C27 C 0.65402(13) 0.21824(18) 0.19874(16) 0.0507(7) Uani 1 1 d . . . H27 H 0.6733 0.1826 0.2368 0.061 Uiso 1 1 calc R . . C28 C 0.66356(14) 0.19345(18) 0.13146(17) 0.0512(7) Uani 1 1 d . . . C29 C 0.63738(14) 0.24398(19) 0.07659(15) 0.0504(7) Uani 1 1 d . . . H29 H 0.6445 0.2255 0.0310 0.060 Uiso 1 1 calc R . . C30 C 0.60050(13) 0.32173(17) 0.08566(13) 0.0424(6) Uani 1 1 d . . . C31 C 0.57656(15) 0.3793(2) 0.02418(13) 0.0570(8) Uani 1 1 d . . . H31A H 0.5878 0.3499 -0.0184 0.086 Uiso 1 1 calc R . . H31B H 0.6032 0.4354 0.0291 0.086 Uiso 1 1 calc R . . H31C H 0.5231 0.3901 0.0217 0.086 Uiso 1 1 calc R . . C32 C 0.60430(16) 0.3230(2) 0.28262(14) 0.0611(8) Uani 1 1 d . . . H32A H 0.6317 0.3775 0.2946 0.092 Uiso 1 1 calc R . . H32B H 0.6223 0.2765 0.3152 0.092 Uiso 1 1 calc R . . H32C H 0.5513 0.3329 0.2854 0.092 Uiso 1 1 calc R . . C33 C 0.72274(19) 0.0612(2) 0.16772(19) 0.0825(11) Uani 1 1 d . . . H33A H 0.7557 0.0913 0.2037 0.124 Uiso 1 1 calc R . . H33B H 0.7487 0.0109 0.1501 0.124 Uiso 1 1 calc R . . H33C H 0.6784 0.0405 0.1875 0.124 Uiso 1 1 calc R . . C34 C 0.19304(12) 0.36155(16) 0.08001(12) 0.0369(6) Uani 1 1 d . . . C35 C 0.16620(13) 0.31346(18) 0.13389(13) 0.0451(7) Uani 1 1 d . . . C36 C 0.13467(14) 0.23191(19) 0.11957(15) 0.0529(7) Uani 1 1 d . . . H36 H 0.1174 0.1986 0.1560 0.063 Uiso 1 1 calc R . . C37 C 0.12791(14) 0.19806(18) 0.05302(16) 0.0522(7) Uani 1 1 d . . . C38 C 0.15186(13) 0.24604(18) -0.00106(15) 0.0484(7) Uani 1 1 d . . . H38 H 0.1461 0.2232 -0.0470 0.058 Uiso 1 1 calc R . . C39 C 0.18478(12) 0.32896(17) 0.01261(13) 0.0410(6) Uani 1 1 d . . . C40 C 0.20759(15) 0.38215(18) -0.04640(13) 0.0505(7) Uani 1 1 d . . . H40A H 0.1697 0.4267 -0.0600 0.076 Uiso 1 1 calc R . . H40B H 0.2130 0.3434 -0.0860 0.076 Uiso 1 1 calc R . . H40C H 0.2550 0.4111 -0.0319 0.076 Uiso 1 1 calc R . . C41 C 0.17027(15) 0.3510(2) 0.20683(13) 0.0556(8) Uani 1 1 d . . . H41A H 0.1438 0.3121 0.2360 0.083 Uiso 1 1 calc R . . H41B H 0.1473 0.4095 0.2051 0.083 Uiso 1 1 calc R . . H41C H 0.2223 0.3558 0.2264 0.083 Uiso 1 1 calc R . . C42 C 0.0901(2) 0.0772(2) -0.02078(19) 0.0820(11) Uani 1 1 d . . . H42A H 0.0575 0.1118 -0.0542 0.123 Uiso 1 1 calc R . . H42B H 0.0702 0.0175 -0.0182 0.123 Uiso 1 1 calc R . . H42C H 0.1399 0.0746 -0.0357 0.123 Uiso 1 1 calc R . . C43 C 0.19712(11) 0.68788(15) 0.12299(12) 0.0324(6) Uani 1 1 d . . . C44 C 0.17599(12) 0.72128(16) 0.18495(12) 0.0366(6) Uani 1 1 d . . . C45 C 0.14193(12) 0.80381(17) 0.18455(13) 0.0399(6) Uani 1 1 d . . . H45 H 0.1271 0.8272 0.2263 0.048 Uiso 1 1 calc R . . C46 C 0.12979(12) 0.85156(16) 0.12348(13) 0.0398(6) Uani 1 1 d . . . C47 C 0.14894(13) 0.81724(17) 0.06228(13) 0.0420(6) Uani 1 1 d . . . H47 H 0.1384 0.8495 0.0204 0.050 Uiso 1 1 calc R . . C48 C 0.18350(12) 0.73612(17) 0.06117(13) 0.0387(6) Uani 1 1 d . . . C49 C 0.20517(14) 0.7004(2) -0.00593(13) 0.0505(7) Uani 1 1 d . . . H49A H 0.1698 0.6548 -0.0236 0.076 Uiso 1 1 calc R . . H49B H 0.2550 0.6749 0.0020 0.076 Uiso 1 1 calc R . . H49C H 0.2049 0.7480 -0.0400 0.076 Uiso 1 1 calc R . . C50 C 0.18935(14) 0.66895(18) 0.25083(12) 0.0447(6) Uani 1 1 d . . . H50A H 0.1633 0.6126 0.2448 0.067 Uiso 1 1 calc R . . H50B H 0.1709 0.7018 0.2889 0.067 Uiso 1 1 calc R . . H50C H 0.2427 0.6583 0.2618 0.067 Uiso 1 1 calc R . . C51 C 0.08853(16) 0.97677(18) 0.18033(14) 0.0540(7) Uani 1 1 d . . . H51A H 0.0517 0.9458 0.2046 0.081 Uiso 1 1 calc R . . H51B H 0.0718 1.0372 0.1703 0.081 Uiso 1 1 calc R . . H51C H 0.1361 0.9778 0.2097 0.081 Uiso 1 1 calc R . . C52 C 0.66068(13) 0.79676(18) 0.18017(14) 0.0454(7) Uani 1 1 d . . . H52 H 0.6803 0.8321 0.1461 0.054 Uiso 1 1 calc R . . C61 C 0.01459(13) 0.6263(2) -0.08349(15) 0.0517(7) Uani 1 1 d . . . H61 H 0.0194 0.6624 -0.1227 0.062 Uiso 1 1 calc R . . C62 C 0.01312(13) 0.66362(19) -0.02091(15) 0.0500(7) Uani 1 1 d . . . H62 H 0.0176 0.7257 -0.0168 0.060 Uiso 1 1 calc R . . C63 C 0.00501(12) 0.61257(19) 0.03999(14) 0.0442(7) Uani 1 1 d . . . C64 C 0.00356(13) 0.6500(2) 0.10560(15) 0.0503(7) Uani 1 1 d . . . H64 H 0.0082 0.7119 0.1109 0.060 Uiso 1 1 calc R . . C65 C -0.00450(14) 0.5988(2) 0.16256(15) 0.0569(8) Uani 1 1 d . . . H65 H -0.0060 0.6258 0.2066 0.068 Uiso 1 1 calc R . . C66 C -0.01056(14) 0.5079(2) 0.15647(15) 0.0547(8) Uani 1 1 d . . . H66 H -0.0158 0.4732 0.1964 0.066 Uiso 1 1 calc R . . C67 C -0.00901(13) 0.46724(19) 0.09217(14) 0.0455(7) Uani 1 1 d . . . C68 C -0.00148(12) 0.52002(18) 0.03320(12) 0.0419(6) Uani 1 1 d . . . C71 C 0.6882(2) 0.9874(2) 0.9016(2) 0.0586(11) Uani 0.794(4) 1 d PD A 1 H71A H 0.6686 0.9761 0.8526 0.070 Uiso 0.794(4) 1 calc PR A 1 H71B H 0.7429 0.9858 0.9041 0.070 Uiso 0.794(4) 1 calc PR A 1 C72 C 0.6643(2) 0.9121(3) 0.9445(3) 0.0709(13) Uani 0.794(4) 1 d PD A 1 H72A H 0.6867 0.9214 0.9929 0.085 Uiso 0.794(4) 1 calc PR A 1 H72B H 0.6865 0.8577 0.9277 0.085 Uiso 0.794(4) 1 calc PR A 1 C73 C 0.5815(3) 0.8950(3) 0.9464(2) 0.0682(13) Uani 0.794(4) 1 d PD A 1 H73A H 0.5755 0.8351 0.9650 0.082 Uiso 0.794(4) 1 calc PR A 1 H73B H 0.5629 0.9370 0.9793 0.082 Uiso 0.794(4) 1 calc PR A 1 C74 C 0.5336(2) 0.9024(3) 0.8781(2) 0.0537(13) Uani 0.794(4) 1 d P A 1 H74A H 0.5657 0.8932 0.8406 0.064 Uiso 0.794(4) 1 calc PR A 1 H74B H 0.4975 0.8534 0.8754 0.064 Uiso 0.794(4) 1 calc PR A 1 C75 C 0.4914(2) 0.9850(2) 0.8626(2) 0.0555(11) Uani 0.794(4) 1 d P A 1 H75A H 0.4593 0.9940 0.9001 0.067 Uiso 0.794(4) 1 calc PR A 1 H75B H 0.4582 0.9757 0.8192 0.067 Uiso 0.794(4) 1 calc PR A 1 C76 C 0.5342(2) 1.0708(3) 0.8546(2) 0.0569(11) Uani 0.794(4) 1 d P A 1 H76A H 0.5655 1.0631 0.8163 0.068 Uiso 0.794(4) 1 calc PR A 1 H76B H 0.4979 1.1179 0.8405 0.068 Uiso 0.794(4) 1 calc PR A 1 C77 C 0.5831(2) 1.1014(3) 0.9181(2) 0.0559(10) Uani 0.794(4) 1 d P A 1 H77A H 0.5648 1.0746 0.9596 0.067 Uiso 0.794(4) 1 calc PR A 1 H77B H 0.5777 1.1659 0.9221 0.067 Uiso 0.794(4) 1 calc PR A 1 C78 C 0.66600(19) 1.0799(2) 0.9194(2) 0.0537(11) Uani 0.794(4) 1 d P A 1 H78A H 0.6870 1.1205 0.8868 0.064 Uiso 0.794(4) 1 calc PR A 1 H78B H 0.6902 1.0936 0.9665 0.064 Uiso 0.794(4) 1 calc PR A 1 C71A C 0.7186(6) 0.9993(10) 0.9469(8) 0.093(6) Uiso 0.206(4) 1 d PD A 2 H71A H 0.7696 0.9859 0.9367 0.111 Uiso 0.206(4) 1 calc PR A 2 H71B H 0.7223 1.0454 0.9833 0.111 Uiso 0.206(4) 1 calc PR A 2 C72A C 0.6872(6) 0.9183(9) 0.9764(8) 0.079(7) Uiso 0.206(4) 1 d PD A 2 H72A H 0.7224 0.8973 1.0158 0.095 Uiso 0.206(4) 1 calc PR A 2 H72B H 0.6833 0.8718 0.9404 0.095 Uiso 0.206(4) 1 calc PR A 2 C73A C 0.6116(6) 0.9309(10) 1.0016(7) 0.070(5) Uiso 0.206(4) 1 d PD A 2 H73A H 0.6121 0.9033 1.0479 0.084 Uiso 0.206(4) 1 calc PR A 2 H73B H 0.6029 0.9947 1.0072 0.084 Uiso 0.206(4) 1 calc PR A 2 C74A C 0.5474(8) 0.8929(13) 0.9540(9) 0.101(10) Uiso 0.206(4) 1 d PD A 2 H74A H 0.5002 0.9137 0.9695 0.121 Uiso 0.206(4) 1 calc PR A 2 H74B H 0.5485 0.8280 0.9581 0.121 Uiso 0.206(4) 1 calc PR A 2 C75A C 0.5490(15) 0.9179(12) 0.8781(8) 0.19(2) Uiso 0.206(4) 1 d PD A 2 H75A H 0.5105 0.8836 0.8495 0.232 Uiso 0.206(4) 1 calc PR A 2 H75B H 0.5977 0.9011 0.8637 0.232 Uiso 0.206(4) 1 calc PR A 2 C76A C 0.5360(7) 1.0152(13) 0.8631(9) 0.089(7) Uiso 0.206(4) 1 d PD A 2 H76A H 0.4912 1.0342 0.8840 0.107 Uiso 0.206(4) 1 calc PR A 2 H76B H 0.5261 1.0235 0.8122 0.107 Uiso 0.206(4) 1 calc PR A 2 C77A C 0.6007(8) 1.0742(10) 0.8907(11) 0.102(9) Uiso 0.206(4) 1 d PD A 2 H77A H 0.5953 1.1314 0.8663 0.123 Uiso 0.206(4) 1 calc PR A 2 H77B H 0.5978 1.0853 0.9406 0.123 Uiso 0.206(4) 1 calc PR A 2 C78A C 0.6765(6) 1.0371(11) 0.8821(7) 0.060(5) Uiso 0.206(4) 1 d PD A 2 H78A H 0.6706 0.9904 0.8464 0.072 Uiso 0.206(4) 1 calc PR A 2 H78B H 0.7069 1.0844 0.8645 0.072 Uiso 0.206(4) 1 calc PR A 2 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 O1 0.0533(11) 0.0431(12) 0.0709(13) -0.0105(10) 0.0085(9) -0.0131(9) O2 0.0755(15) 0.0500(13) 0.0984(17) -0.0003(13) 0.0101(12) 0.0141(11) O3 0.0777(15) 0.0457(13) 0.0932(17) 0.0089(12) -0.0082(12) -0.0211(11) O4 0.0559(11) 0.0387(11) 0.0581(12) 0.0050(10) 0.0043(9) 0.0112(9) C1 0.0306(12) 0.0365(14) 0.0361(13) -0.0031(11) 0.0035(10) -0.0019(11) C2 0.0280(12) 0.0383(15) 0.0430(14) -0.0063(12) 0.0005(10) 0.0021(11) C3 0.0322(12) 0.0346(14) 0.0363(13) -0.0010(11) 0.0032(10) 0.0036(11) C4 0.0382(14) 0.0296(14) 0.0416(14) -0.0021(11) 0.0036(11) 0.0020(11) C5 0.0381(14) 0.0311(14) 0.0398(14) -0.0018(11) 0.0007(10) -0.0036(11) C6 0.0322(13) 0.0319(14) 0.0392(13) 0.0063(11) 0.0015(10) -0.0020(11) C7 0.0262(12) 0.0390(15) 0.0407(13) 0.0042(12) -0.0019(10) -0.0014(11) C8 0.0319(12) 0.0323(14) 0.0350(13) 0.0040(11) 0.0020(10) 0.0004(11) C9 0.0358(13) 0.0311(14) 0.0377(13) -0.0014(11) 0.0016(10) 0.0036(11) C10 0.0347(13) 0.0305(14) 0.0391(13) -0.0058(11) 0.0019(10) -0.0018(11) C11 0.0292(12) 0.0335(14) 0.0351(13) -0.0025(11) 0.0027(9) -0.0003(10) C12 0.0333(12) 0.0323(14) 0.0338(13) -0.0028(11) 0.0042(10) 0.0001(11) C13 0.0295(12) 0.0325(14) 0.0349(13) 0.0001(11) 0.0010(9) -0.0014(10) C14 0.0306(12) 0.0339(14) 0.0319(12) 0.0018(11) 0.0029(9) -0.0007(11) C15 0.0289(12) 0.0328(14) 0.0290(12) 0.0016(11) 0.0031(9) 0.0006(10) C16 0.0281(12) 0.0330(14) 0.0317(12) -0.0015(11) 0.0019(9) 0.0012(10) C17 0.0270(12) 0.0347(14) 0.0417(14) -0.0072(12) 0.0023(10) 0.0031(11) C18 0.0301(13) 0.0480(17) 0.0455(15) -0.0077(13) 0.0059(11) -0.0032(12) C19 0.0362(14) 0.0529(18) 0.0416(15) -0.0149(14) 0.0016(11) -0.0066(13) C20 0.0327(13) 0.0371(15) 0.0578(17) -0.0081(14) 0.0012(12) -0.0010(12) C21 0.0410(14) 0.0399(16) 0.0432(15) -0.0032(13) 0.0002(11) 0.0025(12) C22 0.0677(19) 0.057(2) 0.0507(17) -0.0022(15) 0.0019(14) -0.0124(15) C23 0.0591(18) 0.069(2) 0.0533(17) -0.0063(16) 0.0134(14) -0.0252(16) C24 0.0495(17) 0.066(2) 0.077(2) -0.0255(18) 0.0167(15) -0.0168(15) C25 0.0261(12) 0.0323(14) 0.0499(15) -0.0035(12) 0.0025(10) 0.0001(10) C26 0.0337(13) 0.0410(16) 0.0551(16) 0.0023(14) 0.0036(11) 0.0015(12) C27 0.0334(14) 0.0434(17) 0.074(2) 0.0169(15) 0.0012(13) 0.0013(12) C28 0.0367(15) 0.0331(16) 0.086(2) -0.0171(16) 0.0151(14) 0.0036(12) C29 0.0440(15) 0.0460(18) 0.0612(18) -0.0111(15) 0.0062(13) 0.0030(13) C30 0.0376(14) 0.0391(16) 0.0509(16) -0.0091(13) 0.0074(11) -0.0050(12) C31 0.0580(17) 0.068(2) 0.0448(16) -0.0090(15) 0.0040(13) 0.0049(15) C32 0.0623(19) 0.067(2) 0.0544(18) 0.0088(16) 0.0066(14) 0.0068(16) C33 0.070(2) 0.066(2) 0.109(3) 0.030(2) 0.0033(19) 0.0053(18) C34 0.0270(12) 0.0341(14) 0.0475(15) 0.0055(12) -0.0056(10) -0.0020(11) C35 0.0373(14) 0.0425(17) 0.0530(16) 0.0101(14) -0.0058(12) -0.0048(12) C36 0.0450(15) 0.0495(18) 0.0611(19) 0.0169(15) -0.0076(13) -0.0096(14) C37 0.0479(16) 0.0303(16) 0.075(2) 0.0065(15) -0.0084(14) -0.0080(13) C38 0.0424(15) 0.0404(16) 0.0594(17) -0.0012(14) -0.0077(13) -0.0019(13) C39 0.0318(13) 0.0362(15) 0.0528(16) 0.0047(13) -0.0042(11) -0.0028(11) C40 0.0542(16) 0.0471(17) 0.0505(16) -0.0044(14) 0.0077(13) -0.0081(13) C41 0.0505(16) 0.059(2) 0.0558(17) 0.0174(15) 0.0004(13) -0.0071(14) C42 0.098(3) 0.047(2) 0.095(3) -0.006(2) -0.013(2) -0.0213(19) C43 0.0234(11) 0.0325(14) 0.0407(14) 0.0018(11) 0.0004(10) 0.0005(10) C44 0.0294(12) 0.0361(15) 0.0432(14) 0.0028(12) -0.0013(10) -0.0004(11) C45 0.0335(13) 0.0396(16) 0.0462(15) -0.0067(13) 0.0033(11) -0.0004(11) C46 0.0316(13) 0.0303(15) 0.0554(16) 0.0053(13) -0.0049(11) 0.0002(11) C47 0.0392(14) 0.0435(16) 0.0431(15) 0.0103(13) 0.0034(11) 0.0027(12) C48 0.0278(12) 0.0383(15) 0.0491(15) 0.0052(13) 0.0007(10) 0.0009(11) C49 0.0463(15) 0.0619(19) 0.0443(15) 0.0098(14) 0.0086(12) 0.0125(14) C50 0.0492(15) 0.0431(16) 0.0414(15) 0.0035(13) 0.0028(11) 0.0032(13) C51 0.0614(18) 0.0458(18) 0.0554(17) -0.0062(15) 0.0085(13) 0.0084(14) C52 0.0427(15) 0.0401(16) 0.0530(16) 0.0027(14) 0.0039(12) -0.0046(12) C61 0.0406(15) 0.0533(19) 0.0597(18) 0.0129(16) -0.0019(13) -0.0032(13) C62 0.0345(14) 0.0464(17) 0.0673(19) 0.0063(16) -0.0024(13) -0.0054(12) C63 0.0276(13) 0.0497(18) 0.0532(17) -0.0038(14) -0.0047(11) 0.0008(12) C64 0.0358(14) 0.0490(18) 0.0632(19) -0.0011(16) -0.0070(12) 0.0014(13) C65 0.0393(15) 0.071(2) 0.0580(19) -0.0110(17) -0.0052(13) 0.0025(15) C66 0.0389(15) 0.069(2) 0.0549(18) 0.0088(16) -0.0010(12) 0.0001(14) C67 0.0302(13) 0.0555(19) 0.0490(16) 0.0026(15) -0.0030(11) -0.0010(12) C68 0.0234(12) 0.0508(18) 0.0498(15) 0.0011(14) -0.0035(11) -0.0015(12) C71 0.048(2) 0.053(3) 0.075(3) -0.021(2) 0.005(2) -0.004(2) C72 0.068(3) 0.050(3) 0.091(3) -0.003(2) -0.008(3) 0.009(2) C73 0.075(4) 0.044(3) 0.084(3) 0.019(2) 0.006(3) 0.001(2) C74 0.042(2) 0.038(2) 0.083(3) -0.007(2) 0.0129(18) -0.0095(18) C75 0.052(2) 0.051(2) 0.065(2) -0.006(2) 0.0123(18) -0.0103(19) C76 0.054(2) 0.037(2) 0.077(3) -0.001(2) -0.0091(18) -0.0065(17) C77 0.069(3) 0.034(2) 0.062(2) -0.006(2) -0.004(2) 0.0031(19) C78 0.052(2) 0.040(2) 0.067(2) -0.003(2) -0.0011(18) -0.0049(17) _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 O1 C20 1.385(3) . ? O1 C24 1.404(3) . ? O2 C33 1.376(3) . ? O2 C28 1.396(3) . ? O3 C37 1.378(3) . ? O3 C42 1.413(4) . ? O4 C46 1.374(3) . ? O4 C51 1.404(3) . ? C1 C2 1.386(3) . ? C1 C11 1.409(3) . ? C1 C17 1.495(3) . ? C2 C3 1.385(3) . ? C2 H2 0.9500 . ? C3 C12 1.412(3) . ? C3 C25 1.493(3) . ? C4 C5 1.335(3) . ? C4 C12 1.432(3) . ? C4 H4 0.9500 . ? C5 C13 1.435(3) . ? C5 H5 0.9500 . ? C6 C7 1.390(3) . ? C6 C13 1.411(3) . ? C6 C34 1.497(3) . ? C7 C8 1.386(3) . ? C7 H7 0.9500 . ? C8 C14 1.408(3) . ? C8 C43 1.496(3) . ? C9 C10 1.346(3) . ? C9 C14 1.432(3) . ? C9 H9 0.9500 . ? C10 C11 1.432(3) . ? C10 H10 0.9500 . ? C11 C16 1.426(3) . ? C12 C16 1.419(3) . ? C13 C15 1.418(3) . ? C14 C15 1.421(3) . ? C15 C16 1.436(3) . ? C17 C18 1.397(3) . ? C17 C21 1.406(3) . ? C18 C19 1.398(3) . ? C18 C23 1.497(4) . ? C19 C20 1.366(4) . ? C19 H19 0.9500 . ? C20 C52 1.379(3) . ? C21 C52 1.382(3) . ? C21 C22 1.510(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.394(3) . ? C25 C30 1.416(3) . ? C26 C27 1.401(4) . ? C26 C32 1.495(4) . ? C27 C28 1.386(4) . ? C27 H27 0.9500 . ? C28 C29 1.354(4) . ? C29 C30 1.379(4) . ? C29 H29 0.9500 . ? C30 C31 1.503(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C39 1.389(3) . ? C34 C35 1.406(3) . ? C35 C36 1.381(4) . ? C35 C41 1.519(4) . ? C36 C37 1.381(4) . ? C36 H36 0.9500 . ? C37 C38 1.386(4) . ? C38 C39 1.408(4) . ? C38 H38 0.9500 . ? C39 C40 1.496(3) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.396(3) . ? C43 C48 1.403(3) . ? C44 C45 1.399(3) . ? C44 C50 1.501(3) . ? C45 C46 1.385(3) . ? C45 H45 0.9500 . ? C46 C47 1.375(3) . ? C47 C48 1.385(3) . ? C47 H47 0.9500 . ? C48 C49 1.501(3) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52 0.9500 . ? C61 C62 1.342(4) . ? C61 C67 1.435(4) 3_565 ? C61 H61 0.9500 . ? C62 C63 1.434(4) . ? C62 H62 0.9500 . ? C63 C64 1.396(4) . ? C63 C68 1.417(4) . ? C64 C65 1.371(4) . ? C64 H64 0.9500 . ? C65 C66 1.392(4) . ? C65 H65 0.9500 . ? C66 C67 1.394(4) . ? C66 H66 0.9500 . ? C67 C68 1.415(3) . ? C67 C61 1.435(4) 3_565 ? C68 C68 1.430(5) 3_565 ? C71 C72 1.507(5) . ? C71 C78 1.514(5) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.528(5) . ? C72 H72A 0.9900 . ? C72 H72B 0.9900 . ? C73 C74 1.504(5) . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C74 C75 1.483(5) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 C76 1.536(5) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C76 C77 1.508(5) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 C78 1.536(5) . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C71A C72A 1.497(8) . ? C71A C78A 1.508(8) . ? C71A H71A 0.9900 . ? C71A H71B 0.9900 . ? C72A C73A 1.520(8) . ? C72A H72A 0.9900 . ? C72A H72B 0.9900 . ? C73A C74A 1.517(8) . ? C73A H73A 0.9900 . ? C73A H73B 0.9900 . ? C74A C75A 1.522(8) . ? C74A H74A 0.9900 . ? C74A H74B 0.9900 . ? C75A C76A 1.522(8) . ? C75A H75A 0.9900 . ? C75A H75B 0.9900 . ? C76A C77A 1.525(8) . ? C76A H76A 0.9900 . ? C76A H76B 0.9900 . ? C77A C78A 1.512(8) . ? C77A H77A 0.9900 . ? C77A H77B 0.9900 . ? C78A H78A 0.9900 . ? C78A H78B 0.9900 . ? 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 C20 O1 C24 116.7(2) . . ? C33 O2 C28 115.9(3) . . ? C37 O3 C42 117.2(3) . . ? C46 O4 C51 116.6(2) . . ? C2 C1 C11 118.9(2) . . ? C2 C1 C17 120.7(2) . . ? C11 C1 C17 120.4(2) . . ? C3 C2 C1 123.3(2) . . ? C3 C2 H2 118.4 . . ? C1 C2 H2 118.4 . . ? C2 C3 C12 119.1(2) . . ? C2 C3 C25 120.8(2) . . ? C12 C3 C25 120.0(2) . . ? C5 C4 C12 121.8(2) . . ? C5 C4 H4 119.1 . . ? C12 C4 H4 119.1 . . ? C4 C5 C13 121.9(2) . . ? C4 C5 H5 119.1 . . ? C13 C5 H5 119.1 . . ? C7 C6 C13 119.1(2) . . ? C7 C6 C34 122.0(2) . . ? C13 C6 C34 118.9(2) . . ? C8 C7 C6 122.8(2) . . ? C8 C7 H7 118.6 . . ? C6 C7 H7 118.6 . . ? C7 C8 C14 119.0(2) . . ? C7 C8 C43 121.0(2) . . ? C14 C8 C43 120.0(2) . . ? C10 C9 C14 122.0(2) . . ? C10 C9 H9 119.0 . . ? C14 C9 H9 119.0 . . ? C9 C10 C11 121.8(2) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C1 C11 C16 119.2(2) . . ? C1 C11 C10 122.7(2) . . ? C16 C11 C10 118.09(19) . . ? C3 C12 C16 119.1(2) . . ? C3 C12 C4 122.4(2) . . ? C16 C12 C4 118.5(2) . . ? C6 C13 C15 119.4(2) . . ? C6 C13 C5 122.4(2) . . ? C15 C13 C5 118.15(19) . . ? C8 C14 C15 119.7(2) . . ? C8 C14 C9 122.0(2) . . ? C15 C14 C9 118.30(19) . . ? C13 C15 C14 120.05(19) . . ? C13 C15 C16 120.1(2) . . ? C14 C15 C16 119.8(2) . . ? C12 C16 C11 120.41(19) . . ? C12 C16 C15 119.5(2) . . ? C11 C16 C15 120.1(2) . . ? C18 C17 C21 119.3(2) . . ? C18 C17 C1 120.6(2) . . ? C21 C17 C1 120.2(2) . . ? C17 C18 C19 119.5(2) . . ? C17 C18 C23 120.7(2) . . ? C19 C18 C23 119.7(2) . . ? C20 C19 C18 120.8(2) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C19 C20 C52 119.9(2) . . ? C19 C20 O1 124.6(2) . . ? C52 C20 O1 115.5(2) . . ? C52 C21 C17 119.4(2) . . ? C52 C21 C22 120.4(2) . . ? C17 C21 C22 120.1(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O1 C24 H24A 109.5 . . ? O1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 120.0(2) . . ? C26 C25 C3 121.5(2) . . ? C30 C25 C3 118.5(2) . . ? C25 C26 C27 119.1(2) . . ? C25 C26 C32 120.5(2) . . ? C27 C26 C32 120.4(2) . . ? C28 C27 C26 119.8(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 121.0(2) . . ? C29 C28 O2 114.5(3) . . ? C27 C28 O2 124.5(3) . . ? C28 C29 C30 121.3(3) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C29 C30 C25 118.9(2) . . ? C29 C30 C31 120.0(2) . . ? C25 C30 C31 121.1(2) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 C33 H33A 109.5 . . ? O2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C39 C34 C35 120.2(2) . . ? C39 C34 C6 121.2(2) . . ? C35 C34 C6 118.5(2) . . ? C36 C35 C34 119.2(2) . . ? C36 C35 C41 120.1(2) . . ? C34 C35 C41 120.7(2) . . ? C35 C36 C37 120.9(3) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? O3 C37 C36 115.2(3) . . ? O3 C37 C38 124.3(3) . . ? C36 C37 C38 120.5(2) . . ? C37 C38 C39 119.5(3) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C34 C39 C38 119.7(2) . . ? C34 C39 C40 121.0(2) . . ? C38 C39 C40 119.2(2) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C35 C41 H41A 109.5 . . ? C35 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C35 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O3 C42 H42A 109.5 . . ? O3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C48 120.3(2) . . ? C44 C43 C8 120.9(2) . . ? C48 C43 C8 118.7(2) . . ? C43 C44 C45 119.0(2) . . ? C43 C44 C50 120.3(2) . . ? C45 C44 C50 120.7(2) . . ? C46 C45 C44 120.2(2) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? O4 C46 C47 115.0(2) . . ? O4 C46 C45 124.5(2) . . ? C47 C46 C45 120.4(2) . . ? C46 C47 C48 120.7(2) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C47 C48 C43 119.3(2) . . ? C47 C48 C49 119.9(2) . . ? C43 C48 C49 120.8(2) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C44 C50 H50A 109.5 . . ? C44 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C44 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O4 C51 H51A 109.5 . . ? O4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C20 C52 C21 121.0(3) . . ? C20 C52 H52 119.5 . . ? C21 C52 H52 119.5 . . ? C62 C61 C67 121.1(3) . 3_565 ? C62 C61 H61 119.4 . . ? C67 C61 H61 119.4 3_565 . ? C61 C62 C63 121.9(3) . . ? C61 C62 H62 119.0 . . ? C63 C62 H62 119.0 . . ? C64 C63 C68 118.7(3) . . ? C64 C63 C62 122.9(3) . . ? C68 C63 C62 118.5(2) . . ? C65 C64 C63 121.1(3) . . ? C65 C64 H64 119.5 . . ? C63 C64 H64 119.5 . . ? C64 C65 C66 120.7(3) . . ? C64 C65 H65 119.7 . . ? C66 C65 H65 119.7 . . ? C65 C66 C67 120.5(3) . . ? C65 C66 H66 119.8 . . ? C67 C66 H66 119.8 . . ? C66 C67 C68 118.9(3) . . ? C66 C67 C61 122.4(3) . 3_565 ? C68 C67 C61 118.7(2) . 3_565 ? C67 C68 C63 120.2(2) . . ? C67 C68 C68 120.1(3) . 3_565 ? C63 C68 C68 119.7(3) . 3_565 ? C72 C71 C78 118.8(3) . . ? C72 C71 H71A 107.6 . . ? C78 C71 H71A 107.6 . . ? C72 C71 H71B 107.6 . . ? C78 C71 H71B 107.6 . . ? H71A C71 H71B 107.1 . . ? C71 C72 C73 119.0(3) . . ? C71 C72 H72A 107.6 . . ? C73 C72 H72A 107.6 . . ? C71 C72 H72B 107.6 . . ? C73 C72 H72B 107.6 . . ? H72A C72 H72B 107.0 . . ? C74 C73 C72 116.1(4) . . ? C74 C73 H73A 108.3 . . ? C72 C73 H73A 108.3 . . ? C74 C73 H73B 108.3 . . ? C72 C73 H73B 108.3 . . ? H73A C73 H73B 107.4 . . ? C75 C74 C73 118.4(3) . . ? C75 C74 H74A 107.7 . . ? C73 C74 H74A 107.7 . . ? C75 C74 H74B 107.7 . . ? C73 C74 H74B 107.7 . . ? H74A C74 H74B 107.1 . . ? C74 C75 C76 119.0(3) . . ? C74 C75 H75A 107.6 . . ? C76 C75 H75A 107.6 . . ? C74 C75 H75B 107.6 . . ? C76 C75 H75B 107.6 . . ? H75A C75 H75B 107.0 . . ? C77 C76 C75 115.9(3) . . ? C77 C76 H76A 108.3 . . ? C75 C76 H76A 108.3 . . ? C77 C76 H76B 108.3 . . ? C75 C76 H76B 108.3 . . ? H76A C76 H76B 107.4 . . ? C76 C77 C78 115.6(4) . . ? C76 C77 H77A 108.4 . . ? C78 C77 H77A 108.4 . . ? C76 C77 H77B 108.4 . . ? C78 C77 H77B 108.4 . . ? H77A C77 H77B 107.4 . . ? C71 C78 C77 118.6(3) . . ? C71 C78 H78A 107.7 . . ? C77 C78 H78A 107.7 . . ? C71 C78 H78B 107.7 . . ? C77 C78 H78B 107.7 . . ? H78A C78 H78B 107.1 . . ? C72A C71A C78A 116.9(8) . . ? C72A C71A H71A 108.1 . . ? C78A C71A H71A 108.1 . . ? C72A C71A H71B 108.1 . . ? C78A C71A H71B 108.1 . . ? H71A C71A H71B 107.3 . . ? C71A C72A C73A 114.4(7) . . ? C71A C72A H72A 108.7 . . ? C73A C72A H72A 108.7 . . ? C71A C72A H72B 108.7 . . ? C73A C72A H72B 108.7 . . ? H72A C72A H72B 107.6 . . ? C74A C73A C72A 114.6(7) . . ? C74A C73A H73A 108.6 . . ? C72A C73A H73A 108.6 . . ? C74A C73A H73B 108.6 . . ? C72A C73A H73B 108.6 . . ? H73A C73A H73B 107.6 . . ? C73A C74A C75A 113.4(7) . . ? C73A C74A H74A 108.9 . . ? C75A C74A H74A 108.9 . . ? C73A C74A H74B 108.9 . . ? C75A C74A H74B 108.9 . . ? H74A C74A H74B 107.7 . . ? C74A C75A C76A 114.1(8) . . ? C74A C75A H75A 108.7 . . ? C76A C75A H75A 108.7 . . ? C74A C75A H75B 108.7 . . ? C76A C75A H75B 108.7 . . ? H75A C75A H75B 107.6 . . ? C75A C76A C77A 114.1(7) . . ? C75A C76A H76A 108.7 . . ? C77A C76A H76A 108.7 . . ? C75A C76A H76B 108.7 . . ? C77A C76A H76B 108.7 . . ? H76A C76A H76B 107.6 . . ? C78A C77A C76A 114.6(7) . . ? C78A C77A H77A 108.6 . . ? C76A C77A H77A 108.6 . . ? C78A C77A H77B 108.6 . . ? C76A C77A H77B 108.6 . . ? H77A C77A H77B 107.6 . . ? C71A C78A C77A 115.7(8) . . ? C71A C78A H78A 108.4 . . ? C77A C78A H78A 108.4 . . ? C71A C78A H78B 108.4 . . ? C77A C78A H78B 108.4 . . ? H78A C78A H78B 107.4 . . ? 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 C11 C1 C2 C3 0.1(4) . . . . ? C17 C1 C2 C3 -178.0(2) . . . . ? C1 C2 C3 C12 -1.0(4) . . . . ? C1 C2 C3 C25 175.6(2) . . . . ? C12 C4 C5 C13 0.7(4) . . . . ? C13 C6 C7 C8 -0.4(4) . . . . ? C34 C6 C7 C8 177.1(2) . . . . ? C6 C7 C8 C14 -0.3(3) . . . . ? C6 C7 C8 C43 177.7(2) . . . . ? C14 C9 C10 C11 0.7(3) . . . . ? C2 C1 C11 C16 0.9(3) . . . . ? C17 C1 C11 C16 179.0(2) . . . . ? C2 C1 C11 C10 -179.5(2) . . . . ? C17 C1 C11 C10 -1.4(3) . . . . ? C9 C10 C11 C1 -179.7(2) . . . . ? C9 C10 C11 C16 -0.1(3) . . . . ? C2 C3 C12 C16 0.8(3) . . . . ? C25 C3 C12 C16 -175.8(2) . . . . ? C2 C3 C12 C4 -178.5(2) . . . . ? C25 C3 C12 C4 4.9(3) . . . . ? C5 C4 C12 C3 179.4(2) . . . . ? C5 C4 C12 C16 0.1(3) . . . . ? C7 C6 C13 C15 0.9(3) . . . . ? C34 C6 C13 C15 -176.7(2) . . . . ? C7 C6 C13 C5 179.8(2) . . . . ? C34 C6 C13 C5 2.2(3) . . . . ? C4 C5 C13 C6 -179.8(2) . . . . ? C4 C5 C13 C15 -0.8(3) . . . . ? C7 C8 C14 C15 0.5(3) . . . . ? C43 C8 C14 C15 -177.5(2) . . . . ? C7 C8 C14 C9 -179.8(2) . . . . ? C43 C8 C14 C9 2.2(3) . . . . ? C10 C9 C14 C8 179.4(2) . . . . ? C10 C9 C14 C15 -0.9(3) . . . . ? C6 C13 C15 C14 -0.7(3) . . . . ? C5 C13 C15 C14 -179.7(2) . . . . ? C6 C13 C15 C16 179.1(2) . . . . ? C5 C13 C15 C16 0.2(3) . . . . ? C8 C14 C15 C13 0.0(3) . . . . ? C9 C14 C15 C13 -179.7(2) . . . . ? C8 C14 C15 C16 -179.83(19) . . . . ? C9 C14 C15 C16 0.5(3) . . . . ? C3 C12 C16 C11 0.2(3) . . . . ? C4 C12 C16 C11 179.5(2) . . . . ? C3 C12 C16 C15 179.90(19) . . . . ? C4 C12 C16 C15 -0.8(3) . . . . ? C1 C11 C16 C12 -1.0(3) . . . . ? C10 C11 C16 C12 179.4(2) . . . . ? C1 C11 C16 C15 179.2(2) . . . . ? C10 C11 C16 C15 -0.4(3) . . . . ? C13 C15 C16 C12 0.6(3) . . . . ? C14 C15 C16 C12 -179.6(2) . . . . ? C13 C15 C16 C11 -179.6(2) . . . . ? C14 C15 C16 C11 0.2(3) . . . . ? C2 C1 C17 C18 -91.1(3) . . . . ? C11 C1 C17 C18 90.9(3) . . . . ? C2 C1 C17 C21 89.5(3) . . . . ? C11 C1 C17 C21 -88.6(3) . . . . ? C21 C17 C18 C19 0.7(3) . . . . ? C1 C17 C18 C19 -178.7(2) . . . . ? C21 C17 C18 C23 -179.6(2) . . . . ? C1 C17 C18 C23 0.9(3) . . . . ? C17 C18 C19 C20 0.1(4) . . . . ? C23 C18 C19 C20 -179.5(2) . . . . ? C18 C19 C20 C52 -1.3(4) . . . . ? C18 C19 C20 O1 179.1(2) . . . . ? C24 O1 C20 C19 -5.5(4) . . . . ? C24 O1 C20 C52 174.9(2) . . . . ? C18 C17 C21 C52 -0.4(3) . . . . ? C1 C17 C21 C52 179.1(2) . . . . ? C18 C17 C21 C22 -178.3(2) . . . . ? C1 C17 C21 C22 1.2(3) . . . . ? C2 C3 C25 C26 78.7(3) . . . . ? C12 C3 C25 C26 -104.7(3) . . . . ? C2 C3 C25 C30 -101.5(3) . . . . ? C12 C3 C25 C30 75.0(3) . . . . ? C30 C25 C26 C27 -0.2(3) . . . . ? C3 C25 C26 C27 179.6(2) . . . . ? C30 C25 C26 C32 179.7(2) . . . . ? C3 C25 C26 C32 -0.5(3) . . . . ? C25 C26 C27 C28 -0.9(4) . . . . ? C32 C26 C27 C28 179.2(2) . . . . ? C26 C27 C28 C29 0.9(4) . . . . ? C26 C27 C28 O2 178.4(2) . . . . ? C33 O2 C28 C29 -173.5(3) . . . . ? C33 O2 C28 C27 8.9(4) . . . . ? C27 C28 C29 C30 0.1(4) . . . . ? O2 C28 C29 C30 -177.6(2) . . . . ? C28 C29 C30 C25 -1.1(4) . . . . ? C28 C29 C30 C31 176.0(2) . . . . ? C26 C25 C30 C29 1.1(3) . . . . ? C3 C25 C30 C29 -178.6(2) . . . . ? C26 C25 C30 C31 -175.9(2) . . . . ? C3 C25 C30 C31 4.4(3) . . . . ? C7 C6 C34 C39 97.4(3) . . . . ? C13 C6 C34 C39 -85.0(3) . . . . ? C7 C6 C34 C35 -86.9(3) . . . . ? C13 C6 C34 C35 90.7(3) . . . . ? C39 C34 C35 C36 2.9(3) . . . . ? C6 C34 C35 C36 -172.8(2) . . . . ? C39 C34 C35 C41 -175.9(2) . . . . ? C6 C34 C35 C41 8.4(3) . . . . ? C34 C35 C36 C37 -1.3(4) . . . . ? C41 C35 C36 C37 177.5(2) . . . . ? C42 O3 C37 C36 -175.9(3) . . . . ? C42 O3 C37 C38 6.7(4) . . . . ? C35 C36 C37 O3 -178.4(2) . . . . ? C35 C36 C37 C38 -0.9(4) . . . . ? O3 C37 C38 C39 178.7(2) . . . . ? C36 C37 C38 C39 1.4(4) . . . . ? C35 C34 C39 C38 -2.3(3) . . . . ? C6 C34 C39 C38 173.2(2) . . . . ? C35 C34 C39 C40 175.2(2) . . . . ? C6 C34 C39 C40 -9.2(3) . . . . ? C37 C38 C39 C34 0.2(4) . . . . ? C37 C38 C39 C40 -177.4(2) . . . . ? C7 C8 C43 C44 97.9(3) . . . . ? C14 C8 C43 C44 -84.1(3) . . . . ? C7 C8 C43 C48 -84.5(3) . . . . ? C14 C8 C43 C48 93.5(3) . . . . ? C48 C43 C44 C45 -0.7(3) . . . . ? C8 C43 C44 C45 176.8(2) . . . . ? C48 C43 C44 C50 178.9(2) . . . . ? C8 C43 C44 C50 -3.5(3) . . . . ? C43 C44 C45 C46 -0.3(3) . . . . ? C50 C44 C45 C46 -180.0(2) . . . . ? C51 O4 C46 C47 -169.3(2) . . . . ? C51 O4 C46 C45 12.4(3) . . . . ? C44 C45 C46 O4 -179.8(2) . . . . ? C44 C45 C46 C47 2.0(3) . . . . ? O4 C46 C47 C48 178.9(2) . . . . ? C45 C46 C47 C48 -2.8(4) . . . . ? C46 C47 C48 C43 1.7(3) . . . . ? C46 C47 C48 C49 -179.0(2) . . . . ? C44 C43 C48 C47 0.0(3) . . . . ? C8 C43 C48 C47 -177.5(2) . . . . ? C44 C43 C48 C49 -179.3(2) . . . . ? C8 C43 C48 C49 3.1(3) . . . . ? C19 C20 C52 C21 1.7(4) . . . . ? O1 C20 C52 C21 -178.7(2) . . . . ? C17 C21 C52 C20 -0.8(4) . . . . ? C22 C21 C52 C20 177.1(2) . . . . ? C67 C61 C62 C63 -0.8(4) 3_565 . . . ? C61 C62 C63 C64 179.8(2) . . . . ? C61 C62 C63 C68 0.1(3) . . . . ? C68 C63 C64 C65 -0.5(3) . . . . ? C62 C63 C64 C65 179.8(2) . . . . ? C63 C64 C65 C66 0.8(4) . . . . ? C64 C65 C66 C67 -0.4(4) . . . . ? C65 C66 C67 C68 -0.2(4) . . . . ? C65 C66 C67 C61 179.6(2) . . . 