# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'RSC Advances' _journal_coden_cambridge 1500 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Junwei Ye' _publ_contact_author_email junweiye@dlut.edu.cn _publ_author_name 'Junwei Ye' data_1 _database_code_depnum_ccdc_archive 'CCDC 894149' #TrackingRef '- compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H17 F3' _chemical_formula_weight 362.38 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 14.213(8) _cell_length_b 7.615(4) _cell_length_c 34.237(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3706(3) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 25141 _cell_measurement_theta_min 2.3835 _cell_measurement_theta_max 18.1855 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1504 _exptl_absorpt_coefficient_mu 0.095 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9757 _exptl_absorpt_correction_T_max 0.9831 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 'none ' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 23279 _diffrn_reflns_av_R_equivalents 0.0644 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4206 _reflns_number_gt 1924 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1254P)^2^+0.5799P] 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 0 _refine_ls_number_reflns 4206 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.2603 _refine_ls_wR_factor_gt 0.2068 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.005 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 F1 F -1.1630(3) 0.3556(6) -0.02847(12) 0.2066(19) Uani 1 1 d . . . F2 F -1.1497(3) 0.1008(6) -0.03363(12) 0.225(2) Uani 1 1 d . . . F3 F -1.0898(2) 0.2256(8) 0.01136(9) 0.246(3) Uani 1 1 d . . . C1 C -0.6114(2) 0.3414(4) -0.13829(8) 0.0596(7) Uani 1 1 d . . . C2 C -0.66762(19) 0.3752(4) -0.16951(8) 0.0588(7) Uani 1 1 d . . . C3 C -0.7661(2) 0.3741(4) -0.15620(8) 0.0631(8) Uani 1 1 d . . . H12A H -0.8181 0.3968 -0.1719 0.076 Uiso 1 1 calc R . . C4 C -0.76920(18) 0.3340(4) -0.11692(8) 0.0572(7) Uani 1 1 d . . . C5 C -0.6727(2) 0.3120(4) -0.10325(8) 0.0629(8) Uani 1 1 d . . . H9A H -0.6635 0.1947 -0.0929 0.076 Uiso 1 1 calc R . . H9B H -0.6584 0.3966 -0.0829 0.076 Uiso 1 1 calc R . . C6 C -0.5079(2) 0.3374(4) -0.13480(8) 0.0634(8) Uani 1 1 d . . . C7 C -0.4647(2) 0.2397(5) -0.10553(10) 0.0844(10) Uani 1 1 d . . . H20A H -0.5014 0.1727 -0.0887 0.101 Uiso 1 1 calc R . . C8 C -0.3681(3) 0.2408(6) -0.10115(14) 0.1096(14) Uani 1 1 d . . . H21A H -0.3405 0.1744 -0.0815 0.132 Uiso 1 1 calc R . . C9 C -0.3128(3) 0.3387(7) -0.12548(15) 0.1089(14) Uani 1 1 d . . . H22A H -0.2478 0.3387 -0.1225 0.131 Uiso 1 1 calc R . . C10 C -0.3540(3) 0.4368(6) -0.15436(13) 0.0997(12) Uani 1 1 d . . . H23A H -0.3168 0.5040 -0.1710 0.120 Uiso 1 1 calc R . . C11 C -0.4503(2) 0.4363(5) -0.15890(10) 0.0795(10) Uani 1 1 d . . . H24A H -0.4772 0.5039 -0.1786 0.095 Uiso 1 1 calc R . . C12 C -0.64344(18) 0.4061(4) -0.21087(8) 0.0592(7) Uani 1 1 d . . . C13 C -0.5777(2) 0.3052(5) -0.23066(11) 0.0791(10) Uani 1 1 d . . . H14A H -0.5469 0.2146 -0.2177 0.095 Uiso 1 1 calc R . . C14 C -0.5574(3) 0.3378(6) -0.26950(12) 0.0949(12) Uani 1 1 d . . . H15A H -0.5121 0.2705 -0.2821 0.114 Uiso 1 1 calc R . . C15 C -0.6031(3) 0.4673(7) -0.28964(11) 0.0990(13) Uani 1 1 d . . . H16A H -0.5897 0.4870 -0.3159 0.119 Uiso 1 1 calc R . . C16 C -0.6684(3) 0.5672(6) -0.27076(11) 0.0925(11) Uani 1 1 d . . . H17A H -0.6993 0.6565 -0.2841 0.111 Uiso 1 1 calc R . . C17 C -0.6888(2) 0.5368(4) -0.23191(9) 0.0731(9) Uani 1 1 d . . . H18A H -0.7341 0.6054 -0.2196 0.088 Uiso 1 1 calc R . . C18 C -0.85341(19) 0.3099(4) -0.09309(9) 0.0613(8) Uani 1 1 d . . . C19 C -0.9413(2) 0.2898(5) -0.10994(10) 0.0801(10) Uani 1 1 d . . . H6A H -0.9469 0.2938 -0.1370 0.096 Uiso 1 1 calc R . . C20 C -1.0208(2) 0.2639(5) -0.08754(10) 0.0856(10) Uani 1 1 d . . . H7A H -1.0788 0.2497 -0.0997 0.103 Uiso 1 1 calc R . . C21 C -1.0154(2) 0.2589(5) -0.04754(10) 0.0778(9) Uani 1 1 d . . . C22 C -0.9287(3) 0.2770(6) -0.03047(11) 0.1017(13) Uani 1 1 d . . . H3A H -0.9238 0.2730 -0.0034 0.122 Uiso 1 1 calc R . . C23 C -0.8492(3) 0.3008(6) -0.05253(10) 0.0945(12) Uani 1 1 d . . . H4A H -0.7913 0.3111 -0.0401 0.113 Uiso 1 1 calc R . . C24 C -1.0999(3) 0.2316(8) -0.02403(14) 0.1056(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.130(2) 0.251(5) 0.239(4) 0.055(3) 0.098(3) 0.055(3) F2 0.187(3) 0.240(5) 0.248(4) -0.092(3) 0.130(3) -0.125(3) F3 0.121(2) 0.521(9) 0.096(2) 0.033(3) 0.0372(19) -0.056(3) C1 0.0548(16) 0.0536(17) 0.0703(18) -0.0023(14) -0.0047(14) -0.0015(13) C2 0.0549(16) 0.0540(17) 0.0675(18) -0.0055(14) -0.0015(14) 0.0036(13) C3 0.0561(17) 0.0675(19) 0.0658(18) -0.0030(14) -0.0044(13) 0.0061(14) C4 0.0524(16) 0.0527(17) 0.0665(18) -0.0069(13) -0.0038(13) 0.0011(12) C5 0.0651(18) 0.0585(18) 0.0651(18) -0.0022(13) -0.0033(14) -0.0040(14) C6 0.0525(16) 0.0638(18) 0.0740(19) -0.0065(15) -0.0038(14) -0.0013(14) C7 0.067(2) 0.096(3) 0.090(2) 0.006(2) -0.0127(18) 0.0096(18) C8 0.070(2) 0.138(4) 0.121(3) 0.002(3) -0.026(2) 0.019(2) C9 0.053(2) 0.140(4) 0.134(4) -0.027(3) -0.013(2) 0.006(2) C10 0.065(2) 0.118(3) 0.116(3) -0.021(3) 0.008(2) -0.018(2) C11 0.061(2) 0.091(3) 0.086(2) -0.0044(19) -0.0014(16) -0.0082(17) C12 0.0524(15) 0.0603(18) 0.0648(18) -0.0048(14) -0.0004(13) -0.0028(13) C13 0.070(2) 0.085(2) 0.082(2) -0.0118(18) 0.0015(17) 0.0056(17) C14 0.085(3) 0.114(3) 0.085(3) -0.026(2) 0.022(2) -0.012(2) C15 0.095(3) 0.134(4) 0.068(2) -0.006(2) -0.001(2) -0.034(3) C16 0.089(3) 0.111(3) 0.077(2) 0.019(2) -0.016(2) -0.014(2) C17 0.0680(19) 0.077(2) 0.075(2) 0.0023(17) -0.0028(16) 0.0033(16) C18 0.0572(17) 0.0607(18) 0.0659(18) -0.0062(14) -0.0009(14) -0.0009(13) C19 0.061(2) 0.115(3) 0.064(2) -0.0054(18) 0.0005(15) -0.0002(17) C20 0.0576(19) 0.118(3) 0.082(2) -0.011(2) 0.0033(17) -0.0008(19) C21 0.071(2) 0.087(2) 0.076(2) -0.0048(17) 0.0072(18) -0.0061(18) C22 0.089(3) 0.153(4) 0.063(2) 0.003(2) 0.0043(19) -0.013(2) C23 0.070(2) 0.143(4) 0.070(2) 0.001(2) -0.0056(17) -0.013(2) C24 0.079(3) 0.141(4) 0.097(3) -0.002(3) 0.025(2) -0.015(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 F1 C24 1.311(6) . ? F2 C24 1.266(5) . ? F3 C24 1.221(5) . ? C1 C2 1.359(4) . ? C1 C6 1.475(4) . ? C1 C5 1.500(4) . ? C2 C3 1.471(4) . ? C2 C12 1.476(4) . ? C3 C4 1.380(4) . ? C3 H12A 0.9300 . ? C4 C5 1.458(4) . ? C4 C18 1.460(4) . ? C5 H9A 0.9700 . ? C5 H9B 0.9700 . ? C6 C11 1.385(4) . ? C6 C7 1.391(4) . ? C7 C8 1.381(5) . ? C7 H20A 0.9300 . ? C8 C9 1.366(6) . ? C8 H21A 0.9300 . ? C9 C10 1.371(6) . ? C9 H22A 0.9300 . ? C10 C11 1.377(5) . ? C10 H23A 0.9300 . ? C11 H24A 0.9300 . ? C12 C13 1.386(4) . ? C12 C17 1.388(4) . ? C13 C14 1.383(5) . ? C13 H14A 0.9300 . ? C14 C15 1.367(6) . ? C14 H15A 0.9300 . ? C15 C16 1.363(5) . ? C15 H16A 0.9300 . ? C16 C17 1.381(5) . ? C16 H17A 0.9300 . ? C17 H18A 0.9300 . ? C18 C19 1.384(4) . ? C18 C23 1.392(4) . ? C19 C20 1.379(4) . ? C19 H6A 0.9300 . ? C20 C21 1.372(5) . ? C20 H7A 0.9300 . ? C21 C22 1.370(5) . ? C21 C24 1.461(5) . ? C22 C23 1.371(5) . ? C22 H3A 0.9300 . ? C23 H4A 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 C2 C1 C6 130.8(3) . . ? C2 C1 C5 108.4(2) . . ? C6 C1 C5 120.8(2) . . ? C1 C2 C3 108.3(3) . . ? C1 C2 C12 130.4(3) . . ? C3 C2 C12 121.3(2) . . ? C4 C3 C2 109.5(2) . . ? C4 C3 H12A 125.2 . . ? C2 C3 H12A 125.2 . . ? C3 C4 C5 107.9(2) . . ? C3 C4 C18 126.8(2) . . ? C5 C4 C18 125.2(3) . . ? C4 C5 C1 105.8(2) . . ? C4 C5 H9A 110.6 . . ? C1 C5 H9A 110.6 . . ? C4 C5 H9B 110.6 . . ? C1 C5 H9B 110.6 . . ? H9A C5 H9B 108.7 . . ? C11 C6 C7 117.3(3) . . ? C11 C6 C1 122.0(3) . . ? C7 C6 C1 120.6(3) . . ? C8 C7 C6 120.9(4) . . ? C8 C7 H20A 119.5 . . ? C6 C7 H20A 119.5 . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H21A 119.7 . . ? C7 C8 H21A 119.7 . . ? C8 C9 C10 119.4(4) . . ? C8 C9 H22A 120.3 . . ? C10 C9 H22A 120.3 . . ? C9 C10 C11 120.3(4) . . ? C9 C10 H23A 119.9 . . ? C11 C10 H23A 119.9 . . ? C10 C11 C6 121.4(4) . . ? C10 C11 H24A 119.3 . . ? C6 C11 H24A 119.3 . . ? C13 C12 C17 117.2(3) . . ? C13 C12 C2 122.5(3) . . ? C17 C12 C2 120.3(3) . . ? C14 C13 C12 120.7(4) . . ? C14 C13 H14A 119.6 . . ? C12 C13 H14A 119.6 . . ? C15 C14 C13 121.0(4) . . ? C15 C14 H15A 119.5 . . ? C13 C14 H15A 119.5 . . ? C16 C15 C14 119.1(4) . . ? C16 C15 H16A 120.4 . . ? C14 C15 H16A 120.4 . . ? C15 C16 C17 120.4(4) . . ? C15 C16 H17A 119.8 . . ? C17 C16 H17A 119.8 . . ? C16 C17 C12 121.5(3) . . ? C16 C17 H18A 119.2 . . ? C12 C17 H18A 119.2 . . ? C19 C18 C23 116.7(3) . . ? C19 C18 C4 121.4(3) . . ? C23 C18 C4 121.9(3) . . ? C20 C19 C18 121.5(3) . . ? C20 C19 H6A 119.2 . . ? C18 C19 H6A 119.2 . . ? C21 C20 C19 120.9(3) . . ? C21 C20 H7A 119.6 . . ? C19 C20 H7A 119.6 . . ? C22 C21 C20 118.2(3) . . ? C22 C21 C24 121.2(4) . . ? C20 C21 C24 120.5(3) . . ? C21 C22 C23 121.3(3) . . ? C21 C22 H3A 119.4 . . ? C23 C22 H3A 119.4 . . ? C22 C23 C18 121.4(3) . . ? C22 C23 H4A 119.3 . . ? C18 C23 H4A 119.3 . . ? F3 C24 F2 107.1(5) . . ? F3 C24 F1 102.8(5) . . ? F2 C24 F1 98.8(4) . . ? F3 C24 C21 117.1(4) . . ? F2 C24 C21 115.4(4) . . ? F1 C24 C21 113.3(4) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.394 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.043 # = = = END data_4 _database_code_depnum_ccdc_archive 'CCDC 894150' #TrackingRef '- compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H20' _chemical_formula_weight 308.40 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 5.9678(3) _cell_length_b 18.3299(7) _cell_length_c 15.8727(7) _cell_angle_alpha 90.00 _cell_angle_beta 99.236(2) _cell_angle_gamma 90.00 _cell_volume 1713.79(13) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4305 _cell_measurement_theta_min 2.5755 _cell_measurement_theta_max 27.614 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.195 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9853 _exptl_absorpt_correction_T_max 0.9880 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 'none ' _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 11252 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.70 _reflns_number_total 3999 _reflns_number_gt 3143 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.2355P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3999 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0591 _refine_ls_R_factor_gt 0.0459 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.057 _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 C1 C 0.4694(2) -0.01965(7) 0.23667(8) 0.0412(3) Uani 1 1 d . . . C2 C 0.3545(2) 0.04258(7) 0.24817(8) 0.0418(3) Uani 1 1 d . . . C3 C 0.3867(2) 0.09470(7) 0.18137(8) 0.0455(3) Uani 1 1 d . . . H3A H 0.3218 0.1409 0.1750 0.055 Uiso 1 1 calc R . . C4 C 0.5256(2) 0.06576(7) 0.12980(8) 0.0410(3) Uani 1 1 d . . . C5 C 0.5896(2) -0.00910(7) 0.16111(8) 0.0422(3) Uani 1 1 d . . . H5A H 0.7527 -0.0131 0.1780 0.051 Uiso 1 1 calc R . . H5B H 0.5400 -0.0451 0.1173 0.051 Uiso 1 1 calc R . . C6 C 0.4830(2) -0.08934(7) 0.28312(8) 0.0426(3) Uani 1 1 d . . . C7 C 0.6615(3) -0.13709(8) 0.27875(10) 0.0585(4) Uani 1 1 d . . . H7A H 0.7738 -0.1238 0.2473 0.070 Uiso 1 1 calc R . . C8 C 0.6768(3) -0.20375(9) 0.31982(11) 0.0691(5) Uani 1 1 d . . . H8A H 0.7986 -0.2345 0.3158 0.083 Uiso 1 1 calc R . . C9 C 0.5134(3) -0.22490(9) 0.36646(10) 0.0631(4) Uani 1 1 d . . . H9A H 0.5241 -0.2696 0.3946 0.076 Uiso 1 1 calc R . . C10 C 0.3341(3) -0.17917(8) 0.37100(10) 0.0616(4) Uani 1 1 d . . . H10A H 0.2222 -0.1933 0.4022 0.074 Uiso 1 1 calc R . . C11 C 0.3168(3) -0.11246(8) 0.32998(9) 0.0534(3) Uani 1 1 d . . . H11A H 0.1929 -0.0825 0.3336 0.064 Uiso 1 1 calc R . . C12 C 0.2227(2) 0.06290(7) 0.31648(8) 0.0428(3) Uani 1 1 d . . . C13 C 0.3114(3) 0.05359(8) 0.40250(9) 0.0531(3) Uani 1 1 d . . . H13A H 0.4558 0.0339 0.4180 0.064 Uiso 1 1 calc R . . C14 C 0.1863(3) 0.07344(9) 0.46480(10) 0.0652(4) Uani 1 1 d . . . H14A H 0.2473 0.0675 0.5221 0.078 Uiso 1 1 calc R . . C15 C -0.0285(3) 0.10206(9) 0.44252(11) 0.0690(5) Uani 1 1 d . . . H15A H -0.1145 0.1137 0.4846 0.083 Uiso 1 1 calc R . . C16 C -0.1152(3) 0.11340(9) 0.35810(11) 0.0634(4) Uani 1 1 d . . . H16A H -0.2590 0.1336 0.3431 0.076 Uiso 1 1 calc R . . C17 C 0.0104(2) 0.09487(8) 0.29542(10) 0.0515(3) Uani 1 1 d . . . H17A H -0.0480 0.1039 0.2385 0.062 Uiso 1 1 calc R . . C18 C 0.6108(2) 0.10184(6) 0.05887(7) 0.0393(3) Uani 1 1 d . . . C19 C 0.5017(2) 0.16293(7) 0.01898(8) 0.0465(3) Uani 1 1 d . . . H19A H 0.3674 0.1791 0.0354 0.056 Uiso 1 1 calc R . . C20 C 0.5886(2) 0.19985(7) -0.04409(9) 0.0501(3) Uani 1 1 d . . . H20A H 0.5114 0.2403 -0.0694 0.060 Uiso 1 1 calc R . . C21 C 0.7889(2) 0.17802(7) -0.07071(8) 0.0470(3) Uani 1 1 d . . . C22 C 0.8935(2) 0.11629(7) -0.03340(9) 0.0497(3) Uani 1 1 d . . . H22A H 1.0251 0.0995 -0.0514 0.060 Uiso 1 1 calc R . . C23 C 0.8079(2) 0.07869(7) 0.03020(8) 0.0467(3) Uani 1 1 d . . . H23A H 0.8832 0.0374 0.0541 0.056 Uiso 1 1 calc R . . C24 C 0.8891(3) 0.22207(10) -0.13581(11) 0.0678(4) Uani 1 1 d . . . H24A H 1.0262 0.1992 -0.1468 0.102 Uiso 1 1 calc R . . H24B H 0.9226 0.2705 -0.1143 0.102 Uiso 1 1 calc R . . H24C H 0.7822 0.2246 -0.1878 0.102 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 C1 0.0430(6) 0.0422(6) 0.0386(6) -0.0018(5) 0.0078(5) -0.0034(5) C2 0.0430(6) 0.0445(7) 0.0382(6) -0.0024(5) 0.0074(5) -0.0017(5) C3 0.0501(7) 0.0430(7) 0.0437(7) 0.0005(5) 0.0090(5) 0.0029(5) C4 0.0448(6) 0.0392(6) 0.0391(6) -0.0002(5) 0.0070(5) 0.0012(5) C5 0.0471(6) 0.0408(6) 0.0396(7) -0.0029(5) 0.0093(5) -0.0026(5) C6 0.0477(7) 0.0414(6) 0.0386(6) -0.0012(5) 0.0064(5) -0.0044(5) C7 0.0545(8) 0.0592(9) 0.0640(9) 0.0145(7) 0.0166(7) 0.0068(7) C8 0.0654(9) 0.0599(9) 0.0820(12) 0.0202(8) 0.0114(8) 0.0139(8) C9 0.0813(11) 0.0511(8) 0.0547(9) 0.0126(7) 0.0043(8) -0.0038(8) C10 0.0803(10) 0.0523(8) 0.0566(9) 0.0016(6) 0.0242(7) -0.0157(8) C11 0.0607(8) 0.0450(7) 0.0587(9) -0.0033(6) 0.0216(7) -0.0062(6) C12 