3_565 ? C66 C67 C68 C63 0.6(3) . . . . ? C61 C67 C68 C63 -179.3(2) 3_565 . . . ? C66 C67 C68 C68 179.0(2) . . . 3_565 ? C61 C67 C68 C68 -0.9(4) 3_565 . . 3_565 ? C64 C63 C68 C67 -0.2(3) . . . . ? C62 C63 C68 C67 179.5(2) . . . . ? C64 C63 C68 C68 -178.6(2) . . . 3_565 ? C62 C63 C68 C68 1.1(4) . . . 3_565 ? C78 C71 C72 C73 61.3(5) . . . . ? C71 C72 C73 C74 42.2(5) . . . . ? C72 C73 C74 C75 -99.3(5) . . . . ? C73 C74 C75 C76 64.9(5) . . . . ? C74 C75 C76 C77 -62.9(5) . . . . ? C75 C76 C77 C78 99.5(4) . . . . ? C72 C71 C78 C77 -58.7(5) . . . . ? C76 C77 C78 C71 -47.7(5) . . . . ? C78A C71A C72A C73A -63.8(18) . . . . ? C71A C72A C73A C74A 104.6(12) . . . . ? C72A C73A C74A C75A -48.0(18) . . . . ? C73A C74A C75A C76A -67.2(19) . . . . ? C74A C75A C76A C77A 72(2) . . . . ? C75A C76A C77A C78A 40(2) . . . . ? C72A C71A C78A C77A 66.6(18) . . . . ? C76A C77A C78A C71A -103.1(14) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.300 _refine_diff_density_min -0.273 _refine_diff_density_rms 0.054 #END data_TP-PC _database_code_depnum_ccdc_archive 'CCDC 726026' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra(2,6-dimethyl-4-methoxyphenyl)pyrene ; _chemical_name_common tetra(2,6-dimethyl-4-methoxyphenyl)pyrene _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 O4, C16 H10, C H Cl3' _chemical_formula_sum 'C69 H61 Cl3 O4' _chemical_formula_weight 1060.53 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 25.857(5) _cell_length_b 15.118(3) _cell_length_c 13.916(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.224(4) _cell_angle_gamma 90.00 _cell_volume 5431.1(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3447 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.63 _exptl_crystal_description 'thick needles' _exptl_crystal_colour 'color less' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.297 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2232 _exptl_absorpt_coefficient_mu 0.221 _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 100(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 'Bruker SMART APEX' _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 27548 _diffrn_reflns_av_R_equivalents 0.0708 _diffrn_reflns_av_sigmaI/netI 0.0827 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9512 _reflns_number_gt 5793 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0753P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9512 _refine_ls_number_parameters 685 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.1791 _refine_ls_wR_factor_gt 0.1568 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _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 Cl1 Cl 0.28013(5) 0.42130(7) 0.19080(8) 0.0618(3) Uani 1 1 d . . . Cl2 Cl 0.31907(4) 0.59862(7) 0.18212(8) 0.0533(3) Uani 1 1 d . . . Cl3 Cl 0.22650(4) 0.56258(7) 0.28486(8) 0.0513(3) Uani 1 1 d . . . O1 O 0.44603(10) 0.61812(14) 0.03844(16) 0.0379(6) Uani 1 1 d . . . O2 O 0.38447(9) 1.43363(13) -0.00612(16) 0.0336(6) Uani 1 1 d . . . O3 O 0.04828(9) 1.35178(15) 0.48156(17) 0.0391(6) Uani 1 1 d . . . O4 O 0.11682(9) 0.54973(13) 0.47681(15) 0.0315(6) Uani 1 1 d . . . C1 C 0.34523(12) 0.93546(19) 0.1339(2) 0.0224(7) Uani 1 1 d . . . C2 C 0.35737(12) 1.02022(19) 0.1012(2) 0.0226(7) Uani 1 1 d . . . H2 H 0.3867 1.0274 0.0637 0.027 Uiso 1 1 calc R . . C3 C 0.32784(12) 1.09461(19) 0.1216(2) 0.0223(7) Uani 1 1 d . . . C4 C 0.25343(12) 1.1589(2) 0.2035(2) 0.0234(7) Uani 1 1 d . . . H4 H 0.2622 1.2163 0.1819 0.028 Uiso 1 1 calc R . . C5 C 0.21216(12) 1.14923(19) 0.2571(2) 0.0236(7) Uani 1 1 d . . . H5 H 0.1927 1.2000 0.2729 0.028 Uiso 1 1 calc R . . C6 C 0.15377(12) 1.05270(19) 0.3474(2) 0.0223(7) Uani 1 1 d . . . C7 C 0.14074(12) 0.9676(2) 0.3767(2) 0.0238(7) Uani 1 1 d . . . H7 H 0.1111 0.9602 0.4134 0.029 Uiso 1 1 calc R . . C8 C 0.16950(12) 0.89303(19) 0.3544(2) 0.0228(7) Uani 1 1 d . . . C9 C 0.24528(12) 0.82956(19) 0.2765(2) 0.0229(7) Uani 1 1 d . . . H9 H 0.2366 0.7721 0.2979 0.028 Uiso 1 1 calc R . . C10 C 0.28708(12) 0.83976(19) 0.2246(2) 0.0223(7) Uani 1 1 d . . . H10 H 0.3071 0.7893 0.2103 0.027 Uiso 1 1 calc R . . C11 C 0.30243(12) 0.92480(19) 0.1899(2) 0.0203(7) Uani 1 1 d . . . C12 C 0.28486(12) 1.08444(19) 0.1778(2) 0.0212(7) Uani 1 1 d . . . C13 C 0.19671(12) 1.06385(19) 0.2911(2) 0.0208(7) Uani 1 1 d . . . C14 C 0.21343(12) 0.90285(19) 0.3004(2) 0.0215(7) Uani 1 1 d . . . C15 C 0.22715(12) 0.98870(19) 0.2678(2) 0.0209(7) Uani 1 1 d . . . C16 C 0.27148(12) 0.99962(19) 0.2122(2) 0.0207(7) Uani 1 1 d . . . C17 C 0.37619(12) 0.85616(19) 0.1081(2) 0.0229(7) Uani 1 1 d . . . C18 C 0.35907(12) 0.8059(2) 0.0264(2) 0.0255(7) Uani 1 1 d . . . C19 C 0.38365(13) 0.7278(2) 0.0070(2) 0.0280(8) Uani 1 1 d . . . H19 H 0.3721 0.6942 -0.0478 0.034 Uiso 1 1 calc R . . C20 C 0.42466(13) 0.6973(2) 0.0654(2) 0.0289(8) Uani 1 1 d . . . C21 C 0.44238(13) 0.7463(2) 0.1438(2) 0.0266(8) Uani 1 1 d . . . H21 H 0.4709 0.7255 0.1836 0.032 Uiso 1 1 calc R . . C22 C 0.41863(12) 0.8267(2) 0.1655(2) 0.0233(7) Uani 1 1 d . . . C23 C 0.44019(13) 0.8800(2) 0.2503(2) 0.0333(8) Uani 1 1 d . . . H23A H 0.4731 0.9070 0.2344 0.050 Uiso 1 1 calc R . . H23B H 0.4460 0.8411 0.3062 0.050 Uiso 1 1 calc R . . H23C H 0.4155 0.9265 0.2653 0.050 Uiso 1 1 calc R . . C24 C 0.31527(13) 0.8395(2) -0.0390(2) 0.0357(9) Uani 1 1 d . . . H24A H 0.3112 0.8013 -0.0959 0.054 Uiso 1 1 calc R . . H24B H 0.3228 0.9000 -0.0592 0.054 Uiso 1 1 calc R . . H24C H 0.2832 0.8391 -0.0048 0.054 Uiso 1 1 calc R . . C25 C 0.48484(16) 0.5796(2) 0.1025(3) 0.0465(10) Uani 1 1 d . . . H25A H 0.5161 0.6163 0.1042 0.070 Uiso 1 1 calc R . . H25B H 0.4931 0.5201 0.0800 0.070 Uiso 1 1 calc R . . H25C H 0.4719 0.5758 0.1672 0.070 Uiso 1 1 calc R . . C26 C 0.34249(12) 1.18329(19) 0.0849(2) 0.0217(7) Uani 1 1 d . . . C27 C 0.31586(12) 1.21953(19) 0.0041(2) 0.0233(7) Uani 1 1 d . . . C28 C 0.32932(12) 1.3034(2) -0.0289(2) 0.0260(7) Uani 1 1 d . . . H28 H 0.3114 1.3281 -0.0841 0.031 Uiso 1 1 calc R . . C29 C 0.36893(13) 1.3506(2) 0.0194(2) 0.0260(8) Uani 1 1 d . . . C30 C 0.39591(13) 1.3144(2) 0.0982(2) 0.0277(8) Uani 1 1 d . . . H30 H 0.4235 1.3467 0.1297 0.033 Uiso 1 1 calc R . . C31 C 0.41205(13) 1.1927(2) 0.2190(2) 0.0316(8) Uani 1 1 d . . . H31A H 0.4395 1.2337 0.2416 0.047 Uiso 1 1 calc R . . H31B H 0.4275 1.1360 0.2019 0.047 Uiso 1 1 calc R . . H31C H 0.3881 1.1834 0.2701 0.047 Uiso 1 1 calc R . . C32 C 0.27277(13) 1.1696(2) -0.0482(2) 0.0321(8) Uani 1 1 d . . . H32A H 0.2420 1.1709 -0.0103 0.048 Uiso 1 1 calc R . . H32B H 0.2835 1.1082 -0.0575 0.048 Uiso 1 1 calc R . . H32C H 0.2647 1.1973 -0.1110 0.048 Uiso 1 1 calc R . . C33 C 0.35331(14) 1.4784(2) -0.0780(2) 0.0369(9) Uani 1 1 d . . . H33A H 0.3554 1.4477 -0.1396 0.055 Uiso 1 1 calc R . . H33B H 0.3657 1.5393 -0.0841 0.055 Uiso 1 1 calc R . . H33C H 0.3173 1.4792 -0.0597 0.055 Uiso 1 1 calc R . . C34 C 0.12358(12) 1.1307(2) 0.3801(2) 0.0239(7) Uani 1 1 d . . . C35 C 0.07915(12) 1.1601(2) 0.3290(2) 0.0258(7) Uani 1 1 d . . . C36 C 0.05355(13) 1.2355(2) 0.3606(2) 0.0282(8) Uani 1 1 d . . . H36 H 0.0237 1.2569 0.3252 0.034 Uiso 1 1 calc R . . C37 C 0.07161(13) 1.2788(2) 0.4432(2) 0.0297(8) Uani 1 1 d . . . C38 C 0.11556(13) 1.2488(2) 0.4942(2) 0.0312(8) Uani 1 1 d . . . H38 H 0.1278 1.2794 0.5506 0.037 Uiso 1 1 calc R . . C39 C 0.14182(12) 1.1754(2) 0.4648(2) 0.0275(8) Uani 1 1 d . . . C40 C 0.18798(13) 1.1418(2) 0.5237(3) 0.0369(9) Uani 1 1 d . . . H40A H 0.1942 1.1796 0.5804 0.055 Uiso 1 1 calc R . . H40B H 0.2184 1.1429 0.4848 0.055 Uiso 1 1 calc R . . H40C H 0.1815 1.0811 0.5443 0.055 Uiso 1 1 calc R . . C41 C 0.05723(14) 1.1124(2) 0.2416(2) 0.0373(9) Uani 1 1 d . . . H41A H 0.0855 1.0927 0.2028 0.056 Uiso 1 1 calc R . . H41B H 0.0344 1.1523 0.2034 0.056 Uiso 1 1 calc R . . H41C H 0.0374 1.0610 0.2615 0.056 Uiso 1 1 calc R . . C42 C 0.00336(15) 1.3852(2) 0.4308(3) 0.0494(11) Uani 1 1 d . . . H42A H 0.0127 1.4090 0.3687 0.074 Uiso 1 1 calc R . . H42B H -0.0118 1.4324 0.4686 0.074 Uiso 1 1 calc R . . H42C H -0.0219 1.3374 0.4202 0.074 Uiso 1 1 calc R . . C43 C 0.15504(12) 0.80351(19) 0.3905(2) 0.0212(7) Uani 1 1 d . . . C44 C 0.11811(12) 0.75147(19) 0.3376(2) 0.0233(7) Uani 1 1 d . . . C45 C 0.10622(12) 0.6678(2) 0.3698(2) 0.0257(7) Uani 1 1 d . . . H45 H 0.0810 0.6333 0.3346 0.031 Uiso 1 1 calc R . . C46 C 0.13081(12) 0.63342(19) 0.4535(2) 0.0246(7) Uani 1 1 d . . . C47 C 0.16677(12) 0.6846(2) 0.5061(2) 0.0252(7) Uani 1 1 d . . . H47 H 0.1832 0.6617 0.5636 0.030 Uiso 1 1 calc R . . C48 C 0.17897(12) 0.76969(19) 0.4750(2) 0.0242(7) Uani 1 1 d . . . C49 C 0.21812(13) 0.8241(2) 0.5332(2) 0.0328(8) Uani 1 1 d . . . H49A H 0.2487 0.8335 0.4960 0.049 Uiso 1 1 calc R . . H49B H 0.2283 0.7928 0.5931 0.049 Uiso 1 1 calc R . . H49C H 0.2029 0.8814 0.5485 0.049 Uiso 1 1 calc R . . C50 C 0.09127(14) 0.7877(2) 0.2467(2) 0.0331(8) Uani 1 1 d . . . H50A H 0.0669 0.7436 0.2194 0.050 Uiso 1 1 calc R . . H50B H 0.1171 0.8014 0.2000 0.050 Uiso 1 1 calc R . . H50C H 0.0724 0.8417 0.2619 0.050 Uiso 1 1 calc R . . C51 C 0.14450(14) 0.5086(2) 0.5561(2) 0.0350(9) Uani 1 1 d . . . H51A H 0.1816 0.5089 0.5453 0.053 Uiso 1 1 calc R . . H51B H 0.1326 0.4474 0.5623 0.053 Uiso 1 1 calc R . . H51C H 0.1383 0.5411 0.6153 0.053 Uiso 1 1 calc R . . C52 C 0.38311(12) 1.2310(2) 0.1321(2) 0.0240(7) Uani 1 1 d . . . C61 C 0.41633(14) 0.4807(2) 0.3374(2) 0.0370(9) Uani 1 1 d . . . H61 H 0.3973 0.5116 0.2875 0.044 Uiso 1 1 calc R . . C62 C 0.40785(14) 0.3919(2) 0.3499(3) 0.0395(9) Uani 1 1 d . . . H62 H 0.3823 0.3627 0.3098 0.047 Uiso 1 1 calc R . . C63 C 0.43580(13) 0.3444(2) 0.4196(2) 0.0334(8) Uani 1 1 d . . . H63 H 0.4293 0.2830 0.4266 0.040 Uiso 1 1 calc R . . C64 C 0.47298(12) 0.3847(2) 0.4794(2) 0.0281(8) Uani 1 1 d . . . C65 C 0.48160(12) 0.4781(2) 0.4689(2) 0.0268(8) Uani 1 1 d . . . C66 C 0.45271(13) 0.5263(2) 0.3972(2) 0.0306(8) Uani 1 1 d . . . C67 C 0.46123(14) 0.6194(2) 0.3891(2) 0.0333(8) Uani 1 1 d . . . H67 H 0.4416 0.6525 0.3419 0.040 Uiso 1 1 calc R . . C68 C 0.50312(13) 0.3395(2) 0.5525(2) 0.0321(8) Uani 1 1 d . . . H68 H 0.4979 0.2778 0.5604 0.038 Uiso 1 1 calc R . . C71 C 0.06265(16) 0.4043(3) 0.1615(3) 0.0456(10) Uani 1 1 d . . . H71 H 0.0664 0.3499 0.1955 0.055 Uiso 1 1 calc R . . C72 C 0.09569(15) 0.4746(3) 0.1863(3) 0.0477(10) Uani 1 1 d . . . H72 H 0.1216 0.4676 0.2369 0.057 Uiso 1 1 calc R . . C73 C 0.09136(15) 0.5535(2) 0.1387(3) 0.0411(9) Uani 1 1 d . . . H73 H 0.1146 0.6003 0.1559 0.049 Uiso 1 1 calc R . . C74 C 0.05300(14) 0.5662(2) 0.0646(3) 0.0355(9) Uani 1 1 d . . . C75 C 0.01939(13) 0.4951(2) 0.0375(2) 0.0324(8) Uani 1 1 d . . . C76 C 0.02435(14) 0.4126(2) 0.0879(3) 0.0348(9) Uani 1 1 d . . . C77 C 0.04671(15) 0.6477(2) 0.0113(3) 0.0368(9) Uani 1 1 d . . . H77 H 0.0691 0.6959 0.0270 0.044 Uiso 1 1 calc R . . C78 C 0.00999(14) 0.6569(2) -0.0600(3) 0.0359(9) Uani 1 1 d . . . H78 H 0.0069 0.7120 -0.0927 0.043 Uiso 1 1 calc R . . C81 C 0.28580(18) 0.5210(3) 0.2512(3) 0.0623(12) Uani 1 1 d . . . H81 H 0.3076 0.5103 0.3117 0.075 Uiso 1 1 calc R . . 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 Cl1 0.0713(8) 0.0423(6) 0.0712(8) -0.0169(5) -0.0007(6) -0.0061(5) Cl2 0.0460(6) 0.0461(6) 0.0675(7) 0.0209(5) -0.0003(5) 0.0031(5) Cl3 0.0361(6) 0.0544(6) 0.0631(7) -0.0035(5) 0.0000(5) 0.0016(5) O1 0.0432(15) 0.0260(13) 0.0450(15) -0.0080(11) 0.0050(12) 0.0110(11) O2 0.0412(15) 0.0200(12) 0.0397(14) 0.0079(10) 0.0014(12) -0.0068(11) O3 0.0338(14) 0.0290(14) 0.0541(16) -0.0149(11) 0.0003(13) 0.0040(11) O4 0.0395(14) 0.0183(12) 0.0363(13) 0.0064(10) -0.0016(12) -0.0060(10) C1 0.0249(18) 0.0200(16) 0.0223(17) -0.0002(13) 0.0014(14) -0.0002(14) C2 0.0195(17) 0.0255(17) 0.0232(17) 0.0003(13) 0.0047(14) -0.0007(14) C3 0.0206(18) 0.0232(17) 0.0228(17) 0.0026(13) -0.0001(14) -0.0017(13) C4 0.0246(18) 0.0188(16) 0.0268(17) 0.0014(13) 0.0013(15) -0.0029(14) C5 0.0241(18) 0.0182(16) 0.0288(18) 0.0032(13) 0.0036(15) 0.0033(13) C6 0.0225(18) 0.0197(16) 0.0247(17) -0.0012(13) 0.0006(14) -0.0013(13) C7 0.0215(17) 0.0252(17) 0.0250(17) 0.0016(13) 0.0047(14) -0.0017(14) C8 0.0250(18) 0.0212(17) 0.0227(17) 0.0038(13) 0.0052(15) -0.0006(14) C9 0.0291(19) 0.0159(16) 0.0239(17) 0.0014(13) 0.0019(15) -0.0018(14) C10 0.0245(18) 0.0168(16) 0.0254(17) 0.0011(13) 0.0005(15) 0.0035(13) C11 0.0199(17) 0.0186(16) 0.0224(17) -0.0026(12) 0.0012(14) -0.0019(13) C12 0.0236(18) 0.0181(16) 0.0215(16) 0.0006(12) -0.0009(14) -0.0017(13) C13 0.0239(18) 0.0207(16) 0.0177(16) -0.0020(12) 0.0011(14) -0.0015(13) C14 0.0209(17) 0.0216(16) 0.0218(17) 0.0018(12) 0.0000(14) -0.0008(13) C15 0.0218(17) 0.0208(17) 0.0203(16) 0.0015(12) 0.0017(14) -0.0015(13) C16 0.0217(17) 0.0174(16) 0.0226(16) -0.0003(12) -0.0017(14) -0.0008(13) C17 0.0215(18) 0.0220(17) 0.0259(17) 0.0031(13) 0.0073(15) -0.0009(14) C18 0.0242(18) 0.0250(18) 0.0275(18) 0.0004(14) 0.0027(15) -0.0056(14) C19 0.030(2) 0.0227(17) 0.0313(19) -0.0060(14) 0.0025(16) -0.0039(15) C20 0.032(2) 0.0184(17) 0.037(2) -0.0015(14) 0.0134(17) 0.0001(15) C21 0.0252(18) 0.0296(18) 0.0254(18) 0.0011(14) 0.0043(15) 0.0029(15) C22 0.0232(18) 0.0235(17) 0.0234(17) 0.0004(13) 0.0053(15) -0.0018(14) C23 0.031(2) 0.033(2) 0.035(2) -0.0083(15) -0.0030(17) 0.0054(16) C24 0.035(2) 0.036(2) 0.035(2) -0.0045(16) -0.0069(17) -0.0032(16) C25 0.057(3) 0.037(2) 0.046(2) -0.0054(17) 0.003(2) 0.021(2) C26 0.0192(17) 0.0195(16) 0.0269(18) 0.0008(13) 0.0050(15) 0.0002(13) C27 0.0222(18) 0.0214(17) 0.0269(18) 0.0018(13) 0.0058(15) 0.0002(14) C28 0.0281(19) 0.0239(18) 0.0265(18) 0.0041(13) 0.0068(15) 0.0032(14) C29 0.0278(19) 0.0196(17) 0.0313(19) 0.0021(14) 0.0081(16) -0.0003(14) C30 0.0262(19) 0.0270(18) 0.0297(19) -0.0017(14) 0.0008(16) -0.0071(15) C31 0.032(2) 0.0320(19) 0.0301(19) 0.0040(15) -0.0063(16) -0.0093(16) C32 0.036(2) 0.0284(19) 0.0318(19) 0.0042(15) -0.0025(17) -0.0032(16) C33 0.054(2) 0.0175(17) 0.039(2) 0.0102(15) 0.0001(19) 0.0006(16) C34 0.0239(18) 0.0201(16) 0.0285(18) 0.0033(13) 0.0099(15) 0.0004(14) C35 0.0263(19) 0.0270(18) 0.0247(18) -0.0001(14) 0.0061(15) -0.0010(14) C36 0.0235(18) 0.0305(19) 0.0306(19) 0.0020(15) 0.0026(16) 0.0038(15) C37 0.030(2) 0.0226(18) 0.037(2) -0.0043(15) 0.0087(17) -0.0016(15) C38 0.033(2) 0.0249(19) 0.036(2) -0.0082(15) 0.0032(17) -0.0064(16) C39 0.0247(19) 0.0263(18) 0.0320(19) -0.0009(14) 0.0071(16) -0.0074(15) C40 0.034(2) 0.031(2) 0.044(2) -0.0052(16) -0.0034(18) -0.0032(16) C41 0.040(2) 0.042(2) 0.0297(19) -0.0048(16) 0.0021(18) 0.0130(18) C42 0.041(2) 0.040(2) 0.066(3) -0.018(2) -0.004(2) 0.0107(19) C43 0.0201(17) 0.0178(16) 0.0266(17) 0.0032(13) 0.0077(14) -0.0003(13) C44 0.0239(18) 0.0226(17) 0.0235(17) 0.0025(13) 0.0041(15) -0.0001(14) C45 0.0229(18) 0.0239(17) 0.0302(18) -0.0037(14) 0.0012(15) -0.0052(14) C46 0.0237(18) 0.0182(16) 0.0324(18) 0.0031(14) 0.0072(16) -0.0008(14) C47 0.0274(19) 0.0273(18) 0.0212(17) 0.0051(13) 0.0025(15) 0.0007(14) C48 0.0249(18) 0.0203(17) 0.0278(18) 0.0002(13) 0.0040(15) -0.0009(14) C49 0.038(2) 0.0261(18) 0.034(2) 0.0030(15) -0.0010(17) -0.0055(16) C50 0.038(2) 0.0320(19) 0.0285(19) 0.0032(15) -0.0005(17) -0.0080(16) C51 0.046(2) 0.0200(18) 0.039(2) 0.0066(15) -0.0007(18) -0.0004(16) C52 0.0245(18) 0.0229(17) 0.0252(17) 0.0015(13) 0.0051(15) 0.0000(14) C61 0.034(2) 0.044(2) 0.033(2) -0.0019(17) 0.0001(17) 0.0028(18) C62 0.032(2) 0.050(2) 0.036(2) -0.0049(18) 0.0019(18) -0.0048(18) C63 0.030(2) 0.037(2) 0.034(2) -0.0017(16) 0.0082(17) -0.0014(16) C64 0.0236(19) 0.034(2) 0.0273(18) -0.0017(15) 0.0092(16) 0.0042(15) C65 0.0220(18) 0.0314(19) 0.0277(19) 0.0010(14) 0.0078(15) 0.0037(15) C66 0.028(2) 0.036(2) 0.0281(19) 0.0000(15) 0.0056(16) 0.0056(16) C67 0.034(2) 0.032(2) 0.034(2) 0.0055(16) 0.0080(17) 0.0060(16) C68 0.035(2) 0.0254(18) 0.037(2) 0.0046(15) 0.0143(18) 0.0045(16) C71 0.048(3) 0.047(2) 0.043(2) 0.0043(18) 0.013(2) 0.004(2) C72 0.043(2) 0.059(3) 0.042(2) -0.002(2) 0.001(2) -0.002(2) C73 0.034(2) 0.044(2) 0.046(2) -0.0091(18) 0.0098(19) -0.0028(18) C74 0.034(2) 0.033(2) 0.041(2) -0.0056(16) 0.0157(18) -0.0012(16) C75 0.031(2) 0.035(2) 0.033(2) -0.0072(16) 0.0152(16) -0.0013(16) C76 0.035(2) 0.037(2) 0.034(2) -0.0008(16) 0.0108(18) 0.0025(17) C77 0.039(2) 0.029(2) 0.044(2) -0.0089(16) 0.0194(19) -0.0012(17) C78 0.040(2) 0.029(2) 0.041(2) -0.0002(16) 0.0169(19) -0.0033(17) C81 0.068(3) 0.043(3) 0.078(3) 0.001(2) 0.017(3) 0.004(2) _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 Cl1 C81 1.728(4) . ? Cl2 C81 1.770(4) . ? Cl3 C81 1.745(4) . ? O1 C20 1.379(4) . ? O1 C25 1.429(4) . ? O2 C29 1.371(3) . ? O2 C33 1.420(4) . ? O3 C37 1.379(4) . ? O3 C42 1.418(4) . ? O4 C46 1.360(3) . ? O4 C51 1.424(4) . ? C1 C11 1.398(4) . ? C1 C2 1.402(4) . ? C1 C17 1.496(4) . ? C2 C3 1.398(4) . ? C2 H2 0.9500 . ? C3 C12 1.402(4) . ? C3 C26 1.491(4) . ? C4 C5 1.343(4) . ? C4 C12 1.445(4) . ? C4 H4 0.9500 . ? C5 C13 1.439(4) . ? C5 H5 0.9500 . ? C6 C7 1.397(4) . ? C6 C13 1.404(4) . ? C6 C34 1.499(4) . ? C7 C8 1.395(4) . ? C7 H7 0.9500 . ? C8 C14 1.405(4) . ? C8 C43 1.498(4) . ? C9 C10 1.342(4) . ? C9 C14 1.431(4) . ? C9 H9 0.9500 . ? C10 C11 1.437(4) . ? C10 H10 0.9500 . ? C11 C16 1.430(4) . ? C12 C16 1.419(4) . ? C13 C15 1.430(4) . ? C14 C15 1.426(4) . ? C15 C16 1.428(4) . ? C17 C22 1.394(4) . ? C17 C18 1.418(4) . ? C18 C19 1.375(4) . ? C18 C24 1.501(4) . ? C19 C20 1.379(5) . ? C19 H19 0.9500 . ? C20 C21 1.377(4) . ? C21 C22 1.402(4) . ? C21 H21 0.9500 . ? C22 C23 1.509(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.397(4) . ? C26 C52 1.406(4) . ? C27 C28 1.400(4) . ? C27 C32 1.500(4) . ? C28 C29 1.390(4) . ? C28 H28 0.9500 . ? C29 C30 1.379(4) . ? C30 C52 1.393(4) . ? C30 H30 0.9500 . ? C31 C52 1.502(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.390(4) . ? C34 C39 1.416(4) . ? C35 C36 1.402(4) . ? C35 C41 1.497(4) . ? C36 C37 1.380(4) . ? C36 H36 0.9500 . ? C37 C38 1.383(5) . ? C38 C39 1.375(4) . ? C38 H38 0.9500 . ? C39 C40 1.498(5) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C48 1.395(4) . ? C43 C44 1.412(4) . ? C44 C45 1.383(4) . ? C44 C50 1.510(4) . ? C45 C46 1.395(4) . ? C45 H45 0.9500 . ? C46 C47 1.387(4) . ? C47 C48 1.399(4) . ? C47 H47 0.9500 . ? C48 C49 1.505(4) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C61 C62 1.372(5) . ? C61 C66 1.403(5) . ? C61 H61 0.9500 . ? C62 C63 1.379(5) . ? C62 H62 0.9500 . ? C63 C64 1.377(5) . ? C63 H63 0.9500 . ? C64 C68 1.421(4) . ? C64 C65 1.438(4) . ? C65 C65 1.414(6) 3_666 ? C65 C66 1.415(4) . ? C66 C67 1.429(5) . ? C67 C68 1.347(5) 3_666 ? C67 H67 0.9500 . ? C68 C67 1.347(5) 3_666 ? C68 H68 0.9500 . ? C71 C76 1.390(5) . ? C71 C72 1.395(5) . ? C71 H71 0.9500 . ? C72 C73 1.365(5) . ? C72 H72 0.9500 . ? C73 C74 1.403(5) . ? C73 H73 0.9500 . ? C74 C75 1.419(5) . ? C74 C77 1.443(5) . ? C75 C75 1.415(7) 3_565 ? C75 C76 1.433(5) . ? C76 C78 1.416(5) 3_565 ? C77 C78 1.341(5) . ? C77 H77 0.9500 . ? C78 C76 1.416(5) 3_565 ? C78 H78 0.9500 . ? C81 H81 1.0000 . ? 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 C20 O1 C25 117.6(3) . . ? C29 O2 C33 117.1(2) . . ? C37 O3 C42 117.1(3) . . ? C46 O4 C51 117.5(2) . . ? C11 C1 C2 119.0(3) . . ? C11 C1 C17 119.5(3) . . ? C2 C1 C17 121.5(3) . . ? C3 C2 C1 122.3(3) . . ? C3 C2 H2 118.9 . . ? C1 C2 H2 118.9 . . ? C2 C3 C12 119.0(3) . . ? C2 C3 C26 120.1(3) . . ? C12 C3 C26 120.9(3) . . ? C5 C4 C12 121.9(3) . . ? C5 C4 H4 119.0 . . ? C12 C4 H4 119.0 . . ? C4 C5 C13 121.6(3) . . ? C4 C5 H5 119.2 . . ? C13 C5 H5 119.2 . . ? C7 C6 C13 119.0(3) . . ? C7 C6 C34 119.8(3) . . ? C13 C6 C34 121.1(3) . . ? C8 C7 C6 122.6(3) . . ? C8 C7 H7 118.7 . . ? C6 C7 H7 118.7 . . ? C7 C8 C14 119.4(3) . . ? C7 C8 C43 120.6(3) . . ? C14 C8 C43 120.0(3) . . ? C10 C9 C14 121.8(3) . . ? C10 C9 H9 119.1 . . ? C14 C9 H9 119.1 . . ? C9 C10 C11 122.0(3) . . ? C9 C10 H10 119.0 . . ? C11 C10 H10 119.0 . . ? C1 C11 C16 120.0(3) . . ? C1 C11 C10 122.2(3) . . ? C16 C11 C10 117.8(3) . . ? C3 C12 C16 120.2(3) . . ? C3 C12 C4 121.8(3) . . ? C16 C12 C4 117.9(3) . . ? C6 C13 C15 119.6(3) . . ? C6 C13 C5 122.3(3) . . ? C15 C13 C5 118.1(3) . . ? C8 C14 C15 119.3(3) . . ? C8 C14 C9 122.4(3) . . ? C15 C14 C9 118.3(3) . . ? C14 C15 C16 119.9(3) . . ? C14 C15 C13 120.1(3) . . ? C16 C15 C13 120.0(3) . . ? C12 C16 C15 120.4(3) . . ? C12 C16 C11 119.4(3) . . ? C15 C16 C11 120.2(3) . . ? C22 C17 C18 119.3(3) . . ? C22 C17 C1 122.2(3) . . ? C18 C17 C1 118.3(3) . . ? C19 C18 C17 119.4(3) . . ? C19 C18 C24 120.8(3) . . ? C17 C18 C24 119.8(3) . . ? C18 C19 C20 121.3(3) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C21 C20 C19 119.9(3) . . ? C21 C20 O1 124.2(3) . . ? C19 C20 O1 115.9(3) . . ? C20 C21 C22 120.5(3) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C17 C22 C21 119.6(3) . . ? C17 C22 C23 121.4(3) . . ? C21 C22 C23 119.0(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C25 H25A 109.5 . . ? O1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C52 119.7(3) . . ? C27 C26 C3 120.3(3) . . ? C52 C26 C3 119.9(3) . . ? C26 C27 C28 119.9(3) . . ? C26 C27 C32 120.8(3) . . ? C28 C27 C32 119.2(3) . . ? C29 C28 C27 119.8(3) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? O2 C29 C30 115.3(3) . . ? O2 C29 C28 124.3(3) . . ? C30 C29 C28 120.5(3) . . ? C29 C30 C52 120.6(3) . . ? C29 C30 H30 119.7 . . ? C52 C30 H30 119.7 . . ? C52 C31 H31A 109.5 . . ? C52 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C52 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O2 C33 H33A 109.5 . . ? O2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C39 120.0(3) . . ? C35 C34 C6 121.7(3) . . ? C39 C34 C6 118.2(3) . . ? C34 C35 C36 119.4(3) . . ? C34 C35 C41 121.7(3) . . ? C36 C35 C41 118.9(3) . . ? C37 C36 C35 120.3(3) . . ? C37 C36 H36 119.9 . . ? C35 C36 H36 119.9 . . ? O3 C37 C36 124.6(3) . . ? O3 C37 C38 115.4(3) . . ? C36 C37 C38 120.1(3) . . ? C39 C38 C37 121.1(3) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C38 C39 C34 119.1(3) . . ? C38 C39 C40 120.1(3) . . ? C34 C39 C40 120.8(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C35 C41 H41A 109.5 . . ? C35 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C35 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O3 C42 H42A 109.5 . . ? O3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? O3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 119.4(3) . . ? C48 C43 C8 120.4(3) . . ? C44 C43 C8 120.2(3) . . ? C45 C44 C43 119.8(3) . . ? C45 C44 C50 120.2(3) . . ? C43 C44 C50 120.0(3) . . ? C44 C45 C46 120.8(3) . . ? C44 C45 H45 119.6 . . ? C46 C45 H45 119.6 . . ? O4 C46 C47 124.9(3) . . ? O4 C46 C45 115.5(3) . . ? C47 C46 C45 119.6(3) . . ? C46 C47 C48 120.4(3) . . ? C46 C47 H47 119.8 . . ? C48 C47 H47 119.8 . . ? C43 C48 C47 120.0(3) . . ? C43 C48 C49 120.4(3) . . ? C47 C48 C49 119.5(3) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C44 C50 H50A 109.5 . . ? C44 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C44 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O4 C51 H51A 109.5 . . ? O4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? O4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C30 C52 C26 119.5(3) . . ? C30 C52 C31 120.3(3) . . ? C26 C52 C31 120.2(3) . . ? C62 C61 C66 120.8(3) . . ? C62 C61 H61 119.6 . . ? C66 C61 H61 119.6 . . ? C61 C62 C63 121.2(3) . . ? C61 C62 H62 119.4 . . ? C63 C62 H62 119.4 . . ? C64 C63 C62 121.0(3) . . ? C64 C63 H63 119.5 . . ? C62 C63 H63 119.5 . . ? C63 C64 C68 123.7(3) . . ? C63 C64 C65 118.7(3) . . ? C68 C64 C65 117.6(3) . . ? C65 C65 C66 120.0(4) 3_666 . ? C65 C65 C64 120.1(4) 3_666 . ? C66 C65 C64 119.9(3) . . ? C61 C66 C65 118.4(3) . . ? C61 C66 C67 122.6(3) . . ? C65 C66 C67 119.1(3) . . ? C68 C67 C66 120.6(3) 3_666 . ? C68 C67 H67 119.7 3_666 . ? C66 C67 H67 119.7 . . ? C67 C68 C64 122.7(3) 3_666 . ? C67 C68 H68 118.7 3_666 . ? C64 C68 H68 118.7 . . ? C76 C71 C72 120.9(4) . . ? C76 C71 H71 119.6 . . ? C72 C71 H71 119.6 . . ? C73 C72 C71 120.9(4) . . ? C73 C72 H72 119.5 . . ? C71 C72 H72 119.5 . . ? C72 C73 C74 120.7(4) . . ? C72 C73 H73 119.7 . . ? C74 C73 H73 119.7 . . ? C73 C74 C75 119.3(3) . . ? C73 C74 C77 123.3(3) . . ? C75 C74 C77 117.4(3) . . ? C75 C75 C74 121.0(4) 3_565 . ? C75 C75 C76 119.5(4) 3_565 . ? C74 C75 C76 119.5(3) . . ? C71 C76 C78 123.0(3) . 3_565 ? C71 C76 C75 118.7(3) . . ? C78 C76 C75 118.3(3) 3_565 . ? C78 C77 C74 121.6(3) . . ? C78 C77 H77 119.2 . . ? C74 C77 H77 119.2 . . ? C77 C78 C76 122.2(3) . 3_565 ? C77 C78 H78 118.9 . . ? C76 C78 H78 118.9 3_565 . ? Cl1 C81 Cl3 113.1(3) . . ? Cl1 C81 Cl2 110.2(2) . . ? Cl3 C81 Cl2 111.6(2) . . ? Cl1 C81 H81 107.2 . . ? Cl3 C81 H81 107.2 . . ? Cl2 C81 H81 107.2 . . ? 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 C11 C1 C2 C3 -0.7(5) . . . . ? C17 C1 C2 C3 177.7(3) . . . . ? C1 C2 C3 C12 0.7(4) . . . . ? C1 C2 C3 C26 -180.0(3) . . . . ? C12 C4 C5 C13 -0.6(5) . . . . ? C13 C6 C7 C8 1.6(5) . . . . ? C34 C6 C7 C8 -175.4(3) . . . . ? C6 C7 C8 C14 0.1(5) . . . . ? C6 C7 C8 C43 177.8(3) . . . . ? C14 C9 C10 C11 0.0(5) . . . . ? C2 C1 C11 C16 0.6(4) . . . . ? C17 C1 C11 C16 -177.8(3) . . . . ? C2 C1 C11 C10 178.8(3) . . . . ? C17 C1 C11 C10 0.5(4) . . . . ? C9 C10 C11 C1 -178.5(3) . . . . ? C9 C10 C11 C16 -0.1(4) . . . . ? C2 C3 C12 C16 -0.6(4) . . . . ? C26 C3 C12 C16 -179.9(3) . . . . ? C2 C3 C12 C4 178.5(3) . . . . ? C26 C3 C12 C4 -0.8(4) . . . . ? C5 C4 C12 C3 179.8(3) . . . . ? C5 C4 C12 C16 -1.0(4) . . . . ? C7 C6 C13 C15 -2.1(4) . . . . ? C34 C6 C13 C15 174.9(3) . . . . ? C7 C6 C13 C5 179.2(3) . . . . ? C34 C6 C13 C5 -3.8(4) . . . . ? C4 C5 C13 C6 179.8(3) . . . . ? C4 C5 C13 C15 1.1(4) . . . . ? C7 C8 C14 C15 -1.2(4) . . . . ? C43 C8 C14 C15 -179.0(3) . . . . ? C7 C8 C14 C9 178.8(3) . . . . ? C43 C8 C14 C9 1.0(4) . . . . ? C10 C9 C14 C8 179.8(3) . . . . ? C10 C9 C14 C15 -0.2(4) . . . . ? C8 C14 C15 C16 -179.6(3) . . . . ? C9 C14 C15 C16 0.4(4) . . . . ? C8 C14 C15 C13 0.8(4) . . . . ? C9 C14 C15 C13 -179.2(3) . . . . ? C6 C13 C15 C14 0.9(4) . . . . ? C5 C13 C15 C14 179.7(3) . . . . ? C6 C13 C15 C16 -178.7(3) . . . . ? C5 C13 C15 C16 0.0(4) . . . . ? C3 C12 C16 C15 -178.7(3) . . . . ? C4 C12 C16 C15 2.1(4) . . . . ? C3 C12 C16 C11 0.5(4) . . . . ? C4 C12 C16 C11 -178.6(3) . . . . ? C14 C15 C16 C12 178.7(3) . . . . ? C13 C15 C16 C12 -1.6(4) . . . . ? C14 C15 C16 C11 -0.6(4) . . . . ? C13 C15 C16 C11 179.1(3) . . . . ? C1 C11 C16 C12 -0.5(4) . . . . ? C10 C11 C16 C12 -178.9(3) . . . . ? C1 C11 C16 C15 178.8(3) . . . . ? C10 C11 C16 C15 0.4(4) . . . . ? C11 C1 C17 C22 -90.3(4) . . . . ? C2 C1 C17 C22 91.4(4) . . . . ? C11 C1 C17 C18 84.8(4) . . . . ? C2 C1 C17 C18 -93.5(4) . . . . ? C22 C17 C18 C19 1.9(4) . . . . ? C1 C17 C18 C19 -173.3(3) . . . . ? C22 C17 C18 C24 -176.7(3) . . . . ? C1 C17 C18 C24 8.1(4) . . . . ? C17 C18 C19 C20 0.0(5) . . . . ? C24 C18 C19 C20 178.5(3) . . . . ? C18 C19 C20 C21 -1.3(5) . . . . ? C18 C19 C20 O1 179.9(3) . . . . ? C25 O1 C20 C21 7.8(4) . . . . ? C25 O1 C20 C19 -173.4(3) . . . . ? C19 C20 C21 C22 0.7(5) . . . . ? O1 C20 C21 C22 179.4(3) . . . . ? C18 C17 C22 C21 -2.5(4) . . . . ? C1 C17 C22 C21 172.5(3) . . . . ? C18 C17 C22 C23 176.7(3) . . . . ? C1 C17 C22 C23 -8.2(4) . . . . ? C20 C21 C22 C17 1.2(4) . . . . ? C20 C21 C22 C23 -178.1(3) . . . . ? C2 C3 C26 C27 101.5(3) . . . . ? C12 C3 C26 C27 -79.2(4) . . . . ? C2 C3 C26 C52 -78.9(4) . . . . ? C12 C3 C26 C52 100.4(4) . . . . ? C52 C26 C27 C28 -0.7(4) . . . . ? C3 C26 C27 C28 178.9(3) . . . . ? C52 C26 C27 C32 179.3(3) . . . . ? C3 C26 C27 C32 -1.1(4) . . . . ? C26 C27 C28 C29 -0.5(4) . . . . ? C32 C27 C28 C29 179.5(3) . . . . ? C33 O2 C29 C30 -171.4(3) . . . . ? C33 O2 C29 C28 9.1(4) . . . . ? C27 C28 C29 O2 -178.9(3) . . . . ? C27 C28 C29 C30 1.6(5) . . . . ? O2 C29 C30 C52 178.9(3) . . . . ? C28 C29 C30 C52 -1.5(5) . . . . ? C7 C6 C34 C35 -88.2(4) . . . . ? C13 C6 C34 C35 94.8(4) . . . . ? C7 C6 C34 C39 92.6(4) . . . . ? C13 C6 C34 C39 -84.4(4) . . . . ? C39 C34 C35 C36 1.7(4) . . . . ? C6 C34 C35 C36 -177.5(3) . . . . ? C39 C34 C35 C41 -177.2(3) . . . . ? C6 C34 C35 C41 3.6(5) . . . . ? C34 C35 C36 C37 -1.6(5) . . . . ? C41 C35 C36 C37 177.4(3) . . . . ? C42 O3 C37 C36 -1.6(5) . . . . ? C42 O3 C37 C38 179.4(3) . . . . ? C35 C36 C37 O3 -178.0(3) . . . . ? C35 C36 C37 C38 1.0(5) . . . . ? O3 C37 C38 C39 178.5(3) . . . . ? C36 C37 C38 C39 -0.5(5) . . . . ? C37 C38 C39 C34 0.7(5) . . . . ? C37 C38 C39 C40 -177.3(3) . . . . ? C35 C34 C39 C38 -1.3(4) . . . . ? C6 C34 C39 C38 177.9(3) . . . . ? C35 C34 C39 C40 176.7(3) . . . . ? C6 C34 C39 C40 -4.1(4) . . . . ? C7 C8 C43 C48 -95.2(4) . . . . ? C14 C8 C43 C48 82.6(4) . . . . ? C7 C8 C43 C44 86.7(4) . . . . ? C14 C8 C43 C44 -95.5(4) . . . . ? C48 C43 C44 C45 -0.2(4) . . . . ? C8 C43 C44 C45 177.9(3) . . . . ? C48 C43 C44 C50 179.0(3) . . . . ? C8 C43 C44 C50 -2.8(4) . . . . ? C43 C44 C45 C46 -0.9(4) . . . . ? C50 C44 C45 C46 179.9(3) . . . . ? C51 O4 C46 C47 -6.0(4) . . . . ? C51 O4 C46 C45 173.9(3) . . . . ? C44 C45 C46 O4 -178.5(3) . . . . ? C44 C45 C46 C47 1.5(4) . . . . ? O4 C46 C47 C48 179.1(3) . . . . ? C45 C46 C47 C48 -0.9(4) . . . . ? C44 C43 C48 C47 0.7(4) . . . . ? C8 C43 C48 C47 -177.4(3) . . . . ? C44 C43 C48 C49 -179.5(3) . . . . ? C8 C43 C48 C49 2.4(4) . . . . ? C46 C47 C48 C43 -0.2(5) . . . . ? C46 C47 C48 C49 180.0(3) . . . . ? C29 C30 C52 C26 0.3(5) . . . . ? C29 C30 C52 C31 -178.9(3) . . . . ? C27 C26 C52 C30 0.8(4) . . . . ? C3 C26 C52 C30 -178.9(3) . . . . ? C27 C26 C52 C31 -180.0(3) . . . . ? C3 C26 C52 C31 0.4(4) . . . . ? C66 C61 C62 C63 -1.9(5) . . . . ? C61 C62 C63 C64 0.4(5) . . . . ? C62 C63 C64 C68 -179.9(3) . . . . ? C62 C63 C64 C65 1.1(5) . . . . ? C63 C64 C65 C65 178.1(3) . . . 3_666 ? C68 C64 C65 C65 -0.9(5) . . . 3_666 ? C63 C64 C65 C66 -1.0(4) . . . . ? C68 C64 C65 C66 179.9(3) . . . . ? C62 C61 C66 C65 1.9(5) . . . . ? C62 C61 C66 C67 -177.5(3) . . . . ? C65 C65 C66 C61 -179.6(4) 3_666 . . . ? C64 C65 C66 C61 -0.5(4) . . . . ? C65 C65 C66 C67 -0.2(5) 3_666 . . . ? C64 C65 C66 C67 179.0(3) . . . . ? C61 C66 C67 C68 -179.4(3) . . . 3_666 ? C65 C66 C67 C68 1.2(5) . . . 3_666 ? C63 C64 C68 C67 -179.1(3) . . . 3_666 ? C65 C64 C68 C67 0.0(4) . . . 3_666 ? C76 C71 C72 C73 -0.1(6) . . . . ? C71 C72 C73 C74 1.0(6) . . . . ? C72 C73 C74 C75 -1.7(5) . . . . ? C72 C73 C74 C77 -179.5(3) . . . . ? C73 C74 C75 C75 -179.2(4) . . . 3_565 ? C77 C74 C75 C75 -1.3(5) . . . 3_565 ? C73 C74 C75 C76 1.6(5) . . . . ? C77 C74 C75 C76 179.6(3) . . . . ? C72 C71 C76 C78 179.8(3) . . . 3_565 ? C72 C71 C76 C75 0.1(5) . . . . ? C75 C75 C76 C71 -180.0(4) 3_565 . . . ? C74 C75 C76 C71 -0.8(5) . . . . ? C75 C75 C76 C78 0.3(5) 3_565 . . 3_565 ? C74 C75 C76 C78 179.5(3) . . . 3_565 ? C73 C74 C77 C78 179.1(3) . . . . ? C75 C74 C77 C78 1.3(5) . . . . ? C74 C77 C78 C76 -0.8(5) . . . 3_565 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.243 _refine_diff_density_min -0.172 _refine_diff_density_rms 0.085 #END data_TP-MC _database_code_depnum_ccdc_archive 'CCDC 726027' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra(2,6-dimethyl-4-methoxyphenyl)pyrene ; _chemical_name_common tetra(2,6-dimethyl-4-methoxyphenyl)pyrene _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 O4, C9 H12, C H Cl3' _chemical_formula_sum 'C62 H63 Cl3 O4' _chemical_formula_weight 978.47 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.594(4) _cell_length_b 15.769(4) _cell_length_c 24.726(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.662(5) _cell_angle_gamma 90.00 _cell_volume 5225(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3447 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 22.63 _exptl_crystal_description needles _exptl_crystal_colour 'color less' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_absorpt_coefficient_mu 0.223 _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 100(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 'Bruker SMART APEX' _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 28710 _diffrn_reflns_av_R_equivalents 0.0745 _diffrn_reflns_av_sigmaI/netI 0.0862 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10216 _reflns_number_gt 6561 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0625P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10216 _refine_ls_number_parameters 637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0987 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1515 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Cl1 Cl -0.09499(6) 0.70769(6) 0.10292(4) 0.0626(3) Uani 1 1 d . . . Cl2 Cl 0.00586(7) 0.54613(5) 0.11527(4) 0.0613(3) Uani 1 1 d . . . Cl3 Cl 0.05529(6) 0.67594(6) 0.19739(3) 0.0561(2) Uani 1 1 d . . . O1 O 0.74706(13) 0.29031(10) 0.06811(7) 0.0299(4) Uani 1 1 d . . . O2 O 0.72968(12) 1.06705(11) 0.11219(7) 0.0296(4) Uani 1 1 d . . . O3 O 0.26980(13) 1.00777(11) 0.44171(7) 0.0339(4) Uani 1 1 d . . . O4 O 0.27055(12) 0.22643(10) 0.39582(7) 0.0281(4) Uani 1 1 d . . . C1 C 0.61513(17) 0.58614(15) 0.16385(9) 0.0220(5) Uani 1 1 d . . . C2 C 0.64439(17) 0.66651(15) 0.14995(9) 0.0238(5) Uani 1 1 d . . . H2 H 0.6853 0.6714 0.1225 0.029 Uiso 1 1 calc R . . C3 C 0.61649(17) 0.74035(15) 0.17438(9) 0.0212(5) Uani 1 1 d . . . C4 C 0.55802(17) 0.73272(15) 0.21658(9) 0.0209(5) Uani 1 1 d . . . C5 C 0.52989(17) 0.80525(15) 0.24560(9) 0.0226(5) Uani 1 1 d . . . H5 H 0.5500 0.8601 0.2359 0.027 Uiso 1 1 calc R . . C6 C 0.47555(17) 0.79752(15) 0.28635(9) 0.0217(5) Uani 1 1 d . . . H6 H 0.4588 0.8471 0.3047 0.026 Uiso 1 1 calc R . . C7 C 0.44240(17) 0.71646(15) 0.30271(9) 0.0201(5) Uani 1 1 d . . . C8 C 0.38600(17) 0.70669(15) 0.34544(9) 0.0208(5) Uani 1 1 d . . . C9 C 0.35791(17) 0.62613(15) 0.35975(9) 0.0229(5) Uani 1 1 d . . . H9 H 0.3210 0.6206 0.3889 0.028 Uiso 1 1 calc R . . C10 C 0.38173(17) 0.55340(15) 0.33304(9) 0.0219(5) Uani 1 1 d . . . C11 C 0.43713(17) 0.56098(15) 0.28956(9) 0.0209(5) Uani 1 1 d . . . C12 C 0.46430(17) 0.48841(15) 0.26003(9) 0.0225(5) Uani 1 1 d . . . H12 H 0.4433 0.4336 0.2693 0.027 Uiso 1 1 calc R . . C13 C 0.51885(17) 0.49632(15) 0.21961(9) 0.0220(5) Uani 1 1 d . . . H13 H 0.5347 0.4469 0.2008 0.026 Uiso 1 1 calc R . . C14 C 0.55379(17) 0.57724(15) 0.20410(9) 0.0208(5) Uani 1 1 d . . . C15 C 0.52665(16) 0.65137(15) 0.23120(9) 0.0197(5) Uani 1 1 d . . . C16 C 0.46766(16) 0.64250(15) 0.27432(9) 0.0203(5) Uani 1 1 d . . . C17 C 0.64953(17) 0.50912(15) 0.13642(9) 0.0217(5) Uani 1 1 d . . . C18 C 0.58625(17) 0.47061(16) 0.09295(9) 0.0235(5) Uani 1 1 d . . . C19 C 0.61670(18) 0.39648(15) 0.06956(9) 0.0241(6) Uani 1 1 d . . . H19 H 0.5735 0.3696 0.0404 0.029 Uiso 1 1 calc R . . C20 C 0.70986(18) 0.36208(15) 0.08886(9) 0.0237(6) Uani 1 1 d . . . C21 C 0.77344(18) 0.40157(15) 0.13107(9) 0.0243(6) Uani 1 1 d . . . H21 H 0.8376 0.3781 0.1436 0.029 Uiso 1 1 calc R . . C22 C 0.74465(18) 0.47499(15) 0.15525(9) 0.0237(6) Uani 1 1 d . . . C23 C 0.81427(18) 0.51646(16) 0.20169(10) 0.0292(6) Uani 1 1 d . . . H23A H 0.8786 0.4869 0.2074 0.044 Uiso 1 1 calc R . . H23B H 0.7851 0.5134 0.2353 0.044 Uiso 1 1 calc R . . H23C H 0.8243 0.5760 0.1926 0.044 Uiso 1 1 calc R . . C24 C 0.48467(18) 0.50783(17) 0.07213(10) 0.0305(6) Uani 1 1 d . . . H24A H 0.4428 0.5030 0.1006 0.046 Uiso 1 1 calc R . . H24B H 0.4535 0.4769 0.0393 0.046 Uiso 1 1 calc R . . H24C H 0.4918 0.5677 0.0629 0.046 Uiso 1 1 calc R . . C25 C 0.6834(2) 0.24478(17) 0.02632(11) 0.0357(7) Uani 1 1 d . . . H25A H 0.6225 0.2280 0.0398 0.054 Uiso 1 1 calc R . . H25B H 0.7181 0.1940 0.0164 0.054 Uiso 1 1 calc R . . H25C H 0.6659 0.2810 -0.0061 0.054 Uiso 1 1 calc R . . C26 C 0.65022(17) 0.82485(15) 0.15721(9) 0.0218(5) Uani 1 1 d . . . C27 C 0.73947(17) 0.86021(15) 0.18456(9) 0.0233(5) Uani 1 1 d . . . C28 C 0.76875(18) 0.94088(16) 0.16933(10) 0.0258(6) Uani 1 1 d . . . H28 H 0.8300 0.9645 0.1872 0.031 Uiso 1 1 calc R . . C29 C 0.70906(18) 0.98646(15) 0.12847(9) 0.0236(5) Uani 1 1 d . . . C30 C 0.62232(18) 0.95043(15) 0.10023(9) 0.0236(6) Uani 1 1 d . . . H30 H 0.5831 0.9808 0.0712 0.028 Uiso 1 1 calc R . . C31 C 0.59240(17) 0.87012(15) 0.11417(9) 0.0219(5) Uani 1 1 d . . . C32 C 0.49695(18) 0.83345(16) 0.08279(10) 0.0298(6) Uani 1 1 d . . . H32A H 0.4434 0.8397 0.1045 0.045 Uiso 1 1 calc R . . H32B H 0.5068 0.7732 0.0756 0.045 Uiso 1 1 calc R . . H32C H 0.4788 0.8637 0.0479 0.045 Uiso 1 1 calc R . . C33 C 0.80403(19) 0.81303(16) 0.23018(10) 0.0312(6) Uani 1 1 d . . . H33A H 0.7770 0.8199 0.2642 0.047 Uiso 1 1 calc R . . H33B H 0.8721 0.8358 0.2352 0.047 Uiso 1 1 calc R . . H33C H 0.8051 0.7527 0.2208 0.047 Uiso 1 1 calc R . . C34 C 0.8090(2) 1.11102(17) 0.14511(11) 0.0347(7) Uani 1 1 d . . . H34A H 0.7992 1.1099 0.1835 0.052 Uiso 1 1 calc R . . H34B H 0.8101 1.1700 0.1326 0.052 Uiso 1 1 calc R . . H34C H 0.8725 1.0836 0.1419 0.052 Uiso 1 1 calc R . . C35 C 0.35508(17) 0.78367(15) 0.37409(9) 0.0203(5) Uani 1 1 d . . . C36 C 0.41079(17) 0.81223(15) 0.42309(9) 0.0231(5) Uani 1 1 d . . . C37 C 0.38301(18) 0.88652(16) 0.44725(10) 0.0254(6) Uani 1 1 d . . . H37 H 0.4205 0.9058 0.4809 0.031 Uiso 1 1 calc R . . C38 C 0.30070(18) 0.93226(16) 0.42207(10) 0.0255(6) Uani 1 1 d . . . C39 C 0.24373(18) 0.90241(16) 0.37415(9) 0.0256(6) Uani 1 1 d . . . H39 H 0.1867 0.9335 0.3575 0.031 Uiso 1 1 calc R . . C40 C 0.26867(17) 0.82798(15) 0.35016(9) 0.0230(5) Uani 1 1 d . . . C41 C 0.20262(19) 0.79398(16) 0.29956(10) 0.0311(6) Uani 1 1 d . . . H41A H 0.1423 0.8288 0.2913 0.047 Uiso 1 1 calc R . . H41B H 0.1840 0.7353 0.3061 0.047 Uiso 1 1 calc R . . H41C H 0.2387 0.7958 0.2684 0.047 Uiso 1 1 calc R . . C42 C 0.50157(19) 0.76394(17) 0.45023(10) 0.0320(6) Uani 1 1 d . . . H42A H 0.4819 0.7065 0.4592 0.048 Uiso 1 1 calc R . . H42B H 0.5316 0.7932 0.4839 0.048 Uiso 1 1 calc R . . H42C H 0.5502 0.7607 0.4252 0.048 Uiso 1 1 calc R . . C43 C 0.3234(2) 1.03915(18) 0.49198(11) 0.0394(7) Uani 1 1 d . . . H43A H 0.3151 1.0003 0.5218 0.059 Uiso 1 1 calc R . . H43B H 0.2978 1.0953 0.4994 0.059 Uiso 1 1 calc R . . H43C H 0.3944 1.0435 0.4894 0.059 Uiso 1 1 calc R . . C44 C 0.34920(17) 0.46800(15) 0.34989(9) 0.0212(5) Uani 1 1 d . . . C45 C 0.25960(17) 0.43266(15) 0.32299(9) 0.0226(5) Uani 1 1 d . . . C46 C 0.23085(17) 0.35172(15) 0.33784(9) 0.0232(5) Uani 1 1 d . . . H46 H 0.1703 0.3275 0.3195 0.028 Uiso 1 1 calc R . . C47 C 0.29043(18) 0.30691(15) 0.37916(9) 0.0225(5) Uani 1 1 d . . . C48 C 0.37679(18) 0.34392(15) 0.40713(9) 0.0233(5) Uani 1 1 d . . . H48 H 0.4151 0.3144 0.4370 0.028 Uiso 1 1 calc R . . C49 C 0.40844(18) 0.42296(16) 0.39253(9) 0.0247(6) Uani 1 1 d . . . C50 C 0.50538(18) 0.45877(17) 0.42213(10) 0.0320(6) Uani 1 1 d . . . H50A H 0.5291 0.4244 0.4547 0.048 Uiso 1 1 calc R . . H50B H 0.4950 0.5173 0.4332 0.048 Uiso 1 1 calc R . . H50C H 0.5552 0.4579 0.3977 0.048 Uiso 1 1 calc R . . C51 C 0.19491(19) 0.48036(16) 0.27754(10) 0.0313(6) Uani 1 1 d . . . H51A H 0.2276 0.4818 0.2451 0.047 Uiso 1 1 calc R . . H51B H 0.1849 0.5385 0.2896 0.047 Uiso 1 1 calc R . . H51C H 0.1302 0.4519 0.2683 0.047 Uiso 1 1 calc R . . C52 C 0.19307(19) 0.18021(16) 0.36200(11) 0.0320(6) Uani 1 1 d . . . H52A H 0.1286 0.2074 0.3633 0.048 Uiso 1 1 calc R . . H52B H 0.1919 0.1218 0.3754 0.048 Uiso 1 1 calc R . . H52C H 0.2056 0.1798 0.3241 0.048 Uiso 1 1 calc R . . C53 C 0.1732(2) 0.57244(18) 0.45349(11) 0.0341(6) Uani 1 1 d . . . C54 C 0.19017(19) 0.64849(18) 0.48232(10) 0.0332(6) Uani 1 1 d . . . H54 H 0.2368 0.6498 0.5156 0.040 Uiso 1 1 calc R . . C55 C 0.1403(2) 0.72222(18) 0.46340(11) 0.0340(7) Uani 1 1 d . . . C56 C 0.07305(19) 0.71990(18) 0.41449(11) 0.0346(7) Uani 1 1 d . . . H56 H 0.0396 0.7705 0.4010 0.042 Uiso 1 1 calc R . . C57 C 0.0536(2) 0.64505(19) 0.38472(11) 0.0352(7) Uani 1 1 d . . . C58 C 0.1048(2) 0.57220(19) 0.40478(11) 0.0362(7) Uani 1 1 d . . . H58 H 0.0928 0.5208 0.3847 0.043 Uiso 1 1 calc R . . C59 C 0.2275(2) 0.49289(19) 0.47446(11) 0.0443(8) Uani 1 1 d . . . H59A H 0.1971 0.4692 0.5044 0.066 Uiso 1 1 calc R . . H59B H 0.2977 0.5062 0.4880 0.066 Uiso 1 1 calc R . . H59C H 0.2231 0.4514 0.4446 0.066 Uiso 1 1 calc R . . C60 C 0.1581(2) 0.80361(18) 0.49635(11) 0.0414(7) Uani 1 1 d . . . H60A H 0.1107 0.8071 0.5221 0.062 Uiso 1 1 calc R . . H60B H 0.1487 0.8523 0.4714 0.062 Uiso 1 1 calc R . . H60C H 0.2264 0.8039 0.5168 0.062 Uiso 1 1 calc R . . C61 C -0.0219(2) 0.6437(2) 0.33287(12) 0.0495(8) Uani 1 1 d . . . H61A H -0.0033 0.6002 0.3081 0.074 Uiso 1 1 calc R . . H61B H -0.0236 0.6993 0.3150 0.074 Uiso 1 1 calc R . . H61C H -0.0879 0.6307 0.3417 0.074 Uiso 1 1 calc R . . C62 C 0.0173(2) 0.65569(18) 0.12756(10) 0.0366(7) Uani 1 1 d . . . H62 H 0.0696 0.6782 0.1074 0.044 Uiso 1 1 calc R . . 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 Cl1 0.0354(5) 0.0873(7) 0.0642(6) 0.0184(5) 0.0064(4) 0.0064(4) Cl2 0.0796(6) 0.0449(5) 0.0679(6) -0.0183(4) 0.0373(5) -0.0166(4) Cl3 0.0657(6) 0.0669(6) 0.0327(4) -0.0075(4) -0.0001(4) -0.0095(4) O1 0.0377(11) 0.0213(10) 0.0315(10) -0.0040(8) 0.0077(8) 0.0042(8) O2 0.0342(10) 0.0225(10) 0.0312(10) 0.0045(8) 0.0028(8) -0.0065(8) O3 0.0375(11) 0.0277(10) 0.0361(10) -0.0094(8) 0.0049(8) 0.0093(8) O4 0.0302(10) 0.0203(10) 0.0336(10) 0.0051(8) 0.0044(8) -0.0028(7) C1 0.0226(13) 0.0215(14) 0.0225(12) -0.0015(10) 0.0055(10) -0.0002(10) C2 0.0226(13) 0.0255(14) 0.0243(13) -0.0008(11) 0.0068(10) 0.0002(11) C3 0.0221(13) 0.0206(13) 0.0210(12) 0.0002(10) 0.0043(10) -0.0006(10) C4 0.0198(13) 0.0221(13) 0.0207(12) -0.0004(10) 0.0032(10) 0.0016(10) C5 0.0243(13) 0.0166(13) 0.0272(13) -0.0015(10) 0.0054(10) -0.0025(10) C6 0.0251(13) 0.0161(13) 0.0239(12) -0.0008(10) 0.0042(10) 0.0024(10) C7 0.0200(12) 0.0192(13) 0.0209(12) -0.0009(10) 0.0031(10) 0.0005(10) C8 0.0205(13) 0.0216(13) 0.0199(12) -0.0005(10) 0.0022(10) 0.0029(10) C9 0.0250(13) 0.0242(14) 0.0205(12) 0.0032(10) 0.0062(10) 0.0005(11) C10 0.0232(13) 0.0216(14) 0.0207(12) 0.0026(10) 0.0034(10) -0.0009(10) C11 0.0210(13) 0.0217(13) 0.0197(12) -0.0002(10) 0.0024(10) 0.0010(10) C12 0.0251(13) 0.0169(13) 0.0252(13) -0.0020(10) 0.0037(10) -0.0031(10) C13 0.0250(13) 0.0183(13) 0.0228(12) -0.0029(10) 0.0046(10) 0.0008(10) C14 0.0193(13) 0.0202(13) 0.0227(12) -0.0001(10) 0.0030(10) 0.0005(10) C15 0.0197(13) 0.0189(13) 0.0203(12) 0.0001(10) 0.0029(10) 0.0002(10) C16 0.0199(13) 0.0209(13) 0.0196(12) 0.0004(10) 0.0022(10) -0.0007(10) C17 0.0240(13) 0.0210(13) 0.0221(12) 0.0008(10) 0.0101(10) -0.0012(10) C18 0.0250(14) 0.0253(14) 0.0218(12) 0.0011(11) 0.0089(10) -0.0004(11) C19 0.0283(14) 0.0214(14) 0.0234(13) -0.0022(10) 0.0070(10) -0.0034(11) C20 0.0327(15) 0.0173(13) 0.0237(13) 0.0012(10) 0.0127(11) 0.0009(11) C21 0.0259(14) 0.0244(14) 0.0234(13) 0.0038(11) 0.0064(10) 0.0029(11) C22 0.0276(14) 0.0224(14) 0.0229(13) 0.0033(10) 0.0093(10) -0.0003(11) C23 0.0280(15) 0.0312(15) 0.0289(14) -0.0010(12) 0.0062(11) 0.0012(11) C24 0.0273(15) 0.0339(16) 0.0312(14) -0.0039(12) 0.0071(11) 0.0029(12) C25 0.0454(17) 0.0268(15) 0.0360(15) -0.0091(12) 0.0100(13) -0.0032(13) C26 0.0234(13) 0.0214(13) 0.0227(12) -0.0008(10) 0.0100(10) -0.0006(10) C27 0.0260(14) 0.0228(14) 0.0223(12) -0.0002(10) 0.0080(10) -0.0011(11) C28 0.0255(14) 0.0253(15) 0.0274(13) -0.0023(11) 0.0066(11) -0.0051(11) C29 0.0296(14) 0.0189(13) 0.0243(13) 0.0012(10) 0.0100(11) -0.0044(11) C30 0.0260(14) 0.0259(14) 0.0201(12) 0.0033(11) 0.0072(10) 0.0011(11) C31 0.0236(13) 0.0206(14) 0.0231(12) -0.0014(10) 0.0080(10) -0.0033(10) C32 0.0295(15) 0.0268(15) 0.0329(14) 0.0035(12) 0.0041(11) -0.0042(11) C33 0.0341(15) 0.0257(15) 0.0330(14) 0.0018(12) 0.0032(12) -0.0045(12) C34 0.0362(16) 0.0263(15) 0.0398(16) 0.0013(12) 0.0013(12) -0.0071(12) C35 0.0224(13) 0.0187(13) 0.0224(12) -0.0001(10) 0.0115(10) -0.0022(10) C36 0.0248(13) 0.0234(14) 0.0223(12) 0.0013(10) 0.0079(10) -0.0007(11) C37 0.0287(14) 0.0261(14) 0.0220(12) -0.0028(11) 0.0057(10) -0.0028(11) C38 0.0281(14) 0.0230(14) 0.0280(13) -0.0034(11) 0.0118(11) 0.0008(11) C39 0.0263(14) 0.0252(14) 0.0264(13) 0.0015(11) 0.0071(11) 0.0055(11) C40 0.0262(14) 0.0212(14) 0.0228(12) 0.0017(10) 0.0076(10) -0.0007(11) C41 0.0354(15) 0.0286(15) 0.0285(14) -0.0068(12) 0.0032(11) 0.0023(12) C42 0.0334(15) 0.0295(16) 0.0316(14) -0.0053(12) 0.0008(12) 0.0031(12) C43 0.0440(18) 0.0353(17) 0.0402(16) -0.0165(13) 0.0107(13) 0.0027(13) C44 0.0272(13) 0.0193(13) 0.0195(12) -0.0004(10) 0.0105(10) 0.0012(10) C45 0.0245(14) 0.0224(14) 0.0220(12) -0.0005(10) 0.0069(10) 0.0037(10) C46 0.0231(13) 0.0212(13) 0.0258(13) -0.0020(10) 0.0052(10) -0.0042(10) C47 0.0264(14) 0.0183(13) 0.0249(13) 0.0021(10) 0.0108(10) 0.0023(10) C48 0.0286(14) 0.0200(13) 0.0215(12) 0.0036(10) 0.0042(10) 0.0023(11) C49 0.0273(14) 0.0253(14) 0.0226(13) -0.0006(11) 0.0079(10) 0.0023(11) C50 0.0314(15) 0.0269(15) 0.0360(15) 0.0036(12) 0.0008(12) -0.0039(12) C51 0.0346(16) 0.0265(15) 0.0324(14) 0.0064(12) 0.0042(12) -0.0011(12) C52 0.0321(15) 0.0229(15) 0.0400(15) 0.0022(12) 0.0031(12) -0.0033(11) C53 0.0362(16) 0.0370(17) 0.0323(15) 0.0049(13) 0.0149(12) 0.0005(13) C54 0.0340(16) 0.0405(18) 0.0267(14) 0.0028(13) 0.0098(12) -0.0001(13) C55 0.0326(16) 0.0398(18) 0.0329(15) 0.0034(13) 0.0153(12) -0.0019(13) C56 0.0332(16) 0.0403(18) 0.0326(15) 0.0104(13) 0.0121(12) 0.0041(13) C57 0.0326(16) 0.0444(18) 0.0312(15) 0.0029(13) 0.0129(12) -0.0042(13) C58 0.0392(17) 0.0393(18) 0.0326(15) -0.0002(13) 0.0138(13) -0.0065(13) C59 0.0514(19) 0.0436(19) 0.0400(17) 0.0028(14) 0.0141(14) 0.0075(15) C60 0.0449(18) 0.0410(18) 0.0396(16) 0.0006(14) 0.0110(13) 0.0000(14) C61 0.0448(19) 0.064(2) 0.0391(17) 0.0056(16) 0.0048(14) -0.0060(16) C62 0.0363(16) 0.0414(18) 0.0330(15) -0.0066(13) 0.0082(12) -0.0073(13) _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 Cl1 C62 1.749(3) . ? Cl2 C62 1.756(3) . ? Cl3 C62 1.747(3) . ? O1 C20 1.374(3) . ? O1 C25 1.425(3) . ? O2 C29 1.376(3) . ? O2 C34 1.418(3) . ? O3 C38 1.378(3) . ? O3 C43 1.420(3) . ? O4 C47 1.375(3) . ? O4 C52 1.430(3) . ? C1 C2 1.389(3) . ? C1 C14 1.408(3) . ? C1 C17 1.503(3) . ? C2 C3 1.393(3) . ? C2 H2 0.9500 . ? C3 C4 1.419(3) . ? C3 C26 1.494(3) . ? C4 C15 1.418(3) . ? C4 C5 1.436(3) . ? C5 C6 1.351(3) . ? C5 H5 0.9500 . ? C6 C7 1.436(3) . ? C6 H6 0.9500 . ? C7 C8 1.414(3) . ? C7 C16 1.432(3) . ? C8 C9 1.389(3) . ? C8 C35 1.501(3) . ? C9 C10 1.389(3) . ? C9 H9 0.9500 . ? C10 C11 1.417(3) . ? C10 C44 1.498(3) . ? C11 C16 1.421(3) . ? C11 C12 1.439(3) . ? C12 C13 1.347(3) . ? C12 H12 0.9500 . ? C13 C14 1.436(3) . ? C13 H13 0.9500 . ? C14 C15 1.426(3) . ? C15 C16 1.444(3) . ? C17 C18 1.398(3) . ? C17 C22 1.406(3) . ? C18 C19 1.397(3) . ? C18 C24 1.509(3) . ? C19 C20 1.387(3) . ? C19 H19 0.9500 . ? C20 C21 1.386(3) . ? C21 C22 1.389(3) . ? C21 H21 0.9500 . ? C22 C23 1.509(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.402(3) . ? C26 C31 1.407(3) . ? C27 C28 1.403(3) . ? C27 C33 1.505(3) . ? C28 C29 1.386(3) . ? C28 H28 0.9500 . ? C29 C30 1.387(3) . ? C30 C31 1.391(3) . ? C30 H30 0.9500 . ? C31 C32 1.511(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.391(3) . ? C35 C40 1.409(3) . ? C36 C37 1.396(3) . ? C36 C42 1.508(3) . ? C37 C38 1.388(3) . ? C37 H37 0.9500 . ? C38 C39 1.385(3) . ? C39 C40 1.383(3) . ? C39 H39 0.9500 . ? C40 C41 1.511(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.402(3) . ? C44 C49 1.407(3) . ? C45 C46 1.402(3) . ? C45 C51 1.507(3) . ? C46 C47 1.386(3) . ? C46 H46 0.9500 . ? C47 C48 1.387(3) . ? C48 C49 1.386(3) . ? C48 H48 0.9500 . ? C49 C50 1.506(3) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C58 1.393(4) . ? C53 C54 1.394(4) . ? C53 C59 1.503(4) . ? C54 C55 1.387(4) . ? C54 H54 0.9500 . ? C55 C56 1.389(4) . ? C55 C60 1.518(4) . ? C56 C57 1.393(4) . ? C56 H56 0.9500 . ? C57 C58 1.391(4) . ? C57 C61 1.502(4) . ? C58 H58 0.9500 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62 1.0000 . ? 