0.0467(7) 0.0394(6) 0.0439(7) -0.0044(5) 0.0123(5) -0.0038(5) C13 0.0611(8) 0.0534(8) 0.0456(7) 0.0004(6) 0.0111(6) 0.0031(6) C14 0.0912(12) 0.0623(9) 0.0457(8) -0.0026(7) 0.0223(8) -0.0015(8) C15 0.0829(11) 0.0612(9) 0.0729(11) -0.0160(8) 0.0432(9) -0.0070(8) C16 0.0518(8) 0.0617(9) 0.0806(11) -0.0169(8) 0.0229(8) -0.0009(7) C17 0.0480(7) 0.0531(8) 0.0533(8) -0.0098(6) 0.0079(6) -0.0020(6) C18 0.0437(6) 0.0369(6) 0.0376(6) -0.0031(5) 0.0070(5) -0.0006(5) C19 0.0474(7) 0.0459(7) 0.0466(7) 0.0014(5) 0.0091(5) 0.0066(5) C20 0.0598(8) 0.0422(7) 0.0480(8) 0.0064(5) 0.0076(6) 0.0054(6) C21 0.0574(7) 0.0442(7) 0.0398(7) -0.0026(5) 0.0093(6) -0.0074(6) C22 0.0524(7) 0.0489(7) 0.0509(8) -0.0025(6) 0.0182(6) 0.0013(6) C23 0.0521(7) 0.0401(6) 0.0495(7) 0.0026(5) 0.0133(6) 0.0064(5) C24 0.0851(11) 0.0644(10) 0.0582(9) 0.0096(7) 0.0245(8) -0.0099(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.3582(17) . ? C1 C6 1.4706(17) . ? C1 C5 1.5055(16) . ? C2 C3 1.4627(18) . ? C2 C12 1.4854(17) . ? C3 C4 1.3623(17) . ? C4 C18 1.4653(16) . ? C4 C5 1.4884(17) . ? C6 C7 1.3891(19) . ? C6 C11 1.3976(18) . ? C7 C8 1.381(2) . ? C8 C9 1.371(2) . ? C9 C10 1.370(2) . ? C10 C11 1.381(2) . ? C12 C17 1.3875(19) . ? C12 C13 1.3933(18) . ? C13 C14 1.380(2) . ? C14 C15 1.378(3) . ? C15 C16 1.372(2) . ? C16 C17 1.381(2) . ? C18 C23 1.3939(17) . ? C18 C19 1.3950(18) . ? C19 C20 1.3768(18) . ? C20 C21 1.3891(19) . ? C21 C22 1.379(2) . ? C21 C24 1.5085(19) . ? C22 C23 1.3859(18) . ? 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 C2 C1 C6 130.59(11) . . ? C2 C1 C5 108.33(11) . . ? C6 C1 C5 121.06(11) . . ? C1 C2 C3 108.86(11) . . ? C1 C2 C12 130.28(12) . . ? C3 C2 C12 120.79(11) . . ? C4 C3 C2 110.16(11) . . ? C3 C4 C18 127.26(11) . . ? C3 C4 C5 107.85(11) . . ? C18 C4 C5 124.79(10) . . ? C4 C5 C1 104.77(10) . . ? C7 C6 C11 116.82(12) . . ? C7 C6 C1 120.21(12) . . ? C11 C6 C1 122.91(12) . . ? C8 C7 C6 121.78(14) . . ? C9 C8 C7 120.41(15) . . ? C10 C9 C8 118.97(14) . . ? C9 C10 C11 121.11(14) . . ? C10 C11 C6 120.89(14) . . ? C17 C12 C13 118.46(12) . . ? C17 C12 C2 120.00(12) . . ? C13 C12 C2 121.48(12) . . ? C14 C13 C12 120.37(14) . . ? C15 C14 C13 120.31(15) . . ? C16 C15 C14 119.84(14) . . ? C15 C16 C17 120.21(15) . . ? C16 C17 C12 120.71(14) . . ? C23 C18 C19 116.93(11) . . ? C23 C18 C4 121.91(11) . . ? C19 C18 C4 121.12(11) . . ? C20 C19 C18 121.46(12) . . ? C19 C20 C21 121.49(12) . . ? C22 C21 C20 117.27(12) . . ? C22 C21 C24 122.09(13) . . ? C20 C21 C24 120.62(13) . . ? C21 C22 C23 121.74(12) . . ? C22 C23 C18 121.04(12) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.70 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.173 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.041 # = = = END data_5 _database_code_depnum_ccdc_archive 'CCDC 894151' #TrackingRef '- compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H20' _chemical_formula_weight 344.43 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pca2(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y, z+1/2' 'x+1/2, -y, z' _cell_length_a 14.060(5) _cell_length_b 17.548(6) _cell_length_c 7.824(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1930.4(12) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 10706 _cell_measurement_theta_min 2.322 _cell_measurement_theta_max 17.656 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9867 _exptl_absorpt_correction_T_max 0.9881 _exptl_absorpt_process_details ; Higashi, T. (1995) Progrom for Absorption Correcttion. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID' _diffrn_measurement_method 'Omega scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 10218 _diffrn_reflns_av_R_equivalents 0.0504 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 27.69 _reflns_number_total 4242 _reflns_number_gt 1888 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction PROCESS-AUTO _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0318P)^2^+0.0590P] 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 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 10(10) _refine_ls_number_reflns 4242 _refine_ls_number_parameters 245 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1531 _refine_ls_R_factor_gt 0.0528 _refine_ls_wR_factor_ref 0.1156 _refine_ls_wR_factor_gt 0.0875 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.33647(18) 0.33711(17) 0.3001(4) 0.0545(8) Uani 1 1 d . . . C2 C 0.3935(2) 0.27859(17) 0.2540(4) 0.0550(7) Uani 1 1 d . . . C3 C 0.3359(2) 0.20993(17) 0.2337(4) 0.0610(8) Uani 1 1 d . . . H3A H 0.3594 0.1626 0.2005 0.073 Uiso 1 1 calc R . . C4 C 0.2433(2) 0.22477(16) 0.2699(4) 0.0597(8) Uani 1 1 d . . . C5 C 0.23608(19) 0.30652(15) 0.3149(4) 0.0626(9) Uani 1 1 d . . . H5A H 0.2123 0.3127 0.4304 0.075 Uiso 1 1 calc R . . H5B H 0.1938 0.3329 0.2368 0.075 Uiso 1 1 calc R . . C6 C 0.3582(2) 0.41782(16) 0.3250(4) 0.0578(8) Uani 1 1 d . . . C7 C 0.3115(2) 0.4599(2) 0.4485(4) 0.0779(11) Uani 1 1 d . . . H7A H 0.2658 0.4364 0.5164 0.093 Uiso 1 1 calc R . . C8 C 0.3310(3) 0.5358(3) 0.4731(6) 0.1005(13) Uani 1 1 d . . . H8A H 0.2992 0.5629 0.5577 0.121 Uiso 1 1 calc R . . C9 C 0.3969(3) 0.5714(2) 0.3741(7) 0.1037(15) Uani 1 1 d . . . H9A H 0.4105 0.6227 0.3910 0.124 Uiso 1 1 calc R . . C10 C 0.4427(3) 0.5312(2) 0.2499(6) 0.0942(12) Uani 1 1 d . . . H10A H 0.4875 0.5555 0.1814 0.113 Uiso 1 1 calc R . . C11 C 0.4235(2) 0.45526(18) 0.2246(5) 0.0752(10) Uani 1 1 d . . . H11A H 0.4551 0.4289 0.1385 0.090 Uiso 1 1 calc R . . C12 C 0.4982(2) 0.27582(17) 0.2350(4) 0.0588(8) Uani 1 1 d . . . C13 C 0.5578(2) 0.31583(18) 0.3428(5) 0.0756(10) Uani 1 1 d . . . H13A H 0.5322 0.3461 0.4288 0.091 Uiso 1 1 calc R . . C14 C 0.6558(3) 0.3112(2) 0.3235(6) 0.0948(13) Uani 1 1 d . . . H14A H 0.6956 0.3385 0.3960 0.114 Uiso 1 1 calc R . . C15 C 0.6937(3) 0.2661(3) 0.1973(7) 0.1043(16) Uani 1 1 d . . . H15A H 0.7594 0.2627 0.1845 0.125 Uiso 1 1 calc R . . C16 C 0.6356(3) 0.2266(2) 0.0914(6) 0.0961(14) Uani 1 1 d . . . H16A H 0.6617 0.1962 0.0061 0.115 Uiso 1 1 calc R . . C17 C 0.5380(2) 0.23111(19) 0.1089(4) 0.0750(10) Uani 1 1 d . . . H17A H 0.4988 0.2038 0.0352 0.090 Uiso 1 1 calc R . . C18 C 0.1604(2) 0.17376(18) 0.2572(4) 0.0624(9) Uani 1 1 d . . . C19 C 0.1659(2) 0.09469(19) 0.3021(4) 0.0649(8) Uani 1 1 d . . . C20 C 0.2453(3) 0.06163(19) 0.3809(4) 0.0735(9) Uani 1 1 d . . . H20A H 0.2968 0.0921 0.4103 0.088 Uiso 1 1 calc R . . C21 C 0.2481(3) -0.0149(2) 0.4153(4) 0.0845(10) Uani 1 1 d . . . H21A H 0.3016 -0.0359 0.4668 0.101 Uiso 1 1 calc R . . C22 C 0.1711(3) -0.0614(2) 0.3733(5) 0.1000(13) Uani 1 1 d . . . H22A H 0.1743 -0.1137 0.3925 0.120 Uiso 1 1 calc R . . C23 C 0.0926(3) -0.0309(2) 0.3054(5) 0.0897(12) Uani 1 1 d . . . H23A H 0.0411 -0.0623 0.2810 0.108 Uiso 1 1 calc R . . C24 C 0.0858(3) 0.0475(2) 0.2698(4) 0.0779(10) Uani 1 1 d . . . C25 C 0.0034(3) 0.0799(3) 0.2027(5) 0.0983(13) Uani 1 1 d . . . H25A H -0.0491 0.0489 0.1831 0.118 