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 C20 O1 C25 117.99(19) . . ? C29 O2 C34 117.14(18) . . ? C38 O3 C43 117.87(19) . . ? C47 O4 C52 117.25(18) . . ? C2 C1 C14 119.6(2) . . ? C2 C1 C17 120.1(2) . . ? C14 C1 C17 120.3(2) . . ? C1 C2 C3 123.0(2) . . ? C1 C2 H2 118.5 . . ? C3 C2 H2 118.5 . . ? C2 C3 C4 118.3(2) . . ? C2 C3 C26 120.2(2) . . ? C4 C3 C26 121.4(2) . . ? C15 C4 C3 119.6(2) . . ? C15 C4 C5 118.5(2) . . ? C3 C4 C5 121.9(2) . . ? C6 C5 C4 121.7(2) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 121.8(2) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C8 C7 C16 118.8(2) . . ? C8 C7 C6 122.9(2) . . ? C16 C7 C6 118.3(2) . . ? C9 C8 C7 119.8(2) . . ? C9 C8 C35 120.6(2) . . ? C7 C8 C35 119.6(2) . . ? C10 C9 C8 122.6(2) . . ? C10 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? C9 C10 C11 119.2(2) . . ? C9 C10 C44 120.5(2) . . ? C11 C10 C44 120.4(2) . . ? C10 C11 C16 119.6(2) . . ? C10 C11 C12 122.2(2) . . ? C16 C11 C12 118.3(2) . . ? C13 C12 C11 121.6(2) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 121.9(2) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C1 C14 C15 118.7(2) . . ? C1 C14 C13 122.6(2) . . ? C15 C14 C13 118.7(2) . . ? C4 C15 C14 120.6(2) . . ? C4 C15 C16 120.3(2) . . ? C14 C15 C16 119.1(2) . . ? C11 C16 C7 120.1(2) . . ? C11 C16 C15 120.4(2) . . ? C7 C16 C15 119.4(2) . . ? C18 C17 C22 120.1(2) . . ? C18 C17 C1 120.0(2) . . ? C22 C17 C1 119.9(2) . . ? C19 C18 C17 119.7(2) . . ? C19 C18 C24 120.1(2) . . ? C17 C18 C24 120.2(2) . . ? C20 C19 C18 120.1(2) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? O1 C20 C21 115.4(2) . . ? O1 C20 C19 124.5(2) . . ? C21 C20 C19 120.1(2) . . ? C20 C21 C22 120.9(2) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C17 119.1(2) . . ? C21 C22 C23 120.2(2) . . ? C17 C22 C23 120.7(2) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C25 H25A 109.5 . . ? O1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 C31 119.4(2) . . ? C27 C26 C3 120.0(2) . . ? C31 C26 C3 120.6(2) . . ? C26 C27 C28 119.5(2) . . ? C26 C27 C33 120.9(2) . . ? C28 C27 C33 119.6(2) . . ? C29 C28 C27 120.5(2) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? O2 C29 C28 124.7(2) . . ? O2 C29 C30 115.4(2) . . ? C28 C29 C30 119.9(2) . . ? C29 C30 C31 120.5(2) . . ? C29 C30 H30 119.8 . . ? C31 C30 H30 119.8 . . ? C30 C31 C26 120.0(2) . . ? C30 C31 C32 118.9(2) . . ? C26 C31 C32 121.1(2) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 H33A 109.5 . . ? C27 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C27 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O2 C34 H34A 109.5 . . ? O2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 119.9(2) . . ? C36 C35 C8 121.2(2) . . ? C40 C35 C8 118.9(2) . . ? C35 C36 C37 119.8(2) . . ? C35 C36 C42 120.6(2) . . ? C37 C36 C42 119.6(2) . . ? C38 C37 C36 120.0(2) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? O3 C38 C39 115.8(2) . . ? O3 C38 C37 124.2(2) . . ? C39 C38 C37 120.0(2) . . ? C40 C39 C38 120.9(2) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C39 C40 C35 119.2(2) . . ? C39 C40 C41 120.1(2) . . ? C35 C40 C41 120.6(2) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C36 C42 H42A 109.5 . . ? C36 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C36 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O3 C43 H43A 109.5 . . ? O3 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O3 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C49 119.8(2) . . ? C45 C44 C10 119.9(2) . . ? C49 C44 C10 120.2(2) . . ? C44 C45 C46 119.7(2) . . ? C44 C45 C51 120.5(2) . . ? C46 C45 C51 119.8(2) . . ? C47 C46 C45 120.2(2) . . ? C47 C46 H46 119.9 . . ? C45 C46 H46 119.9 . . ? O4 C47 C46 124.8(2) . . ? O4 C47 C48 115.6(2) . . ? C46 C47 C48 119.6(2) . . ? C49 C48 C47 121.5(2) . . ? C49 C48 H48 119.3 . . ? C47 C48 H48 119.3 . . ? C48 C49 C44 119.0(2) . . ? C48 C49 C50 119.7(2) . . ? C44 C49 C50 121.3(2) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C45 C51 H51A 109.5 . . ? C45 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C45 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O4 C52 H52A 109.5 . . ? O4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C58 C53 C54 118.3(3) . . ? C58 C53 C59 120.9(3) . . ? C54 C53 C59 120.8(2) . . ? C55 C54 C53 121.3(3) . . ? C55 C54 H54 119.4 . . ? C53 C54 H54 119.4 . . ? C54 C55 C56 119.0(3) . . ? C54 C55 C60 120.2(2) . . ? C56 C55 C60 120.8(3) . . ? C55 C56 C57 121.4(3) . . ? C55 C56 H56 119.3 . . ? C57 C56 H56 119.3 . . ? C58 C57 C56 118.2(3) . . ? C58 C57 C61 121.5(3) . . ? C56 C57 C61 120.4(3) . . ? C57 C58 C53 121.9(3) . . ? C57 C58 H58 119.1 . . ? C53 C58 H58 119.1 . . ? C53 C59 H59A 109.5 . . ? C53 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C53 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C55 C60 H60A 109.5 . . ? C55 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C55 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C57 C61 H61A 109.5 . . ? C57 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C57 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Cl3 C62 Cl1 110.78(15) . . ? Cl3 C62 Cl2 110.72(16) . . ? Cl1 C62 Cl2 110.75(15) . . ? Cl3 C62 H62 108.2 . . ? Cl1 C62 H62 108.2 . . ? Cl2 C62 H62 108.2 . . ? 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 C14 C1 C2 C3 0.5(3) . . . . ? C17 C1 C2 C3 -179.0(2) . . . . ? C1 C2 C3 C4 2.0(3) . . . . ? C1 C2 C3 C26 -179.7(2) . . . . ? C2 C3 C4 C15 -2.4(3) . . . . ? C26 C3 C4 C15 179.3(2) . . . . ? C2 C3 C4 C5 177.1(2) . . . . ? C26 C3 C4 C5 -1.2(3) . . . . ? C15 C4 C5 C6 0.6(3) . . . . ? C3 C4 C5 C6 -178.9(2) . . . . ? C4 C5 C6 C7 -0.4(4) . . . . ? C5 C6 C7 C8 179.6(2) . . . . ? C5 C6 C7 C16 -0.5(3) . . . . ? C16 C7 C8 C9 1.2(3) . . . . ? C6 C7 C8 C9 -178.9(2) . . . . ? C16 C7 C8 C35 -177.4(2) . . . . ? C6 C7 C8 C35 2.5(3) . . . . ? C7 C8 C9 C10 -1.0(3) . . . . ? C35 C8 C9 C10 177.6(2) . . . . ? C8 C9 C10 C11 0.2(3) . . . . ? C8 C9 C10 C44 -179.7(2) . . . . ? C9 C10 C11 C16 0.3(3) . . . . ? C44 C10 C11 C16 -179.7(2) . . . . ? C9 C10 C11 C12 -179.9(2) . . . . ? C44 C10 C11 C12 0.0(3) . . . . ? C10 C11 C12 C13 -178.5(2) . . . . ? C16 C11 C12 C13 1.3(3) . . . . ? C11 C12 C13 C14 0.7(3) . . . . ? C2 C1 C14 C15 -2.5(3) . . . . ? C17 C1 C14 C15 176.9(2) . . . . ? C2 C1 C14 C13 178.6(2) . . . . ? C17 C1 C14 C13 -2.0(3) . . . . ? C12 C13 C14 C1 176.7(2) . . . . ? C12 C13 C14 C15 -2.2(3) . . . . ? C3 C4 C15 C14 0.4(3) . . . . ? C5 C4 C15 C14 -179.2(2) . . . . ? C3 C4 C15 C16 179.6(2) . . . . ? C5 C4 C15 C16 0.1(3) . . . . ? C1 C14 C15 C4 2.1(3) . . . . ? C13 C14 C15 C4 -178.9(2) . . . . ? C1 C14 C15 C16 -177.1(2) . . . . ? C13 C14 C15 C16 1.8(3) . . . . ? C10 C11 C16 C7 -0.1(3) . . . . ? C12 C11 C16 C7 -179.9(2) . . . . ? C10 C11 C16 C15 178.2(2) . . . . ? C12 C11 C16 C15 -1.6(3) . . . . ? C8 C7 C16 C11 -0.7(3) . . . . ? C6 C7 C16 C11 179.4(2) . . . . ? C8 C7 C16 C15 -179.0(2) . . . . ? C6 C7 C16 C15 1.1(3) . . . . ? C4 C15 C16 C11 -179.2(2) . . . . ? C14 C15 C16 C11 0.0(3) . . . . ? C4 C15 C16 C7 -0.9(3) . . . . ? C14 C15 C16 C7 178.33(19) . . . . ? C2 C1 C17 C18 -99.2(3) . . . . ? C14 C1 C17 C18 81.3(3) . . . . ? C2 C1 C17 C22 82.0(3) . . . . ? C14 C1 C17 C22 -97.5(3) . . . . ? C22 C17 C18 C19 2.1(3) . . . . ? C1 C17 C18 C19 -176.6(2) . . . . ? C22 C17 C18 C24 -179.1(2) . . . . ? C1 C17 C18 C24 2.1(3) . . . . ? C17 C18 C19 C20 -1.0(3) . . . . ? C24 C18 C19 C20 -179.7(2) . . . . ? C25 O1 C20 C21 177.2(2) . . . . ? C25 O1 C20 C19 -4.3(3) . . . . ? C18 C19 C20 O1 -179.0(2) . . . . ? C18 C19 C20 C21 -0.6(3) . . . . ? O1 C20 C21 C22 179.6(2) . . . . ? C19 C20 C21 C22 1.1(4) . . . . ? C20 C21 C22 C17 0.1(4) . . . . ? C20 C21 C22 C23 179.1(2) . . . . ? C18 C17 C22 C21 -1.7(3) . . . . ? C1 C17 C22 C21 177.1(2) . . . . ? C18 C17 C22 C23 179.3(2) . . . . ? C1 C17 C22 C23 -2.0(3) . . . . ? C2 C3 C26 C27 -91.0(3) . . . . ? C4 C3 C26 C27 87.3(3) . . . . ? C2 C3 C26 C31 89.9(3) . . . . ? C4 C3 C26 C31 -91.8(3) . . . . ? C31 C26 C27 C28 1.3(3) . . . . ? C3 C26 C27 C28 -177.9(2) . . . . ? C31 C26 C27 C33 -179.0(2) . . . . ? C3 C26 C27 C33 1.9(3) . . . . ? C26 C27 C28 C29 1.5(4) . . . . ? C33 C27 C28 C29 -178.2(2) . . . . ? C34 O2 C29 C28 -10.2(3) . . . . ? C34 O2 C29 C30 170.8(2) . . . . ? C27 C28 C29 O2 177.5(2) . . . . ? C27 C28 C29 C30 -3.6(4) . . . . ? O2 C29 C30 C31 -178.2(2) . . . . ? C28 C29 C30 C31 2.8(4) . . . . ? C29 C30 C31 C26 0.0(3) . . . . ? C29 C30 C31 C32 179.4(2) . . . . ? C27 C26 C31 C30 -2.0(3) . . . . ? C3 C26 C31 C30 177.1(2) . . . . ? C27 C26 C31 C32 178.6(2) . . . . ? C3 C26 C31 C32 -2.3(3) . . . . ? C9 C8 C35 C36 85.6(3) . . . . ? C7 C8 C35 C36 -95.8(3) . . . . ? C9 C8 C35 C40 -95.3(3) . . . . ? C7 C8 C35 C40 83.3(3) . . . . ? C40 C35 C36 C37 -2.5(3) . . . . ? C8 C35 C36 C37 176.7(2) . . . . ? C40 C35 C36 C42 178.0(2) . . . . ? C8 C35 C36 C42 -2.9(3) . . . . ? C35 C36 C37 C38 -0.8(4) . . . . ? C42 C36 C37 C38 178.8(2) . . . . ? C43 O3 C38 C39 177.4(2) . . . . ? C43 O3 C38 C37 -2.4(4) . . . . ? C36 C37 C38 O3 -177.5(2) . . . . ? C36 C37 C38 C39 2.6(4) . . . . ? O3 C38 C39 C40 178.9(2) . . . . ? C37 C38 C39 C40 -1.2(4) . . . . ? C38 C39 C40 C35 -2.0(4) . . . . ? C38 C39 C40 C41 176.8(2) . . . . ? C36 C35 C40 C39 3.8(3) . . . . ? C8 C35 C40 C39 -175.3(2) . . . . ? C36 C35 C40 C41 -174.9(2) . . . . ? C8 C35 C40 C41 5.9(3) . . . . ? C9 C10 C44 C45 93.7(3) . . . . ? C11 C10 C44 C45 -86.3(3) . . . . ? C9 C10 C44 C49 -86.5(3) . . . . ? C11 C10 C44 C49 93.5(3) . . . . ? C49 C44 C45 C46 -1.6(3) . . . . ? C10 C44 C45 C46 178.2(2) . . . . ? C49 C44 C45 C51 179.5(2) . . . . ? C10 C44 C45 C51 -0.7(3) . . . . ? C44 C45 C46 C47 0.4(3) . . . . ? C51 C45 C46 C47 179.2(2) . . . . ? C52 O4 C47 C46 11.6(3) . . . . ? C52 O4 C47 C48 -169.0(2) . . . . ? C45 C46 C47 O4 -178.1(2) . . . . ? C45 C46 C47 C48 2.4(3) . . . . ? O4 C47 C48 C49 176.5(2) . . . . ? C46 C47 C48 C49 -4.0(4) . . . . ? C47 C48 C49 C44 2.8(4) . . . . ? C47 C48 C49 C50 -176.9(2) . . . . ? C45 C44 C49 C48 0.1(3) . . . . ? C10 C44 C49 C48 -179.7(2) . . . . ? C45 C44 C49 C50 179.7(2) . . . . ? C10 C44 C49 C50 -0.1(3) . . . . ? C58 C53 C54 C55 0.2(4) . . . . ? C59 C53 C54 C55 -179.9(2) . . . . ? C53 C54 C55 C56 -0.6(4) . . . . ? C53 C54 C55 C60 178.4(2) . . . . ? C54 C55 C56 C57 1.1(4) . . . . ? C60 C55 C56 C57 -177.9(2) . . . . ? C55 C56 C57 C58 -1.1(4) . . . . ? C55 C56 C57 C61 178.1(2) . . . . ? C56 C57 C58 C53 0.7(4) . . . . ? C61 C57 C58 C53 -178.5(3) . . . . ? C54 C53 C58 C57 -0.3(4) . . . . ? C59 C53 C58 C57 179.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.356 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.067 #END data_TP-BM _database_code_depnum_ccdc_archive 'CCDC 726987' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra(2,6-dimethyl-4-methoxyphenyl)pyrene ; _chemical_name_common tetra(2,6-dimethyl-4-methoxyphenyl)pyrene _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 O4, C4 H9 N O, C7 H6 O' _chemical_formula_sum 'C63 H65 N O6' _chemical_formula_weight 932.16 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 orthorhombic _symmetry_space_group_name_H-M Pca21 _symmetry_space_group_name_Hall 'P 2c -2ac' _symmetry_Int_Tables_number 29 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 14.829(4) _cell_length_b 15.582(5) _cell_length_c 23.732(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5484(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2179 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 17.49 _exptl_crystal_description 'thin needles' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Thin needle shape crystals. It losses crystallinity both at low (guest molecules freezes and broken into many pieces)and moderate temperatures. ; _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 'Bruker SMART APEX' _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 27514 _diffrn_reflns_av_R_equivalents 0.0681 _diffrn_reflns_av_sigmaI/netI 0.0826 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9470 _reflns_number_gt 5228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.1156P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 2(3) _refine_ls_number_reflns 9470 _refine_ls_number_parameters 705 _refine_ls_number_restraints 207 _refine_ls_R_factor_all 0.1601 _refine_ls_R_factor_gt 0.0944 _refine_ls_wR_factor_ref 0.2424 _refine_ls_wR_factor_gt 0.2098 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.101 _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 O1 O 0.0583(3) -0.1612(3) 0.4942(2) 0.0814(14) Uani 1 1 d . . . O2 O 0.0580(3) 0.6087(3) 0.5352(2) 0.0914(15) Uani 1 1 d . . . O3 O 0.6379(4) 0.6458(3) 0.1984(2) 0.1025(18) Uani 1 1 d . . . O4 O 0.6212(4) -0.1184(3) 0.1557(2) 0.0883(15) Uani 1 1 d . . . C1 C 0.2091(4) 0.1552(3) 0.4295(3) 0.0504(14) Uani 1 1 d . . . C2 C 0.1818(4) 0.2315(4) 0.4551(3) 0.0575(16) Uani 1 1 d . . . H2 H 0.1391 0.2279 0.4837 0.069 Uiso 1 1 calc R . . C3 C 0.2135(4) 0.3117(3) 0.4411(2) 0.0487(14) Uani 1 1 d . . . C4 C 0.2788(4) 0.3179(3) 0.3990(3) 0.0491(14) Uani 1 1 d . . . C5 C 0.3167(4) 0.3975(3) 0.3817(3) 0.0538(15) Uani 1 1 d . . . H5 H 0.2980 0.4478 0.3994 0.065 Uiso 1 1 calc R . . C6 C 0.3801(4) 0.4023(3) 0.3398(3) 0.0544(15) Uani 1 1 d . . . H6 H 0.4024 0.4557 0.3294 0.065 Uiso 1 1 calc R . . C7 C 0.4123(4) 0.3292(3) 0.3123(2) 0.0418(13) Uani 1 1 d . . . C8 C 0.4804(4) 0.3339(3) 0.2705(3) 0.0527(15) Uani 1 1 d . . . C9 C 0.5085(4) 0.2582(3) 0.2441(3) 0.0494(14) Uani 1 1 d . . . H9 H 0.5527 0.2614 0.2164 0.059 Uiso 1 1 calc R . . C10 C 0.4734(4) 0.1795(4) 0.2577(3) 0.0564(16) Uani 1 1 d . . . C11 C 0.4069(4) 0.1716(3) 0.3006(2) 0.0425(12) Uani 1 1 d . . . C12 C 0.3694(4) 0.0924(3) 0.3177(2) 0.0479(14) Uani 1 1 d . . . H12 H 0.3891 0.0424 0.3002 0.058 Uiso 1 1 calc R . . C13 C 0.3074(4) 0.0865(3) 0.3575(2) 0.0481(14) Uani 1 1 d . . . H13 H 0.2844 0.0327 0.3664 0.058 Uiso 1 1 calc R . . C14 C 0.2746(4) 0.1594(3) 0.3872(3) 0.0501(14) Uani 1 1 d . . . C15 C 0.3104(4) 0.2422(3) 0.3709(2) 0.0431(13) Uani 1 1 d . . . C16 C 0.3771(4) 0.2469(3) 0.3282(2) 0.0474(14) Uani 1 1 d . . . C17 C 0.1674(4) 0.0719(3) 0.4465(2) 0.0449(13) Uani 1 1 d . . . C18 C 0.0933(4) 0.0415(4) 0.4166(2) 0.0549(15) Uani 1 1 d . . . C19 C 0.0558(4) -0.0388(4) 0.4321(3) 0.0571(16) Uani 1 1 d . . . H19 H 0.0077 -0.0611 0.4116 0.069 Uiso 1 1 calc R . . C20 C 0.0897(4) -0.0835(4) 0.4767(3) 0.0582(15) Uani 1 1 d . . . C21 C 0.1585(4) -0.0507(4) 0.5079(3) 0.0614(16) Uani 1 1 d . . . H21 H 0.1789 -0.0800 0.5395 0.074 Uiso 1 1 calc R . . C22 C 0.1982(4) 0.0264(4) 0.4924(3) 0.0584(16) Uani 1 1 d . . . C23 C 0.2766(5) 0.0606(5) 0.5266(3) 0.089(2) Uani 1 1 d . . . H23A H 0.3278 0.0687 0.5024 0.134 Uiso 1 1 calc R . . H23B H 0.2915 0.0204 0.5557 0.134 Uiso 1 1 calc R . . H23C H 0.2601 0.1145 0.5432 0.134 Uiso 1 1 calc R . . C24 C 0.0561(5) 0.0885(4) 0.3669(3) 0.083(2) Uani 1 1 d . . . H24A H 0.0471 0.1477 0.3765 0.124 Uiso 1 1 calc R . . H24B H -0.0004 0.0634 0.3561 0.124 Uiso 1 1 calc R . . H24C H 0.0978 0.0845 0.3360 0.124 Uiso 1 1 calc R . . C25 C -0.0039(5) -0.2037(4) 0.4576(4) 0.089(2) Uani 1 1 d . . . H25A H -0.0588 -0.1712 0.4556 0.133 Uiso 1 1 calc R . . H25B H -0.0166 -0.2600 0.4720 0.133 Uiso 1 1 calc R . . H25C H 0.0219 -0.2085 0.4207 0.133 Uiso 1 1 calc R . . C26 C 0.1729(4) 0.3904(3) 0.4685(3) 0.0531(15) Uani 1 1 d . . . C27 C 0.2163(5) 0.4294(4) 0.5141(3) 0.0614(17) Uani 1 1 d . . . C28 C 0.1780(4) 0.5031(4) 0.5360(3) 0.0597(15) Uani 1 1 d . . . H28 H 0.2061 0.5306 0.5660 0.072 Uiso 1 1 calc R . . C29 C 0.1005(5) 0.5364(4) 0.5148(3) 0.0657(18) Uani 1 1 d . . . C30 C 0.0584(5) 0.4951(4) 0.4727(3) 0.0716(18) Uani 1 1 d . . . H30 H 0.0041 0.5172 0.4596 0.086 Uiso 1 1 calc R . . C31 C 0.0919(4) 0.4209(4) 0.4475(3) 0.0585(16) Uani 1 1 d . . . C32 C 0.0423(5) 0.3799(5) 0.3986(3) 0.084(2) Uani 1 1 d . . . H32A H 0.0849 0.3621 0.3705 0.127 Uiso 1 1 calc R . . H32B H 0.0012 0.4207 0.3825 0.127 Uiso 1 1 calc R . . H32C H 0.0092 0.3309 0.4118 0.127 Uiso 1 1 calc R . . C33 C 0.3027(5) 0.3936(5) 0.5366(4) 0.101(3) Uani 1 1 d . . . H33A H 0.3121 0.4140 0.5743 0.151 Uiso 1 1 calc R . . H33B H 0.3518 0.4118 0.5131 0.151 Uiso 1 1 calc R . . H33C H 0.2996 0.3321 0.5368 0.151 Uiso 1 1 calc R . . C34 C 0.1072(6) 0.6623(5) 0.5732(4) 0.102(3) Uani 1 1 d . . . H34A H 0.1215 0.6305 0.6066 0.153 Uiso 1 1 calc R . . H34B H 0.0711 0.7113 0.5830 0.153 Uiso 1 1 calc R . . H34C H 0.1618 0.6812 0.5554 0.153 Uiso 1 1 calc R . . C35 C 0.5207(4) 0.4158(3) 0.2523(3) 0.0518(15) Uani 1 1 d . . . C36 C 0.5900(4) 0.4538(4) 0.2850(3) 0.0603(17) Uani 1 1 d . . . C37 C 0.6291(4) 0.5294(4) 0.2665(3) 0.0647(18) Uani 1 1 d . . . H37 H 0.6747 0.5544 0.2877 0.078 Uiso 1 1 calc R . . C38 C 0.6025(5) 0.5676(4) 0.2182(3) 0.0678(18) Uani 1 1 d . . . C39 C 0.5361(5) 0.5308(4) 0.1856(3) 0.077(2) Uani 1 1 d . . . H39 H 0.5196 0.5565 0.1518 0.093 Uiso 1 1 calc R . . C40 C 0.4942(5) 0.4573(4) 0.2022(3) 0.0657(17) Uani 1 1 d . . . C41 C 0.4191(6) 0.4203(5) 0.1657(3) 0.110(3) Uani 1 1 d . . . H41A H 0.4294 0.4355 0.1270 0.165 Uiso 1 1 calc R . . H41B H 0.3622 0.4432 0.1778 0.165 Uiso 1 1 calc R . . H41C H 0.4184 0.3590 0.1693 0.165 Uiso 1 1 calc R . . C42 C 0.6242(5) 0.4088(4) 0.3368(3) 0.077(2) Uani 1 1 d . . . H42A H 0.6583 0.4483 0.3594 0.116 Uiso 1 1 calc R . . H42B H 0.6620 0.3616 0.3259 0.116 Uiso 1 1 calc R . . H42C H 0.5740 0.3876 0.3583 0.116 Uiso 1 1 calc R . . C43 C 0.6935(6) 0.6943(5) 0.2341(5) 0.118(3) Uani 1 1 d . . . H43A H 0.6628 0.7046 0.2691 0.177 Uiso 1 1 calc R . . H43B H 0.7075 0.7481 0.2165 0.177 Uiso 1 1 calc R . . H43C H 0.7483 0.6633 0.2412 0.177 Uiso 1 1 calc R . . C44 C 0.5099(4) 0.1016(3) 0.2296(2) 0.0507(14) Uani 1 1 d . . . C45 C 0.4658(4) 0.0635(3) 0.1840(3) 0.0571(15) Uani 1 1 d . . . C46 C 0.5019(5) -0.0108(4) 0.1583(3) 0.0702(18) Uani 1 1 d . . . H46 H 0.4713 -0.0369 0.1287 0.084 Uiso 1 1 calc R . . C47 C 0.5822(5) -0.0446(4) 0.1771(3) 0.0635(18) Uani 1 1 d . . . C48 C 0.6284(5) -0.0065(4) 0.2217(3) 0.0675(18) Uani 1 1 d . . . H48 H 0.6820 -0.0302 0.2348 0.081 Uiso 1 1 calc R . . C49 C 0.5938(4) 0.0669(3) 0.2462(2) 0.0554(15) Uani 1 1 d . . . C50 C 0.6475(5) 0.1081(4) 0.2926(3) 0.0743(19) Uani 1 1 d . . . H50A H 0.7053 0.0806 0.2953 0.112 Uiso 1 1 calc R . . H50B H 0.6158 0.1019 0.3276 0.112 Uiso 1 1 calc R . . H50C H 0.6557 0.1679 0.2844 0.112 Uiso 1 1 calc R . . C51 C 0.3791(5) 0.0997(4) 0.1615(3) 0.089(2) Uani 1 1 d . . . H51A H 0.3372 0.1074 0.1920 0.134 Uiso 1 1 calc R . . H51B H 0.3540 0.0608 0.1344 0.134 Uiso 1 1 calc R . . H51C H 0.3906 0.1540 0.1439 0.134 Uiso 1 1 calc R . . C52 C 0.5699(6) -0.1677(5) 0.1192(4) 0.109(3) Uani 1 1 d . . . H52A H 0.5142 -0.1830 0.1371 0.164 Uiso 1 1 calc R . . H52B H 0.6025 -0.2189 0.1095 0.164 Uiso 1 1 calc R . . H52C H 0.5576 -0.1354 0.0856 0.164 Uiso 1 1 calc R . . O6 O 0.6600(8) 0.2042(9) -0.0431(4) 0.230(9) Uani 0.650(11) 1 d PDU A 1 N1 N 0.5318(9) 0.2366(11) 0.0437(5) 0.218(9) Uani 0.650(11) 1 d PDU A 1 H1B H 0.5259 0.2386 0.0814 0.262 Uiso 0.650(11) 1 d PR A 1 C60 C 0.6429(8) 0.2877(7) -0.0262(6) 0.098(4) Uani 0.650(11) 1 d PDU A 1 H60A H 0.6084 0.3135 -0.0559 0.117 Uiso 0.650(11) 1 d PR A 1 H60B H 0.6992 0.3180 -0.0241 0.117 Uiso 0.650(11) 1 d PR A 1 C61 C 0.5973(11) 0.2995(8) 0.0292(6) 0.180(11) Uani 0.650(11) 1 d PDU A 1 H61A H 0.6412 0.3055 0.0587 0.217 Uiso 0.650(11) 1 d PR A 1 H61B H 0.5655 0.3531 0.0266 0.217 Uiso 0.650(11) 1 d PR A 1 C62 C 0.5538(9) 0.1511(9) 0.0281(6) 0.136(6) Uani 0.650(11) 1 d PDU A 1 H62A H 0.4994 0.1177 0.0281 0.163 Uiso 0.650(11) 1 d PR A 1 H62B H 0.5929 0.1275 0.0564 0.163 Uiso 0.650(11) 1 d PR A 1 C63 C 0.6022(11) 0.1404(7) -0.0265(7) 0.164(8) Uani 0.650(11) 1 d PDU A 1 H63A H 0.6310 0.0852 -0.0276 0.196 Uiso 0.650(11) 1 d PR A 1 H63B H 0.5562 0.1404 -0.0550 0.196 Uiso 0.650(11) 1 d PR A 1 O6A O 0.7205(18) 0.2618(16) -0.0705(11) 0.252(14) Uiso 0.350(11) 1 d PDU A 2 N1A N 0.5816(14) 0.2892(15) 0.0105(10) 0.120(9) Uiso 0.350(11) 1 d PDU A 2 H1AB H 0.5531 0.2764 0.0429 0.144 Uiso 0.350(11) 1 d PR A 2 C60A C 0.6954(14) 0.3466(13) -0.0553(9) 0.108(9) Uiso 0.350(11) 1 d PDU A 2 H60A H 0.6557 0.3673 -0.0842 0.130 Uiso 0.350(11) 1 d PR A 2 H60B H 0.7392 0.3904 -0.0476 0.130 Uiso 0.350(11) 1 d PR A 2 C61A C 0.6524(16) 0.3505(13) 0.0025(9) 0.137(10) Uiso 0.350(11) 1 d PDU A 2 H61A H 0.6928 0.3343 0.0323 0.164 Uiso 0.350(11) 1 d PR A 2 H61B H 0.6209 0.4013 0.0141 0.164 Uiso 0.350(11) 1 d PR A 2 C62A C 0.608(2) 0.2040(12) -0.0073(14) 0.188(15) Uiso 0.350(11) 1 d PDU A 2 H62A H 0.5642 0.1607 -0.0162 0.226 Uiso 0.350(11) 1 d PR A 2 H62B H 0.6472 0.1815 0.0213 0.226 Uiso 0.350(11) 1 d PR A 2 C63A C 0.646(3) 0.2050(16) -0.0672(13) 0.251(19) Uiso 0.350(11) 1 d PDU A 2 H63A H 0.6777 0.1547 -0.0792 0.301 Uiso 0.350(11) 1 d PR A 2 H63B H 0.6061 0.2222 -0.0971 0.301 Uiso 0.350(11) 1 d PR A 2 O5 O 0.9303(18) 0.1128(11) 0.2591(11) 0.334(14) Uani 0.496(10) 1 d PDU B 1 C59 C 0.9195(10) 0.1895(10) 0.2588(6) 0.127(6) Uani 0.496(10) 1 d PDU B 1 H59A H 0.9593 0.2249 0.2783 0.152 Uiso 0.496(10) 1 calc PR B 1 C53 C 0.8425(10) 0.2275(7) 0.2273(5) 0.101(5) Uani 0.496(10) 1 d PGDU B 1 C54 C 0.8200(10) 0.3133(7) 0.2353(5) 0.081(5) Uani 0.496(10) 1 d PGDU B 1 H54A H 0.8478 0.3449 0.2636 0.097 Uiso 0.496(10) 1 calc PR B 1 C55 C 0.7559(11) 0.3518(7) 0.2008(6) 0.109(5) Uani 0.496(10) 1 d PGU B 1 H55A H 0.7408 0.4092 0.2061 0.130 Uiso 0.496(10) 1 calc PR B 1 C56 C 0.7143(10) 0.3046(9) 0.1585(6) 0.111(5) Uani 0.496(10) 1 d PGU B 1 H56A H 0.6714 0.3304 0.1354 0.133 Uiso 0.496(10) 1 calc PR B 1 C57 C 0.7369(11) 0.2188(8) 0.1505(6) 0.112(6) Uani 0.496(10) 1 d PGU B 1 H57A H 0.7091 0.1873 0.1222 0.134 Uiso 0.496(10) 1 calc PR B 1 C58 C 0.8010(11) 0.1803(7) 0.1850(6) 0.112(5) Uani 0.496(10) 1 d PGDU B 1 H58A H 0.8161 0.1230 0.1797 0.134 Uiso 0.496(10) 1 calc PR B 1 O5A O 0.9007(19) 0.3619(14) 0.3046(10) 0.349(15) Uani 0.504(10) 1 d PDU B 2 C59A C 0.8488(12) 0.3768(9) 0.2667(8) 0.155(8) Uani 0.504(10) 1 d PDU B 2 H59B H 0.8237 0.4313 0.2636 0.186 Uiso 0.504(10) 1 calc PR B 2 C53A C 0.8242(13) 0.3097(8) 0.2248(8) 0.153(8) Uani 0.504(10) 1 d PGDU B 2 C54A C 0.8657(12) 0.2298(9) 0.2277(8) 0.165(8) Uani 0.504(10) 1 d PGDU B 2 H54B H 0.9154 0.2219 0.2510 0.197 Uiso 0.504(10) 1 calc PR B 2 C55A C 0.8330(14) 0.1619(8) 0.1958(9) 0.175(9) Uani 0.504(10) 1 d PGU B 2 H55B H 0.8608 0.1084 0.1977 0.210 Uiso 0.504(10) 1 calc PR B 2 C56A C 0.7587(14) 0.1737(10) 0.1609(9) 0.172(9) Uani 0.504(10) 1 d PGU B 2 H56B H 0.7368 0.1282 0.1395 0.206 Uiso 0.504(10) 1 calc PR B 2 C57A C 0.7172(13) 0.2536(12) 0.1579(8) 0.171(8) Uani 0.504(10) 1 d PGU B 2 H57B H 0.6675 0.2615 0.1346 0.205 Uiso 0.504(10) 1 calc PR B 2 C58A C 0.7499(14) 0.3215(9) 0.1899(9) 0.160(8) Uani 0.504(10) 1 d PGDU B 2 H58B H 0.7222 0.3750 0.1879 0.192 Uiso 0.504(10) 1 calc PR B 2 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 O1 0.095(4) 0.065(3) 0.084(3) 0.016(2) -0.003(3) -0.033(2) O2 0.099(4) 0.069(3) 0.106(4) -0.031(3) 0.002(3) 0.027(3) O3 0.109(4) 0.082(3) 0.116(4) 0.048(3) 0.002(4) -0.037(3) O4 0.117(4) 0.060(3) 0.087(3) -0.019(3) 0.020(3) 0.000(3) C1 0.045(3) 0.053(3) 0.053(4) 0.000(3) 0.008(3) -0.002(3) C2 0.056(4) 0.062(4) 0.055(4) -0.006(3) 0.009(3) 0.002(3) C3 0.050(4) 0.048(3) 0.048(3) 0.000(3) 0.005(3) -0.010(3) C4 0.045(3) 0.040(3) 0.062(4) -0.004(3) -0.005(3) 0.003(2) C5 0.058(4) 0.041(3) 0.062(4) 0.003(3) -0.003(3) 0.002(3) C6 0.056(4) 0.043(3) 0.065(4) 0.008(3) 0.000(3) -0.009(3) C7 0.044(3) 0.034(3) 0.047(3) 0.000(2) 0.000(3) 0.000(2) C8 0.054(4) 0.039(3) 0.066(4) 0.010(3) 0.013(3) -0.003(2) C9 0.053(3) 0.042(3) 0.053(4) 0.006(3) 0.018(3) -0.006(3) C10 0.058(4) 0.058(4) 0.054(4) 0.001(3) -0.002(3) 0.014(3) C11 0.045(3) 0.041(3) 0.041(3) -0.001(2) 0.007(3) 0.008(2) C12 0.052(4) 0.035(3) 0.057(4) -0.010(2) 0.013(3) 0.001(2) C13 0.056(4) 0.030(3) 0.057(4) -0.002(2) 0.008(3) -0.001(2) C14 0.043(3) 0.044(3) 0.064(4) 0.003(3) 0.000(3) -0.004(2) C15 0.043(3) 0.046(3) 0.040(3) 0.006(2) 0.008(3) -0.002(2) C16 0.044(3) 0.054(3) 0.044(3) 0.003(3) -0.007(3) 0.001(3) C17 0.052(4) 0.044(3) 0.039(3) -0.004(3) 0.007(3) -0.005(3) C18 0.062(4) 0.059(3) 0.044(3) 0.002(3) 0.002(3) -0.007(3) C19 0.052(4) 0.062(4) 0.057(4) -0.006(3) -0.004(3) -0.018(3) C20 0.069(4) 0.060(3) 0.046(4) 0.011(3) -0.004(3) -0.012(3) C21 0.065(4) 0.063(4) 0.056(4) 0.016(3) -0.005(3) -0.017(3) C22 0.058(4) 0.071(4) 0.046(3) -0.001(3) 0.002(3) -0.014(3) C23 0.075(5) 0.092(5) 0.100(6) 0.010(4) -0.015(4) -0.024(4) C24 0.094(6) 0.069(4) 0.086(5) 0.017(4) -0.013(4) 0.000(4) C25 0.093(6) 0.062(4) 0.113(7) 0.009(4) -0.003(5) -0.028(4) C26 0.058(4) 0.044(3) 0.057(4) 0.003(3) 0.016(3) 0.002(3) C27 0.075(5) 0.050(3) 0.059(4) -0.003(3) 0.001(4) -0.005(3) C28 0.068(4) 0.058(3) 0.054(4) -0.014(3) 0.007(3) -0.001(3) C29 0.080(5) 0.051(4) 0.066(4) -0.006(3) 0.016(4) -0.003(3) C30 0.072(5) 0.070(4) 0.073(5) 0.010(4) -0.001(4) 0.004(3) C31 0.056(4) 0.053(3) 0.067(4) -0.007(3) 0.020(3) 0.011(3) C32 0.083(5) 0.094(5) 0.076(5) -0.020(4) -0.014(4) 0.005(4) C33 0.092(6) 0.109(6) 0.100(6) -0.021(5) -0.026(5) 0.006(5) C34 0.117(7) 0.084(5) 0.105(6) -0.035(5) 0.002(6) 0.013(5) C35 0.053(4) 0.044(3) 0.058(4) -0.009(3) -0.001(3) 0.001(3) C36 0.057(4) 0.057(4) 0.067(4) 0.003(3) 0.009(3) 0.009(3) C37 0.060(4) 0.052(4) 0.083(5) 0.002(3) 0.007(4) -0.010(3) C38 0.066(4) 0.064(4) 0.073(5) 0.026(4) 0.007(4) -0.002(3) C39 0.088(5) 0.072(4) 0.072(5) 0.027(4) -0.013(4) -0.002(4) C40 0.076(5) 0.054(3) 0.067(4) 0.016(3) -0.012(4) -0.012(3) C41 0.140(8) 0.097(5) 0.094(6) 0.028(5) -0.048(6) -0.027(5) C42 0.075(5) 0.083(4) 0.073(5) 0.024(4) -0.021(4) -0.013(4) C43 0.109(7) 0.080(5) 0.165(9) 0.030(6) -0.015(7) -0.059(5) C44 0.053(4) 0.053(3) 0.046(3) 0.005(3) 0.015(3) -0.009(3) C45 0.051(4) 0.052(3) 0.068(4) 0.001(3) 0.006(3) -0.009(3) C46 0.074(5) 0.077(4) 0.059(4) -0.016(4) 0.011(4) -0.024(4) C47 0.063(4) 0.052(4) 0.075(5) -0.012(3) 0.021(4) 0.004(3) C48 0.060(4) 0.064(4) 0.079(5) -0.015(4) 0.014(4) 0.018(3) C49 0.066(4) 0.052(3) 0.048(3) 0.002(3) 0.009(3) -0.001(3) C50 0.081(5) 0.080(4) 0.062(4) -0.010(4) -0.004(4) 0.010(4) C51 0.068(5) 0.102(5) 0.097(6) -0.016(5) -0.014(4) 0.015(4) C52 0.129(7) 0.086(5) 0.113(7) -0.056(5) 0.036(6) -0.026(5) O6 0.213(14) 0.193(13) 0.285(17) 0.070(12) -0.193(13) -0.001(11) N1 0.130(13) 0.34(2) 0.180(14) 0.054(16) -0.064(12) -0.005(14) C60 0.092(9) 0.085(8) 0.116(11) 0.024(8) -0.026(8) -0.009(7) C61 0.185(17) 0.203(17) 0.154(16) 0.017(13) -0.137(15) -0.028(14) C62 0.119(12) 0.171(14) 0.118(12) 0.006(11) -0.065(10) 0.027(10) C63 0.163(16) 0.149(13) 0.179(17) 0.017(13) -0.065(14) 0.014(12) O5 0.339(19) 0.36(2) 0.305(19) -0.003(16) -0.008(16) 0.023(16) C59 0.124(10) 0.165(11) 0.092(9) 0.037(9) -0.001(8) 0.077(9) C53 0.097(10) 0.147(10) 0.058(8) 0.016(8) 0.025(8) 0.023(8) C54 0.080(9) 0.125(11) 0.037(7) -0.012(8) 0.027(7) 0.007(9) C55 0.097(10) 0.145(11) 0.083(9) -0.006(9) 0.037(9) -0.006(9) C56 0.088(9) 0.151(11) 0.093(9) -0.010(9) 0.014(8) -0.014(9) C57 0.094(10) 0.139(10) 0.103(10) -0.015(9) 0.018(8) 0.002(9) C58 0.097(11) 0.151(11) 0.088(10) 0.011(9) 0.029(9) 0.001(9) O5A 0.30(3) 0.37(3) 0.37(3) -0.05(2) 0.10(2) -0.07(2) C59A 0.120(13) 0.169(13) 0.176(16) -0.113(12) 0.088(12) -0.096(10) C53A 0.122(13) 0.150(12) 0.186(15) -0.072(11) 0.095(12) -0.053(10) C54A 0.132(13) 0.164(14) 0.198(17) -0.045(13) 0.118(12) -0.005(11) C55A 0.150(15) 0.169(13) 0.207(18) -0.022(13) 0.122(13) -0.006(12) C56A 0.156(15) 0.163(14) 0.196(17) -0.013(14) 0.083(14) -0.025(13) C57A 0.153(14) 0.178(15) 0.182(16) -0.016(14) 0.070(14) -0.016(13) C58A 0.138(14) 0.163(13) 0.179(17) -0.053(12) 0.071(13) -0.046(12) _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 O1 C20 1.363(6) . ? O1 C25 1.430(8) . ? O2 C29 1.378(7) . ? O2 C34 1.429(9) . ? O3 C43 1.403(10) . ? O3 C38 1.406(7) . ? O4 C47 1.385(7) . ? O4 C52 1.386(9) . ? C1 C2 1.396(7) . ? C1 C14 1.398(7) . ? C1 C17 1.493(7) . ? C2 C3 1.376(8) . ? C2 H2 0.9300 . ? C3 C4 1.393(7) . ? C3 C26 1.513(8) . ? C4 C5 1.422(7) . ? C4 C15 1.435(7) . ? C5 C6 1.371(8) . ? C5 H5 0.9300 . ? C6 C7 1.396(7) . ? C6 H6 0.9300 . ? C7 C8 1.419(7) . ? C7 C16 1.434(7) . ? C8 C9 1.398(7) . ? C8 C35 1.474(7) . ? C9 C10 1.371(7) . ? C9 H9 0.9300 . ? C10 C11 1.423(8) . ? C10 C44 1.487(8) . ? C11 C12 1.413(7) . ? C11 C16 1.415(7) . ? C12 C13 1.321(7) . ? C12 H12 0.9300 . ? C13 C14 1.423(7) . ? C13 H13 0.9300 . ? C14 C15 1.448(7) . ? C15 C16 1.417(6) . ? C17 C22 1.378(8) . ? C17 C18 1.391(8) . ? C18 C19 1.417(8) . ? C18 C24 1.494(9) . ? C19 C20 1.364(8) . ? C19 H19 0.9300 . ? C20 C21 1.359(8) . ? C21 C22 1.388(8) . ? C21 H21 0.9300 . ? C22 C23 1.514(8) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C31 1.384(8) . ? C26 C27 1.399(8) . ? C27 C28 1.383(8) . ? C27 C33 1.495(9) . ? C28 C29 1.359(8) . ? C28 H28 0.9300 . ? C29 C30 1.342(9) . ? C30 C31 1.393(8) . ? C30 H30 0.9300 . ? C31 C32 1.516(9) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C40 1.409(8) . ? C35 C36 1.418(8) . ? C36 C37 1.385(8) . ? C36 C42 1.504(9) . ? C37 C38 1.350(9) . ? C37 H37 0.9300 . ? C38 C39 1.378(9) . ? C39 C40 1.361(8) . ? C39 H39 0.9300 . ? C40 C41 1.524(9) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 C45 1.397(8) . ? C44 C49 1.413(8) . ? C45 C46 1.415(8) . ? C45 C51 1.502(9) . ? C46 C47 1.376(9) . ? C46 H46 0.9300 . ? C47 C48 1.393(9) . ? C48 C49 1.383(8) . ? C48 H48 0.9300 . ? C49 C50 1.501(9) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? O6 C63 1.371(5) . ? O6 C60 1.386(5) . ? O6 H63A 1.1827 . ? N1 C62 1.422(6) . ? N1 C61 1.423(6) . ? N1 H1B 0.8999 . ? N1 H1AB 0.6961 . ? C60 C61 1.491(5) . ? C60 H60A 0.9601 . ? C60 H60B 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9599 . ? C61 H1AB 0.8160 . ? C61 H61A 1.5174 . ? C62 C63 1.492(6) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62A 1.0731 . ? C62 H62B 1.4727 . ? C63 H63A 0.9600 . ? C63 H63B 0.9601 . ? C63 H62A 0.6919 . ? C63 H62B 1.4653 . ? O6A C60A 1.419(7) . ? O6A C63A 1.420(7) . ? O6A H60B 1.4420 . ? N1A C61A 1.433(7) . ? N1A C62A 1.448(7) . ? N1A H61A 1.4678 . ? N1A H61B 1.0919 . ? N1A H1AB 0.8999 . ? C60A C61A 1.515(7) . ? C60A H60A 1.3897 . ? C60A H60B 0.8660 . ? C60A H60A 0.9600 . ? C60A H60B 0.9600 . ? C61A H60B 1.0660 . ? C61A H61A 1.5163 . ? C61A H61B 1.4099 . ? C61A H61A 0.9599 . ? C61A H61B 0.9600 . ? C62A C63A 1.528(7) . ? C62A H62A 0.9600 . ? C62A H62B 0.9600 . ? C63A H63A 0.9600 . ? C63A H63B 0.9600 . ? O5 C59 1.207(6) . ? C59 C53 1.487(5) . ? C59 H59A 0.9300 . ? C53 C54 1.3900 . ? C53 C58 1.3900 . ? C54 C55 1.3900 . ? C54 H54A 0.9300 . ? C55 C56 1.3900 . ? C55 H55A 0.9300 . ? C56 C57 1.3900 . ? C56 H56A 0.9300 . ? C57 C58 1.3900 . ? C57 H57A 0.9300 . ? C58 H58A 0.9300 . ? O5A C59A 1.207(6) . ? C59A C53A 1.489(5) . ? C59A H59B 0.9300 . ? C53A C54A 1.3900 . ? C53A C58A 1.3900 . ? C54A C55A 1.3900 . ? C54A H54B 0.9300 . ? C55A C56A 1.3900 . ? C55A H55B 0.9300 . ? C56A C57A 1.3900 . ? C56A H56B 0.9300 . ? C57A C58A 1.3900 . ? C57A H57B 0.9300 . ? C58A H58B 0.9300 . ? 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 C20 O1 C25 116.6(5) . . ? C29 O2 C34 117.8(6) . . ? C43 O3 C38 119.0(6) . . ? C47 O4 C52 117.4(6) . . ? C2 C1 C14 118.4(5) . . ? C2 C1 C17 120.1(5) . . ? C14 C1 C17 121.5(5) . . ? C3 C2 C1 124.6(5) . . ? C3 C2 H2 117.7 . . ? C1 C2 H2 117.7 . . ? C2 C3 C4 118.4(5) . . ? C2 C3 C26 119.7(5) . . ? C4 C3 C26 121.8(5) . . ? C3 C4 C5 122.9(5) . . ? C3 C4 C15 120.2(5) . . ? C5 C4 C15 116.9(5) . . ? C6 C5 C4 121.8(5) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 121.9(5) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C6 C7 C8 121.8(4) . . ? C6 C7 C16 118.8(5) . . ? C8 C7 C16 119.3(4) . . ? C9 C8 C7 118.8(4) . . ? C9 C8 C35 118.6(5) . . ? C7 C8 C35 122.6(5) . . ? C10 C9 C8 122.5(5) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C9 C10 C11 120.6(5) . . ? C9 C10 C44 119.2(5) . . ? C11 C10 C44 120.1(5) . . ? C12 C11 C16 118.0(5) . . ? C12 C11 C10 123.6(4) . . ? C16 C11 C10 118.4(4) . . ? C13 C12 C11 122.6(5) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 C13 C14 122.5(5) . . ? C12 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? C1 C14 C13 123.8(5) . . ? C1 C14 C15 119.2(5) . . ? C13 C14 C15 116.9(5) . . ? C16 C15 C4 121.2(4) . . ? C16 C15 C14 119.6(4) . . ? C4 C15 C14 119.2(5) . . ? C11 C16 C15 120.4(4) . . ? C11 C16 C7 120.4(5) . . ? C15 C16 C7 119.2(4) . . ? C22 C17 C18 119.3(5) . . ? C22 C17 C1 121.6(5) . . ? C18 C17 C1 119.0(5) . . ? C17 C18 C19 118.6(5) . . ? C17 C18 C24 121.8(5) . . ? C19 C18 C24 119.4(6) . . ? C20 C19 C18 120.5(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C21 C20 O1 115.1(5) . . ? C21 C20 C19 120.5(5) . . ? O1 C20 C19 124.4(6) . . ? C20 C21 C22 120.0(6) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C17 C22 C21 120.9(6) . . ? C17 C22 C23 119.8(5) . . ? C21 C22 C23 119.3(6) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O1 C25 H25A 109.5 . . ? O1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C26 C27 121.9(5) . . ? C31 C26 C3 118.0(5) . . ? C27 C26 C3 120.1(5) . . ? C28 C27 C26 117.5(6) . . ? C28 C27 C33 121.9(6) . . ? C26 C27 C33 120.6(6) . . ? C29 C28 C27 121.7(6) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? C30 C29 C28 119.1(6) . . ? C30 C29 O2 116.2(7) . . ? C28 C29 O2 124.7(6) . . ? C29 C30 C31 123.5(7) . . ? C29 C30 H30 118.3 . . ? C31 C30 H30 118.3 . . ? C26 C31 C30 116.1(6) . . ? C26 C31 C32 123.5(5) . . ? C30 C31 C32 120.3(6) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C27 C33 H33A 109.5 . . ? C27 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C27 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O2 C34 H34A 109.5 . . ? O2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C40 C35 C36 118.2(5) . . ? C40 C35 C8 122.1(5) . . ? C36 C35 C8 119.6(5) . . ? C37 C36 C35 119.0(6) . . ? C37 C36 C42 121.1(6) . . ? C35 C36 C42 119.8(5) . . ? C38 C37 C36 121.6(7) . . ? C38 C37 H37 119.2 . . ? C36 C37 H37 119.2 . . ? C37 C38 C39 120.0(6) . . ? C37 C38 O3 123.8(7) . . ? C39 C38 O3 116.1(6) . . ? C40 C39 C38 121.0(6) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C39 C40 C35 120.2(6) . . ? C39 C40 C41 119.2(6) . . ? C35 C40 C41 120.6(5) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C36 C42 H42A 109.5 . . ? C36 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C36 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O3 C43 H43A 109.5 . . ? O3 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O3 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 C49 117.8(5) . . ? C45 C44 C10 121.6(5) . . ? C49 C44 C10 120.5(5) . . ? C44 C45 C46 120.4(6) . . ? C44 C45 C51 121.1(6) . . ? C46 C45 C51 118.5(6) . . ? C47 C46 C45 120.0(6) . . ? C47 C46 H46 120.0 . . ? C45 C46 H46 120.0 . . ? C46 C47 O4 124.1(7) . . ? C46 C47 C48 120.6(6) . . ? O4 C47 C48 115.3(6) . . ? C49 C48 C47 119.3(6) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C48 C49 C44 121.7(6) . . ? C48 C49 C50 117.7(6) . . ? C44 C49 C50 120.6(5) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C45 C51 H51A 109.5 . . ? C45 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C45 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O4 C52 H52A 109.5 . . ? O4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C63 O6 C60 118.9(5) . . ? C63 O6 H63A 82.7 . . ? C60 O6 H63A 149.6 . . ? C62 N1 C61 115.2(5) . . ? C62 N1 H1B 108.3 . . ? C61 N1 H1B 106.4 . . ? C62 N1 H1AB 136.3 . . ? C61 N1 H1AB 21.5 . . ? H1B N1 H1AB 92.2 . . ? O6 C60 C61 117.0(5) . . ? O6 C60 H60A 106.2 . . ? C61 C60 H60A 110.7 . . ? O6 C60 H60B 108.6 . . ? C61 C60 H60B 106.7 . . ? H60A C60 H60B 107.3 . . ? N1 C61 C60 116.0(5) . . ? N1 C61 H61A 110.7 . . ? C60 C61 H61A 110.4 . . ? N1 C61 H61B 106.2 . . ? C60 C61 H61B 105.8 . . ? H61A C61 H61B 107.2 . . ? N1 C61 H1AB 18.2 . . ? C60 C61 H1AB 131.4 . . ? H61A C61 H1AB 107.2 . . ? H61B C61 H1AB 90.9 . . ? N1 C61 H61A 150.6 . . ? C60 C61 H61A 70.3 . . ? H61A C61 H61A 45.5 . . ? H61B C61 H61A 98.7 . . ? H1AB C61 H61A 152.6 . . ? N1 C62 C63 116.2(5) . . ? N1 C62 H62A 108.4 . . ? C63 C62 H62A 110.1 . . ? N1 C62 H62B 108.4 . . ? C63 C62 H62B 105.9 . . ? H62A C62 H62B 107.5 . . ? N1 C62 H62A 99.0 . . ? C63 C62 H62A 25.1 . . ? H62A C62 H62A 101.3 . . ? H62B C62 H62A 130.7 . . ? N1 C62 H62B 86.7 . . ? C63 C62 H62B 59.2 . . ? H62A C62 H62B 164.8 . . ? H62B C62 H62B 68.4 . . ? H62A C62 H62B 73.3 . . ? O6 C63 C62 118.0(5) . . ? O6 C63 H63A 111.2 . . ? C62 C63 H63A 109.7 . . ? O6 C63 H63B 104.0 . . ? C62 C63 H63B 105.7 . . ? H63A C63 H63B 107.4 . . ? O6 C63 H62A 106.2 . . ? C62 C63 H62A 41.2 . . ? H63A C63 H62A 141.5 . . ? H63B C63 H62A 70.8 . . ? O6 C63 H62B 67.7 . . ? C62 C63 H62B 59.7 . . ? H63A C63 H62B 102.1 . . ? H63B C63 H62B 150.4 . . ? H62A C63 H62B 84.0 . . ? C60A O6A C63A 111.2(8) . . ? C60A O6A H60B 35.2 . . ? C63A O6A H60B 99.6 . . ? C61A N1A C62A 112.0(8) . . ? C61A N1A H61A 63.0 . . ? C62A N1A H61A 102.9 . . ? C61A N1A H61B 66.3 . . ? C62A N1A H61B 175.5 . . ? H61A N1A H61B 72.6 . . ? C61A N1A H1AB 127.2 . . ? C62A N1A H1AB 100.0 . . ? H61A N1A H1AB 69.8 . . ? H61B N1A H1AB 78.5 . . ? O6A C60A C61A 112.2(7) . . ? O6A C60A H60A 84.0 . . ? C61A C60A H60A 68.5 . . ? O6A C60A H60B 73.8 . . ? C61A C60A H60B 43.4 . . ? H60A C60A H60B 83.1 . . ? O6A C60A H60A 107.0 . . ? C61A C60A H60A 112.1 . . ? H60A C60A H60A 63.1 . . ? H60B C60A H60A 145.5 . . ? O6A C60A H60B 122.3 . . ? C61A C60A H60B 94.8 . . ? H60A C60A H60B 153.3 . . ? H60B C60A H60B 99.2 . . ? H60A C60A H60B 108.1 . . ? N1A C61A C60A 113.7(7) . . ? N1A C61A H60B 103.8 . . ? C60A C61A H60B 33.9 . . ? N1A C61A H61A 59.6 . . ? C60A C61A H61A 145.6 . . ? H60B C61A H61A 111.9 . . ? N1A C61A H61B 45.2 . . ? C60A C61A H61B 138.8 . . ? H60B C61A H61B 148.0 . . ? H61A C61A H61B 63.7 . . ? N1A C61A H61A 100.6 . . ? C60A C61A H61A 113.2 . . ? H60B C61A H61A 84.6 . . ? H61A C61A H61A 45.5 . . ? H61B C61A H61A 106.2 . . ? N1A C61A H61B 98.9 . . ? C60A C61A H61B 119.9 . . ? H60B C61A H61B 151.4 . . ? H61A C61A H61B 94.4 . . ? H61B C61A H61B 54.3 . . ? H61A C61A H61B 108.1 . . ? N1A C62A C63A 111.2(8) . . ? N1A C62A H62A 121.6 . . ? C63A C62A H62A 93.0 . . ? N1A C62A H62B 106.9 . . ? C63A C62A H62B 116.2 . . ? H62A C62A H62B 108.0 . . ? O6A C63A C62A 110.1(8) . . ? O6A C63A H63A 96.2 . . ? C62A C63A H63A 116.6 . . ? O6A C63A H63B 105.4 . . ? C62A C63A H63B 117.8 . . ? H63A C63A H63B 108.1 . . ? O5 C59 C53 120.0(7) . . ? O5 C59 H59A 120.0 . . ? C53 C59 H59A 120.0 . . ? C54 C53 C58 120.0 . . ? C54 C53 C59 120.0(3) . . ? C58 C53 C59 119.5(3) . . ? C55 C54 C53 120.0 . . ? C55 C54 H54A 120.0 . . ? C53 C54 H54A 120.0 . . ? C54 C55 C56 120.0 . . ? C54 C55 H55A 120.0 . . ? C56 C55 H55A 120.0 . . ? C57 C56 C55 120.0 . . ? C57 C56 H56A 120.0 . . ? C55 C56 H56A 120.0 . . ? C56 C57 C58 120.0 . . ? C56 C57 H57A 120.0 . . ? C58 C57 H57A 120.0 . . ? C57 C58 C53 120.0 . . ? C57 C58 H58A 120.0 . . ? C53 C58 H58A 120.0 . . ? O5A C59A C53A 121.3(6) . . ? O5A C59A H59B 119.3 . . ? C53A C59A H59B 119.3 . . ? C54A C53A C58A 120.0 . . ? C54A C53A C59A 119.1(3) . . ? C58A C53A C59A 119.9(3) . . ? C55A C54A C53A 120.0 . . ? C55A C54A H54B 120.0 . . ? C53A C54A H54B 120.0 . . ? C54A C55A C56A 120.0 . . ? C54A C55A H55B 120.0 . . ? C56A C55A H55B 120.0 . . ? C57A C56A C55A 120.0 . . ? C57A C56A H56B 120.0 . . ? C55A C56A H56B 120.0 . . ? C56A C57A C58A 120.0 . . ? C56A C57A H57B 120.0 . . ? C58A C57A H57B 120.0 . . ? C57A C58A C53A 120.0 . . ? C57A C58A H58B 120.0 . . ? C53A C58A H58B 120.0 . . ? 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 C14 C1 C2 C3 1.3(9) . . . . ? C17 C1 C2 C3 -177.5(6) . . . . ? C1 C2 C3 C4 -1.2(9) . . . . ? C1 C2 C3 C26 174.8(6) . . . . ? C2 C3 C4 C5 -179.3(6) . . . . ? C26 C3 C4 C5 4.8(8) . . . . ? C2 C3 C4 C15 0.9(8) . . . . ? C26 C3 C4 C15 -175.0(5) . . . . ? C3 C4 C5 C6 -179.2(5) . . . . ? C15 C4 C5 C6 0.5(8) . . . . ? C4 C5 C6 C7 -1.1(9) . . . . ? C5 C6 C7 C8 -177.5(5) . . . . ? C5 C6 C7 C16 0.6(8) . . . . ? C6 C7 C8 C9 -179.2(5) . . . . ? C16 C7 C8 C9 2.7(8) . . . . ? C6 C7 C8 C35 -1.3(9) . . . . ? C16 C7 C8 C35 -179.4(5) . . . . ? C7 C8 C9 C10 -0.7(9) . . . . ? C35 C8 C9 C10 -178.7(6) . . . . ? C8 C9 C10 C11 -1.2(9) . . . . ? C8 C9 C10 C44 -177.2(6) . . . . ? C9 C10 C11 C12 -178.5(6) . . . . ? C44 C10 C11 C12 -2.5(8) . . . . ? C9 C10 C11 C16 1.1(8) . . . . ? C44 C10 C11 C16 177.0(5) . . . . ? C16 C11 C12 C13 0.8(8) . . . . ? C10 C11 C12 C13 -179.7(6) . . . . ? C11 C12 C13 C14 -1.2(9) . . . . ? C2 C1 C14 C13 -179.3(5) . . . . ? C17 C1 C14 C13 -0.5(9) . . . . ? C2 C1 C14 C15 -1.1(8) . . . . ? C17 C1 C14 C15 177.8(5) . . . . ? C12 C13 C14 C1 180.0(6) . . . . ? C12 C13 C14 C15 1.7(8) . . . . ? C3 C4 C15 C16 -179.7(5) . . . . ? C5 C4 C15 C16 0.5(7) . . . . ? C3 C4 C15 C14 -0.8(8) . . . . ? C5 C4 C15 C14 179.4(5) . . . . ? C1 C14 C15 C16 179.8(5) . . . . ? C13 C14 C15 C16 -1.8(7) . . . . ? C1 C14 C15 C4 0.8(8) . . . . ? C13 C14 C15 C4 179.2(5) . . . . ? C12 C11 C16 C15 -1.0(7) . . . . ? C10 C11 C16 C15 179.4(5) . . . . ? C12 C11 C16 C7 -179.5(5) . . . . ? C10 C11 C16 C7 1.0(8) . . . . ? C4 C15 C16 C11 -179.5(5) . . . . ? C14 C15 C16 C11 1.6(7) . . . . ? C4 C15 C16 C7 -1.0(7) . . . . ? C14 C15 C16 C7 -179.9(5) . . . . ? C6 C7 C16 C11 179.0(5) . . . . ? C8 C7 C16 C11 -2.9(7) . . . . ? C6 C7 C16 C15 0.5(7) . . . . ? C8 C7 C16 C15 178.6(5) . . . . ? C2 C1 C17 C22 -84.2(7) . . . . ? C14 C1 C17 C22 96.9(7) . . . . ? C2 C1 C17 C18 93.0(7) . . . . ? C14 C1 C17 C18 -85.8(7) . . . . ? C22 C17 C18 C19 -4.4(8) . . . . ? C1 C17 C18 C19 178.2(5) . . . . ? C22 C17 C18 C24 179.3(6) . . . . ? C1 C17 C18 C24 1.9(8) . . . . ? C17 C18 C19 C20 2.4(8) . . . . ? C24 C18 C19 C20 178.8(6) . . . . ? C25 O1 C20 C21 -170.6(6) . . . . ? C25 O1 C20 C19 10.5(9) . . . . ? C18 C19 C20 C21 1.7(9) . . . . ? C18 C19 C20 O1 -179.4(6) . . . . ? O1 C20 C21 C22 177.3(6) . . . . ? C19 C20 C21 C22 -3.7(9) . . . . ? C18 C17 C22 C21 2.5(9) . . . . ? C1 C17 C22 C21 179.8(5) . . . . ? C18 C17 C22 C23 -177.7(6) . . . . ? C1 C17 C22 C23 -0.5(9) . . . . ? C20 C21 C22 C17 1.6(9) . . . . ? C20 C21 C22 C23 -178.1(6) . . . . ? C2 C3 C26 C31 -80.2(7) . . . . ? C4 C3 C26 C31 95.6(7) . . . . ? C2 C3 C26 C27 98.8(7) . . . . ? C4 C3 C26 C27 -85.3(7) . . . . ? C31 C26 C27 C28 -3.5(8) . . . . ? C3 C26 C27 C28 177.4(5) . . . . ? C31 C26 C27 C33 178.6(6) . . . . ? C3 C26 C27 C33 -0.4(9) . . . . ? C26 C27 C28 C29 0.9(9) . . . . ? C33 C27 C28 C29 178.7(7) . . . . ? C27 C28 C29 C30 2.2(10) . . . . ? C27 C28 C29 O2 178.9(6) . . . . ? C34 O2 C29 C30 -169.8(6) . . . . ? C34 O2 C29 C28 13.4(10) . . . . ? C28 C29 C30 C31 -2.7(9) . . . . ? O2 C29 C30 C31 -179.7(6) . . . . ? C27 C26 C31 C30 3.0(8) . . . . ? C3 C26 C31 C30 -177.9(5) . . . . ? C27 C26 C31 C32 -179.2(6) . . . . ? C3 C26 C31 C32 -0.2(8) . . . . ? C29 C30 C31 C26 0.1(9) . . . . ? C29 C30 C31 C32 -177.6(6) . . . . ? C9 C8 C35 C40 77.4(8) . . . . ? C7 C8 C35 C40 -100.5(7) . . . . ? C9 C8 C35 C36 -100.9(7) . . . . ? C7 C8 C35 C36 81.2(7) . . . . ? C40 C35 C36 C37 -0.3(8) . . . . ? C8 C35 C36 C37 178.0(5) . . . . ? C40 C35 C36 C42 -176.2(6) . . . . ? C8 C35 C36 C42 2.2(8) . . . . ? C35 C36 C37 C38 0.2(9) . . . . ? C42 C36 C37 C38 176.0(6) . . . . ? C36 C37 C38 C39 -1.1(10) . . . . ? C36 C37 C38 O3 177.9(6) . . . . ? C43 O3 C38 C37 -10.3(11) . . . . ? C43 O3 C38 C39 168.7(7) . . . . ? C37 C38 C39 C40 2.1(11) . . . . ? O3 C38 C39 C40 -176.9(6) . . . . ? C38 C39 C40 C35 -2.3(11) . . . . ? C38 C39 C40 C41 178.1(7) . . . . ? C36 C35 C40 C39 1.4(9) . . . . ? C8 C35 C40 C39 -176.9(6) . . . . ? C36 C35 C40 C41 -179.0(6) . . . . ? C8 C35 C40 C41 2.7(10) . . . . ? C9 C10 C44 C45 -99.3(7) . . . . ? C11 C10 C44 C45 84.7(7) . . . . ? C9 C10 C44 C49 76.6(7) . . . . ? C11 C10 C44 C49 -99.4(7) . . . . ? C49 C44 C45 C46 4.3(8) . . . . ? C10 C44 C45 C46 -179.7(5) . . . . ? C49 C44 C45 C51 -176.4(6) . . . . ? C10 C44 C45 C51 -0.3(8) . . . . ? C44 C45 C46 C47 -1.9(9) . . . . ? C51 C45 C46 C47 178.7(6) . . . . ? C45 C46 C47 O4 178.0(5) . . . . ? C45 C46 C47 C48 0.4(9) . . . . ? C52 O4 C47 C46 -9.9(9) . . . . ? C52 O4 C47 C48 167.8(6) . . . . ? C46 C47 C48 C49 -1.4(9) . . . . ? O4 C47 C48 C49 -179.2(5) . . . . ? C47 C48 C49 C44 3.9(9) . . . . ? C47 C48 C49 C50 -177.6(6) . . . . ? C45 C44 C49 C48 -5.4(8) . . . . ? C10 C44 C49 C48 178.6(5) . . . . ? C45 C44 C49 C50 176.2(5) . . . . ? C10 C44 C49 C50 0.1(8) . . . . ? C63 O6 C60 C61 31.1(17) . . . . ? C62 N1 C61 C60 38.5(17) . . . . ? O6 C60 C61 N1 -35.6(17) . . . . ? C61 N1 C62 C63 -36.8(17) . . . . ? C60 O6 C63 C62 -29.7(19) . . . . ? N1 C62 C63 O6 32.4(19) . . . . ? C63A O6A C60A C61A 55.5(18) . . . . ? C62A N1A C61A C60A 48(2) . . . . ? O6A C60A C61A N1A -50(2) . . . . ? C61A N1A C62A C63A -52(2) . . . . ? C60A O6A C63A C62A -59.4(18) . . . . ? N1A C62A C63A O6A 57.7(19) . . . . ? O5 C59 C53 C54 168(2) . . . . ? O5 C59 C53 C58 -20(3) . . . . ? C58 C53 C54 C55 0.0 . . . . ? C59 C53 C54 C55 171.8(15) . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C57 0.0 . . . . ? C55 C56 C57 C58 0.0 . . . . ? C56 C57 C58 C53 0.0 . . . . ? C54 C53 C58 C57 0.0 . . . . ? C59 C53 C58 C57 -171.8(15) . . . . ? O5A C59A C53A C54A -4(3) . . . . ? O5A C59A C53A C58A 165(2) . . . . ? C58A C53A C54A C55A 0.0 . . . . ? C59A C53A C54A C55A 168.7(19) . . . . ? C53A C54A C55A C56A 0.0 . . . . ? C54A C55A C56A C57A 0.0 . . . . ? C55A C56A C57A C58A 0.0 . . . . ? C56A C57A C58A C53A 0.0 . . . . ? C54A C53A C58A C57A 0.0 . . . . ? C59A C53A C58A C57A -168.6(19) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.515 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.053 #END #END data_TP-NP _database_code_depnum_ccdc_archive 'CCDC 751674' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra(2,6-dimethyl-4-methoxyphenyl)pyrene ; _chemical_name_common tetra(2,6-dimethyl-4-methoxyphenyl)pyrene _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 O4, C10 H8, C8 H6' _chemical_formula_sum 'C70 H64 O4' _chemical_formula_weight 969.21 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 14.001(5) _cell_length_b 14.840(5) _cell_length_c 14.493(5) _cell_angle_alpha 90.00 _cell_angle_beta 117.081(7) _cell_angle_gamma 90.00 _cell_volume 2681.2(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2805 _cell_measurement_theta_min 2.74 _cell_measurement_theta_max 26.77 _exptl_crystal_description cubes _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_absorpt_coefficient_mu 0.073 _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 100(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 'Bruker SMART APEX' _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 13498 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0546 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4694 _reflns_number_gt 3464 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0924P)^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 4694 _refine_ls_number_parameters 369 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0768 _refine_ls_R_factor_gt 0.0571 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1452 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 O1 O 0.13978(10) 0.91121(8) 0.43078(9) 0.0361(4) Uani 1 1 d . . . O2 O -0.00071(10) 0.90685(8) -0.39955(9) 0.0348(3) Uani 1 1 d . . . C1 C 0.04304(13) 0.58155(11) 0.21127(12) 0.0244(4) Uani 1 1 d . . . C2 C 0.03367(13) 0.50062(11) 0.25447(13) 0.0259(4) Uani 1 1 d . . . H2 H 0.0426 0.5009 0.3235 0.031 Uiso 1 1 calc R . . C3 C -0.01178(13) 0.58087(11) -0.20133(12) 0.0244(4) Uani 1 1 d . . . C4 C 0.00063(13) 0.58216(11) -0.09906(12) 0.0230(4) Uani 1 1 d . . . C5 C 0.02070(14) 0.66399(11) -0.04012(12) 0.0260(4) Uani 1 1 d . . . H5 H 0.0248 0.7194 -0.0710 0.031 Uiso 1 1 calc R . . C6 C 0.03377(13) 0.66395(11) 0.05765(12) 0.0257(4) Uani 1 1 d . . . H6 H 0.0470 0.7194 0.0942 0.031 Uiso 1 1 calc R . . C7 C 0.02835(13) 0.58253(11) 0.10841(12) 0.0234(4) Uani 1 1 d . . . C8 C 0.00684(13) 0.50014(11) 0.05198(12) 0.0228(4) Uani 1 1 d . . . C9 C 0.07058(14) 0.66692(11) 0.27400(12) 0.0246(4) Uani 1 1 d . . . C10 C 0.17787(14) 0.69402(12) 0.32693(12) 0.0280(4) Uani 1 1 d . . . C11 C 0.20337(15) 0.77539(12) 0.38141(12) 0.0302(4) Uani 1 1 d . . . H11 H 0.2761 0.7942 0.4174 0.036 Uiso 1 1 calc R . . C12 C 0.12303(15) 0.82857(12) 0.38309(12) 0.0282(4) Uani 1 1 d . . . C13 C 0.01758(15) 0.80025(12) 0.33329(14) 0.0332(5) Uani 1 1 d . . . H13 H -0.0367 0.8359 0.3374 0.040 Uiso 1 1 calc R . . C14 C -0.01010(15) 0.72038(12) 0.27723(13) 0.0304(4) Uani 1 1 d . . . C15 C -0.12605(15) 0.69365(14) 0.21828(16) 0.0460(6) Uani 1 1 d . . . H15A H -0.1710 0.7393 0.2284 0.069 Uiso 1 1 calc R . . H15B H -0.1371 0.6353 0.2437 0.069 Uiso 1 1 calc R . . H15C H -0.1457 0.6889 0.1444 0.069 Uiso 1 1 calc R . . C16 C 0.26608(15) 0.63711(13) 0.32601(16) 0.0417(5) Uani 1 1 d . . . H16A H 0.3349 0.6682 0.3639 0.063 Uiso 1 1 calc R . . H16B H 0.2525 0.6269 0.2543 0.063 Uiso 1 1 calc R . . H16C H 0.2684 0.5791 0.3593 0.063 Uiso 1 1 calc R . . C17 C 0.23911(15) 0.95466(13) 0.45711(14) 0.0398(5) Uani 1 1 d . . . H17A H 0.2970 0.9213 0.5129 0.060 Uiso 1 1 calc R . . H17B H 0.2367 1.0163 0.4803 0.060 Uiso 1 1 calc R . . H17C H 0.2523 0.9565 0.3963 0.060 Uiso 1 1 calc R . . C18 C -0.00534(14) 0.66626(11) -0.25326(12) 0.0252(4) Uani 1 1 d . . . C19 C -0.10074(14) 0.71306(12) -0.31701(12) 0.0282(4) Uani 1 1 d . . . C20 C -0.09455(15) 0.79236(12) -0.36483(13) 0.0306(4) Uani 1 1 d . . . H20 H -0.1586 0.8236 -0.4084 0.037 Uiso 1 1 calc R . . C21 C 0.00310(15) 0.82665(11) -0.35019(12) 0.0278(4) Uani 1 1 d . . . C22 C 0.09694(15) 0.78105(12) -0.28784(13) 0.0313(4) Uani 1 1 d . . . H22 H 0.1641 0.8045 -0.2780 0.038 Uiso 1 1 calc R . . C23 C 0.09317(14) 0.70036(12) -0.23922(13) 0.0295(4) Uani 1 1 d . . . C24 C 0.19626(15) 0.65123(14) -0.17340(16) 0.0451(5) Uani 1 1 d . . . H24A H 0.1983 0.6347 -0.1071 0.068 Uiso 1 1 calc R . . H24B H 0.2573 0.6904 -0.1609 0.068 Uiso 1 1 calc R . . H24C H 0.2002 0.5966 -0.2095 0.068 Uiso 1 1 calc R . . C25 C -0.20748(15) 0.67727(14) -0.33409(16) 0.0413(5) Uani 1 1 d . . . H25A H -0.2639 0.7198 -0.3767 0.062 Uiso 1 1 calc R . . H25B H -0.2079 0.6695 -0.2671 0.062 Uiso 1 1 calc R . . H25C H -0.2205 0.6190 -0.3696 0.062 Uiso 1 1 calc R . . C26 C 0.09862(15) 0.95154(13) -0.37231(14) 0.0362(5) Uani 1 1 d . . . H26A H 0.1348 0.9627 -0.2975 0.054 Uiso 1 1 calc R . . H26B H 0.0851 1.0091 -0.4094 0.054 Uiso 1 1 calc R . . H26C H 0.1442 0.9136 -0.3913 0.054 Uiso 1 1 calc R . . C27 C -0.1808(3) 0.5658(2) 0.44611(18) 0.0723(8) Uani 1 1 d . . . H27 H -0.2406 0.6047 0.4280 0.087 Uiso 1 1 calc R . . C28 C -0.0829(2) 0.60179(19) 0.47431(17) 0.0623(7) Uani 1 1 d . . . H28 H -0.0752 0.6655 0.4754 0.075 Uiso 1 1 calc R . . C29 C 0.0063(2) 0.54807(17) 0.50149(14) 0.0518(6) Uani 1 1 d . . . C30 C 0.1103(2) 0.58409(18) 0.53129(16) 0.0603(7) Uani 1 1 d . . . H30 H 0.1200 0.6476 0.5333 0.072 Uiso 1 1 calc R . . C31 C 0.1964(2) 0.5286(2) 0.55709(16) 0.0701(8) Uani 1 1 d . . . H31 H 0.2658 0.5529 0.5769 0.084 Uiso 1 1 calc R . . C32 C -0.0071(3) 0.0061(2) -0.01974(16) 0.0322(12) Uani 0.50 1 d PGD A -1 C33 C 0.0373(3) -0.06943(19) 0.04166(19) 0.0346(9) Uani 0.50 1 d PG A -1 H33A H 0.0625(12) -0.125(3) 0.0120(13) 0.042 Uiso 0.50 1 d PR A -1 C34 C 0.0485(2) -0.07240(16) 0.14196(19) 0.0343(9) Uani 0.50 1 d PG A -1 H34A H 0.0795(12) -0.125(2) 0.1849(17) 0.041 Uiso 0.50 1 d PR A -1 C35 C 0.0154(3) 0.00020(19) 0.18086(16) 0.037(2) Uani 0.50 1 d PG A -1 H35A H 0.0241(6) -0.0021(3) 0.259(3) 0.045 Uiso 0.50 1 d PR A -1 C36 C -0.0290(2) 0.07577(15) 0.11946(19) 0.0274(8) Uani 0.50 1 d PG A -1 H36A H -0.0473(9) 0.1158(19) 0.1409(11) 0.033 Uiso 0.50 1 d PR A -1 C37 C -0.0402(2) 0.07875(17) 0.01916(18) 0.0386(11) Uani 0.50 1 d PG A -1 H37A H -0.0681(15) 0.126(3) -0.020(2) 0.046 Uiso 0.50 1 d PR A -1 C38 C -0.0160(4) 0.0045(3) -0.1240(4) 0.0418(12) Uani 0.50 1 d PD A -1 C39 C -0.0254(6) 0.0008(4) -0.2076(6) 0.0384(16) Uani 0.50 1 d PD A -1 H39A H -0.0331 -0.0021 -0.2761 0.046 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0418(8) 0.0297(8) 0.0370(7) -0.0110(5) 0.0182(6) -0.0055(6) O2 0.0413(8) 0.0281(7) 0.0369(7) 0.0105(5) 0.0196(6) 0.0031(6) C1 0.0240(9) 0.0265(10) 0.0226(9) -0.0002(7) 0.0105(7) 0.0007(7) C2 0.0278(9) 0.0294(10) 0.0232(9) 0.0003(7) 0.0140(7) 0.0019(7) C3 0.0252(9) 0.0253(10) 0.0236(9) 0.0020(7) 0.0119(7) 0.0003(7) C4 0.0228(9) 0.0244(10) 0.0222(9) 0.0014(7) 0.0106(7) 0.0019(7) C5 0.0295(10) 0.0207(9) 0.0287(9) 0.0029(7) 0.0141(8) -0.0004(7) C6 0.0275(10) 0.0236(10) 0.0263(9) -0.0013(7) 0.0126(8) -0.0009(7) C7 0.0209(9) 0.0260(10) 0.0230(9) -0.0016(7) 0.0098(7) -0.0003(7) C8 0.0226(9) 0.0257(9) 0.0217(8) 0.0001(7) 0.0115(7) 0.0008(7) C9 0.0310(10) 0.0250(9) 0.0201(8) 0.0005(7) 0.0135(7) 0.0003(7) C10 0.0302(10) 0.0287(10) 0.0241(9) 0.0004(7) 0.0115(8) 0.0014(8) C11 0.0283(10) 0.0344(11) 0.0235(9) -0.0008(8) 0.0079(7) -0.0031(8) C12 0.0358(11) 0.0270(10) 0.0235(9) -0.0034(7) 0.0149(8) -0.0023(8) C13 0.0327(11) 0.0348(11) 0.0371(10) -0.0070(8) 0.0202(9) 0.0013(8) C14 0.0317(10) 0.0350(11) 0.0294(9) -0.0056(8) 0.0180(8) -0.0033(8) C15 0.0311(11) 0.0495(13) 0.0615(14) -0.0203(10) 0.0248(10) -0.0040(9) C16 0.0284(10) 0.0414(12) 0.0488(12) -0.0077(9) 0.0120(9) 0.0029(9) C17 0.0431(12) 0.0308(11) 0.0392(11) -0.0064(9) 0.0132(9) -0.0059(9) C18 0.0326(10) 0.0255(9) 0.0206(8) -0.0002(7) 0.0147(8) 0.0017(7) C19 0.0287(10) 0.0305(10) 0.0250(9) -0.0020(7) 0.0120(8) 0.0004(8) C20 0.0289(10) 0.0323(11) 0.0284(9) 0.0047(8) 0.0113(8) 0.0070(8) C21 0.0377(11) 0.0253(10) 0.0240(9) 0.0042(7) 0.0172(8) 0.0036(8) C22 0.0300(10) 0.0343(11) 0.0339(10) 0.0064(8) 0.0182(8) -0.0009(8) C23 0.0303(10) 0.0322(11) 0.0280(9) 0.0073(8) 0.0149(8) 0.0045(8) C24 0.0339(11) 0.0445(13) 0.0555(13) 0.0221(10) 0.0192(10) 0.0052(9) C25 0.0296(11) 0.0400(12) 0.0505(12) 0.0061(9) 0.0150(9) 0.0022(9) C26 0.0436(12) 0.0325(11) 0.0373(10) 0.0061(9) 0.0225(9) -0.0014(9) C27 0.093(2) 0.089(2) 0.0427(14) 0.0163(13) 0.0376(14) 0.0392(18) C28 0.092(2) 0.0626(17) 0.0443(14) 0.0066(11) 0.0409(14) 0.0190(15) C29 0.0757(17) 0.0624(14) 0.0250(10) 0.0027(10) 0.0297(11) 0.0162(14) C30 0.087(2) 0.0643(17) 0.0337(12) -0.0040(11) 0.0312(13) -0.0057(15) C31 0.0694(18) 0.108(3) 0.0328(13) 0.0060(14) 0.0232(12) 0.0083(17) C32 0.025(2) 0.040(2) 0.025(4) 0.003(3) 0.006(2) -0.0043(17) C33 0.028(2) 0.037(3) 0.033(2) -0.007(2) 0.0093(19) 0.0053(18) C34 0.035(2) 0.036(2) 0.028(2) -0.0001(18) 0.0107(16) 0.0065(18) C35 0.034(4) 0.057(5) 0.021(4) -0.002(3) 0.012(3) -0.001(3) C36 0.0253(19) 0.030(2) 0.0244(18) -0.0051(15) 0.0093(15) -0.0044(15) C37 0.032(2) 0.045(3) 0.029(2) 0.0076(19) 0.0045(19) -0.0149(19) C38 0.035(2) 0.047(3) 0.040(3) 0.005(3) 0.013(2) -0.010(2) C39 0.035(3) 0.033(4) 0.042(3) -0.0057(19) 0.014(2) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C12 1.374(2) . ? O1 C17 1.419(2) . ? O2 C21 1.377(2) . ? O2 C26 1.425(2) . ? C1 C2 1.388(2) . ? C1 C7 1.409(2) . ? C1 C9 1.504(2) . ? C2 C3 1.391(2) 3_565 ? C2 H2 0.9500 . ? C3 C2 1.391(2) 3_565 ? C3 C4 1.412(2) . ? C3 C18 1.497(2) . ? C4 C8 1.426(2) 3_565 ? C4 C5 1.437(2) . ? C5 C6 1.344(2) . ? C5 H5 0.9500 . ? C6 C7 1.434(2) . ? C6 H6 0.9500 . ? C7 C8 1.425(2) . ? C8 C4 1.426(2) 3_565 ? C8 C8 1.430(3) 3_565 ? C9 C14 1.398(2) . ? C9 C10 1.399(2) . ? C10 C11 1.397(2) . ? C10 C16 1.501(3) . ? C11 C12 1.383(3) . ? C11 H11 0.9500 . ? C12 C13 1.381(3) . ? C13 C14 1.389(2) . ? C13 H13 0.9500 . ? C14 C15 1.503(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.394(3) . ? C18 C19 1.413(2) . ? C19 C20 1.388(2) . ? C19 C25 1.497(3) . ? C20 C21 1.382(3) . ? C20 H20 0.9500 . ? C21 C22 1.385(2) . ? C22 C23 1.402(2) . ? C22 H22 0.9500 . ? C23 C24 1.507(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.350(4) . ? C27 C31 1.415(4) 3_566 ? C27 H27 0.9500 . ? C28 C29 1.379(3) . ? C28 H28 0.9500 . ? C29 C30 1.422(4) . ? C29 C29 1.436(5) 3_566 ? C30 C31 1.364(4) . ? C30 H30 0.9500 . ? C31 C27 1.415(4) 3_566 ? C31 H31 0.9500 . ? C32 C33 1.3900 . ? C32 C37 1.3900 . ? C32 C38 1.458(5) . ? C33 C34 1.3900 . ? C33 H33A 1.0585 . ? C34 C35 1.3900 . ? C34 H34A 0.9728 . ? C35 C36 1.3900 . ? C35 H35A 1.0780 . ? C36 C37 1.3900 . ? C36 H36A 0.7663 . ? C37 H37A 0.8760 . ? C38 C39 1.159(6) . ? C39 H39A 0.9500 . ? 