Uiso 1 1 calc R . . C26 C -0.0026(3) 0.1552(3) 0.1649(6) 0.0993(13) Uani 1 1 d . . . H26A H -0.0590 0.1757 0.1230 0.119 Uiso 1 1 calc R . . C27 C 0.0779(2) 0.2021(2) 0.1901(5) 0.0783(11) Uani 1 1 d . . . H27A H 0.0747 0.2533 0.1604 0.094 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 C1 0.0555(18) 0.0599(19) 0.0482(18) -0.0014(18) -0.0003(16) -0.0089(17) C2 0.0615(18) 0.0562(18) 0.0474(19) 0.0000(16) -0.0004(16) -0.0057(18) C3 0.0685(19) 0.058(2) 0.057(2) -0.0010(17) 0.0004(18) -0.0067(18) C4 0.0653(19) 0.0584(19) 0.056(2) 0.0033(17) -0.0001(17) -0.0089(19) C5 0.0678(19) 0.069(2) 0.0507(19) 0.0047(18) 0.0037(17) -0.0067(17) C6 0.0576(18) 0.059(2) 0.057(2) -0.004(2) -0.0056(17) 0.0028(17) C7 0.082(3) 0.073(3) 0.079(3) -0.009(2) 0.004(2) 0.010(2) C8 0.122(4) 0.079(3) 0.100(3) -0.027(3) -0.014(3) 0.024(3) C9 0.107(3) 0.055(3) 0.149(4) -0.010(3) -0.043(3) 0.008(3) C10 0.088(3) 0.064(3) 0.131(4) 0.015(3) -0.010(3) -0.011(2) C11 0.078(2) 0.062(2) 0.085(3) -0.002(2) 0.009(2) -0.0037(19) C12 0.0628(19) 0.0518(18) 0.062(2) 0.0044(19) -0.0014(19) -0.0012(18) C13 0.072(2) 0.075(2) 0.080(2) 0.008(2) -0.011(2) -0.012(2) C14 0.069(3) 0.101(3) 0.115(4) 0.033(3) -0.031(3) -0.024(2) C15 0.065(3) 0.111(4) 0.136(4) 0.049(4) 0.006(3) 0.016(3) C16 0.085(3) 0.090(3) 0.113(4) 0.022(3) 0.025(3) 0.020(3) C17 0.069(2) 0.068(2) 0.089(3) 0.007(2) 0.009(2) 0.002(2) C18 0.066(2) 0.072(2) 0.050(2) 0.0008(19) 0.0017(17) -0.0117(19) C19 0.073(2) 0.076(2) 0.0458(19) -0.0029(19) 0.0040(18) -0.019(2) C20 0.092(3) 0.071(2) 0.058(2) 0.0024(19) 0.001(2) -0.019(2) C21 0.109(3) 0.080(3) 0.064(2) 0.006(2) 0.001(2) -0.011(3) C22 0.142(4) 0.081(3) 0.078(3) 0.009(2) 0.010(3) -0.027(3) C23 0.109(3) 0.088(3) 0.072(3) 0.001(2) 0.008(2) -0.041(3) C24 0.091(3) 0.087(3) 0.056(2) 0.001(2) -0.001(2) -0.029(2) C25 0.083(3) 0.132(4) 0.080(3) 0.002(3) -0.006(2) -0.042(3) C26 0.075(3) 0.130(4) 0.093(3) 0.013(3) -0.017(2) -0.020(3) C27 0.067(2) 0.094(3) 0.074(3) 0.008(2) -0.0122(19) -0.011(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 C1 C2 1.352(3) . ? C1 C6 1.462(4) . ? C1 C5 1.514(3) . ? C2 C3 1.460(4) . ? C2 C12 1.481(4) . ? C3 C4 1.358(4) . ? C3 H3A 0.9300 . ? C4 C18 1.473(4) . ? C4 C5 1.481(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C11 1.376(4) . ? C6 C7 1.383(4) . ? C7 C8 1.373(4) . ? C7 H7A 0.9300 . ? C8 C9 1.359(5) . ? C8 H8A 0.9300 . ? C9 C10 1.363(6) . ? C9 H9A 0.9300 . ? C10 C11 1.375(4) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C17 1.379(4) . ? C12 C13 1.381(4) . ? C13 C14 1.387(4) . ? C13 H13A 0.9300 . ? C14 C15 1.373(5) . ? C14 H14A 0.9300 . ? C15 C16 1.354(5) . ? C15 H15A 0.9300 . ? C16 C17 1.383(4) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C27 1.366(4) . ? C18 C19 1.433(4) . ? C19 C20 1.401(4) . ? C19 C24 1.420(4) . ? C20 C21 1.371(4) . ? C20 H20A 0.9300 . ? C21 C22 1.396(5) . ? C21 H21A 0.9300 . ? C22 C23 1.337(4) . ? C22 H22A 0.9300 . ? C23 C24 1.406(5) . ? C23 H23A 0.9300 . ? C24 C25 1.392(5) . ? C25 C26 1.357(5) . ? C25 H25A 0.9300 . ? C26 C27 1.414(4) . ? C26 H26A 0.9300 . ? C27 H27A 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 C2 C1 C6 130.4(3) . . ? C2 C1 C5 107.7(2) . . ? C6 C1 C5 121.9(3) . . ? C1 C2 C3 109.1(2) . . ? C1 C2 C12 129.9(3) . . ? C3 C2 C12 120.9(3) . . ? C4 C3 C2 110.5(3) . . ? C4 C3 H3A 124.7 . . ? C2 C3 H3A 124.7 . . ? C3 C4 C18 128.9(3) . . ? C3 C4 C5 107.5(3) . . ? C18 C4 C5 123.4(3) . . ? C4 C5 C1 105.2(2) . . ? C4 C5 H5A 110.7 . . ? C1 C5 H5A 110.7 . . ? C4 C5 H5B 110.7 . . ? C1 C5 H5B 110.7 . . ? H5A C5 H5B 108.8 . . ? C11 C6 C7 117.5(3) . . ? C11 C6 C1 121.8(3) . . ? C7 C6 C1 120.8(3) . . ? C8 C7 C6 121.4(4) . . ? C8 C7 H7A 119.3 . . ? C6 C7 H7A 119.3 . . ? C9 C8 C7 120.2(4) . . ? C9 C8 H8A 119.9 . . ? C7 C8 H8A 119.9 . . ? C10 C9 C8 119.4(4) . . ? C10 C9 H9A 120.3 . . ? C8 C9 H9A 120.3 . . ? C9 C10 C11 120.8(4) . . ? C9 C10 H10A 119.6 . . ? C11 C10 H10A 119.6 . . ? C6 C11 C10 120.8(4) . . ? C6 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C17 C12 C13 118.7(3) . . ? C17 C12 C2 119.6(3) . . ? C13 C12 C2 121.7(3) . . ? C12 C13 C14 120.4(4) . . ? C12 C13 H13A 119.8 . . ? C14 C13 H13A 119.8 . . ? C15 C14 C13 119.9(4) . . ? C15 C14 H14A 120.1 . . ? C13 C14 H14A 120.1 . . ? C16 C15 C14 120.0(4) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 120.6(4) . . ? C15 C16 H16A 119.7 . . ? C17 C16 H16A 119.7 . . ? C12 C17 C16 120.4(4) . . ? C12 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C27 C18 C19 119.5(3) . . ? C27 C18 C4 118.4(3) . . ? C19 C18 C4 122.0(3) . . ? C20 C19 C24 117.9(3) . . ? C20 C19 C18 123.5(3) . . ? C24 C19 C18 118.6(3) . . ? C21 C20 C19 121.0(3) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C20 C21 C22 120.3(4) . . ? C20 C21 H21A 119.9 . . ? C22 C21 H21A 119.9 . . ? C23 C22 C21 120.0(4) . . ? C23 C22 H22A 120.0 . . ? C21 C22 H22A 120.0 . . ? C22 C23 C24 121.8(4) . . ? C22 C23 H23A 119.1 . . ? C24 C23 H23A 119.1 . . ? C25 C24 C23 122.0(4) . . ? C25 C24 C19 119.2(4) . . ? C23 C24 C19 118.7(4) . . ? C26 C25 C24 122.1(4) . . ? C26 C25 H25A 118.9 . . ? C24 C25 H25A 118.9 . . ? C25 C26 C27 119.1(4) . . ? C25 C26 H26A 120.5 . . ? C27 C26 H26A 120.5 . . ? C18 C27 C26 121.4(3) . . ? C18 C27 H27A 119.3 . . ? C26 C27 H27A 119.3 . . ? 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 -175.5(3) . . . . ? C5 C1 C2 C3 1.1(3) . . . . ? C6 C1 C2 C12 8.6(5) . . . . ? C5 C1 C2 C12 -174.8(3) . . . . ? C1 C2 C3 C4 -1.1(4) . . . . ? C12 C2 C3 C4 175.2(3) . . . . ? C2 C3 C4 C18 176.3(3) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? C3 C4 C5 C1 0.0(3) . . . . ? C18 C4 C5 C1 -176.0(3) . . . . ? C2 C1 C5 C4 -0.7(3) . . . . ? C6 C1 C5 C4 176.3(3) . . . . ? C2 C1 C6 C11 35.7(5) . . . . ? C5 C1 C6 C11 -140.5(3) . . . . ? C2 C1 C6 C7 -146.0(3) . . . . ? C5 C1 C6 C7 37.8(4) . . . . ? C11 C6 C7 C8 -1.5(5) . . . . ? C1 C6 C7 C8 -179.9(3) . . . . ? C6 C7 C8 C9 0.6(6) . . . . ? C7 C8 C9 C10 0.4(7) . . . . ? C8 C9 C10 C11 -0.4(6) . . . . ? C7 C6 C11 C10 1.5(5) . . . . ? C1 C6 C11 C10 179.8(3) . . . . ? C9 C10 C11 C6 -0.6(6) . . . . ? C1 C2 C12 C17 -145.1(3) . . . . ? C3 C2 C12 C17 39.5(4) . . . . ? C1 C2 C12 C13 36.3(5) . . . . ? C3 C2 C12 C13 -139.2(3) . . . . ? C17 C12 C13 C14 0.3(5) . . . . ? C2 C12 C13 C14 179.0(3) . . . . ? C12 C13 C14 C15 -0.4(5) . . . . ? C13 C14 C15 C16 0.3(6) . . . . ? C14 C15 C16 C17 0.0(6) . . . . ? C13 C12 C17 C16 0.0(5) . . . . ? C2 C12 C17 C16 -178.7(3) . . . . ? C15 C16 C17 C12 -0.1(6) . . . . ? C3 C4 C18 C27 -137.5(4) . . . . ? C5 C4 C18 C27 37.6(4) . . . . ? C3 C4 C18 C19 38.3(5) . . . . ? C5 C4 C18 C19 -146.7(3) . . . . ? C27 C18 C19 C20 -176.1(3) . . . . ? C4 C18 C19 C20 8.3(5) . . . . ? C27 C18 C19 C24 2.1(4) . . . . ? C4 C18 C19 C24 -173.6(3) . . . . ? C24 C19 C20 C21 4.3(5) . . . . ? C18 C19 C20 C21 -177.5(3) . . . . ? C19 C20 C21 C22 -0.5(5) . . . . ? C20 C21 C22 C23 -2.7(6) . . . . ? C21 C22 C23 C24 1.9(6) . . . . ? C22 C23 C24 C25 -178.5(4) . . . . ? C22 C23 C24 C19 2.0(5) . . . . ? C20 C19 C24 C25 175.5(3) . . . . ? C18 C19 C24 C25 -2.7(4) . . . . ? C20 C19 C24 C23 -5.0(4) . . . . ? C18 C19 C24 C23 176.7(3) . . . . ? C23 C24 C25 C26 -178.6(4) . . . . ? C19 C24 C25 C26 0.8(6) . . . . ? C24 C25 C26 C27 1.7(6) . . . . ? C19 C18 C27 C26 0.4(5) . . . . ? C4 C18 C27 C26 176.3(3) . . . . ? C25 C26 C27 C18 -2.