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 C12 O1 C17 117.57(14) . . ? C21 O2 C26 117.15(13) . . ? C2 C1 C7 119.21(15) . . ? C2 C1 C9 120.48(15) . . ? C7 C1 C9 120.31(14) . . ? C1 C2 C3 123.01(16) . 3_565 ? C1 C2 H2 118.5 . . ? C3 C2 H2 118.5 3_565 . ? C2 C3 C4 118.94(15) 3_565 . ? C2 C3 C18 120.40(15) 3_565 . ? C4 C3 C18 120.63(14) . . ? C3 C4 C8 119.35(15) . 3_565 ? C3 C4 C5 122.20(15) . . ? C8 C4 C5 118.45(15) 3_565 . ? C6 C5 C4 121.50(15) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 121.85(15) . . ? C5 C6 H6 119.1 . . ? C7 C6 H6 119.1 . . ? C1 C7 C8 119.29(15) . . ? C1 C7 C6 122.35(15) . . ? C8 C7 C6 118.37(15) . . ? C7 C8 C4 120.18(15) . 3_565 ? C7 C8 C8 119.94(18) . 3_565 ? C4 C8 C8 119.88(18) 3_565 3_565 ? C14 C9 C10 120.04(16) . . ? C14 C9 C1 120.63(15) . . ? C10 C9 C1 119.31(15) . . ? C11 C10 C9 119.51(16) . . ? C11 C10 C16 119.45(16) . . ? C9 C10 C16 121.04(16) . . ? C12 C11 C10 120.15(17) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? O1 C12 C13 115.56(16) . . ? O1 C12 C11 124.32(16) . . ? C13 C12 C11 120.11(16) . . ? C12 C13 C14 120.85(17) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C13 C14 C9 119.29(17) . . ? C13 C14 C15 119.95(17) . . ? C9 C14 C15 120.73(16) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16A 109.5 . . ? C10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 119.66(16) . . ? C23 C18 C3 121.04(15) . . ? C19 C18 C3 119.30(16) . . ? C20 C19 C18 119.20(16) . . ? C20 C19 C25 120.19(16) . . ? C18 C19 C25 120.61(16) . . ? C21 C20 C19 121.18(16) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? O2 C21 C20 115.90(15) . . ? O2 C21 C22 124.19(16) . . ? C20 C21 C22 119.91(16) . . ? C21 C22 C23 120.22(17) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C18 C23 C22 119.83(16) . . ? C18 C23 C24 121.03(16) . . ? C22 C23 C24 119.13(16) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C19 C25 H25A 109.5 . . ? C19 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C19 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O2 C26 H26A 109.5 . . ? O2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C31 121.5(3) . 3_566 ? C28 C27 H27 119.3 . . ? C31 C27 H27 119.3 3_566 . ? C27 C28 C29 121.4(3) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C28 C29 C30 122.6(3) . . ? C28 C29 C29 118.9(3) . 3_566 ? C30 C29 C29 118.5(3) . 3_566 ? C31 C30 C29 120.8(3) . . ? C31 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C30 C31 C27 119.0(3) . 3_566 ? C30 C31 H31 120.5 . . ? C27 C31 H31 120.5 3_566 . ? C33 C32 C37 120.0 . . ? C33 C32 C38 116.9(3) . . ? C37 C32 C38 123.1(3) . . ? C34 C33 C32 120.0 . . ? C35 C34 C33 120.0 . . ? C34 C35 C36 120.0 . . ? C35 C36 C37 120.0 . . ? C36 C37 C32 120.0 . . ? C39 C38 C32 177.8(6) . . ? C38 C39 H39A 180.0 . . ? 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 C7 C1 C2 C3 1.0(3) . . . 3_565 ? C9 C1 C2 C3 -177.88(16) . . . 3_565 ? C2 C3 C4 C8 1.6(2) 3_565 . . 3_565 ? C18 C3 C4 C8 179.45(15) . . . 3_565 ? C2 C3 C4 C5 -178.44(15) 3_565 . . . ? C18 C3 C4 C5 -0.6(2) . . . . ? C3 C4 C5 C6 -179.09(16) . . . . ? C8 C4 C5 C6 0.9(2) 3_565 . . . ? C4 C5 C6 C7 0.0(3) . . . . ? C2 C1 C7 C8 -1.5(2) . . . . ? C9 C1 C7 C8 177.33(15) . . . . ? C2 C1 C7 C6 178.18(15) . . . . ? C9 C1 C7 C6 -3.0(2) . . . . ? C5 C6 C7 C1 179.32(16) . . . . ? C5 C6 C7 C8 -1.0(2) . . . . ? C1 C7 C8 C4 0.5(2) . . . 3_565 ? C6 C7 C8 C4 -179.17(15) . . . 3_565 ? C1 C7 C8 C8 -179.17(18) . . . 3_565 ? C6 C7 C8 C8 1.1(3) . . . 3_565 ? C2 C1 C9 C14 -88.0(2) . . . . ? C7 C1 C9 C14 93.2(2) . . . . ? C2 C1 C9 C10 93.9(2) . . . . ? C7 C1 C9 C10 -84.9(2) . . . . ? C14 C9 C10 C11 -1.0(2) . . . . ? C1 C9 C10 C11 177.07(14) . . . . ? C14 C9 C10 C16 179.04(16) . . . . ? C1 C9 C10 C16 -2.8(2) . . . . ? C9 C10 C11 C12 0.1(2) . . . . ? C16 C10 C11 C12 -179.94(16) . . . . ? C17 O1 C12 C13 -162.61(15) . . . . ? C17 O1 C12 C11 16.4(2) . . . . ? C10 C11 C12 O1 -177.16(15) . . . . ? C10 C11 C12 C13 1.8(3) . . . . ? O1 C12 C13 C14 176.21(15) . . . . ? C11 C12 C13 C14 -2.8(3) . . . . ? C12 C13 C14 C9 1.9(3) . . . . ? C12 C13 C14 C15 -176.27(17) . . . . ? C10 C9 C14 C13 0.0(3) . . . . ? C1 C9 C14 C13 -178.05(15) . . . . ? C10 C9 C14 C15 178.20(17) . . . . ? C1 C9 C14 C15 0.1(3) . . . . ? C2 C3 C18 C23 -96.9(2) 3_565 . . . ? C4 C3 C18 C23 85.2(2) . . . . ? C2 C3 C18 C19 83.4(2) 3_565 . . . ? C4 C3 C18 C19 -94.47(19) . . . . ? C23 C18 C19 C20 0.1(2) . . . . ? C3 C18 C19 C20 179.80(15) . . . . ? C23 C18 C19 C25 179.37(16) . . . . ? C3 C18 C19 C25 -0.9(2) . . . . ? C18 C19 C20 C21 -0.7(3) . . . . ? C25 C19 C20 C21 -179.99(17) . . . . ? C26 O2 C21 C20 169.67(15) . . . . ? C26 O2 C21 C22 -9.5(2) . . . . ? C19 C20 C21 O2 -178.44(15) . . . . ? C19 C20 C21 C22 0.8(3) . . . . ? O2 C21 C22 C23 178.95(15) . . . . ? C20 C21 C22 C23 -0.2(3) . . . . ? C19 C18 C23 C22 0.4(3) . . . . ? C3 C18 C23 C22 -179.25(15) . . . . ? C19 C18 C23 C24 -178.82(16) . . . . ? C3 C18 C23 C24 1.5(3) . . . . ? C21 C22 C23 C18 -0.4(3) . . . . ? C21 C22 C23 C24 178.88(17) . . . . ? C31 C27 C28 C29 -0.2(3) 3_566 . . . ? C27 C28 C29 C30 179.9(2) . . . . ? C27 C28 C29 C29 0.6(3) . . . 3_566 ? C28 C29 C30 C31 -179.6(2) . . . . ? C29 C29 C30 C31 -0.4(3) 3_566 . . . ? C29 C30 C31 C27 -0.1(3) . . . 3_566 ? C37 C32 C33 C34 0.0 . . . . ? C38 C32 C33 C34 179.9(4) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C32 0.0 . . . . ? C33 C32 C37 C36 0.0 . . . . ? C38 C32 C37 C36 -179.9(4) . . . . ? C33 C32 C38 C39 63(19) . . . . ? C37 C32 C38 C39 -117(19) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.305 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.052 #END data_TP-FB _database_code_depnum_ccdc_archive 'CCDC 751675' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra(2,6-dimethyl-4-methoxyphenyl)pyrene ; _chemical_name_common tetra(2,6-dimethyl-4-methoxyphenyl)pyrene _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 O4, C13 H10, C6 H6' _chemical_formula_sum 'C71 H66 O4' _chemical_formula_weight 983.24 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 14.4322(15) _cell_length_b 14.1880(14) _cell_length_c 14.8641(15) _cell_angle_alpha 90.00 _cell_angle_beta 118.016(2) _cell_angle_gamma 90.00 _cell_volume 2687.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1628 _cell_measurement_theta_min 2.17 _cell_measurement_theta_max 22.14 _exptl_crystal_description 'SMALL CUBES' _exptl_crystal_colour 'color less' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.074 _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 100(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 'Bruker SMART APEX' _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 13616 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4674 _reflns_number_gt 3038 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0640P)^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 4674 _refine_ls_number_parameters 397 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.0903 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1432 _refine_ls_wR_factor_gt 0.1279 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.024 _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 O1 O 0.10797(12) 0.04461(10) 0.84482(11) 0.0401(4) Uani 1 1 d . . . O2 O 0.09421(14) 0.90492(11) 1.02569(13) 0.0562(5) Uani 1 1 d . . . C1 C 0.28885(16) 0.40632(14) 0.95188(15) 0.0284(5) Uani 1 1 d . . . C2 C 0.24184(17) 0.48875(14) 0.96247(15) 0.0307(5) Uani 1 1 d . . . H2A H 0.1717 0.4856 0.9519 0.037 Uiso 1 1 calc R . . C3 C 0.29297(16) 0.57469(14) 0.98770(15) 0.0290(5) Uani 1 1 d . . . C4 C 0.39625(15) 0.58074(13) 1.00111(15) 0.0275(5) Uani 1 1 d . . . C5 C 0.44732(15) 0.49740(14) 0.99275(15) 0.0272(5) Uani 1 1 d . . . C6 C 0.39308(16) 0.41013(13) 0.96829(15) 0.0269(5) Uani 1 1 d . . . C7 C 0.44784(16) 0.32776(14) 0.96165(15) 0.0303(5) Uani 1 1 d . . . H7A H 0.4130 0.2686 0.9466 0.036 Uiso 1 1 calc R . . C8 C 0.45347(16) 0.66776(13) 1.02392(15) 0.0301(5) Uani 1 1 d . . . H8A H 0.4203 0.7239 1.0289 0.036 Uiso 1 1 calc R . . C9 C 0.23090(15) 0.31477(14) 0.92135(16) 0.0290(5) Uani 1 1 d . . . C10 C 0.17840(17) 0.28951(14) 0.81848(17) 0.0330(5) Uani 1 1 d . . . C11 C 0.13381(16) 0.20013(14) 0.79056(17) 0.0328(5) Uani 1 1 d . . . H11A H 0.0972 0.1831 0.7206 0.039 Uiso 1 1 calc R . . C12 C 0.14266(16) 0.13628(14) 0.86435(16) 0.0318(5) Uani 1 1 d . . . C13 C 0.19028(16) 0.16278(14) 0.96610(16) 0.0330(5) Uani 1 1 d . . . H13A H 0.1920 0.1200 1.0161 0.040 Uiso 1 1 calc R . . C14 C 0.23526(16) 0.25111(14) 0.99530(16) 0.0316(5) Uani 1 1 d . . . C15 C 0.16882(19) 0.35755(16) 0.73666(17) 0.0454(6) Uani 1 1 d . . . H15A H 0.1257 0.3293 0.6695 0.068 Uiso 1 1 calc R . . H15B H 0.2388 0.3716 0.7447 0.068 Uiso 1 1 calc R . . H15C H 0.1358 0.4159 0.7425 0.068 Uiso 1 1 calc R . . C16 C 0.2909(2) 0.27841(17) 1.10657(17) 0.0456(6) Uani 1 1 d . . . H16A H 0.2779 0.2304 1.1467 0.068 Uiso 1 1 calc R . . H16B H 0.2645 0.3394 1.1154 0.068 Uiso 1 1 calc R . . H16C H 0.3665 0.2831 1.1297 0.068 Uiso 1 1 calc R . . C17 C 0.0673(2) 0.01457(16) 0.74167(18) 0.0486(7) Uani 1 1 d . . . H17A H 0.0029 0.0496 0.6988 0.073 Uiso 1 1 calc R . . H17B H 0.0516 -0.0530 0.7370 0.073 Uiso 1 1 calc R . . H17C H 0.1193 0.0265 0.7182 0.073 Uiso 1 1 calc R . . C18 C 0.23971(16) 0.66122(13) 0.99987(16) 0.0283(5) Uani 1 1 d . . . C19 C 0.17653(17) 0.71628(15) 0.91455(17) 0.0362(6) Uani 1 1 d . . . C20 C 0.1306(2) 0.79708(16) 0.92769(18) 0.0445(6) Uani 1 1 d . . . H20A H 0.0878 0.8347 0.8701 0.053 Uiso 1 1 calc R . . C21 C 0.14575(19) 0.82409(15) 1.02300(18) 0.0389(6) Uani 1 1 d . . . C22 C 0.20715(18) 0.77039(15) 1.10677(17) 0.0370(6) Uani 1 1 d . . . H22A H 0.2176 0.7891 1.1722 0.044 Uiso 1 1 calc R . . C23 C 0.25435(17) 0.68830(15) 1.09605(16) 0.0351(5) Uani 1 1 d . . . C24 C 0.1573(2) 0.68738(18) 0.81006(17) 0.0482(7) Uani 1 1 d . . . H24A H 0.1121 0.7341 0.7601 0.072 Uiso 1 1 calc R . . H24B H 0.1228 0.6257 0.7932 0.072 Uiso 1 1 calc R . . H24C H 0.2244 0.6836 0.8086 0.072 Uiso 1 1 calc R . . C25 C 0.3185(2) 0.62886(19) 1.18912(18) 0.0573(8) Uani 1 1 d . . . H25A H 0.3079 0.6512 1.2460 0.086 Uiso 1 1 calc R . . H25B H 0.3930 0.6339 1.2073 0.086 Uiso 1 1 calc R . . H25C H 0.2963 0.5629 1.1744 0.086 Uiso 1 1 calc R . . C26 C 0.1030(2) 0.93341(17) 1.1206(2) 0.0550(7) Uani 1 1 d . . . H26A H 0.0754 0.8837 1.1472 0.082 Uiso 1 1 calc R . . H26B H 0.0627 0.9915 1.1115 0.082 Uiso 1 1 calc R . . H26C H 0.1769 0.9448 1.1688 0.082 Uiso 1 1 calc R . . C27 C 0.4021(2) -0.01339(18) 0.9923(2) 0.0574(8) Uani 1 1 d . . . H27A H 0.3348 -0.0233 0.9874 0.069 Uiso 1 1 calc R . . C28 C 0.4160(2) 0.05539(18) 0.93542(19) 0.0558(8) Uani 1 1 d . . . H28A H 0.3587 0.0937 0.8910 0.067 Uiso 1 1 calc R . . C29 C 0.5138(2) 0.06861(17) 0.94311(19) 0.0565(8) Uani 1 1 d . . . H29A H 0.5238 0.1162 0.9036 0.068 Uiso 1 1 calc R . . C30 C 0.5034(6) -0.0357(5) 0.5275(5) 0.090(4) Uani 0.50 1 d PD . 1 C31 C 0.5083(5) -0.1220(4) 0.5751(4) 0.0567(19) Uani 0.50 1 d PD . 1 H31A H 0.4854 -0.1783 0.5347 0.068 Uiso 0.50 1 d PR . 1 C32 C 0.5421(6) -0.1253(3) 0.6790(4) 0.0265(16) Uani 0.50 1 d PD . 1 H32A H 0.5450 -0.1849 0.7108 0.032 Uiso 0.50 1 d PR . 1 C33 C 0.5737(18) -0.0436(6) 0.7372(6) 0.121(8) Uani 0.50 1 d PD . 1 H33A H 0.5953 -0.0466 0.8088 0.145 Uiso 0.50 1 d PR . 1 C34 C 0.5718(8) 0.0423(4) 0.6902(6) 0.061(2) Uani 0.50 1 d PD . 1 H34A H 0.5991 0.0979 0.7311 0.074 Uiso 0.50 1 d PR . 1 C35 C 0.5392(11) 0.0454(5) 0.5871(6) 0.136(7) Uani 0.50 1 d PD . 1 C36 C 0.5226(4) 0.1227(4) 0.5133(5) 0.0418(12) Uani 0.50 1 d P . 1 H36A H 0.5902 0.1490 0.5305 0.050 Uiso 0.50 1 d PR . 1 H36B H 0.4758 0.1719 0.5107 0.050 Uiso 0.50 1 d PR . 1 C37 C 0.4663(8) -0.0279(4) 0.4211(5) 0.030(2) Uani 0.50 1 d PD . 1 C42 C 0.4796(7) 0.0690(4) 0.4181(6) 0.086(4) Uani 0.50 1 d PD . 1 C41 C 0.4520(17) 0.1121(5) 0.3236(7) 0.159(10) Uani 0.50 1 d PD . 1 H41A H 0.4602 0.1790 0.3205 0.191 Uiso 0.50 1 d PR . 1 C40 C 0.4142(11) 0.0586(4) 0.2361(6) 0.050(2) Uani 0.50 1 d PD . 1 H40A H 0.3980 0.0882 0.1724 0.060 Uiso 0.50 1 d PR . 1 C39 C 0.3977(5) -0.0385(4) 0.2383(4) 0.0491(15) Uani 0.50 1 d PD . 1 H39A H 0.3699 -0.0754 0.1770 0.059 Uiso 0.50 1 d PR . 1 C38 C 0.4244(8) -0.0815(4) 0.3326(6) 0.070(3) Uani 0.50 1 d PD . 1 H38A H 0.4144 -0.1481 0.3355 0.085 Uiso 0.50 1 d PR . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0501(10) 0.0298(9) 0.0432(10) -0.0027(7) 0.0241(8) -0.0096(7) O2 0.0802(14) 0.0469(10) 0.0571(11) 0.0125(9) 0.0453(10) 0.0322(9) C1 0.0262(12) 0.0263(11) 0.0316(12) -0.0002(9) 0.0127(9) -0.0021(9) C2 0.0236(12) 0.0353(13) 0.0343(12) 0.0024(10) 0.0145(10) -0.0010(9) C3 0.0256(12) 0.0314(12) 0.0302(12) 0.0017(10) 0.0133(9) 0.0025(9) C4 0.0248(12) 0.0275(11) 0.0302(12) 0.0000(9) 0.0130(9) 0.0022(9) C5 0.0245(12) 0.0278(11) 0.0287(12) -0.0015(9) 0.0122(9) -0.0013(9) C6 0.0264(12) 0.0271(11) 0.0275(11) 0.0024(9) 0.0130(9) 0.0002(9) C7 0.0266(12) 0.0257(12) 0.0369(13) -0.0029(10) 0.0134(10) -0.0009(9) C8 0.0329(13) 0.0233(11) 0.0347(12) -0.0030(9) 0.0165(10) 0.0018(9) C9 0.0225(12) 0.0285(12) 0.0354(12) 0.0017(10) 0.0131(10) 0.0009(9) C10 0.0298(13) 0.0334(13) 0.0363(13) 0.0052(10) 0.0159(10) 0.0008(10) C11 0.0277(13) 0.0335(13) 0.0340(12) -0.0002(10) 0.0118(10) -0.0054(10) C12 0.0288(13) 0.0280(12) 0.0400(13) -0.0018(10) 0.0174(10) -0.0038(9) C13 0.0332(13) 0.0331(13) 0.0366(13) 0.0048(10) 0.0197(10) -0.0024(10) C14 0.0270(13) 0.0342(13) 0.0377(13) 0.0020(10) 0.0185(10) 0.0002(10) C15 0.0512(16) 0.0389(14) 0.0401(14) 0.0040(11) 0.0163(12) -0.0089(11) C16 0.0539(17) 0.0487(15) 0.0335(13) -0.0017(11) 0.0200(12) -0.0110(12) C17 0.0644(19) 0.0357(14) 0.0439(15) -0.0095(11) 0.0240(13) -0.0138(12) C18 0.0237(12) 0.0289(12) 0.0348(12) 0.0008(10) 0.0159(10) 0.0004(9) C19 0.0352(14) 0.0382(13) 0.0392(14) 0.0044(11) 0.0208(11) 0.0053(10) C20 0.0543(17) 0.0455(14) 0.0410(14) 0.0160(12) 0.0284(12) 0.0220(12) C21 0.0457(15) 0.0314(13) 0.0492(15) 0.0051(11) 0.0302(12) 0.0113(11) C22 0.0377(14) 0.0395(13) 0.0369(13) -0.0006(11) 0.0202(11) 0.0064(11) C23 0.0317(13) 0.0399(13) 0.0357(13) 0.0000(10) 0.0176(10) 0.0056(10) C24 0.0521(17) 0.0571(16) 0.0382(14) 0.0058(12) 0.0236(12) 0.0180(13) C25 0.0584(18) 0.0653(18) 0.0427(15) 0.0087(13) 0.0192(13) 0.0296(14) C26 0.0621(19) 0.0507(16) 0.0620(18) -0.0062(14) 0.0372(15) 0.0188(13) C27 0.067(2) 0.0449(16) 0.0475(16) -0.0141(13) 0.0160(14) 0.0037(14) C28 0.069(2) 0.0378(16) 0.0444(16) -0.0062(13) 0.0127(14) 0.0124(14) C29 0.079(2) 0.0358(15) 0.0435(16) -0.0070(12) 0.0192(15) 0.0050(14) C30 0.030(4) 0.055(8) 0.196(13) 0.063(7) 0.062(6) 0.025(5) C31 0.039(4) 0.089(6) 0.052(4) 0.036(4) 0.029(3) 0.029(4) C32 0.016(4) 0.034(3) 0.033(4) 0.004(3) 0.014(3) 0.005(3) C33 0.046(8) 0.20(2) 0.121(11) 0.062(13) 0.044(8) 0.034(12) C34 0.045(4) 0.112(7) 0.032(4) 0.004(5) 0.022(4) 0.010(5) C35 0.017(6) 0.36(2) 0.031(6) 0.004(9) 0.007(5) 0.025(10) C36 0.026(3) 0.040(3) 0.067(4) 0.006(3) 0.028(3) 0.003(2) C37 0.030(5) 0.020(3) 0.048(6) -0.002(3) 0.025(4) -0.006(3) C42 0.046(5) 0.017(4) 0.209(14) -0.020(7) 0.071(8) 0.004(5) C41 0.117(15) 0.23(2) 0.16(2) 0.090(18) 0.092(17) 0.073(16) C40 0.049(6) 0.038(4) 0.075(5) -0.010(3) 0.040(5) 0.003(3) C39 0.043(4) 0.056(4) 0.059(4) -0.008(4) 0.033(3) -0.004(3) C38 0.036(4) 0.113(7) 0.081(7) 0.046(6) 0.043(5) 0.018(5) _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 O1 C12 1.375(2) . ? O1 C17 1.425(3) . ? O2 C21 1.378(2) . ? O2 C26 1.415(3) . ? C1 C2 1.397(3) . ? C1 C6 1.407(3) . ? C1 C9 1.495(3) . ? C2 C3 1.383(3) . ? C2 H2A 0.9500 . ? C3 C4 1.411(3) . ? C3 C18 1.504(3) . ? C4 C5 1.429(3) . ? C4 C8 1.435(3) . ? C5 C6 1.418(3) . ? C5 C5 1.434(4) 3_667 ? C6 C7 1.440(3) . ? C7 C8 1.339(3) 3_667 ? C7 H7A 0.9500 . ? C8 C7 1.339(3) 3_667 ? C8 H8A 0.9500 . ? C9 C10 1.397(3) . ? C9 C14 1.401(3) . ? C10 C11 1.394(3) . ? C10 C15 1.507(3) . ? C11 C12 1.381(3) . ? C11 H11A 0.9500 . ? C12 C13 1.387(3) . ? C13 C14 1.384(3) . ? C13 H13A 0.9500 . ? C14 C16 1.511(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.397(3) . ? C18 C19 1.401(3) . ? C19 C20 1.383(3) . ? C19 C24 1.501(3) . ? C20 C21 1.382(3) . ? C20 H20A 0.9500 . ? C21 C22 1.371(3) . ? C22 C23 1.396(3) . ? C22 H22A 0.9500 . ? C23 C25 1.510(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.366(4) . ? C27 C29 1.384(3) 3_657 ? C27 H27A 0.9500 . ? C28 C29 1.374(4) . ? C28 H28A 0.9500 . ? C29 C27 1.384(3) 3_657 ? C29 H29A 0.9500 . ? C30 C42 0.868(9) 3_656 ? C30 C37 1.129(9) 3_656 ? C30 C30 1.276(10) 3_656 ? C30 C36 1.348(8) 3_656 ? C30 C35 1.394(7) . ? C30 C31 1.399(6) . ? C30 C37 1.416(7) . ? C30 C35 1.522(12) 3_656 ? C31 C42 0.767(7) 3_656 ? C31 C36 1.171(8) 3_656 ? C31 C41 1.345(11) 3_656 ? C31 C32 1.385(5) . ? C31 H31A 0.9600 . ? C32 C41 0.216(13) 3_656 ? C32 C33 1.388(6) . ? C32 C40 1.462(9) 3_656 ? C32 C42 1.547(10) 3_656 ? C32 H32A 0.9600 . ? C33 C40 0.410(13) 3_656 ? C33 C39 1.233(10) 3_656 ? C33 C41 1.258(12) 3_656 ? C33 C34 1.399(7) . ? C33 H33A 0.9599 . ? C34 C38 0.667(7) 3_656 ? C34 C39 0.941(9) 3_656 ? C34 C35 1.376(6) . ? C34 C37 1.492(9) 3_656 ? C34 C40 1.756(9) 3_656 ? C34 H34A 0.9600 . ? C35 C37 0.271(9) 3_656 ? C35 C38 1.172(11) 3_656 ? C35 C36 1.489(8) . ? C35 C30 1.522(12) 3_656 ? C35 C42 1.641(9) 3_656 ? C36 C31 1.171(8) 3_656 ? C36 C30 1.348(8) 3_656 ? C36 C42 1.463(9) . ? C36 C37 1.625(7) 3_656 ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C37 C35 0.271(9) 3_656 ? C37 C30 1.129(9) 3_656 ? C37 C38 1.388(6) . ? C37 C42 1.392(6) . ? C37 C34 1.492(10) 3_656 ? C37 C36 1.625(7) 3_656 ? C42 C31 0.767(7) 3_656 ? C42 C30 0.868(9) 3_656 ? C42 C41 1.407(7) . ? C42 C32 1.547(10) 3_656 ? C42 C35 1.641(9) 3_656 ? C41 C32 0.216(13) 3_656 ? C41 C33 1.258(12) 3_656 ? C41 C31 1.345(11) 3_656 ? C41 C40 1.377(6) . ? C41 H41A 0.9601 . ? C40 C33 0.410(13) 3_656 ? C40 C39 1.401(6) . ? C40 C32 1.462(9) 3_656 ? C40 C34 1.756(9) 3_656 ? C40 H40A 0.9600 . ? C39 C34 0.941(9) 3_656 ? C39 C33 1.233(10) 3_656 ? C39 C38 1.406(6) . ? C39 H39A 0.9600 . ? C38 C34 0.667(7) 3_656 ? C38 C35 1.172(11) 3_656 ? C38 H38A 0.9599 . ? 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 C12 O1 C17 115.80(17) . . ? C21 O2 C26 118.04(18) . . ? C2 C1 C6 118.97(18) . . ? C2 C1 C9 121.95(19) . . ? C6 C1 C9 119.07(18) . . ? C3 C2 C1 122.9(2) . . ? C3 C2 H2A 118.6 . . ? C1 C2 H2A 118.6 . . ? C2 C3 C4 119.07(19) . . ? C2 C3 C18 120.98(19) . . ? C4 C3 C18 119.95(18) . . ? C3 C4 C5 119.42(18) . . ? C3 C4 C8 122.58(18) . . ? C5 C4 C8 117.99(19) . . ? C6 C5 C4 119.97(18) . . ? C6 C5 C5 120.1(2) . 3_667 ? C4 C5 C5 119.9(2) . 3_667 ? C1 C6 C5 119.63(18) . . ? C1 C6 C7 122.23(18) . . ? C5 C6 C7 118.14(19) . . ? C8 C7 C6 121.83(19) 3_667 . ? C8 C7 H7A 119.1 3_667 . ? C6 C7 H7A 119.1 . . ? C7 C8 C4 122.00(19) 3_667 . ? C7 C8 H8A 119.0 3_667 . ? C4 C8 H8A 119.0 . . ? C10 C9 C14 119.65(19) . . ? C10 C9 C1 119.56(18) . . ? C14 C9 C1 120.62(18) . . ? C11 C10 C9 119.75(19) . . ? C11 C10 C15 119.2(2) . . ? C9 C10 C15 121.06(19) . . ? C12 C11 C10 120.2(2) . . ? C12 C11 H11A 119.9 . . ? C10 C11 H11A 119.9 . . ? O1 C12 C11 124.34(19) . . ? O1 C12 C13 115.55(18) . . ? C11 C12 C13 120.10(19) . . ? C14 C13 C12 120.43(19) . . ? C14 C13 H13A 119.8 . . ? C12 C13 H13A 119.8 . . ? C13 C14 C9 119.7(2) . . ? C13 C14 C16 120.35(19) . . ? C9 C14 C16 119.89(19) . . ? C10 C15 H15A 109.5 . . ? C10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 119.61(19) . . ? C23 C18 C3 120.49(18) . . ? C19 C18 C3 119.89(18) . . ? C20 C19 C18 119.0(2) . . ? C20 C19 C24 120.3(2) . . ? C18 C19 C24 120.65(19) . . ? C21 C20 C19 121.3(2) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C22 C21 O2 124.3(2) . . ? C22 C21 C20 120.0(2) . . ? O2 C21 C20 115.6(2) . . ? C21 C22 C23 120.1(2) . . ? C21 C22 H22A 119.9 . . ? C23 C22 H22A 119.9 . . ? C22 C23 C18 119.9(2) . . ? C22 C23 C25 118.9(2) . . ? C18 C23 C25 121.1(2) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O2 C26 H26A 109.5 . . ? O2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 119.8(3) . 3_657 ? C28 C27 H27A 120.1 . . ? C29 C27 H27A 120.1 3_657 . ? C27 C28 C29 119.3(3) . . ? C27 C28 H28A 120.3 . . ? C29 C28 H28A 120.3 . . ? C28 C29 C27 120.8(3) . 3_657 ? C28 C29 H29A 119.6 . . ? C27 C29 H29A 119.6 3_657 . ? C42 C30 C37 87.4(9) 3_656 3_656 ? C42 C30 C30 159.0(13) 3_656 3_656 ? C37 C30 C30 71.9(6) 3_656 3_656 ? C42 C30 C36 79.4(7) 3_656 3_656 ? C37 C30 C36 166.6(6) 3_656 3_656 ? C30 C30 C36 121.1(9) 3_656 3_656 ? C42 C30 C35 90.0(7) 3_656 . ? C37 C30 C35 2.6(5) 3_656 . ? C30 C30 C35 69.3(7) 3_656 . ? C36 C30 C35 169.2(6) 3_656 . ? C42 C30 C31 29.1(6) 3_656 . ? C37 C30 C31 116.4(6) 3_656 . ? C30 C30 C31 171.4(9) 3_656 . ? C36 C30 C31 50.4(4) 3_656 . ? C35 C30 C31 119.0(4) . . ? C42 C30 C37 151.3(9) 3_656 . ? C37 C30 C37 121.1(5) 3_656 . ? C30 C30 C37 49.3(5) 3_656 . ? C36 C30 C37 71.9(5) 3_656 . ? C35 C30 C37 118.6(6) . . ? C31 C30 C37 122.4(6) . . ? C42 C30 C35 141.6(10) 3_656 3_656 ? C37 C30 C35 130.9(6) 3_656 3_656 ? C30 C30 C35 59.0(5) 3_656 3_656 ? C36 C30 C35 62.2(5) 3_656 3_656 ? C35 C30 C35 128.3(5) . 3_656 ? C31 C30 C35 112.6(6) . 3_656 ? C37 C30 C35 9.8(3) . 3_656 ? C42 C31 C36 95.8(8) 3_656 3_656 ? C42 C31 C41 78.4(9) 3_656 3_656 ? C36 C31 C41 174.0(7) 3_656 3_656 ? C42 C31 C32 86.9(8) 3_656 . ? C36 C31 C32 177.1(7) 3_656 . ? C41 C31 C32 8.9(5) 3_656 . ? C42 C31 C30 33.3(8) 3_656 . ? C36 C31 C30 62.5(5) 3_656 . ? C41 C31 C30 111.7(5) 3_656 . ? C32 C31 C30 120.1(4) . . ? C42 C31 H31A 152.7 3_656 . ? C36 C31 H31A 56.9 3_656 . ? C41 C31 H31A 128.9 3_656 . ? C32 C31 H31A 120.4 . . ? C30 C31 H31A 119.4 . . ? C41 C32 C31 75(3) 3_656 . ? C41 C32 C33 49(4) 3_656 . ? C31 C32 C33 120.4(4) . . ? C41 C32 C40 63(3) 3_656 3_656 ? C31 C32 C40 136.3(5) . 3_656 ? C33 C32 C40 16.3(5) . 3_656 ? C41 C32 C42 47(3) 3_656 3_656 ? C31 C32 C42 29.7(3) . 3_656 ? C33 C32 C42 90.8(4) . 3_656 ? C40 C32 C42 106.7(5) 3_656 3_656 ? C41 C32 H32A 156.7 3_656 . ? C31 C32 H32A 119.4 . . ? C33 C32 H32A 120.1 . . ? C40 C32 H32A 104.1 3_656 . ? C42 C32 H32A 149.0 3_656 . ? C40 C33 C39 106(2) 3_656 3_656 ? C40 C33 C41 98.2(17) 3_656 3_656 ? C39 C33 C41 152.5(12) 3_656 3_656 ? C40 C33 C32 92.1(16) 3_656 . ? C39 C33 C32 159.9(8) 3_656 . ? C41 C33 C32 7.5(7) 3_656 . ? C40 C33 C34 147(3) 3_656 . ? C39 C33 C34 41.3(5) 3_656 . ? C41 C33 C34 112.7(6) 3_656 . ? C32 C33 C34 119.5(4) . . ? C40 C33 H33A 30.1 3_656 . ? C39 C33 H33A 79.9 3_656 . ? C41 C33 H33A 126.5 3_656 . ? C32 C33 H33A 119.7 . . ? C34 C33 H33A 120.8 . . ? C38 C34 C39 121.0(13) 3_656 3_656 ? C38 C34 C35 58.3(9) 3_656 . ? C39 C34 C35 172.9(14) 3_656 . ? C38 C34 C33 173(2) 3_656 . ? C39 C34 C33 59.8(6) 3_656 . ? C35 C34 C33 119.9(4) . . ? C38 C34 C37 68.1(8) 3_656 3_656 ? C39 C34 C37 167.6(9) 3_656 3_656 ? C35 C34 C37 9.8(3) . 3_656 ? C33 C34 C37 110.1(4) . 3_656 ? C38 C34 C40 169.8(19) 3_656 3_656 ? C39 C34 C40 52.7(4) 3_656 3_656 ? C35 C34 C40 126.8(5) . 3_656 ? C33 C34 C40 7.4(7) . 3_656 ? C37 C34 C40 117.0(5) 3_656 3_656 ? C38 C34 H34A 62.0 3_656 . ? C39 C34 H34A 59.8 3_656 . ? C35 C34 H34A 120.2 . . ? C33 C34 H34A 119.6 . . ? C37 C34 H34A 130.0 3_656 . ? C40 C34 H34A 112.4 3_656 . ? C37 C35 C38 139(2) 3_656 3_656 ? C37 C35 C34 110(2) 3_656 . ? C38 C35 C34 28.9(4) 3_656 . ? C37 C35 C30 11(2) 3_656 . ? C38 C35 C30 149.6(6) 3_656 . ? C34 C35 C30 120.8(4) . . ? C37 C35 C36 116(2) 3_656 . ? C38 C35 C36 105.6(7) 3_656 . ? C34 C35 C36 134.1(7) . . ? C30 C35 C36 104.8(6) . . ? C37 C35 C30 62(2) 3_656 3_656 ? C38 C35 C30 158.7(7) 3_656 3_656 ? C34 C35 C30 172.2(7) . 3_656 ? C30 C35 C30 51.7(5) . 3_656 ? C36 C35 C30 53.2(3) . 3_656 ? C37 C35 C42 21.1(19) 3_656 3_656 ? C38 C35 C42 117.7(6) 3_656 3_656 ? C34 C35 C42 89.1(5) . 3_656 ? C30 C35 C42 31.9(4) . 3_656 ? C36 C35 C42 136.7(8) . 3_656 ? C30 C35 C42 83.5(7) 3_656 3_656 ? C31 C36 C30 67.0(5) 3_656 3_656 ? C31 C36 C42 31.4(4) 3_656 . ? C30 C36 C42 35.6(4) 3_656 . ? C31 C36 C35 131.6(5) 3_656 . ? C30 C36 C35 64.6(5) 3_656 . ? C42 C36 C35 100.3(5) . . ? C31 C36 C37 123.0(5) 3_656 3_656 ? C30 C36 C37 56.0(3) 3_656 3_656 ? C42 C36 C37 91.6(4) . 3_656 ? C35 C36 C37 8.7(4) . 3_656 ? C31 C36 H36A 96.2 3_656 . ? C30 C36 H36A 120.6 3_656 . ? C42 C36 H36A 112.1 . . ? C35 C36 H36A 107.3 . . ? C37 C36 H36A 111.1 3_656 . ? C31 C36 H36B 94.1 3_656 . ? C30 C36 H36B 127.4 3_656 . ? C42 C36 H36B 111.7 . . ? C35 C36 H36B 115.6 . . ? C37 C36 H36B 119.7 3_656 . ? H36A C36 H36B 109.6 . . ? C35 C37 C30 167(3) 3_656 3_656 ? C35 C37 C38 34(2) 3_656 . ? C30 C37 C38 159.6(6) 3_656 . ? C35 C37 C42 155(2) 3_656 . ? C30 C37 C42 38.5(5) 3_656 . ? C38 C37 C42 121.1(4) . . ? C35 C37 C30 108(2) 3_656 . ? C30 C37 C30 58.9(5) 3_656 . ? C38 C37 C30 141.6(6) . . ? C42 C37 C30 97.3(6) . . ? C35 C37 C34 60(2) 3_656 3_656 ? C30 C37 C34 133.2(6) 3_656 3_656 ? C38 C37 C34 26.5(3) . 3_656 ? C42 C37 C34 94.9(4) . 3_656 ? C30 C37 C34 167.6(7) . 3_656 ? C35 C37 C36 56(2) 3_656 3_656 ? C30 C37 C36 110.9(6) 3_656 3_656 ? C38 C37 C36 89.5(4) . 3_656 ? C42 C37 C36 149.4(5) . 3_656 ? C30 C37 C36 52.1(4) . 3_656 ? C34 C37 C36 115.7(5) 3_656 3_656 ? C31 C42 C30 117.6(12) 3_656 3_656 ? C31 C42 C37 171.6(10) 3_656 . ? C30 C42 C37 54.1(6) 3_656 . ? C31 C42 C41 69.4(9) 3_656 . ? C30 C42 C41 172.6(8) 3_656 . ? C37 C42 C41 118.9(4) . . ? C31 C42 C36 52.8(7) 3_656 . ? C30 C42 C36 64.9(8) 3_656 . ? C37 C42 C36 119.0(6) . . ? C41 C42 C36 122.1(6) . . ? C31 C42 C32 63.4(7) 3_656 3_656 ? C30 C42 C32 175.0(12) 3_656 3_656 ? C37 C42 C32 124.7(5) . 3_656 ? C41 C42 C32 6.4(6) . 3_656 ? C36 C42 C32 116.2(5) . 3_656 ? C31 C42 C35 175.4(12) 3_656 3_656 ? C30 C42 C35 58.1(5) 3_656 3_656 ? C37 C42 C35 4.0(4) . 3_656 ? C41 C42 C35 114.8(5) . 3_656 ? C36 C42 C35 123.0(7) . 3_656 ? C32 C42 C35 120.7(6) 3_656 3_656 ? C32 C41 C33 123(4) 3_656 3_656 ? C32 C41 C31 96(3) 3_656 3_656 ? C33 C41 C31 135.3(8) 3_656 3_656 ? C32 C41 C40 109(3) 3_656 . ? C33 C41 C40 17.1(6) 3_656 . ? C31 C41 C40 152.4(6) 3_656 . ? C32 C41 C42 127(4) 3_656 . ? C33 C41 C42 103.3(6) 3_656 . ? C31 C41 C42 32.3(3) 3_656 . ? C40 C41 C42 120.2(4) . . ? C32 C41 H41A 21.4 3_656 . ? C33 C41 H41A 136.9 3_656 . ? C31 C41 H41A 87.4 3_656 . ? C40 C41 H41A 120.2 . . ? C42 C41 H41A 119.6 . . ? C33 C40 C41 64.7(16) 3_656 . ? C33 C40 C39 57.9(16) 3_656 . ? C41 C40 C39 121.1(4) . . ? C33 C40 C32 71.6(16) 3_656 3_656 ? C41 C40 C32 8.0(6) . 3_656 ? C39 C40 C32 128.7(5) . 3_656 ? C33 C40 C34 26(2) 3_656 3_656 ? C41 C40 C34 89.0(4) . 3_656 ? C39 C40 C34 32.3(3) . 3_656 ? C32 C40 C34 96.5(5) 3_656 3_656 ? C33 C40 H40A 168.0 3_656 . ? C41 C40 H40A 119.7 . . ? C39 C40 H40A 119.2 . . ? C32 C40 H40A 112.0 3_656 . ? C34 C40 H40A 151.2 3_656 . ? C34 C39 C33 78.8(7) 3_656 3_656 ? C34 C39 C40 95.1(5) 3_656 . ? C33 C39 C40 16.4(6) 3_656 . ? C34 C39 C38 24.0(5) 3_656 . ? C33 C39 C38 102.6(5) 3_656 . ? C40 C39 C38 118.7(4) . . ? C34 C39 H39A 143.7 3_656 . ? C33 C39 H39A 136.7 3_656 . ? C40 C39 H39A 120.9 . . ? C38 C39 H39A 120.4 . . ? C34 C38 C35 92.8(10) 3_656 3_656 ? C34 C38 C37 85.5(9) 3_656 . ? C35 C38 C37 7.4(4) 3_656 . ? C34 C38 C39 35.0(8) 3_656 . ? C35 C38 C39 127.4(5) 3_656 . ? C37 C38 C39 120.0(4) . . ? C34 C38 H38A 153.3 3_656 . ? C35 C38 H38A 113.0 3_656 . ? C37 C38 H38A 120.4 . . ? C39 C38 H38A 119.6 . . ? 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(3) . . . . ? C9 C1 C2 C3 -178.05(19) . . . . ? C1 C2 C3 C4 1.6(3) . . . . ? C1 C2 C3 C18 -179.02(18) . . . . ? C2 C3 C4 C5 -2.7(3) . . . . ? C18 C3 C4 C5 177.89(18) . . . . ? C2 C3 C4 C8 177.84(19) . . . . ? C18 C3 C4 C8 -1.6(3) . . . . ? C3 C4 C5 C6 1.8(3) . . . . ? C8 C4 C5 C6 -178.74(18) . . . . ? C3 C4 C5 C5 -179.4(2) . . . 3_667 ? C8 C4 C5 C5 0.1(3) . . . 3_667 ? C2 C1 C6 C5 -1.5(3) . . . . ? C9 C1 C6 C5 177.15(18) . . . . ? C2 C1 C6 C7 178.22(19) . . . . ? C9 C1 C6 C7 -3.1(3) . . . . ? C4 C5 C6 C1 0.3(3) . . . . ? C5 C5 C6 C1 -178.5(2) 3_667 . . . ? C4 C5 C6 C7 -179.39(18) . . . . ? C5 C5 C6 C7 1.8(3) 3_667 . . . ? C1 C6 C7 C8 179.12(19) . . . 3_667 ? C5 C6 C7 C8 -1.2(3) . . . 3_667 ? C3 C4 C8 C7 178.72(19) . . . 3_667 ? C5 C4 C8 C7 -0.7(3) . . . 3_667 ? C2 C1 C9 C10 92.7(3) . . . . ? C6 C1 C9 C10 -85.9(2) . . . . ? C2 C1 C9 C14 -92.1(2) . . . . ? C6 C1 C9 C14 89.3(2) . . . . ? C14 C9 C10 C11 -2.1(3) . . . . ? C1 C9 C10 C11 173.17(19) . . . . ? C14 C9 C10 C15 177.8(2) . . . . ? C1 C9 C10 C15 -7.0(3) . . . . ? C9 C10 C11 C12 -0.9(3) . . . . ? C15 C10 C11 C12 179.3(2) . . . . ? C17 O1 C12 C11 4.4(3) . . . . ? C17 O1 C12 C13 -174.76(19) . . . . ? C10 C11 C12 O1 -175.1(2) . . . . ? C10 C11 C12 C13 4.0(3) . . . . ? O1 C12 C13 C14 175.04(19) . . . . ? C11 C12 C13 C14 -4.2(3) . . . . ? C12 C13 C14 C9 1.2(3) . . . . ? C12 C13 C14 C16 -177.5(2) . . . . ? C10 C9 C14 C13 1.9(3) . . . . ? C1 C9 C14 C13 -173.29(19) . . . . ? C10 C9 C14 C16 -179.4(2) . . . . ? C1 C9 C14 C16 5.4(3) . . . . ? C2 C3 C18 C23 95.0(3) . . . . ? C4 C3 C18 C23 -85.7(2) . . . . ? C2 C3 C18 C19 -86.3(3) . . . . ? C4 C3 C18 C19 93.1(2) . . . . ? C23 C18 C19 C20 0.6(3) . . . . ? C3 C18 C19 C20 -178.2(2) . . . . ? C23 C18 C19 C24 -178.4(2) . . . . ? C3 C18 C19 C24 2.9(3) . . . . ? C18 C19 C20 C21 -0.1(4) . . . . ? C24 C19 C20 C21 178.8(2) . . . . ? C26 O2 C21 C22 -1.6(4) . . . . ? C26 O2 C21 C20 177.1(2) . . . . ? C19 C20 C21 C22 -0.1(4) . . . . ? C19 C20 C21 O2 -178.8(2) . . . . ? O2 C21 C22 C23 178.5(2) . . . . ? C20 C21 C22 C23 -0.1(4) . . . . ? C21 C22 C23 C18 0.5(3) . . . . ? C21 C22 C23 C25 -177.9(2) . . . . ? C19 C18 C23 C22 -0.8(3) . . . . ? C3 C18 C23 C22 178.0(2) . . . . ? C19 C18 C23 C25 177.7(2) . . . . ? C3 C18 C23 C25 -3.6(3) . . . . ? C29 C27 C28 C29 0.2(4) 3_657 . . . ? C27 C28 C29 C27 -0.2(4) . . . 3_657 ? C37 C30 C31 C42 -1.9(16) 3_656 . . 3_656 ? C30 C30 C31 C42 163(8) 3_656 . . 3_656 ? C36 C30 C31 C42 175.1(18) 3_656 . . 3_656 ? C35 C30 C31 C42 -2.2(16) . . . 3_656 ? C37 C30 C31 C42 176(2) . . . 3_656 ? C35 C30 C31 C42 175.8(19) 3_656 . . 3_656 ? C42 C30 C31 C36 -175.1(18) 3_656 . . 3_656 ? C37 C30 C31 C36 -176.9(9) 3_656 . . 3_656 ? C30 C30 C31 C36 -12(7) 3_656 . . 3_656 ? C35 C30 C31 C36 -177.2(12) . . . 3_656 ? C37 C30 C31 C36 0.6(9) . . . 3_656 ? C35 C30 C31 C36 0.7(8) 3_656 . . 3_656 ? C42 C30 C31 C41 3.0(18) 3_656 . . 3_656 ? C37 C30 C31 C41 1.1(15) 3_656 . . 3_656 ? C30 C30 C31 C41 166(7) 3_656 . . 3_656 ? C36 C30 C31 C41 178.1(12) 3_656 . . 3_656 ? C35 C30 C31 C41 0.8(16) . . . 3_656 ? C37 C30 C31 C41 178.7(14) . . . 3_656 ? C35 C30 C31 C41 178.8(12) 3_656 . . 3_656 ? C42 C30 C31 C32 6.3(16) 3_656 . . . ? C37 C30 C31 C32 4.4(13) 3_656 . . . ? C30 C30 C31 C32 169(7) 3_656 . . . ? C36 C30 C31 C32 -178.6(8) 3_656 . . . ? C35 C30 C31 C32 4.1(14) . . . . ? C37 C30 C31 C32 -178.0(9) . . . . ? C35 C30 C31 C32 -177.9(8) 3_656 . . . ? C42 C31 C32 C41 -17(8) 3_656 . . 3_656 ? C36 C31 C32 C41 -175(100) 3_656 . . 3_656 ? C30 C31 C32 C41 -20(8) . . . 3_656 ? C42 C31 C32 C33 1.9(15) 3_656 . . . ? C36 C31 C32 C33 -157(14) 3_656 . . . ? C41 C31 C32 C33 19(8) 3_656 . . . ? C30 C31 C32 C33 -1.6(14) . . . . ? C42 C31 C32 C40 -2.6(17) 3_656 . . 3_656 ? C36 C31 C32 C40 -161(14) 3_656 . . 3_656 ? C41 C31 C32 C40 14(7) 3_656 . . 3_656 ? C30 C31 C32 C40 -6.0(17) . . . 3_656 ? C36 C31 C32 C42 -158(15) 3_656 . . 3_656 ? C41 C31 C32 C42 17(8) 3_656 . . 3_656 ? C30 C31 C32 C42 -3.5(9) . . . 3_656 ? C41 C32 C33 C40 -145(14) 3_656 . . 3_656 ? C31 C32 C33 C40 -169(5) . . . 3_656 ? C42 C32 C33 C40 -168(5) 3_656 . . 3_656 ? C41 C32 C33 C39 9(9) 3_656 . . 3_656 ? C31 C32 C33 C39 -16(6) . . . 3_656 ? C40 C32 C33 C39 153(11) 3_656 . . 3_656 ? C42 C32 C33 C39 -15(6) 3_656 . . 3_656 ? C31 C32 C33 C41 -24(10) . . . 3_656 ? C40 C32 C33 C41 145(14) 3_656 . . 3_656 ? C42 C32 C33 C41 -23(10) 3_656 . . 3_656 ? C41 C32 C33 C34 24(9) 3_656 . . . ? C31 C32 C33 C34 0(2) . . . . ? C40 C32 C33 C34 169(7) 3_656 . . . ? C42 C32 C33 C34 0.6(17) 3_656 . . . ? C40 C33 C34 C38 86(13) 3_656 . . 3_656 ? C39 C33 C34 C38 99(11) 3_656 . . 3_656 ? C41 C33 C34 C38 -70(12) 3_656 . . 3_656 ? C32 C33 C34 C38 -73(11) . . . 3_656 ? C40 C33 C34 C39 -13(10) 3_656 . . 3_656 ? C41 C33 C34 C39 -169(3) 3_656 . . 3_656 ? C32 C33 C34 C39 -172(2) . . . 3_656 ? C40 C33 C34 C35 159(10) 3_656 . . . ? C39 C33 C34 C35 171.8(16) 3_656 . . . ? C41 C33 C34 C35 3(3) 3_656 . . . ? C32 C33 C34 C35 0(3) . . . . ? C40 C33 C34 C37 159(10) 3_656 . . 3_656 ? C39 C33 C34 C37 172.0(13) 3_656 . . 3_656 ? C41 C33 C34 C37 3(3) 3_656 . . 3_656 ? C32 C33 C34 C37 0(2) . . . 3_656 ? C39 C33 C34 C40 13(10) 3_656 . . 3_656 ? C41 C33 C34 C40 -156(13) 3_656 . . 3_656 ? C32 C33 C34 C40 -159(12) . . . 3_656 ? C38 C34 C35 C37 173(7) 3_656 . . 3_656 ? C39 C34 C35 C37 87(8) 3_656 . . 3_656 ? C33 C34 C35 C37 1(7) . . . 3_656 ? C40 C34 C35 C37 4(7) 3_656 . . 3_656 ? C39 C34 C35 C38 -86(6) 3_656 . . 3_656 ? C33 C34 C35 C38 -173(3) . . . 3_656 ? C37 C34 C35 C38 -173(7) 3_656 . . 3_656 ? C40 C34 C35 C38 -169(3) 3_656 . . 3_656 ? C38 C34 C35 C30 176(2) 3_656 . . . ? C39 C34 C35 C30 89(6) 3_656 . . . ? C33 C34 C35 C30 3(2) . . . . ? C37 C34 C35 C30 2(5) 3_656 . . . ? C40 C34 C35 C30 6(2) 3_656 . . . ? C38 C34 C35 C36 -11(2) 3_656 . . . ? C39 C34 C35 C36 -97(6) 3_656 . . . ? C33 C34 C35 C36 176.4(16) . . . . ? C37 C34 C35 C36 176(8) 3_656 . . . ? C40 C34 C35 C36 179.8(12) 3_656 . . . ? C38 C34 C35 C30 -170(9) 3_656 . . 3_656 ? C39 C34 C35 C30 104(11) 3_656 . . 3_656 ? C33 C34 C35 C30 17(10) . . . 3_656 ? C37 C34 C35 C30 17(5) 3_656 . . 3_656 ? C40 C34 C35 C30 21(10) 3_656 . . 3_656 ? C38 C34 C35 C42 172(2) 3_656 . . 3_656 ? C39 C34 C35 C42 86(6) 3_656 . . 3_656 ? C33 C34 C35 C42 -0.2(17) . . . 3_656 ? C37 C34 C35 C42 -1(6) 3_656 . . 3_656 ? C40 C34 C35 C42 3.2(14) 3_656 . . 3_656 ? C42 C30 C35 C37 5(25) 3_656 . . 3_656 ? C30 C30 C35 C37 -172(25) 3_656 . . 3_656 ? C36 C30 C35 C37 -5(29) 3_656 . . 3_656 ? C31 C30 C35 C37 6(26) . . . 3_656 ? C37 C30 C35 C37 -172(24) . . . 3_656 ? C35 C30 C35 C37 -172(25) 3_656 . . 3_656 ? C42 C30 C35 C38 -2(3) 3_656 . . 3_656 ? C37 C30 C35 C38 -7(23) 3_656 . . 3_656 ? C30 C30 C35 C38 -178(3) 3_656 . . 3_656 ? C36 C30 C35 C38 -12(8) 3_656 . . 3_656 ? C31 C30 C35 C38 -1(4) . . . 3_656 ? C37 C30 C35 C38 -179(2) . . . 3_656 ? C35 C30 C35 C38 -178(3) 3_656 . . 3_656 ? C42 C30 C35 C34 -5.9(18) 3_656 . . . ? C37 C30 C35 C34 -11(24) 3_656 . . . ? C30 C30 C35 C34 177.5(14) 3_656 . . . ? C36 C30 C35 C34 -16(7) 3_656 . . . ? C31 C30 C35 C34 -5(2) . . . . ? C37 C30 C35 C34 177.2(7) . . . . ? C35 C30 C35 C34 177.5(14) 3_656 . . . ? C42 C30 C35 C36 179.0(11) 3_656 . . . ? C37 C30 C35 C36 174(26) 3_656 . . . ? C30 C30 C35 C36 2.4(11) 3_656 . . . ? C36 C30 C35 C36 169(5) 3_656 . . . ? C31 C30 C35 C36 -180.0(7) . . . . ? C37 C30 C35 C36 2.1(19) . . . . ? C35 C30 C35 C36 2.4(11) 3_656 . . . ? C42 C30 C35 C30 176.6(15) 3_656 . . 3_656 ? C37 C30 C35 C30 172(25) 3_656 . . 3_656 ? C36 C30 C35 C30 166(6) 3_656 . . 3_656 ? C31 C30 C35 C30 177.6(13) . . . 3_656 ? C37 C30 C35 C30 -0.3(10) . . . 3_656 ? C35 C30 C35 C30 0.0 3_656 . . 3_656 ? C37 C30 C35 C42 -5(25) 3_656 . . 3_656 ? C30 C30 C35 C42 -176.6(15) 3_656 . . 3_656 ? C36 C30 C35 C42 -10(5) 3_656 . . 3_656 ? C31 C30 C35 C42 1.1(8) . . . 3_656 ? C37 C30 C35 C42 -176.9(18) . . . 3_656 ? C35 C30 C35 C42 -176.6(15) 3_656 . . 3_656 ? C37 C35 C36 C31 -2(7) 3_656 . . 3_656 ? C38 C35 C36 C31 177.0(9) 3_656 . . 3_656 ? C34 C35 C36 C31 -177.5(12) . . . 3_656 ? C30 C35 C36 C31 -3.3(16) . . . 3_656 ? C30 C35 C36 C31 -0.9(10) 3_656 . . 3_656 ? C42 C35 C36 C31 -2(2) 3_656 . . 3_656 ? C37 C35 C36 C30 -1(6) 3_656 . . 3_656 ? C38 C35 C36 C30 178.0(13) 3_656 . . 3_656 ? C34 C35 C36 C30 -176.5(18) . . . 3_656 ? C30 C35 C36 C30 -2.3(10) . . . 3_656 ? C42 C35 C36 C30 -1.5(13) 3_656 . . 3_656 ? C37 C35 C36 C42 0(6) 3_656 . . . ? C38 C35 C36 C42 179.0(11) 3_656 . . . ? C34 C35 C36 C42 -175.5(16) . . . . ? C30 C35 C36 C42 -1.4(11) . . . . ? C30 C35 C36 C42 1.0(6) 3_656 . . . ? C42 C35 C36 C42 -0.6(17) 3_656 . . . ? C38 C35 C36 C37 179(100) 3_656 . . 3_656 ? C34 C35 C36 C37 -175(8) . . . 3_656 ? C30 C35 C36 C37 -1(5) . . . 3_656 ? C30 C35 C36 C37 1(6) 3_656 . . 3_656 ? C42 C35 C36 C37 0(5) 3_656 . . 3_656 ? C42 C30 C37 C35 5(8) 3_656 . . 3_656 ? C37 C30 C37 C35 178(6) 3_656 . . 3_656 ? C30 C30 C37 C35 178(6) 3_656 . . 3_656 ? C36 C30 C37 C35 1(6) 3_656 . . 3_656 ? C35 C30 C37 C35 178(5) . . . 3_656 ? C31 C30 C37 C35 1(6) . . . 3_656 ? C42 C30 C37 C30 -173(3) 3_656 . . 3_656 ? C37 C30 C37 C30 0.000(1) 3_656 . . 3_656 ? C36 C30 C37 C30 -177.0(10) 3_656 . . 3_656 ? C35 C30 C37 C30 0.4(13) . . . 3_656 ? C31 C30 C37 C30 -177.5(14) . . . 3_656 ? C35 C30 C37 C30 -178(6) 3_656 . . 3_656 ? C42 C30 C37 C38 7(4) 3_656 . . . ? C37 C30 C37 C38 -179.9(18) 3_656 . . . ? C30 C30 C37 C38 -179.9(18) 3_656 . . . ? C36 C30 C37 C38 3.2(17) 3_656 . . . ? C35 C30 C37 C38 -179.5(9) . . . . ? C31 C30 C37 C38 3(2) . . . . ? C35 C30 C37 C38 2(5) 3_656 . . . ? C42 C30 C37 C42 -175(2) 3_656 . . . ? C37 C30 C37 C42 -2.1(9) 3_656 . . . ? C30 C30 C37 C42 -2.1(9) 3_656 . . . ? C36 C30 C37 C42 -179.0(8) 3_656 . . . ? C35 C30 C37 C42 -1.6(18) . . . . ? C31 C30 C37 C42 -179.5(8) . . . . ? C35 C30 C37 C42 180(6) 3_656 . . . ? C42 C30 C37 C34 -5(7) 3_656 . . 3_656 ? C37 C30 C37 C34 168(5) 3_656 . . 3_656 ? C30 C30 C37 C34 168(5) 3_656 . . 3_656 ? C36 C30 C37 C34 -9(5) 3_656 . . 3_656 ? C35 C30 C37 C34 168(4) . . . 3_656 ? C31 C30 C37 C34 -10(5) . . . 3_656 ? C35 C30 C37 C34 -10(3) 3_656 . . 3_656 ? C42 C30 C37 C36 4(3) 3_656 . . 3_656 ? C37 C30 C37 C36 177.0(10) 3_656 . . 3_656 ? C30 C30 C37 C36 177.0(10) 3_656 . . 3_656 ? C35 C30 C37 C36 177.4(13) . . . 3_656 ? C31 C30 C37 C36 -0.5(7) . . . 3_656 ? C35 C30 C37 C36 -1(6) 3_656 . . 3_656 ? C35 C37 C42 C31 -167(13) 3_656 . . 3_656 ? C30 C37 C42 C31 10(9) 3_656 . . 3_656 ? C38 C37 C42 C31 -169(9) . . . 3_656 ? C30 C37 C42 C31 13(10) . . . 3_656 ? C34 C37 C42 C31 -165(9) 3_656 . . 3_656 ? C36 C37 C42 C31 12(10) 3_656 . . 3_656 ? C35 C37 C42 C30 -177(14) 3_656 . . 3_656 ? C38 C37 C42 C30 -178.7(14) . . . 3_656 ? C30 C37 C42 C30 2.8(13) . . . 3_656 ? C34 C37 C42 C30 -175.0(12) 3_656 . . 3_656 ? C36 C37 C42 C30 1(2) 3_656 . . 3_656 ? C35 C37 C42 C41 0(14) 3_656 . . . ? C30 C37 C42 C41 177.2(17) 3_656 . . . ? C38 C37 C42 C41 -1.5(18) . . . . ? C30 C37 C42 C41 -179.9(13) . . . . ? C34 C37 C42 C41 2.2(15) 3_656 . . . ? C36 C37 C42 C41 178.5(17) 3_656 . . . ? C35 C37 C42 C36 -180(100) 3_656 . . . ? C30 C37 C42 C36 -2.3(8) 3_656 . . . ? C38 C37 C42 C36 179.0(9) . . . . ? C30 C37 C42 C36 0.6(12) . . . . ? C34 C37 C42 C36 -177.3(7) 3_656 . . . ? C36 C37 C42 C36 -1(2) 3_656 . . . ? C35 C37 C42 C32 -3(14) 3_656 . . 3_656 ? C30 C37 C42 C32 174.1(15) 3_656 . . 3_656 ? C38 C37 C42 C32 -4.6(16) . . . 3_656 ? C30 C37 C42 C32 176.9(7) . . . 3_656 ? C34 C37 C42 C32 -0.9(12) 3_656 . . 3_656 ? C36 C37 C42 C32 175.4(13) 3_656 . . 3_656 ? C30 C37 C42 C35 177(14) 3_656 . . 3_656 ? C38 C37 C42 C35 -1(13) . . . 3_656 ? C30 C37 C42 C35 -180(100) . . . 3_656 ? C34 C37 C42 C35 2(13) 3_656 . . 3_656 ? C36 C37 C42 C35 179(100) 3_656 . . 3_656 ? C30 C36 C42 C31 -175.7(16) 3_656 . . 3_656 ? C35 C36 C42 C31 -177.2(12) . . . 3_656 ? C37 C36 C42 C31 -177.3(10) 3_656 . . 3_656 ? C31 C36 C42 C30 175.7(16) 3_656 . . 3_656 ? C35 C36 C42 C30 -1.5(10) . . . 3_656 ? C37 C36 C42 C30 -1.5(10) 3_656 . . 3_656 ? C31 C36 C42 C37 177.7(16) 3_656 . . . ? C30 C36 C42 C37 2.0(7) 3_656 . . . ? C35 C36 C42 C37 0.5(8) . . . . ? C37 C36 C42 C37 0.5(11) 3_656 . . . ? C31 C36 C42 C41 -1.7(12) 3_656 . . . ? C30 C36 C42 C41 -177.4(18) 3_656 . . . ? C35 C36 C42 C41 -179.0(14) . . . . ? C37 C36 C42 C41 -179.0(13) 3_656 . . . ? C31 C36 C42 C32 1.1(7) 3_656 . . 3_656 ? C30 C36 C42 C32 -174.6(14) 3_656 . . 3_656 ? C35 C36 C42 C32 -176.2(9) . . . 3_656 ? C37 C36 C42 C32 -176.2(7) 3_656 . . 3_656 ? C31 C36 C42 C35 177.7(16) 3_656 . . 3_656 ? C30 C36 C42 C35 2.0(10) 3_656 . . 3_656 ? C35 C36 C42 C35 0.5(14) . . . 3_656 ? C37 C36 C42 C35 0.4(7) 3_656 . . 3_656 ? C31 C42 C41 C32 22(10) 3_656 . . 3_656 ? C30 C42 C41 C32 -139(10) 3_656 . . 3_656 ? C37 C42 C41 C32 -156(10) . . . 3_656 ? C36 C42 C41 C32 23(11) . . . 3_656 ? C35 C42 C41 C32 -156(10) 3_656 . . 3_656 ? C31 C42 C41 C33 174(3) 3_656 . . 3_656 ? C30 C42 C41 C33 14(13) 3_656 . . 3_656 ? C37 C42 C41 C33 -4(3) . . . 3_656 ? C36 C42 C41 C33 175.3(18) . . . 3_656 ? C32 C42 C41 C33 152(12) 3_656 . . 3_656 ? C35 C42 C41 C33 -4(3) 3_656 . . 3_656 ? C30 C42 C41 C31 -160(12) 3_656 . . 3_656 ? C37 C42 C41 C31 -178.0(16) . . . 3_656 ? C36 C42 C41 C31 1.5(11) . . . 3_656 ? C32 C42 C41 C31 -22(10) 3_656 . . 3_656 ? C35 C42 C41 C31 -178.0(14) 3_656 . . 3_656 ? C31 C42 C41 C40 177(2) 3_656 . . . ? C30 C42 C41 C40 17(13) 3_656 . . . ? C37 C42 C41 C40 -1(2) . . . . ? C36 C42 C41 C40 178.4(11) . . . . ? C32 C42 C41 C40 155(12) 3_656 . . . ? C35 C42 C41 C40 -1(2) 3_656 . . . ? C32 C41 C40 C33 149(12) 3_656 . . 3_656 ? C31 C41 C40 C33 -7(6) 3_656 . . 3_656 ? C42 C41 C40 C33 -10(5) . . . 3_656 ? C32 C41 C40 C39 162(8) 3_656 . . . ? C33 C41 C40 C39 13(5) 3_656 . . . ? C31 C41 C40 C39 7(4) 3_656 . . . ? C42 C41 C40 C39 3(2) . . . . ? C33 C41 C40 C32 -149(12) 3_656 . . 3_656 ? C31 C41 C40 C32 -156(12) 3_656 . . 3_656 ? C42 C41 C40 C32 -159(10) . . . 3_656 ? C32 C41 C40 C34 159(9) 3_656 . . 3_656 ? C33 C41 C40 C34 10(5) 3_656 . . 3_656 ? C31 C41 C40 C34 3(4) 3_656 . . 3_656 ? C42 C41 C40 C34 -0.6(16) . . . 3_656 ? C33 C40 C39 C34 7(6) 3_656 . . 3_656 ? C41 C40 C39 C34 -6.9(15) . . . 3_656 ? C32 C40 C39 C34 -3.8(17) 3_656 . . 3_656 ? C41 C40 C39 C33 -14(5) . . . 3_656 ? C32 C40 C39 C33 -11(5) 3_656 . . 3_656 ? C34 C40 C39 C33 -7(6) 3_656 . . 3_656 ? C33 C40 C39 C38 12(6) 3_656 . . . ? C41 C40 C39 C38 -2.5(15) . . . . ? C32 C40 C39 C38 0.6(19) 3_656 . . . ? C34 C40 C39 C38 4.5(11) 3_656 . . . ? C35 C37 C38 C34 -171(9) 3_656 . . 3_656 ? C30 C37 C38 C34 6(4) 3_656 . . 3_656 ? C42 C37 C38 C34 8(2) . . . 3_656 ? C30 C37 C38 C34 -174.2(19) . . . 3_656 ? C36 C37 C38 C34 -171.7(17) 3_656 . . 3_656 ? C30 C37 C38 C35 177(12) 3_656 . . 3_656 ? C42 C37 C38 C35 179(100) . . . 3_656 ? C30 C37 C38 C35 -4(8) . . . 3_656 ? C34 C37 C38 C35 171(9) 3_656 . . 3_656 ? C36 C37 C38 C35 -1(9) 3_656 . . 3_656 ? C35 C37 C38 C39 -177(9) 3_656 . . . ? C30 C37 C38 C39 0(4) 3_656 . . . ? C42 C37 C38 C39 2.1(16) . . . . ? C30 C37 C38 C39 179.6(13) . . . . ? C34 C37 C38 C39 -6.2(11) 3_656 . . . ? C36 C37 C38 C39 -177.9(8) 3_656 . . . ? C33 C39 C38 C34 -8(3) 3_656 . . 3_656 ? C40 C39 C38 C34 -11(3) . . . 3_656 ? C34 C39 C38 C35 10.4(19) 3_656 . . 3_656 ? C33 C39 C38 C35 2.7(19) 3_656 . . 3_656 ? C40 C39 C38 C35 -0.7(17) . . . 3_656 ? C34 C39 C38 C37 10.9(18) 3_656 . . . ? C33 C39 C38 C37 3.2(16) 3_656 . . . ? C40 C39 C38 C37 -0.1(14) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.221 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.044 #END data_TP-AO _database_code_depnum_ccdc_archive 'CCDC 751677' _audit_creation_method SHELXL-97 _chemical_name_systematic ; tetra(2,6-dimethyl-4-methoxyphenyl)pyrene ; _chemical_name_common tetra(2,6-dimethyl-4-methoxyphenyl)pyrene _chemical_melting_point ? _chemical_formula_moiety 'C52 H50 O4, 0.5(C14 H10), C8 H16' _chemical_formula_sum 'C67 H71 O4' _chemical_formula_weight 940.24 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' 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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 18.050(6) _cell_length_b 15.120(5) _cell_length_c 19.430(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.437(6) _cell_angle_gamma 90.00 _cell_volume 5245(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3977 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 23.24 _exptl_crystal_description square _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.191 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2020 _exptl_absorpt_coefficient_mu 0.072 _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 100(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 'Bruker SMART APEX' _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 26547 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9162 _reflns_number_gt 6113 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXS-97 _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^)+(0.0985P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9162 _refine_ls_number_parameters 714 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1003 _refine_ls_R_factor_gt 0.0673 _refine_ls_wR_factor_ref 0.1827 _refine_ls_wR_factor_gt 0.1645 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.132 _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 O4 O 0.29196(10) 0.39881(10) 0.23900(9) 0.0403(5) Uani 1 1 d . . . O1 O 0.90677(10) 0.42522(10) 0.38232(9) 0.0418(5) Uani 1 1 d . . . C14 C 0.68966(13) 0.08886(14) 0.36037(11) 0.0263(5) Uani 1 1 d . . . C10 C 0.45189(13) 0.08151(14) 0.31017(12) 0.0279(5) Uani 1 1 d . . . C13 C 0.64725(13) 0.16614(15) 0.33825(12) 0.0295(5) Uani 1 1 d . . . H13 H 0.6728 0.2206 0.3351 0.035 Uiso 1 1 calc R . . C44 C 0.40782(12) 0.16375(14) 0.28938(12) 0.0284(5) Uani 1 1 d . . . C7 C 0.53119(13) -0.07461(14) 0.35505(11) 0.0274(5) Uani 1 1 d . . . C16 C 0.57069(13) 0.00630(14) 0.34854(11) 0.0263(5) Uani 1 1 d . . . C9 C 0.41518(13) 0.00185(14) 0.31622(12) 0.0303(6) Uani 1 1 d . . . H9 H 0.3623 0.0001 0.3042 0.036 Uiso 1 1 calc R . . O3 O 0.29599(10) -0.38442(11) 0.39448(9) 0.0468(5) Uani 1 1 d . . . C12 C 0.57200(13) 0.16424(15) 0.32175(12) 0.0302(6) Uani 1 1 d . . . H12 H 0.5461 0.2171 0.3068 0.036 Uiso 1 1 calc R . . C11 C 0.53052(13) 0.08466(14) 0.32628(11) 0.0262(5) Uani 1 1 d . . . C21 C 0.86140(13) 0.29437(15) 0.31546(12) 0.0308(6) Uani 1 1 d . . . H21 H 0.8738 0.3185 0.2735 0.037 Uiso 1 1 calc R . . C17 C 0.80973(12) 0.17590(14) 0.37725(12) 0.0268(5) Uani 1 1 d . . . C5 C 0.64862(13) -0.15033(15) 0.39240(12) 0.0307(6) Uani 1 1 d . . . H5 H 0.6745 -0.2034 0.4067 0.037 Uiso 1 1 calc R . . C6 C 0.57365(13) -0.15191(15) 0.37694(12) 0.0305(6) Uani 1 1 d . . . H6 H 0.5480 -0.2062 0.3807 0.037 Uiso 1 1 calc R . . C35 C 0.40986(12) -0.15750(14) 0.35073(12) 0.0279(5) Uani 1 1 d . . . C4 C 0.69051(13) -0.07066(14) 0.38789(12) 0.0281(5) Uani 1 1 d . . . C2 C 0.80588(13) 0.01253(14) 0.39989(12) 0.0310(6) Uani 1 1 d . . . H2 H 0.8588 0.0141 0.4119 0.037 Uiso 1 1 calc R . . O2 O 0.92354(11) -0.38895(11) 0.46939(10) 0.0513(5) Uani 1 1 d . . . C20 C 0.87680(13) 0.34149(15) 0.37703(13) 0.0317(6) Uani 1 1 d . . . C30 C 0.85798(14) -0.26205(15) 0.50974(14) 0.0366(6) Uani 1 1 d . . . H30 H 0.8637 -0.2840 0.5560 0.044 Uiso 1 1 calc R . . C3 C 0.76918(13) -0.06695(15) 0.40437(12) 0.0296(5) Uani 1 1 d . . . C15 C 0.65027(13) 0.00855(14) 0.36557(11) 0.0264(5) Uani 1 1 d . . . C31 C 0.82028(13) -0.18187(15) 0.49304(13) 0.0331(6) Uani 1 1 d . . . C1 C 0.76810(13) 0.09067(14) 0.37839(12) 0.0286(5) Uani 1 1 d . . . C18 C 0.82779(13) 0.22347(15) 0.43956(12) 0.0319(6) Uani 1 1 d . . . C49 C 0.38483(14) 0.21803(15) 0.34069(13) 0.0332(6) Uani 1 1 d . . . C48 C 0.34537(14) 0.29528(16) 0.32155(13) 0.0367(6) Uani 1 1 d . . . H48 H 0.3292 0.3317 0.3563 0.044 Uiso 1 1 calc R . . C26 C 0.81234(12) -0.15044(14) 0.42502(12) 0.0293(5) Uani 1 1 d . . . C8 C 0.45251(13) -0.07558(14) 0.33912(11) 0.0275(5) Uani 1 1 d . . . C27 C 0.84319(13) -0.19699(15) 0.37373(13) 0.0337(6) Uani 1 1 d . . . C28 C 0.88051(14) -0.27602(16) 0.39144(14) 0.0382(6) Uani 1 1 d . . . H28 H 0.9019 -0.3078 0.3571 0.046 Uiso 1 1 calc R . . C36 C 0.39445(13) -0.17576(15) 0.41818(12) 0.0302(6) Uani 1 1 d . . . C37 C 0.35703(14) -0.25266(15) 0.43015(13) 0.0339(6) Uani 1 1 d . . . H37 H 0.3472 -0.2657 0.4758 0.041 Uiso 1 1 calc R . . C19 C 0.86183(14) 0.30496(16) 0.43844(13) 0.0359(6) Uani 1 1 d . . . H19 H 0.8752 0.3365 0.4808 0.043 Uiso 1 1 calc R . . C29 C 0.88685(14) -0.30904(16) 0.45848(14) 0.0382(6) Uani 1 1 d . . . C47 C 0.32938(13) 0.31961(15) 0.25222(13) 0.0309(6) Uani 1 1 d . . . C52 C 0.28155(15) 0.42936(17) 0.16956(13) 0.0407(6) Uani 1 1 d . . . H52A H 0.3298 0.4302 0.1522 0.061 Uiso 1 1 calc R . . H52B H 0.2606 0.4892 0.1677 0.061 Uiso 1 1 calc R . . H52C H 0.2470 0.3898 0.1406 0.061 Uiso 1 1 calc R . . C40 C 0.38665(13) -0.21676(15) 0.29670(13) 0.0322(6) Uani 1 1 d . . . C46 C 0.35093(13) 0.26591(15) 0.20185(13) 0.0344(6) Uani 1 1 d . . . H46 H 0.3388 0.2821 0.1543 0.041 Uiso 1 1 calc R . . C22 C 0.82740(13) 0.21098(15) 0.31526(12) 0.0291(5) Uani 1 1 d . . . C45 C 0.39046(13) 0.18786(15) 0.21941(12) 0.0320(6) Uani 1 1 d . . . C51 C 0.41289(16) 0.13185(17) 0.16173(14) 0.0481(7) Uani 1 1 d . . . H51A H 0.3737 0.1347 0.1211 0.072 Uiso 1 1 calc R . . H51B H 0.4195 0.0704 0.1775 0.072 Uiso 1 1 calc R . . H51C H 0.4601 0.1540 0.1490 0.072 Uiso 1 1 calc R . . C23 C 0.81085(15) 0.15987(17) 0.24852(13) 0.0404(6) Uani 1 1 d . . . H23A H 0.8346 0.1015 0.2545 0.061 Uiso 1 1 calc R . . H23B H 0.8306 0.1920 0.2114 0.061 Uiso 1 1 calc R . . H23C H 0.7566 0.1527 0.2362 0.061 Uiso 1 1 calc R . . C33 C 0.83533(15) -0.16305(17) 0.30044(13) 0.0429(7) Uani 1 1 d . . . H33A H 0.8606 -0.2035 0.2721 0.064 Uiso 1 1 calc R . . H33B H 0.8582 -0.1043 0.3002 0.064 Uiso 1 1 calc R . . H33C H 0.7821 -0.1592 0.2812 0.064 Uiso 1 1 calc R . . C42 C 0.41556(15) -0.11060(16) 0.47687(13) 0.0410(7) Uani 1 1 d . . . H42A H 0.3853 -0.0569 0.4679 0.061 Uiso 1 1 calc R . . H42B H 0.4688 -0.0956 0.4800 0.061 Uiso 1 1 calc R . . H42C H 0.4063 -0.1372 0.5208 0.061 Uiso 1 1 calc R . . C25 C 0.91320(16) 0.47029(16) 0.32002(14) 0.0447(7) Uani 1 1 d . . . H25A H 0.9503 0.4404 0.2960 0.067 Uiso 1 1 calc R . . H25B H 0.9292 0.5313 0.3306 0.067 Uiso 1 1 calc R . . H25C H 0.8646 0.4705 0.2900 0.067 Uiso 1 1 calc R . . C32 C 0.79195(15) -0.13029(17) 0.54957(14) 0.0433(7) Uani 1 1 d . . . H32A H 0.8259 -0.0808 0.5635 0.065 Uiso 1 1 calc R . . H32B H 0.7896 -0.1689 0.5897 0.065 Uiso 1 1 calc R . . H32C H 0.7418 -0.1074 0.5325 0.065 Uiso 1 1 calc R . . C38 C 0.33361(14) -0.31108(15) 0.37641(13) 0.0354(6) Uani 1 1 d . . . C39 C 0.34832(14) -0.29349(15) 0.30973(13) 0.0353(6) Uani 1 1 d . . . H39 H 0.3323 -0.3337 0.2730 0.042 Uiso 1 1 calc R . . C34 C 0.92114(17) -0.43161(18) 0.53445(16) 0.0562(8) Uani 1 1 d . . . H34A H 0.9463 -0.3945 0.5722 0.084 Uiso 1 1 calc R . . H34B H 0.9466 -0.4889 0.5349 0.084 Uiso 1 1 calc R . . H34C H 0.8689 -0.4408 0.5410 0.084 Uiso 1 1 calc R . . C43 C 0.27919(17) -0.45114(17) 0.34331(15) 0.0524(8) Uani 1 1 d . . . H43A H 0.2450 -0.4274 0.3038 0.079 Uiso 1 1 calc R . . H43B H 0.2555 -0.5013 0.3634 0.079 Uiso 1 1 calc R . . H43C H 0.3255 -0.4708 0.3274 0.079 Uiso 1 1 calc R . . C24 C 0.80987(15) 0.18747(17) 0.50733(13) 0.0420(7) Uani 1 1 d . . . H24A H 0.8489 0.1455 0.5266 0.063 Uiso 1 1 calc R . . H24B H 0.7614 0.1572 0.4994 0.063 Uiso 1 1 calc R . . H24C H 0.8077 0.2362 0.5402 0.063 Uiso 1 1 calc R . . C41 C 0.40137(17) -0.19792(18) 0.22377(13) 0.0477(7) Uani 1 1 d . . . H41A H 0.3824 -0.2469 0.1932 0.072 Uiso 1 1 calc R . . H41B H 0.4554 -0.1915 0.2237 0.072 Uiso 1 1 calc R . . H41C H 0.3759 -0.1431 0.2070 0.072 Uiso 1 1 calc R . . C50 C 0.40447(17) 0.19531(18) 0.41669(13) 0.0500(7) Uani 