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 27.69 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.099 _refine_diff_density_min -0.139 _refine_diff_density_rms 0.028 # = = = END data_6 _database_code_depnum_ccdc_archive 'CCDC 894152' #TrackingRef '- compounds.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H22' _chemical_formula_weight 370.47 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.3555(5) _cell_length_b 11.4727(6) _cell_length_c 21.3695(12) _cell_angle_alpha 92.113(4) _cell_angle_beta 97.850(4) _cell_angle_gamma 91.027(4) _cell_volume 2027.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15280 _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 27.53 _exptl_crystal_description blcok _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9851 _exptl_absorpt_correction_T_max 0.9891 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER CCD area detector diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 21743 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.53 _reflns_number_total 15280 _reflns_number_gt 8471 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 1997)' _computing_publication_material 'SHELXL97 ' _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^)+(0.0450P)^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 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0(6) _refine_ls_number_reflns 15280 _refine_ls_number_parameters 1045 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1130 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1267 _refine_ls_wR_factor_gt 0.1026 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9443(4) 0.1146(3) 0.95798(17) 0.0508(10) Uani 1 1 d . . . C2 C 0.9449(4) 0.2323(3) 0.95411(17) 0.0495(10) Uani 1 1 d . . . C3 C 0.9741(5) 0.2620(4) 0.88978(18) 0.0570(11) Uani 1 1 d . . . H3 H 0.9832 0.3372 0.8756 0.068 Uiso 1 1 calc R . . C4 C 0.9856(5) 0.1616(3) 0.85454(19) 0.0534(10) Uani 1 1 d . . . C5 C 0.9662(5) 0.0626(3) 0.89446(18) 0.0593(11) Uani 1 1 d . . . H5A H 1.0611 0.0145 0.8976 0.071 Uiso 1 1 calc R . . H5B H 0.8725 0.0148 0.8771 0.071 Uiso 1 1 calc R . . C6 C 0.9394(4) 0.0404(3) 1.01249(18) 0.0477(9) Uani 1 1 d . . . C7 C 0.8643(5) -0.0694(4) 1.0056(2) 0.0591(11) Uani 1 1 d . . . H7A H 0.8152 -0.0959 0.9659 0.071 Uiso 1 1 calc R . . C8 C 0.8609(5) -0.1395(4) 1.0561(2) 0.0697(13) Uani 1 1 d . . . H8A H 0.8091 -0.2122 1.0501 0.084 Uiso 1 1 calc R . . C9 C 0.9336(5) -0.1029(4) 1.1155(2) 0.0705(13) Uani 1 1 d . . . H9A H 0.9298 -0.1501 1.1498 0.085 Uiso 1 1 calc R . . C10 C 1.0120(5) 0.0044(4) 1.12351(19) 0.0665(11) Uani 1 1 d . . . H10A H 1.0625 0.0295 1.1633 0.080 Uiso 1 1 calc R . . C11 C 1.0161(4) 0.0747(3) 1.07286(17) 0.0557(10) Uani 1 1 d . . . H11A H 1.0709 0.1464 1.0789 0.067 Uiso 1 1 calc R . . C12 C 0.9212(4) 0.3243(3) 1.00198(18) 0.0494(9) Uani 1 1 d . . . C13 C 0.8231(5) 0.3073(3) 1.04891(19) 0.0626(11) Uani 1 1 d . . . H13A H 0.7683 0.2363 1.0500 0.075 Uiso 1 1 calc R . . C14 C 0.8063(5) 0.3936(4) 1.0934(2) 0.0715(12) Uani 1 1 d . . . H14A H 0.7449 0.3791 1.1255 0.086 Uiso 1 1 calc R . . C15 C 0.8799(6) 0.5022(4) 1.0910(2) 0.0737(13) Uani 1 1 d . . . H15A H 0.8678 0.5608 1.1211 0.088 Uiso 1 1 calc R . . C16 C 0.9712(5) 0.5219(4) 1.0434(2) 0.0700(12) Uani 1 1 d . . . H16A H 1.0198 0.5948 1.0408 0.084 Uiso 1 1 calc R . . C17 C 0.9909(5) 0.4346(4) 0.9997(2) 0.0629(11) Uani 1 1 d . . . H17A H 1.0527 0.4496 0.9678 0.076 Uiso 1 1 calc R . . C18 C 1.0132(5) 0.1530(3) 0.78845(19) 0.0544(11) Uani 1 1 d . . . C19 C 0.9645(5) 0.0558(3) 0.74871(16) 0.0642(10) Uani 1 1 d . . . H19A H 0.9137 -0.0071 0.7648 0.077 Uiso 1 1 calc R . . C20 C 0.9897(4) 0.0503(3) 0.68583(16) 0.0635(10) Uani 1 1 d . . . H20A H 0.9550 -0.0155 0.6606 0.076 Uiso 1 1 calc R . . C21 C 1.0666(5) 0.1425(3) 0.66000(17) 0.0522(10) Uani 1 1 d . . . C22 C 1.1120(5) 0.2389(3) 0.69869(18) 0.0662(11) Uani 1 1 d . . . H22A H 1.1616 0.3022 0.6826 0.079 Uiso 1 1 calc R . . C23 C 1.0856(5) 0.2438(3) 0.76110(18) 0.0654(11) Uani 1 1 d . . . H23A H 1.1178 0.3108 0.7857 0.079 Uiso 1 1 calc R . . C24 C 1.0942(5) 0.1377(3) 0.59263(18) 0.0529(10) Uani 1 1 d . . . C25 C 0.9944(4) 0.0691(3) 0.54705(15) 0.0645(9) Uani 1 1 d . . . H25A H 0.9105 0.0245 0.5591 0.077 Uiso 1 1 calc R . . C26 C 1.0191(5) 0.0670(3) 0.48422(17) 0.0737(11) Uani 1 1 d . . . H26A H 0.9514 0.0215 0.4544 0.088 Uiso 1 1 calc R . . C27 C 1.1434(6) 0.1318(4) 0.4656(2) 0.0769(13) Uani 1 1 d . . . H27A H 1.1598 0.1300 0.4234 0.092 Uiso 1 1 calc R . . C28 C 1.2424(5) 0.1988(3) 0.50947(18) 0.0717(11) Uani 1 1 d . . . H28A H 1.3266 0.2426 0.4972 0.086 Uiso 1 1 calc R . . C29 C 1.2171(5) 0.2013(3) 0.57252(17) 0.0623(10) Uani 1 1 d . . . H29A H 1.2853 0.2474 0.6019 0.075 Uiso 1 1 calc R . . C59 C 0.2016(4) 0.5560(3) 0.40025(17) 0.0508(10) Uani 1 1 d . . . C60 C 0.2149(4) 0.6738(3) 0.40267(17) 0.0499(10) Uani 1 1 d . . . C61 C 0.1854(5) 0.7172(4) 0.46582(19) 0.0565(10) Uani 1 1 d . . . H61 H 0.1881 0.7952 0.4794 0.068 Uiso 1 1 calc R . . C62 C 0.1533(4) 0.6237(4) 0.50172(19) 0.0527(10) Uani 1 1 d . . . C63 C 0.1622(5) 0.5163(3) 0.46267(18) 0.0591(11) Uani 1 1 d . . . H63A H 0.0598 0.4735 0.4572 0.071 Uiso 1 1 calc R . . H63B H 0.2458 0.4664 0.4821 0.071 Uiso 1 1 calc R . . C64 C 0.2134(4) 0.4710(3) 0.34752(18) 0.0491(9) Uani 1 1 d . . . C65 C 0.2878(4) 0.3640(3) 0.3591(2) 0.0557(10) Uani 1 1 d . . . H65A H 0.3321 0.3481 0.4001 0.067 Uiso 1 1 calc R . . C66 C 0.2970(5) 0.2814(4) 0.3110(2) 0.0667(12) Uani 1 1 d . . . H66A H 0.3467 0.2110 0.3200 0.080 Uiso 1 1 calc R . . C67 C 0.2332(5) 0.3032(4) 0.2506(2) 0.0717(13) Uani 1 1 d . . . H67A H 0.2395 0.2479 0.2181 0.086 Uiso 1 1 calc R . . C68 C 0.1593(5) 0.4076(4) 0.23803(19) 0.0709(12) Uani 1 1 d . . . H68A H 0.1161 0.4227 0.1967 0.085 Uiso 1 1 calc R . . C69 C 0.1481(5) 0.4903(4) 0.28562(19) 0.0643(11) Uani 1 1 d . . . H69A H 0.0962 0.5598 0.2761 0.077 Uiso 1 1 calc R . . C70 C 0.2483(4) 0.7550(3) 0.35361(17) 0.0488(10) Uani 1 1 d . . . C71 C 0.3536(5) 0.7305(3) 0.31149(18) 0.0575(10) Uani 1 1 d . . . H71A H 0.4080 0.6605 0.3137 0.069 Uiso 1 1 calc R . . C72 C 0.3809(5) 0.8076(4) 0.2657(2) 0.0661(11) Uani 1 1 d . . . H72A H 0.4518 0.7885 0.2371 0.079 Uiso 1 1 calc R . . C73 C 0.3042(5) 0.9117(4) 0.2622(2) 0.0726(13) Uani 1 1 d . . . H73A H 0.3217 0.9628 0.2309 0.087 Uiso 1 1 calc R . . C74 C 0.2014(5) 0.9412(4) 0.3047(2) 0.0680(12) Uani 1 1 d . . . H74A H 0.1517 1.0131 0.3035 0.082 Uiso 1 1 calc R . . C75 C 0.1731(5) 0.8618(3) 0.34942(19) 0.0607(11) Uani 1 1 d . . . H75A H 0.1012 0.8807 0.3776 0.073 Uiso 1 1 calc R . . C76 C 0.1205(5) 