1 1 d . . . H50A H 0.4569 0.2106 0.4326 0.075 Uiso 1 1 calc R . . H50B H 0.3971 0.1318 0.4232 0.075 Uiso 1 1 calc R . . H50C H 0.3721 0.2287 0.4437 0.075 Uiso 1 1 calc R . . C53 C 0.49548(14) 0.5547(2) 0.05859(19) 0.0542(8) Uani 1 1 d . . . C57 C 0.48503(16) 0.4227(2) 0.1296(2) 0.0641(9) Uani 1 1 d . . . H57 H 0.4830 0.3602 0.1341 0.077 Uiso 1 1 calc R . . C59 C 0.50278(14) 0.5913(2) -0.0052(2) 0.0582(9) Uani 1 1 d . . . H59 H 0.5043 0.6538 -0.0092 0.070 Uiso 1 1 calc R . . C58 C 0.49197(15) 0.4599(2) 0.06378(19) 0.0551(8) Uani 1 1 d . . . C54 C 0.49278(16) 0.6065(2) 0.1192(2) 0.0632(9) Uani 1 1 d . . . H54 H 0.4959 0.6691 0.1164 0.076 Uiso 1 1 calc R . . C56 C 0.48126(17) 0.4742(2) 0.1862(2) 0.0708(10) Uani 1 1 d . . . H56 H 0.4756 0.4476 0.2295 0.085 Uiso 1 1 calc R . . C55 C 0.48575(18) 0.5678(2) 0.1810(2) 0.0702(10) Uani 1 1 d . . . H55 H 0.4838 0.6035 0.2209 0.084 Uiso 1 1 calc R . . C60 C 0.7865(4) 1.0016(4) 0.0621(3) 0.063(2) Uani 0.524(6) 1 d PD A 1 H60A H 0.7321 1.0074 0.0633 0.076 Uiso 0.524(6) 1 calc PR A 1 H60B H 0.7927 0.9645 0.0213 0.076 Uiso 0.524(6) 1 calc PR A 1 C61 C 0.8176(3) 1.0916(4) 0.0515(4) 0.062(2) Uani 0.524(6) 1 d PD A 1 H61A H 0.7886 1.1163 0.0086 0.074 Uiso 0.524(6) 1 calc PR A 1 H61B H 0.8068 1.1291 0.0906 0.074 Uiso 0.524(6) 1 calc PR A 1 C62 C 0.8986(3) 1.1031(5) 0.0457(3) 0.047(2) Uani 0.524(6) 1 d PD A 1 H62A H 0.9057 1.1637 0.0284 0.056 Uiso 0.524(6) 1 calc PR A 1 H62B H 0.9114 1.0614 0.0100 0.056 Uiso 0.524(6) 1 calc PR A 1 C63 C 0.9538(3) 1.0894(4) 0.1112(3) 0.050(2) Uani 0.524(6) 1 d PD A 1 H63A H 0.9267 1.0943 0.1519 0.060 Uiso 0.524(6) 1 calc PR A 1 H63B H 0.9915 1.1375 0.1149 0.060 Uiso 0.524(6) 1 calc PR A 1 C64 C 0.9941(3) 1.0016(4) 0.1148(4) 0.113(6) Uani 0.524(6) 1 d PD A 1 H64A H 1.0390 1.0074 0.0914 0.135 Uiso 0.524(6) 1 calc PR A 1 H64B H 1.0114 0.9868 0.1642 0.135 Uiso 0.524(6) 1 calc PR A 1 C65 C 0.9467(4) 0.9268(4) 0.0817(4) 0.072(3) Uani 0.524(6) 1 d PD A 1 H65A H 0.9218 0.9459 0.0353 0.086 Uiso 0.524(6) 1 calc PR A 1 H65B H 0.9796 0.8762 0.0748 0.086 Uiso 0.524(6) 1 calc PR A 1 C66 C 0.8878(4) 0.8963(5) 0.1237(5) 0.101(4) Uani 0.524(6) 1 d PD A 1 H66A H 0.8694 0.8380 0.1053 0.122 Uiso 0.524(6) 1 calc PR A 1 H66B H 0.9125 0.8868 0.1721 0.122 Uiso 0.524(6) 1 calc PR A 1 C67 C 0.8210(4) 0.9542(6) 0.1264(4) 0.094(4) Uani 0.524(6) 1 d PD A 1 H67A H 0.7815 0.9173 0.1423 0.112 Uiso 0.524(6) 1 calc PR A 1 H67B H 0.8354 0.9994 0.1628 0.112 Uiso 0.524(6) 1 calc PR A 1 C60A C 0.7980(5) 1.0028(6) 0.1010(5) 0.136(8) Uani 0.476(6) 1 d PD A 2 H60A H 0.8338 1.0266 0.1401 0.164 Uiso 0.476(6) 1 calc PR A 2 H60B H 0.7476 1.0035 0.1153 0.164 Uiso 0.476(6) 1 calc PR A 2 C61A C 0.7975(6) 1.0633(6) 0.0389(6) 0.215(13) Uani 0.476(6) 1 d PD A 2 H61A H 0.7639 1.0377 -0.0010 0.257 Uiso 0.476(6) 1 calc PR A 2 H61B H 0.7763 1.1211 0.0499 0.257 Uiso 0.476(6) 1 calc PR A 2 C62A C 0.8736(8) 1.0786(8) 0.0174(5) 0.261(15) Uani 0.476(6) 1 d PD A 2 H62A H 0.8703 1.1284 -0.0159 0.314 Uiso 0.476(6) 1 calc PR A 2 H62B H 0.8886 1.0252 -0.0066 0.314 Uiso 0.476(6) 1 calc PR A 2 C63A C 0.9332(7) 1.0992(6) 0.0790(7) 0.222(14) Uani 0.476(6) 1 d PD A 2 H63A H 0.9628 1.1508 0.0674 0.267 Uiso 0.476(6) 1 calc PR A 2 H63B H 0.9084 1.1155 0.1194 0.267 Uiso 0.476(6) 1 calc PR A 2 C64A C 0.9858(5) 1.0220(7) 0.0990(6) 0.151(8) Uani 0.476(6) 1 d PD A 2 H64A H 1.0310 1.0445 0.1289 0.182 Uiso 0.476(6) 1 calc PR A 2 H64B H 1.0019 0.9979 0.0562 0.182 Uiso 0.476(6) 1 calc PR A 2 C65A C 0.9530(6) 0.9470(8) 0.1371(5) 0.233(11) Uani 0.476(6) 1 d PD A 2 H65A H 0.9940 0.9095 0.1608 0.280 Uiso 0.476(6) 1 calc PR A 2 H65B H 0.9250 0.9716 0.1729 0.280 Uiso 0.476(6) 1 calc PR A 2 C66A C 0.9010(4) 0.8915(4) 0.0861(5) 0.088(4) Uani 0.476(6) 1 d PD A 2 H66A H 0.9118 0.9035 0.0385 0.105 Uiso 0.476(6) 1 calc PR A 2 H66B H 0.9116 0.8282 0.0963 0.105 Uiso 0.476(6) 1 calc PR A 2 C67A C 0.8188(4) 0.9086(5) 0.0882(5) 0.066(3) Uani 0.476(6) 1 d PD A 2 H67A H 0.7901 0.8892 0.0434 0.079 Uiso 0.476(6) 1 calc PR A 2 H67B H 0.8028 0.8712 0.1252 0.079 Uiso 0.476(6) 1 calc PR A 2 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 O4 0.0441(11) 0.0344(10) 0.0420(11) 0.0043(8) 0.0047(8) 0.0101(8) O1 0.0491(12) 0.0348(10) 0.0407(11) -0.0007(8) 0.0040(8) -0.0127(8) C14 0.0267(13) 0.0263(12) 0.0260(13) -0.0010(10) 0.0040(10) -0.0001(10) C10 0.0263(13) 0.0303(13) 0.0268(13) 0.0011(10) 0.0031(10) -0.0009(10) C13 0.0292(14) 0.0283(13) 0.0314(13) 0.0024(10) 0.0056(10) -0.0028(11) C44 0.0190(12) 0.0306(13) 0.0354(14) 0.0013(11) 0.0033(10) -0.0023(10) C7 0.0273(13) 0.0287(12) 0.0259(13) -0.0006(10) 0.0026(10) 0.0003(10) C16 0.0249(13) 0.0301(13) 0.0236(13) -0.0017(10) 0.0022(9) 0.0012(10) C9 0.0219(13) 0.0355(14) 0.0329(14) 0.0031(11) 0.0026(10) -0.0012(11) O3 0.0537(12) 0.0342(10) 0.0538(12) -0.0009(9) 0.0120(9) -0.0134(9) C12 0.0312(14) 0.0273(13) 0.0322(14) 0.0056(10) 0.0046(11) 0.0027(11) C11 0.0252(13) 0.0284(12) 0.0251(13) 0.0006(10) 0.0038(9) -0.0001(10) C21 0.0249(13) 0.0356(14) 0.0322(14) 0.0037(11) 0.0049(10) -0.0023(11) C17 0.0189(12) 0.0282(12) 0.0330(14) -0.0003(10) 0.0027(10) 0.0015(10) C5 0.0312(14) 0.0274(13) 0.0329(14) -0.0003(10) 0.0019(11) 0.0008(11) C6 0.0327(14) 0.0279(13) 0.0307(13) -0.0001(10) 0.0038(10) -0.0028(11) C35 0.0218(12) 0.0283(12) 0.0328(14) 0.0019(10) 0.0021(10) -0.0010(10) C4 0.0276(13) 0.0272(12) 0.0286(13) -0.0012(10) 0.0013(10) 0.0007(10) C2 0.0235(13) 0.0329(14) 0.0354(14) -0.0025(11) 0.0005(10) -0.0021(11) O2 0.0503(12) 0.0322(10) 0.0687(14) 0.0015(9) -0.0008(10) 0.0134(9) C20 0.0248(13) 0.0289(13) 0.0400(15) -0.0025(11) 0.0000(11) -0.0035(10) C30 0.0290(14) 0.0339(14) 0.0440(16) 0.0027(12) -0.0044(11) -0.0008(11) C3 0.0266(13) 0.0303(13) 0.0304(13) -0.0035(10) -0.0006(10) 0.0020(10) C15 0.0247(13) 0.0300(13) 0.0237(13) 0.0009(10) 0.0004(9) -0.0014(10) C31 0.0245(13) 0.0318(13) 0.0413(16) -0.0012(11) -0.0012(11) -0.0029(11) C1 0.0269(13) 0.0290(13) 0.0299(13) -0.0021(10) 0.0037(10) -0.0025(10) C18 0.0292(14) 0.0329(13) 0.0333(14) -0.0001(11) 0.0028(11) -0.0011(11) C49 0.0340(14) 0.0310(13) 0.0342(14) 0.0005(11) 0.0032(11) -0.0042(11) C48 0.0408(15) 0.0338(14) 0.0364(15) -0.0037(11) 0.0081(12) 0.0061(12) C26 0.0197(12) 0.0286(13) 0.0377(14) -0.0023(11) -0.0023(10) -0.0006(10) C8 0.0262(13) 0.0288(13) 0.0268(13) -0.0005(10) 0.0019(10) -0.0007(10) C27 0.0275(14) 0.0328(13) 0.0386(15) -0.0089(11) -0.0022(11) -0.0011(11) C28 0.0301(14) 0.0362(14) 0.0468(17) -0.0102(12) 0.0009(12) 0.0047(11) C36 0.0275(13) 0.0305(13) 0.0317(14) 0.0023(11) 0.0018(10) 0.0022(11) C37 0.0367(15) 0.0326(13) 0.0326(14) 0.0024(11) 0.0060(11) 0.0025(12) C19 0.0360(15) 0.0375(14) 0.0327(15) -0.0056(11) 0.0002(11) -0.0044(12) C29 0.0306(14) 0.0295(14) 0.0514(18) -0.0032(12) -0.0044(12) 0.0011(11) C47 0.0258(13) 0.0302(13) 0.0365(15) 0.0006(11) 0.0037(11) 0.0013(11) C52 0.0334(15) 0.0417(15) 0.0475(17) 0.0103(13) 0.0082(12) 0.0114(12) C40 0.0279(13) 0.0339(14) 0.0348(14) -0.0031(11) 0.0045(11) 0.0000(11) C46 0.0323(14) 0.0392(14) 0.0307(14) 0.0043(11) 0.0014(11) 0.0065(12) C22 0.0236(13) 0.0301(13) 0.0326(14) -0.0025(11) 0.0005(10) 0.0013(10) C45 0.0240(13) 0.0368(14) 0.0345(14) 0.0042(11) 0.0026(10) 0.0026(11) C51 0.0536(18) 0.0524(17) 0.0400(16) 0.0031(13) 0.0124(13) 0.0238(14) C23 0.0416(16) 0.0436(15) 0.0363(15) -0.0045(12) 0.0073(12) -0.0042(12) C33 0.0369(15) 0.0480(16) 0.0424(16) -0.0087(13) 0.0015(12) 0.0053(13) C42 0.0455(16) 0.0427(15) 0.0346(15) -0.0010(12) 0.0053(12) -0.0042(13) C25 0.0501(18) 0.0376(14) 0.0472(17) 0.0042(13) 0.0096(13) -0.0079(13) C32 0.0426(16) 0.0439(15) 0.0429(16) 0.0035(13) 0.0044(12) 0.0071(13) C38 0.0311(14) 0.0295(13) 0.0455(16) 0.0026(12) 0.0052(12) -0.0021(11) C39 0.0310(14) 0.0333(14) 0.0406(15) -0.0075(12) 0.0025(11) -0.0042(11) C34 0.0498(19) 0.0395(16) 0.076(2) 0.0116(15) -0.0025(16) 0.0128(14) C43 0.061(2) 0.0346(15) 0.061(2) -0.0057(14) 0.0102(15) -0.0138(14) C24 0.0443(16) 0.0464(16) 0.0354(15) -0.0019(12) 0.0060(12) -0.0074(13) C41 0.0561(19) 0.0509(17) 0.0372(16) -0.0064(13) 0.0100(13) -0.0109(14) C50 0.066(2) 0.0499(17) 0.0330(16) 0.0005(13) 0.0032(14) 0.0109(15) C53 0.0188(14) 0.0502(18) 0.090(3) -0.0085(18) -0.0050(14) 0.0022(13) C57 0.0322(17) 0.057(2) 0.100(3) 0.001(2) -0.0018(17) 0.0039(15) C59 0.0222(15) 0.0396(17) 0.109(3) -0.0065(19) -0.0044(16) 0.0029(13) C58 0.0220(15) 0.0455(18) 0.095(3) -0.0055(18) -0.0021(15) 0.0012(13) C54 0.0314(17) 0.0539(19) 0.099(3) -0.016(2) -0.0072(17) 0.0063(14) C56 0.0389(19) 0.073(2) 0.096(3) 0.001(2) -0.0052(18) 0.0015(17) C55 0.0400(19) 0.075(3) 0.090(3) -0.016(2) -0.0110(18) 0.0081(17) C60 0.075(5) 0.074(5) 0.039(4) -0.005(4) 0.003(4) -0.009(4) C61 0.057(5) 0.042(4) 0.075(6) -0.001(4) -0.024(4) -0.015(3) C62 0.089(5) 0.043(4) 0.008(4) 0.002(3) 0.002(3) -0.002(4) C63 0.034(3) 0.063(5) 0.053(5) -0.012(3) 0.005(3) 0.006(3) C64 0.097(7) 0.100(8) 0.165(10) 0.109(8) 0.097(7) 0.054(7) C65 0.062(5) 0.012(3) 0.151(8) -0.008(4) 0.048(5) 0.008(3) C66 0.093(8) 0.097(8) 0.113(9) 0.073(7) 0.009(7) 0.002(6) C67 0.094(9) 0.111(8) 0.071(7) 0.046(6) -0.005(6) -0.059(7) C60A 0.041(6) 0.29(2) 0.087(10) -0.144(13) 0.024(7) -0.044(10) C61A 0.224(19) 0.063(9) 0.29(2) -0.081(11) -0.194(17) 0.043(10) C62A 0.54(4) 0.214(17) 0.028(7) 0.048(8) 0.020(12) 0.27(2) C63A 0.48(4) 0.100(12) 0.116(15) -0.089(10) 0.147(17) -0.196(18) C64A 0.219(18) 0.100(10) 0.126(11) -0.030(9) -0.006(10) -0.138(12) C65A 0.152(16) 0.40(3) 0.119(12) -0.071(17) -0.071(12) 0.041(19) C66A 0.135(11) 0.019(4) 0.104(9) -0.004(5) -0.002(8) -0.010(5) C67A 0.048(5) 0.074(6) 0.070(6) 0.019(4) -0.008(4) -0.025(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 O4 C47 1.380(3) . ? O4 C52 1.412(3) . ? O1 C20 1.375(3) . ? O1 C25 1.409(3) . ? C14 C1 1.408(3) . ? C14 C15 1.418(3) . ? C14 C13 1.428(3) . ? C10 C9 1.388(3) . ? C10 C11 1.409(3) . ? C10 C44 1.499(3) . ? C13 C12 1.349(3) . ? C13 H13 0.9500 . ? C44 C45 1.398(3) . ? C44 C49 1.400(3) . ? C7 C8 1.409(3) . ? C7 C6 1.428(3) . ? C7 C16 1.431(3) . ? C16 C11 1.423(3) . ? C16 C15 1.426(3) . ? C9 C8 1.391(3) . ? C9 H9 0.9500 . ? O3 C38 1.372(3) . ? O3 C43 1.418(3) . ? C12 C11 1.427(3) . ? C12 H12 0.9500 . ? C21 C20 1.385(3) . ? C21 C22 1.402(3) . ? C21 H21 0.9500 . ? C17 C22 1.395(3) . ? C17 C18 1.405(3) . ? C17 C1 1.494(3) . ? C5 C6 1.343(3) . ? C5 C4 1.432(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C35 C40 1.397(3) . ? C35 C36 1.406(3) . ? C35 C8 1.493(3) . ? C4 C3 1.410(3) . ? C4 C15 1.434(3) . ? C2 C3 1.381(3) . ? C2 C1 1.397(3) . ? C2 H2 0.9500 . ? O2 C29 1.379(3) . ? O2 C34 1.425(3) . ? C20 C19 1.377(3) . ? C30 C29 1.386(4) . ? C30 C31 1.405(3) . ? C30 H30 0.9500 . ? C3 C26 1.507(3) . ? C31 C26 1.392(3) . ? C31 C32 1.497(3) . ? C18 C19 1.378(3) . ? C18 C24 1.503(3) . ? C49 C48 1.390(3) . ? C49 C50 1.507(3) . ? C48 C47 1.385(3) . ? C48 H48 0.9500 . ? C26 C27 1.401(3) . ? C27 C28 1.390(3) . ? C27 C33 1.501(3) . ? C28 C29 1.384(4) . ? C28 H28 0.9500 . ? C36 C37 1.382(3) . ? C36 C42 1.513(3) . ? C37 C38 1.386(3) . ? C37 H37 0.9500 . ? C19 H19 0.9500 . ? C47 C46 1.371(3) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C40 C39 1.393(3) . ? C40 C41 1.507(3) . ? C46 C45 1.395(3) . ? C46 H46 0.9500 . ? C22 C23 1.501(3) . ? C45 C51 1.507(3) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C38 C39 1.386(3) . ? C39 H39 0.9500 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C53 C59 1.381(4) . ? C53 C54 1.421(5) . ? C53 C58 1.439(4) . ? C57 C56 1.358(5) . ? C57 C58 1.419(5) . ? C57 H57 0.9500 . ? C59 C58 1.391(4) 3_665 ? C59 H59 0.9500 . ? C58 C59 1.391(4) 3_665 ? C54 C55 1.358(5) . ? C54 H54 0.9500 . ? C56 C55 1.423(5) . ? C56 H56 0.9500 . ? C55 H55 0.9500 . ? C60 C67 1.494(4) . ? C60 C61 1.498(4) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.493(4) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.511(4) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.511(4) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.506(4) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.504(4) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C67 1.497(4) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C60A C67A 1.503(4) . ? C60A C61A 1.512(4) . ? C60A H60A 0.9900 . ? C60A H60B 0.9900 . ? C61A C62A 1.512(4) . ? C61A H61A 0.9900 . ? C61A H61B 0.9900 . ? C62A C63A 1.519(4) . ? C62A H62A 0.9900 . ? C62A H62B 0.9900 . ? C63A C64A 1.518(4) . ? C63A H63A 0.9900 . ? C63A H63B 0.9900 . ? C64A C65A 1.520(4) . ? C64A H64A 0.9900 . ? C64A H64B 0.9900 . ? C65A C66A 1.514(4) . ? C65A H65A 0.9900 . ? C65A H65B 0.9900 . ? C66A C67A 1.512(4) . ? C66A H66A 0.9900 . ? C66A H66B 0.9900 . ? C67A H67A 0.9900 . ? C67A H67B 0.9900 . ? 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 C47 O4 C52 117.02(18) . . ? C20 O1 C25 117.53(18) . . ? C1 C14 C15 119.7(2) . . ? C1 C14 C13 122.3(2) . . ? C15 C14 C13 118.0(2) . . ? C9 C10 C11 119.2(2) . . ? C9 C10 C44 120.1(2) . . ? C11 C10 C44 120.61(19) . . ? C12 C13 C14 122.0(2) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C45 C44 C49 119.5(2) . . ? C45 C44 C10 120.8(2) . . ? C49 C44 C10 119.7(2) . . ? C8 C7 C6 122.5(2) . . ? C8 C7 C16 119.3(2) . . ? C6 C7 C16 118.3(2) . . ? C11 C16 C15 120.10(19) . . ? C11 C16 C7 120.0(2) . . ? C15 C16 C7 119.9(2) . . ? C10 C9 C8 122.9(2) . . ? C10 C9 H9 118.6 . . ? C8 C9 H9 118.6 . . ? C38 O3 C43 117.3(2) . . ? C13 C12 C11 121.5(2) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C10 C11 C16 119.4(2) . . ? C10 C11 C12 122.4(2) . . ? C16 C11 C12 118.2(2) . . ? C20 C21 C22 119.8(2) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C22 C17 C18 119.7(2) . . ? C22 C17 C1 121.3(2) . . ? C18 C17 C1 118.8(2) . . ? C6 C5 C4 121.7(2) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 122.1(2) . . ? C5 C6 H6 119.0 . . ? C7 C6 H6 119.0 . . ? C40 C35 C36 119.7(2) . . ? C40 C35 C8 121.5(2) . . ? C36 C35 C8 118.7(2) . . ? C3 C4 C5 122.9(2) . . ? C3 C4 C15 118.9(2) . . ? C5 C4 C15 118.2(2) . . ? C3 C2 C1 122.5(2) . . ? C3 C2 H2 118.8 . . ? C1 C2 H2 118.8 . . ? C29 O2 C34 117.2(2) . . ? O1 C20 C19 115.4(2) . . ? O1 C20 C21 124.4(2) . . ? C19 C20 C21 120.1(2) . . ? C29 C30 C31 119.8(2) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C2 C3 C4 119.8(2) . . ? C2 C3 C26 120.8(2) . . ? C4 C3 C26 119.4(2) . . ? C14 C15 C16 120.2(2) . . ? C14 C15 C4 120.0(2) . . ? C16 C15 C4 119.88(19) . . ? C26 C31 C30 119.5(2) . . ? C26 C31 C32 121.3(2) . . ? C30 C31 C32 119.1(2) . . ? C2 C1 C14 119.1(2) . . ? C2 C1 C17 120.6(2) . . ? C14 C1 C17 120.18(19) . . ? C19 C18 C17 119.4(2) . . ? C19 C18 C24 119.4(2) . . ? C17 C18 C24 121.1(2) . . ? C48 C49 C44 119.7(2) . . ? C48 C49 C50 119.4(2) . . ? C44 C49 C50 120.8(2) . . ? C47 C48 C49 120.6(2) . . ? C47 C48 H48 119.7 . . ? C49 C48 H48 119.7 . . ? C31 C26 C27 120.5(2) . . ? C31 C26 C3 121.1(2) . . ? C27 C26 C3 118.4(2) . . ? C9 C8 C7 119.1(2) . . ? C9 C8 C35 120.7(2) . . ? C7 C8 C35 120.08(19) . . ? C28 C27 C26 119.0(2) . . ? C28 C27 C33 120.3(2) . . ? C26 C27 C33 120.7(2) . . ? C29 C28 C27 120.9(2) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C37 C36 C35 119.4(2) . . ? C37 C36 C42 119.8(2) . . ? C35 C36 C42 120.8(2) . . ? C36 C37 C38 120.8(2) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C20 C19 C18 121.1(2) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? O2 C29 C28 115.6(2) . . ? O2 C29 C30 124.1(2) . . ? C28 C29 C30 120.2(2) . . ? C46 C47 O4 124.3(2) . . ? C46 C47 C48 119.8(2) . . ? O4 C47 C48 116.0(2) . . ? O4 C52 H52A 109.5 . . ? O4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? O4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C39 C40 C35 120.0(2) . . ? C39 C40 C41 119.3(2) . . ? C35 C40 C41 120.7(2) . . ? C47 C46 C45 121.0(2) . . ? C47 C46 H46 119.5 . . ? C45 C46 H46 119.5 . . ? C17 C22 C21 119.7(2) . . ? C17 C22 C23 120.5(2) . . ? C21 C22 C23 119.8(2) . . ? C46 C45 C44 119.5(2) . . ? C46 C45 C51 118.5(2) . . ? C44 C45 C51 122.0(2) . . ? C45 C51 H51A 109.5 . . ? C45 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C45 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C27 C33 H33A 109.5 . . ? C27 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C27 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C36 C42 H42A 109.5 . . ? C36 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C36 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O1 C25 H25A 109.5 . . ? O1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O3 C38 C37 115.5(2) . . ? O3 C38 C39 124.3(2) . . ? C37 C38 C39 120.2(2) . . ? C38 C39 C40 119.9(2) . . ? C38 C39 H39 120.1 . . ? C40 C39 H39 120.1 . . ? O2 C34 H34A 109.5 . . ? O2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? O2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O3 C43 H43A 109.5 . . ? O3 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? O3 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C18 C24 H24A 109.5 . . ? C18 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C18 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C59 C53 C54 122.8(3) . . ? C59 C53 C58 118.2(3) . . ? C54 C53 C58 118.9(3) . . ? C56 C57 C58 121.7(3) . . ? C56 C57 H57 119.2 . . ? C58 C57 H57 119.2 . . ? C53 C59 C58 122.6(3) . 3_665 ? C53 C59 H59 118.7 . . ? C58 C59 H59 118.7 3_665 . ? C59 C58 C57 122.9(3) 3_665 . ? C59 C58 C53 119.2(3) 3_665 . ? C57 C58 C53 117.9(3) . . ? C55 C54 C53 121.0(3) . . ? C55 C54 H54 119.5 . . ? C53 C54 H54 119.5 . . ? C57 C56 C55 120.1(4) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C54 C55 C56 120.4(3) . . ? C54 C55 H55 119.8 . . ? C56 C55 H55 119.8 . . ? C67 C60 C61 115.5(5) . . ? C67 C60 H60A 108.4 . . ? C61 C60 H60A 108.4 . . ? C67 C60 H60B 108.4 . . ? C61 C60 H60B 108.4 . . ? H60A C60 H60B 107.5 . . ? C62 C61 C60 120.5(5) . . ? C62 C61 H61A 107.2 . . ? C60 C61 H61A 107.2 . . ? C62 C61 H61B 107.2 . . ? C60 C61 H61B 107.2 . . ? H61A C61 H61B 106.8 . . ? C61 C62 C63 116.9(5) . . ? C61 C62 H62A 108.1 . . ? C63 C62 H62A 108.1 . . ? C61 C62 H62B 108.1 . . ? C63 C62 H62B 108.1 . . ? H62A C62 H62B 107.3 . . ? C62 C63 C64 114.4(5) . . ? C62 C63 H63A 108.7 . . ? C64 C63 H63A 108.7 . . ? C62 C63 H63B 108.7 . . ? C64 C63 H63B 108.7 . . ? H63A C63 H63B 107.6 . . ? C65 C64 C63 113.6(4) . . ? C65 C64 H64A 108.8 . . ? C63 C64 H64A 108.8 . . ? C65 C64 H64B 108.8 . . ? C63 C64 H64B 108.8 . . ? H64A C64 H64B 107.7 . . ? C66 C65 C64 113.7(5) . . ? C66 C65 H65A 108.8 . . ? C64 C65 H65A 108.8 . . ? C66 C65 H65B 108.8 . . ? C64 C65 H65B 108.8 . . ? H65A C65 H65B 107.7 . . ? C67 C66 C65 118.4(5) . . ? C67 C66 H66A 107.7 . . ? C65 C66 H66A 107.7 . . ? C67 C66 H66B 107.7 . . ? C65 C66 H66B 107.7 . . ? H66A C66 H66B 107.1 . . ? C60 C67 C66 119.4(5) . . ? C60 C67 H67A 107.5 . . ? C66 C67 H67A 107.5 . . ? C60 C67 H67B 107.5 . . ? C66 C67 H67B 107.5 . . ? H67A C67 H67B 107.0 . . ? C67A C60A C61A 114.5(5) . . ? C67A C60A H60A 108.6 . . ? C61A C60A H60A 108.6 . . ? C67A C60A H60B 108.6 . . ? C61A C60A H60B 108.6 . . ? H60A C60A H60B 107.6 . . ? C62A C61A C60A 114.4(5) . . ? C62A C61A H61A 108.6 . . ? C60A C61A H61A 108.6 . . ? C62A C61A H61B 108.6 . . ? C60A C61A H61B 108.6 . . ? H61A C61A H61B 107.6 . . ? C61A C62A C63A 112.4(6) . . ? C61A C62A H62A 109.1 . . ? C63A C62A H62A 109.1 . . ? C61A C62A H62B 109.1 . . ? C63A C62A H62B 109.1 . . ? H62A C62A H62B 107.9 . . ? C64A C63A C62A 112.8(6) . . ? C64A C63A H63A 109.0 . . ? C62A C63A H63A 109.0 . . ? C64A C63A H63B 109.0 . . ? C62A C63A H63B 109.0 . . ? H63A C63A H63B 107.8 . . ? C63A C64A C65A 115.2(6) . . ? C63A C64A H64A 108.5 . . ? C65A C64A H64A 108.5 . . ? C63A C64A H64B 108.5 . . ? C65A C64A H64B 108.5 . . ? H64A C64A H64B 107.5 . . ? C66A C65A C64A 110.1(6) . . ? C66A C65A H65A 109.6 . . ? C64A C65A H65A 109.6 . . ? C66A C65A H65B 109.6 . . ? C64A C65A H65B 109.6 . . ? H65A C65A H65B 108.2 . . ? C67A C66A C65A 113.9(6) . . ? C67A C66A H66A 108.8 . . ? C65A C66A H66A 108.8 . . ? C67A C66A H66B 108.8 . . ? C65A C66A H66B 108.8 . . ? H66A C66A H66B 107.7 . . ? C60A C67A C66A 115.9(5) . . ? C60A C67A H67A 108.3 . . ? C66A C67A H67A 108.3 . . ? C60A C67A H67B 108.3 . . ? C66A C67A H67B 108.3 . . ? H67A C67A H67B 107.4 . . ? 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 C1 C14 C13 C12 -179.3(2) . . . . ? C15 C14 C13 C12 -0.7(3) . . . . ? C9 C10 C44 C45 -90.8(3) . . . . ? C11 C10 C44 C45 91.6(3) . . . . ? C9 C10 C44 C49 90.4(3) . . . . ? C11 C10 C44 C49 -87.2(3) . . . . ? C8 C7 C16 C11 0.1(3) . . . . ? C6 C7 C16 C11 179.45(19) . . . . ? C8 C7 C16 C15 179.0(2) . . . . ? C6 C7 C16 C15 -1.6(3) . . . . ? C11 C10 C9 C8 1.4(3) . . . . ? C44 C10 C9 C8 -176.2(2) . . . . ? C14 C13 C12 C11 0.7(4) . . . . ? C9 C10 C11 C16 -0.1(3) . . . . ? C44 C10 C11 C16 177.50(19) . . . . ? C9 C10 C11 C12 -179.6(2) . . . . ? C44 C10 C11 C12 -1.9(3) . . . . ? C15 C16 C11 C10 -179.5(2) . . . . ? C7 C16 C11 C10 -0.6(3) . . . . ? C15 C16 C11 C12 -0.1(3) . . . . ? C7 C16 C11 C12 178.9(2) . . . . ? C13 C12 C11 C10 179.2(2) . . . . ? C13 C12 C11 C16 -0.3(3) . . . . ? C4 C5 C6 C7 0.1(4) . . . . ? C8 C7 C6 C5 -179.6(2) . . . . ? C16 C7 C6 C5 1.0(3) . . . . ? C6 C5 C4 C3 179.5(2) . . . . ? C6 C5 C4 C15 -0.6(3) . . . . ? C25 O1 C20 C19 -171.2(2) . . . . ? C25 O1 C20 C21 8.5(3) . . . . ? C22 C21 C20 O1 -176.9(2) . . . . ? C22 C21 C20 C19 2.9(3) . . . . ? C1 C2 C3 C4 -1.0(4) . . . . ? C1 C2 C3 C26 177.5(2) . . . . ? C5 C4 C3 C2 -179.0(2) . . . . ? C15 C4 C3 C2 1.0(3) . . . . ? C5 C4 C3 C26 2.5(3) . . . . ? C15 C4 C3 C26 -177.5(2) . . . . ? C1 C14 C15 C16 179.0(2) . . . . ? C13 C14 C15 C16 0.4(3) . . . . ? C1 C14 C15 C4 -1.1(3) . . . . ? C13 C14 C15 C4 -179.71(19) . . . . ? C11 C16 C15 C14 0.0(3) . . . . ? C7 C16 C15 C14 -178.92(19) . . . . ? C11 C16 C15 C4 -179.92(19) . . . . ? C7 C16 C15 C4 1.2(3) . . . . ? C3 C4 C15 C14 0.0(3) . . . . ? C5 C4 C15 C14 -180.0(2) . . . . ? C3 C4 C15 C16 179.9(2) . . . . ? C5 C4 C15 C16 -0.1(3) . . . . ? C29 C30 C31 C26 0.0(3) . . . . ? C29 C30 C31 C32 -177.7(2) . . . . ? C3 C2 C1 C14 -0.2(3) . . . . ? C3 C2 C1 C17 177.4(2) . . . . ? C15 C14 C1 C2 1.2(3) . . . . ? C13 C14 C1 C2 179.7(2) . . . . ? C15 C14 C1 C17 -176.3(2) . . . . ? C13 C14 C1 C17 2.2(3) . . . . ? C22 C17 C1 C2 101.9(3) . . . . ? C18 C17 C1 C2 -81.5(3) . . . . ? C22 C17 C1 C14 -80.6(3) . . . . ? C18 C17 C1 C14 96.0(3) . . . . ? C22 C17 C18 C19 0.9(3) . . . . ? C1 C17 C18 C19 -175.8(2) . . . . ? C22 C17 C18 C24 -179.7(2) . . . . ? C1 C17 C18 C24 3.5(3) . . . . ? C45 C44 C49 C48 -0.3(3) . . . . ? C10 C44 C49 C48 178.6(2) . . . . ? C45 C44 C49 C50 -178.3(2) . . . . ? C10 C44 C49 C50 0.6(3) . . . . ? C44 C49 C48 C47 -0.8(4) . . . . ? C50 C49 C48 C47 177.2(2) . . . . ? C30 C31 C26 C27 -1.6(3) . . . . ? C32 C31 C26 C27 176.1(2) . . . . ? C30 C31 C26 C3 177.1(2) . . . . ? C32 C31 C26 C3 -5.2(3) . . . . ? C2 C3 C26 C31 98.5(3) . . . . ? C4 C3 C26 C31 -83.0(3) . . . . ? C2 C3 C26 C27 -82.7(3) . . . . ? C4 C3 C26 C27 95.8(3) . . . . ? C10 C9 C8 C7 -2.0(3) . . . . ? C10 C9 C8 C35 174.5(2) . . . . ? C6 C7 C8 C9 -178.2(2) . . . . ? C16 C7 C8 C9 1.2(3) . . . . ? C6 C7 C8 C35 5.3(3) . . . . ? C16 C7 C8 C35 -175.3(2) . . . . ? C40 C35 C8 C9 86.5(3) . . . . ? C36 C35 C8 C9 -95.0(3) . . . . ? C40 C35 C8 C7 -97.1(3) . . . . ? C36 C35 C8 C7 81.5(3) . . . . ? C31 C26 C27 C28 1.3(3) . . . . ? C3 C26 C27 C28 -177.4(2) . . . . ? C31 C26 C27 C33 -179.5(2) . . . . ? C3 C26 C27 C33 1.8(3) . . . . ? C26 C27 C28 C29 0.5(3) . . . . ? C33 C27 C28 C29 -178.7(2) . . . . ? C40 C35 C36 C37 0.6(3) . . . . ? C8 C35 C36 C37 -178.0(2) . . . . ? C40 C35 C36 C42 -177.0(2) . . . . ? C8 C35 C36 C42 4.4(3) . . . . ? C35 C36 C37 C38 -1.0(3) . . . . ? C42 C36 C37 C38 176.6(2) . . . . ? O1 C20 C19 C18 176.3(2) . . . . ? C21 C20 C19 C18 -3.5(4) . . . . ? C17 C18 C19 C20 1.6(4) . . . . ? C24 C18 C19 C20 -177.8(2) . . . . ? C34 O2 C29 C28 -170.6(2) . . . . ? C34 O2 C29 C30 10.1(3) . . . . ? C27 C28 C29 O2 178.5(2) . . . . ? C27 C28 C29 C30 -2.1(4) . . . . ? C31 C30 C29 O2 -178.8(2) . . . . ? C31 C30 C29 C28 1.8(4) . . . . ? C52 O4 C47 C46 -5.9(3) . . . . ? C52 O4 C47 C48 173.9(2) . . . . ? C49 C48 C47 C46 1.7(4) . . . . ? C49 C48 C47 O4 -178.1(2) . . . . ? C36 C35 C40 C39 0.1(3) . . . . ? C8 C35 C40 C39 178.7(2) . . . . ? C36 C35 C40 C41 179.0(2) . . . . ? C8 C35 C40 C41 -2.5(3) . . . . ? O4 C47 C46 C45 178.2(2) . . . . ? C48 C47 C46 C45 -1.6(4) . . . . ? C18 C17 C22 C21 -1.5(3) . . . . ? C1 C17 C22 C21 175.1(2) . . . . ? C18 C17 C22 C23 178.0(2) . . . . ? C1 C17 C22 C23 -5.4(3) . . . . ? C20 C21 C22 C17 -0.4(3) . . . . ? C20 C21 C22 C23 -179.9(2) . . . . ? C47 C46 C45 C44 0.5(4) . . . . ? C47 C46 C45 C51 -179.7(2) . . . . ? C49 C44 C45 C46 0.4(3) . . . . ? C10 C44 C45 C46 -178.5(2) . . . . ? C49 C44 C45 C51 -179.4(2) . . . . ? C10 C44 C45 C51 1.8(3) . . . . ? C43 O3 C38 C37 -172.4(2) . . . . ? C43 O3 C38 C39 7.8(3) . . . . ? C36 C37 C38 O3 -179.0(2) . . . . ? C36 C37 C38 C39 0.8(4) . . . . ? O3 C38 C39 C40 179.6(2) . . . . ? C37 C38 C39 C40 -0.1(4) . . . . ? C35 C40 C39 C38 -0.3(4) . . . . ? C41 C40 C39 C38 -179.2(2) . . . . ? C54 C53 C59 C58 177.7(2) . . . 3_665 ? C58 C53 C59 C58 -1.1(4) . . . 3_665 ? C56 C57 C58 C59 178.9(3) . . . 3_665 ? C56 C57 C58 C53 0.4(4) . . . . ? C59 C53 C58 C59 1.0(4) . . . 3_665 ? C54 C53 C58 C59 -177.8(2) . . . 3_665 ? C59 C53 C58 C57 179.5(2) . . . . ? C54 C53 C58 C57 0.7(4) . . . . ? C59 C53 C54 C55 -179.8(3) . . . . ? C58 C53 C54 C55 -1.1(4) . . . . ? C58 C57 C56 C55 -1.3(5) . . . . ? C53 C54 C55 C56 0.3(5) . . . . ? C57 C56 C55 C54 0.9(5) . . . . ? C67 C60 C61 C62 59.7(9) . . . . ? C60 C61 C62 C63 -70.6(9) . . . . ? C61 C62 C63 C64 102.7(7) . . . . ? C62 C63 C64 C65 -34.8(8) . . . . ? C63 C64 C65 C66 -73.3(7) . . . . ? C64 C65 C66 C67 73.0(9) . . . . ? C61 C60 C67 C66 -89.7(9) . . . . ? C65 C66 C67 C60 39.4(12) . . . . ? C67A C60A C61A C62A -66.4(11) . . . . ? C60A C61A C62A C63A -46.2(13) . . . . ? C61A C62A C63A C64A 105.2(9) . . . . ? C62A C63A C64A C65A -75.0(11) . . . . ? C63A C64A C65A C66A 76.9(10) . . . . ? C64A C65A C66A C67A -103.4(9) . . . . ? C61A C60A C67A C66A 75.3(10) . . . . ? C65A C66A C67A C60A 36.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.643 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.056