0.6297(3) 0.56746(18) 0.0518(10) Uani 1 1 d . . . C77 C 0.0415(4) 0.5395(3) 0.59345(16) 0.0617(9) Uani 1 1 d . . . H77A H 0.0112 0.4720 0.5689 0.074 Uiso 1 1 calc R . . C78 C 0.0067(4) 0.5478(3) 0.65535(15) 0.0593(9) Uani 1 1 d . . . H78A H -0.0464 0.4859 0.6713 0.071 Uiso 1 1 calc R . . C79 C 0.0501(5) 0.6473(3) 0.69398(17) 0.0512(10) Uani 1 1 d . . . C80 C 0.1277(5) 0.7367(3) 0.66786(17) 0.0609(10) Uani 1 1 d . . . H80A H 0.1578 0.8044 0.6922 0.073 Uiso 1 1 calc R . . C81 C 0.1619(5) 0.7280(3) 0.60615(17) 0.0630(10) Uani 1 1 d . . . H81A H 0.2144 0.7902 0.5903 0.076 Uiso 1 1 calc R . . C82 C 0.0125(5) 0.6559(3) 0.76012(18) 0.0520(10) Uani 1 1 d . . . C83 C -0.1044(4) 0.5843(3) 0.78099(16) 0.0618(9) Uani 1 1 d . . . H83A H -0.1608 0.5292 0.7529 0.074 Uiso 1 1 calc R . . C84 C -0.1383(5) 0.5935(3) 0.84246(17) 0.0725(10) Uani 1 1 d . . . H84A H -0.2168 0.5448 0.8552 0.087 Uiso 1 1 calc R . . C85 C -0.0562(5) 0.6746(4) 0.8851(2) 0.0693(12) Uani 1 1 d . . . H85A H -0.0782 0.6801 0.9266 0.083 Uiso 1 1 calc R . . C86 C 0.0577(5) 0.7464(3) 0.86551(18) 0.0671(10) Uani 1 1 d . . . H86A H 0.1133 0.8015 0.8938 0.080 Uiso 1 1 calc R . . C87 C 0.0906(4) 0.7378(3) 0.80391(17) 0.0612(9) Uani 1 1 d . . . H87A H 0.1675 0.7883 0.7914 0.073 Uiso 1 1 calc R . . C30 C 0.7173(4) 0.3167(3) 0.40773(17) 0.0496(10) Uani 1 1 d . . . C31 C 0.7035(4) 0.4337(3) 0.40225(17) 0.0475(9) Uani 1 1 d . . . C32 C 0.6637(5) 0.4857(3) 0.46400(17) 0.0558(10) Uani 1 1 d . . . H32A H 0.7461 0.5426 0.4819 0.067 Uiso 1 1 calc R . . H32B H 0.5602 0.5236 0.4578 0.067 Uiso 1 1 calc R . . C33 C 0.6580(5) 0.3875(3) 0.50569(18) 0.0526(10) Uani 1 1 d . . . C34 C 0.6910(5) 0.2873(4) 0.47138(18) 0.0586(11) Uani 1 1 d . . . H34A H 0.6955 0.2125 0.4868 0.070 Uiso 1 1 calc R . . C35 C 0.7481(5) 0.2260(3) 0.35968(18) 0.0510(10) Uani 1 1 d . . . C36 C 0.6760(5) 0.1156(4) 0.35946(19) 0.0630(11) Uani 1 1 d . . . H36A H 0.6107 0.0998 0.3902 0.076 Uiso 1 1 calc R . . C37 C 0.6983(5) 0.0287(4) 0.3150(2) 0.0704(12) Uani 1 1 d . . . H37A H 0.6509 -0.0449 0.3167 0.084 Uiso 1 1 calc R . . C38 C 0.7908(6) 0.0520(4) 0.2687(2) 0.0731(13) Uani 1 1 d . . . H38A H 0.8042 -0.0050 0.2378 0.088 Uiso 1 1 calc R . . C39 C 0.8634(5) 0.1596(4) 0.2679(2) 0.0701(12) Uani 1 1 d . . . H39A H 0.9264 0.1752 0.2364 0.084 Uiso 1 1 calc R . . C40 C 0.8447(5) 0.2454(3) 0.31323(18) 0.0582(10) Uani 1 1 d . . . H40A H 0.8977 0.3172 0.3125 0.070 Uiso 1 1 calc R . . C41 C 0.7130(4) 0.5079(3) 0.34725(17) 0.0470(9) Uani 1 1 d . . . C42 C 0.6400(4) 0.4721(3) 0.28714(16) 0.0565(10) Uani 1 1 d . . . H42A H 0.5849 0.4006 0.2810 0.068 Uiso 1 1 calc R . . C43 C 0.6488(5) 0.5421(4) 0.23633(18) 0.0629(11) Uani 1 1 d . . . H43A H 0.5995 0.5172 0.1963 0.076 Uiso 1 1 calc R . . C44 C 0.7291(5) 0.6474(4) 0.2444(2) 0.0691(13) Uani 1 1 d . . . H44A H 0.7365 0.6930 0.2098 0.083 Uiso 1 1 calc R . . C45 C 0.7994(5) 0.6862(4) 0.3038(2) 0.0673(12) Uani 1 1 d . . . H45A H 0.8518 0.7587 0.3096 0.081 Uiso 1 1 calc R . . C46 C 0.7912(5) 0.6157(3) 0.35503(19) 0.0574(10) Uani 1 1 d . . . H46A H 0.8392 0.6416 0.3951 0.069 Uiso 1 1 calc R . . C47 C 0.6225(4) 0.3939(3) 0.57111(18) 0.0510(10) Uani 1 1 d . . . C48 C 0.6617(4) 0.3039(3) 0.61207(17) 0.0608(10) Uani 1 1 d . . . H48A H 0.7139 0.2391 0.5980 0.073 Uiso 1 1 calc R . . C49 C 0.6249(4) 0.3090(3) 0.67295(17) 0.0591(10) Uani 1 1 d . . . H49A H 0.6533 0.2475 0.6990 0.071 Uiso 1 1 calc R . . C50 C 0.5461(4) 0.4036(3) 0.69669(16) 0.0507(10) Uani 1 1 d . . . C51 C 0.5032(4) 0.4920(3) 0.65496(15) 0.0588(9) Uani 1 1 d . . . H51A H 0.4470 0.5553 0.6685 0.071 Uiso 1 1 calc R . . C52 C 0.5419(4) 0.4882(3) 0.59415(15) 0.0587(9) Uani 1 1 d . . . H52A H 0.5136 0.5497 0.5680 0.070 Uiso 1 1 calc R . . C53 C 0.5077(5) 0.4099(3) 0.76259(17) 0.0516(10) Uani 1 1 d . . . C54 C 0.5831(4) 0.3390(3) 0.80881(16) 0.0602(9) Uani 1 1 d . . . H54A H 0.6578 0.2855 0.7978 0.072 Uiso 1 1 calc R . . C55 C 0.5502(5) 0.3458(3) 0.87038(18) 0.0662(10) Uani 1 1 d . . . H55A H 0.6033 0.2975 0.9001 0.079 Uiso 1 1 calc R . . C56 C 0.4405(5) 0.4229(3) 0.88804(19) 0.0670(12) Uani 1 1 d . . . H56A H 0.4200 0.4287 0.9297 0.080 Uiso 1 1 calc R . . C57 C 0.3599(5) 0.4926(3) 0.84265(17) 0.0700(10) Uani 1 1 d . . . H57A H 0.2829 0.5440 0.8538 0.084 Uiso 1 1 calc R . . C58 C 0.3930(4) 0.4860(3) 0.78161(16) 0.0614(9) Uani 1 1 d . . . H58A H 0.3378 0.5335 0.7520 0.074 Uiso 1 1 calc R . . C88 C 0.4467(4) 0.8706(3) 0.95764(18) 0.0524(10) Uani 1 1 d . . . C89 C 0.4453(4) 0.9900(3) 0.95831(18) 0.0507(10) Uani 1 1 d . . . C90 C 0.4690(5) 1.0279(3) 0.89410(17) 0.0578(11) Uani 1 1 d . . . H90A H 0.3758 1.0696 0.8752 0.069 Uiso 1 1 calc R . . H90B H 0.5641 1.0785 0.8964 0.069 Uiso 1 1 calc R . . C91 C 0.4893(5) 0.9201(3) 0.85701(19) 0.0531(10) Uani 1 1 d . . . C92 C 0.4776(5) 0.8275(4) 0.89512(18) 0.0575(11) Uani 1 1 d . . . H92A H 0.4877 0.7495 0.8831 0.069 Uiso 1 1 calc R . . C93 C 0.4174(4) 0.7899(3) 1.00719(18) 0.0518(10) Uani 1 1 d . . . C94 C 0.4909(5) 0.6811(4) 1.0100(2) 0.0617(11) Uani 1 1 d . . . H94A H 0.5586 0.6603 0.9805 0.074 Uiso 1 1 calc R . . C95 C 0.4642(6) 0.6040(4) 1.0562(2) 0.0728(13) Uani 1 1 d . . . H95A H 0.5165 0.5331 1.0581 0.087 Uiso 1 1 calc R . . C96 C 0.3609(5) 0.6315(4) 1.0994(2) 0.0747(14) Uani 1 1 d . . . H96A H 0.3424 0.5792 1.1300 0.090 Uiso 1 1 calc R . . C97 C 0.2856(5) 0.7373(4) 1.0966(2) 0.0706(12) Uani 1 1 d . . . H97A H 0.2170 0.7567 1.1260 0.085 Uiso 1 1 calc R . . C98 C 0.3101(5) 0.8151(4) 1.05092(18) 0.0609(11) Uani 1 1 d . . . H98A H 0.2551 0.8849 1.0490 0.073 Uiso 1 1 calc R . . C99 C 0.4371(4) 1.0767(3) 1.01053(17) 0.0483(9) Uani 1 1 d . . . C100 C 0.5076(5) 1.0581(3) 1.07252(18) 0.0598(10) Uani 1 1 d . . . H10B H 0.5584 0.9881 1.0817 0.072 Uiso 1 1 calc R . . C101 C 0.5031(5) 1.1422(4) 1.12047(19) 0.0679(11) Uani 1 1 d . . . H10C H 0.5494 1.1283 1.1615 0.082 Uiso 1 1 calc R . . C102 C 0.4288(5) 1.2471(4) 1.1067(2) 0.0673(12) Uani 1 1 d . . . H10D H 0.4252 1.3041 1.1385 0.081 Uiso 1 1 calc R . . C103 C 0.3609(5) 1.2665(4) 1.0461(2) 0.0660(12) Uani 1 1 d . . . H10E H 0.3111 1.3369 1.0371 0.079 Uiso 1 1 calc R . . C104 C 0.3653(5) 1.1839(3) 0.99867(19) 0.0581(11) Uani 1 1 d . . . H10F H 0.3196 1.1994 0.9578 0.070 Uiso 1 1 calc R . . C105 C 0.5162(5) 0.9133(3) 0.79032(19) 0.0548(11) Uani 1 1 d . . . C106 C 0.5858(5) 0.8164(3) 0.76550(17) 0.0619(10) Uani 1 1 d . . . H10G H 0.6167 0.7557 0.7918 0.074 Uiso 1 1 calc R . . C107 C 0.6108(5) 0.8071(3) 0.70344(18) 0.0642(11) Uani 1 1 d . . . H10H H 0.6577 0.7403 0.6888 0.077 Uiso 1 1 calc R . . C108 C 0.5676(5) 0.8953(4) 0.66194(17) 0.0523(10) Uani 1 1 d . . . C109 C 0.4931(5) 0.9914(3) 0.68592(16) 0.0646(10) Uani 1 1 d . . . H10I H 0.4576 1.0504 0.6591 0.078 Uiso 1 1 calc R . . C110 C 0.4705(5) 1.0010(3) 0.74902(16) 0.0628(10) Uani 1 1 d . . . H11B H 0.4238 1.0676 0.7639 0.075 Uiso 1 1 calc R . . C111 C 0.5929(5) 0.8832(3) 0.59425(17) 0.0523(10) Uani 1 1 d . . . C112 C 0.7131(5) 0.8153(3) 0.57552(16) 0.0623(10) Uani 1 1 d . . . H11C H 0.7812 0.7770 0.6058 0.075 Uiso 1 1 calc R . . C113 C 0.7349(5) 0.8026(3) 0.51232(18) 0.0703(11) Uani 1 1 d . . . H11D H 0.8173 0.7564 0.5009 0.084 Uiso 1 1 calc R . . C114 C 0.6364(6) 0.8574(4) 0.4671(2) 0.0739(13) Uani 1 1 d . . . H11E H 0.6510 0.8484 0.4249 0.089 Uiso 1 1 calc R . . C115 C 0.5149(5) 0.9264(3) 0.48418(17) 0.0720(10) Uani 1 1 d . . . H11F H 0.4470 0.9636 0.4534 0.086 Uiso 1 1 calc R . . C116 C 0.4937(4) 0.9403(3) 0.54734(15) 0.0622(9) Uani 1 1 d . . . H11G H 0.4128 0.9882 0.5586 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 C1 0.052(2) 0.050(3) 0.050(2) -0.0047(19) 0.0043(17) 0.0014(18) C2 0.048(2) 0.045(2) 0.053(2) -0.001(2) -0.0006(18) 0.0034(17) C3 0.068(3) 0.051(3) 0.053(3) 0.008(2) 0.008(2) 0.012(2) C4 0.062(3) 0.050(3) 0.048(2) 0.006(2) 0.0054(18) 0.0028(19) C5 0.060(2) 0.058(3) 0.059(3) 0.001(2) 0.0050(19) 0.0042(19) C6 0.047(2) 0.043(2) 0.054(2) 0.0021(19) 0.0092(18) 0.0041(17) C7 0.055(3) 0.051(3) 0.071(3) 0.001(2) 0.009(2) 0.001(2) C8 0.061(3) 0.048(3) 0.105(4) 0.015(3) 0.024(3) 0.000(2) C9 0.071(3) 0.069(3) 0.079(3) 0.024(3) 0.026(3) 0.017(2) C10 0.077(3) 0.067(3) 0.056(3) 0.008(2) 0.010(2) 0.014(2) C11 0.058(2) 0.051(2) 0.058(2) 0.003(2) 0.0064(19) 0.0042(18) C12 0.047(2) 0.048(3) 0.051(2) 0.0018(19) -0.0017(18) 0.0055(18) C13 0.058(3) 0.053(3) 0.079(3) -0.002(2) 0.019(2) 0.0016(19) C14 0.075(3) 0.067(3) 0.074(3) -0.013(3) 0.020(2) 0.008(2) C15 0.080(3) 0.063(3) 0.075(3) -0.018(3) 0.003(3) 0.014(3) C16 0.079(3) 0.048(3) 0.079(3) -0.002(2) -0.003(2) -0.004(2) C17 0.066(3) 0.054(3) 0.067(3) 0.006(2) 0.005(2) 0.004(2) C18 0.066(3) 0.044(2) 0.052(3) -0.003(2) 0.002(2) 0.0014(19) C19 0.081(3) 0.047(2) 0.065(2) 0.0028(18) 0.013(2) -0.0042(19) C20 0.083(3) 0.049(2) 0.057(2) -0.0050(18) 0.0095(19) -0.0085(19) C21 0.064(2) 0.044(2) 0.048(2) 0.0038(19) 0.0045(18) 0.0033(18) C22 0.087(3) 0.052(2) 0.060(3) 0.0017(19) 0.013(2) -0.012(2) C23 0.090(3) 0.047(2) 0.057(2) -0.0055(18) 0.008(2) -0.007(2) C24 0.057(2) 0.047(2) 0.054(2) 0.0022(18) 0.0060(18) 0.0072(18) C25 0.069(2) 0.067(2) 0.056(2) -0.0037(18) 0.0065(18) -0.0025(19) C26 0.077(3) 0.080(3) 0.061(2) -0.014(2) 0.002(2) 0.000(2) C27 0.095(4) 0.081(3) 0.057(3) 0.011(2) 0.016(2) 0.004(3) C28 0.087(3) 0.065(3) 0.065(3) 0.012(2) 0.014(2) -0.002(2) C29 0.074(3) 0.055(2) 0.056(2) 0.0021(18) 0.0040(19) -0.002(2) C59 0.050(2) 0.053(3) 0.048(2) 0.001(2) 0.0042(17) 0.0039(18) C60 0.049(2) 0.049(3) 0.052(2) 0.002(2) 0.0066(18) 0.0012(18) C61 0.063(3) 0.045(2) 0.061(3) -0.006(2) 0.008(2) 0.0056(19) C62 0.050(2) 0.053(3) 0.054(3) -0.002(2) 0.0022(18) 0.0024(19) C63 0.052(2) 0.059(3) 0.066(3) 0.003(2) 0.0059(19) 0.0008(19) C64 0.049(2) 0.048(2) 0.051(2) -0.0008(19) 0.0091(18) -0.0021(18) C65 0.053(2) 0.048(3) 0.066(3) 0.005(2) 0.008(2) -0.0001(19) C66 0.068(3) 0.046(3) 0.088(3) 0.001(3) 0.019(3) 0.003(2) C67 0.072(3) 0.063(3) 0.083(3) -0.016(3) 0.026(3) -0.014(2) C68 0.078(3) 0.082(4) 0.051(3) -0.005(3) 0.007(2) -0.014(3) C69 0.064(3) 0.063(3) 0.065(3) 0.004(2) 0.005(2) 0.004(2) C70 0.052(2) 0.040(2) 0.053(2) 0.0025(19) 0.0009(18) -0.0008(18) C71 0.062(3) 0.051(3) 0.061(3) 0.008(2) 0.008(2) 0.0073(19) C72 0.061(3) 0.070(3) 0.068(3) 0.006(2) 0.011(2) 0.005(2) C73 0.070(3) 0.068(3) 0.079(3) 0.030(3) 0.001(2) -0.001(2) C74 0.072(3) 0.055(3) 0.074(3) 0.011(2) -0.002(2) 0.010(2) C75 0.066(3) 0.053(3) 0.064(3) -0.004(2) 0.012(2) 0.008(2) C76 0.057(2) 0.048(3) 0.050(3) 0.0035(19) 0.0021(18) 0.0010(19) C77 0.070(3) 0.051(2) 0.061(2) -0.0058(18) 0.0039(19) -0.0072(19) C78 0.076(3) 0.045(2) 0.058(2) 0.0037(17) 0.0110(18) -0.0046(18) C79 0.055(2) 0.043(2) 0.053(3) 0.0016(19) 0.0007(18) 0.0067(17) C80 0.077(3) 0.048(2) 0.055(2) -0.0053(19) 0.005(2) -0.0142(19) C81 0.069(3) 0.054(2) 0.067(3) 0.0018(19) 0.013(2) -0.012(2) C82 0.055(2) 0.047(2) 0.053(2) 0.0056(18) 0.0014(18) 0.0040(18) C83 0.070(2) 0.060(2) 0.055(2) -0.0010(17) 0.0066(17) -0.0083(19) C84 0.084(3) 0.066(3) 0.070(3) 0.008(2) 0.020(2) -0.001(2) C85 0.094(3) 0.062(3) 0.055(2) 0.006(2) 0.015(2) 0.014(2) C86 0.083(3) 0.057(2) 0.060(3) -0.0071(19) 0.006(2) 0.005(2) C87 0.065(2) 0.057(2) 0.062(2) 0.0034(19) 0.0096(19) -0.0041(19) C30 0.049(2) 0.052(3) 0.047(2) 0.0015(19) 0.0044(17) -0.0005(18) C31 0.046(2) 0.048(3) 0.049(2) 0.0080(19) 0.0069(17) 0.0043(17) C32 0.053(2) 0.060(3) 0.054(2) 0.001(2) 0.0046(17) -0.0015(19) C33 0.057(2) 0.049(3) 0.051(3) 0.001(2) 0.0031(18) 0.0020(19) C34 0.069(3) 0.052(3) 0.054(3) 0.002(2) 0.006(2) -0.002(2) C35 0.051(2) 0.047(2) 0.054(2) 0.0076(19) 0.0009(18) 0.0049(18) C36 0.075(3) 0.054(3) 0.061(3) 0.005(2) 0.012(2) -0.009(2) C37 0.076(3) 0.052(3) 0.082(3) -0.005(2) 0.008(3) -0.004(2) C38 0.073(3) 0.066(3) 0.078(3) -0.014(3) 0.007(3) 0.006(2) C39 0.060(3) 0.073(3) 0.080(3) -0.006(3) 0.024(2) 0.001(2) C40 0.054(2) 0.051(3) 0.070(3) -0.004(2) 0.013(2) 0.0017(18) C41 0.045(2) 0.048(2) 0.048(2) 0.0052(19) 0.0047(17) 0.0069(18) C42 0.062(3) 0.056(3) 0.051(2) 0.001(2) 0.0042(19) 0.000(2) C43 0.065(3) 0.072(3) 0.052(3) 0.010(2) 0.008(2) 0.012(2) C44 0.074(3) 0.072(3) 0.068(3) 0.023(3) 0.026(2) 0.012(3) C45 0.067(3) 0.051(3) 0.087(3) 0.007(3) 0.021(2) -0.001(2) C46 0.060(3) 0.052(3) 0.058(3) 0.001(2) 0.0030(19) 0.001(2) C47 0.056(2) 0.045(3) 0.051(3) 0.005(2) 0.0026(18) 0.0020(18) C48 0.071(3) 0.055(2) 0.057(2) -0.0023(19) 0.0107(19) 0.012(2) C49 0.071(3) 0.048(2) 0.058(2) 0.0062(18) 0.0058(19) 0.0069(18) C50 0.058(2) 0.047(2) 0.046(2) 0.0024(19) 0.0028(17) -0.0002(17) C51 0.063(2) 0.055(2) 0.057(2) -0.0006(18) 0.0045(18) 0.0098(18) C52 0.074(3) 0.049(2) 0.053(2) 0.0087(17) 0.0065(18) 0.0057(18) C53 0.060(2) 0.042(2) 0.051(2) 0.0033(17) 0.0011(18) -0.0038(18) C54 0.066(2) 0.059(2) 0.056(2) 0.0045(18) 0.0085(18) 0.0090(19) C55 0.080(3) 0.056(2) 0.061(3) 0.0111(19) 0.001(2) -0.002(2) C56 0.094(3) 0.056(3) 0.051(2) 0.001(2) 0.013(2) -0.008(2) C57 0.083(3) 0.061(2) 0.069(3) 0.002(2) 0.020(2) 0.008(2) C58 0.074(2) 0.055(2) 0.056(2) 0.0073(17) 0.0068(18) 0.0087(19) C88 0.051(2) 0.051(3) 0.053(3) -0.004(2) 0.0002(18) 0.0046(19) C89 0.050(2) 0.046(3) 0.055(2) 0.004(2) 0.0035(18) 0.0022(17) C90 0.062(2) 0.055(3) 0.054(2) -0.001(2) 0.0026(19) 0.0038(19) C91 0.064(3) 0.045(3) 0.049(2) -0.004(2) 0.0035(18) 0.0009(19) C92 0.068(3) 0.052(3) 0.052(2) -0.007(2) 0.0076(19) -0.002(2) C93 0.048(2) 0.054(3) 0.051(2) -0.003(2) 0.0002(18) 0.0006(19) C94 0.064(3) 0.052(3) 0.067(3) 0.001(2) 0.001(2) 0.003(2) C95 0.067(3) 0.049(3) 0.098(4) 0.013(3) -0.006(3) 0.007(2) C96 0.064(3) 0.079(4) 0.078(3) 0.027(3) -0.004(3) -0.003(3) C97 0.066(3) 0.079(3) 0.068(3) 0.017(3) 0.011(2) 0.000(2) C98 0.057(3) 0.057(3) 0.067(3) 0.007(2) 0.003(2) 0.001(2) C99 0.046(2) 0.046(2) 0.054(2) 0.0016(19) 0.0098(18) -0.0002(18) C100 0.066(3) 0.053(3) 0.058(2) -0.002(2) 0.003(2) 0.0004(19) C101 0.068(3) 0.079(3) 0.055(3) -0.005(2) 0.005(2) -0.009(2) C102 0.069(3) 0.060(3) 0.076(3) -0.020(2) 0.029(2) -0.011(2) C103 0.062(3) 0.055(3) 0.084(3) -0.008(3) 0.022(2) 0.000(2) C104 0.062(3) 0.053(3) 0.061(3) -0.001(2) 0.012(2) 0.004(2) C105 0.061(3) 0.047(3) 0.056(3) -0.001(2) 0.005(2) -0.0020(19) C106 0.083(3) 0.050(2) 0.053(2) 0.0083(18) 0.0073(19) 0.011(2) C107 0.086(3) 0.050(2) 0.057(2) -0.0009(19) 0.010(2) 0.011(2) C108 0.061(2) 0.045(2) 0.050(2) 0.000(2) 0.0061(18) -0.0015(17) C109 0.082(3) 0.049(2) 0.063(2) 0.0049(18) 0.010(2) 0.0076(19) C110 0.086(3) 0.051(2) 0.053(2) -0.0017(18) 0.0150(19) 0.011(2) C111 0.066(3) 0.040(2) 0.050(2) -0.0022(18) 0.0063(19) -0.0034(18) C112 0.076(3) 0.054(2) 0.057(2) 0.0024(18) 0.0086(19) 0.0049(19) C113 0.085(3) 0.062(3) 0.065(3) -0.012(2) 0.019(2) -0.003(2) C114 0.088(3) 0.078(3) 0.056(3) -0.007(2) 0.016(2) -0.011(3) C115 0.076(3) 0.078(3) 0.060(2) 0.012(2) 0.004(2) -0.007(2) C116 0.063(2) 0.066(2) 0.056(2) 0.0087(18) 0.0047(17) 0.0024(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.356(5) . ? C1 C6 1.472(5) . ? C1 C5 1.498(5) . ? C2 C12 1.478(5) . ? C2 C3 1.479(5) . ? C3 C4 1.365(5) . ? C3 H3 0.9300 . ? C4 C18 1.462(6) . ? C4 C5 1.465(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.391(5) . ? C6 C11 1.399(5) . ? C7 C8 1.372(5) . ? C7 H7A 0.9300 . ? C8 C9 1.377(6) . ? C8 H8A 0.9300 . ? C9 C10 1.379(6) . ? C9 H9A 0.9300 . ? C10 C11 1.377(5) . ? C10 H10A 0.9300 . ? C11 H11A 0.9300 . ? C12 C17 1.388(5) . ? C12 C13 1.396(5) . ? C13 C14 1.369(5) . ? C13 H13A 0.9300 . ? C14 C15 1.386(6) . ? C14 H14A 0.9300 . ? C15 C16 1.375(6) . ? C15 H15A 0.9300 . ? C16 C17 1.371(5) . ? C16 H16A 0.9300 . ? C17 H17A 0.9300 . ? C18 C23 1.383(5) . ? C18 C19 1.397(5) . ? C19 C20 1.388(4) . ? C19 H19A 0.9300 . ? C20 C21 1.397(5) . ? C20 H20A 0.9300 . ? C21 C22 1.372(5) . ? C21 C24 1.488(5) . ? C22 C23 1.380(5) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C29 1.374(5) . ? C24 C25 1.401(5) . ? C25 C26 1.385(4) . ? C25 H25A 0.9300 . ? C26 C27 1.377(6) . ? C26 H26A 0.9300 . ? C27 C28 1.366(6) . ? C27 H27A 0.9300 . ? C28 C29 1.391(5) . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C59 C60 1.353(5) . ? C59 C64 1.478(5) . ? C59 C63 1.502(5) . ? C60 C61 1.475(5) . ? C60 C70 1.478(5) . ? C61 C62 1.385(5) . ? C61 H61 0.9300 . ? C62 C76 1.467(6) . ? C62 C63 1.472(5) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 C69 1.388(5) . ? C64 C65 1.401(5) . ? C65 C66 1.382(5) . ? C65 H65A 0.9300 . ? C66 C67 1.363(6) . ? C66 H66A 0.9300 . ? C67 C68 1.377(6) . ? C67 H67A 0.9300 . ? C68 C69 1.379(5) . ? C68 H68A 0.9300 . ? C69 H69A 0.9300 . ? C70 C71 1.367(5) . ? C70 C75 1.387(5) . ? C71 C72 1.383(5) . ? C71 H71A 0.9300 . ? C72 C73 1.366(6) . ? C72 H72A 0.9300 . ? C73 C74 1.370(6) . ? C73 H73A 0.9300 . ? C74 C75 1.385(5) . ? C74 H74A 0.9300 . ? C75 H75A 0.9300 . ? C76 C81 1.383(5) . ? C76 C77 1.390(5) . ? C77 C78 1.393(4) . ? C77 H77A 0.9300 . ? C78 C79 1.396(5) . ? C78 H78A 0.9300 . ? C79 C80 1.379(5) . ? C79 C82 1.489(5) . ? C80 C81 1.387(5) . ? C80 H80A 0.9300 . ? C81 H81A 0.9300 . ? C82 C87 1.390(5) . ? C82 C83 1.395(5) . ? C83 C84 1.382(4) . ? C83 H83A 0.9300 . ? C84 C85 1.382(5) . ? C84 H84A 0.9300 . ? C85 C86 1.366(5) . ? C85 H85A 0.9300 . ? C86 C87 1.381(5) . ? C86 H86A 0.9300 . ? C87 H87A 0.9300 . ? C30 C31 1.358(5) . ? C30 C34 1.458(5) . ? C30 C35 1.485(5) . ? C31 C41 1.486(5) . ? C31 C32 1.509(5) . ? C32 C33 1.466(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 C34 1.393(5) . ? C33 C47 1.468(5) . ? C34 H34A 0.9300 . ? C35 C40 1.383(5) . ? C35 C36 1.392(5) . ? C36 C37 1.384(5) . ? C36 H36A 0.9300 . ? C37 C38 1.369(6) . ? C37 H37A 0.9300 . ? C38 C39 1.367(6) . ? C38 H38A 0.9300 . ? C39 C40 1.382(5) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 C46 1.383(5) . ? C41 C42 1.389(5) . ? C42 C43 1.383(5) . ? C42 H42A 0.9300 . ? C43 C44 1.365(6) . ? C43 H43A 0.9300 . ? C44 C45 1.377(6) . ? C44 H44A 0.9300 . ? C45 C46 1.393(5) . ? C45 H45A 0.9300 . ? C46 H46A 0.9300 . ? C47 C48 1.393(5) . ? C47 C52 1.394(5) . ? C48 C49 1.377(5) . ? C48 H48A 0.9300 . ? C49 C50 1.395(5) . ? C49 H49A 0.9300 . ? C50 C51 1.394(4) . ? C50 C53 1.486(5) . ? C51 C52 1.380(4) . ? C51 H51A 0.9300 . ? C52 H52A 0.9300 . ? C53 C54 1.393(5) . ? C53 C58 1.398(5) . ? C54 C55 1.380(4) . ? C54 H54A 0.9300 . ? C55 C56 1.366(5) . ? C55 H55A 0.9300 . ? C56 C57 1.390(5) . ? C56 H56A 0.9300 . ? C57 C58 1.370(4) . ? C57 H57A 0.9300 . ? C58 H58A 0.9300 . ? C88 C89 1.370(5) . ? C88 C92 1.465(5) . ? C88 C93 1.474(5) . ? C89 C99 1.476(5) . ? C89 C90 1.492(5) . ? C90 C91 1.469(5) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C91 C92 1.372(5) . ? C91 C105 1.472(5) . ? C92 H92A 0.9300 . ? C93 C94 1.400(5) . ? C93 C98 1.407(5) . ? C94 C95 1.388(5) . ? C94 H94A 0.9300 . ? C95 C96 1.379(6) . ? C95 H95A 0.9300 . ? C96 C97 1.377(6) . ? C96 H96A 0.9300 . ? C97 C98 1.379(5) . ? C97 H97A 0.9300 . ? C98 H98A 0.9300 . ? C99 C104 1.394(5) . ? C99 C100 1.400(5) . ? C100 C101 1.386(5) . ? C100 H10B 0.9300 . ? C101 C102 1.387(6) . ? C101 H10C 0.9300 . ? C102 C103 1.368(6) . ? C102 H10D 0.9300 . ? C103 C104 1.367(5) . ? C103 H10E 0.9300 . ? C104 H10F 0.9300 . ? C105 C106 1.385(5) . ? C105 C110 1.387(5) . ? C106 C107 1.371(5) . ? C106 H10G 0.9300 . ? C107 C108 1.390(5) . ? C107 H10H 0.9300 . ? C108 C109 1.391(5) . ? C108 C111 1.492(5) . ? C109 C110 1.387(4) . ? C109 H10I 0.9300 . ? C110 H11B 0.9300 . ? C111 C112 1.375(5) . ? C111 C116 1.401(5) . ? C112 C113 1.390(5) . ? C112 H11C 0.9300 . ? C113 C114 1.361(5) . ? C113 H11D 0.9300 . ? C114 C115 1.377(5) . ? C114 H11E 0.9300 . ? C115 C116 1.389(4) . ? C115 H11F 0.9300 . ? C116 H11G 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 C2 C1 C6 130.9(4) . . ? C2 C1 C5 108.0(3) . . ? C6 C1 C5 120.9(3) . . ? C1 C2 C12 130.2(4) . . ? C1 C2 C3 108.7(4) . . ? C12 C2 C3 121.1(3) . . ? C4 C3 C2 109.2(4) . . ? C4 C3 H3 125.4 . . ? C2 C3 H3 125.4 . . ? C3 C4 C18 126.4(4) . . ? C3 C4 C5 108.2(4) . . ? C18 C4 C5 125.4(4) . . ? C4 C5 C1 105.8(3) . . ? C4 C5 H5A 110.6 . . ? C1 C5 H5A 110.6 . . ? C4 C5 H5B 110.6 . . ? C1 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? C7 C6 C11 116.9(4) . . ? C7 C6 C1 121.3(3) . . ? C11 C6 C1 121.7(3) . . ? C8 C7 C6 121.6(4) . . ? C8 C7 H7A 119.2 . . ? C6 C7 H7A 119.2 . . ? C7 C8 C9 120.5(4) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C8 C9 C10 119.1(4) . . ? C8 C9 H9A 120.4 . . ? C10 C9 H9A 120.4 . . ? C11 C10 C9 120.4(4) . . ? C11 C10 H10A 119.8 . . ? C9 C10 H10A 119.8 . . ? C10 C11 C6 121.3(4) . . ? C10 C11 H11A 119.3 . . ? C6 C11 H11A 119.3 . . ? C17 C12 C13 117.1(4) . . ? C17 C12 C2 120.3(4) . . ? C13 C12 C2 122.5(4) . . ? C14 C13 C12 121.0(4) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C13 C14 C15 120.7(4) . . ? C13 C14 H14A 119.7 . . ? C15 C14 H14A 119.7 . . ? C16 C15 C14 118.9(4) . . ? C16 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? C17 C16 C15 120.3(4) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C12 121.8(4) . . ? C16 C17 H17A 119.1 . . ? C12 C17 H17A 119.1 . . ? C23 C18 C19 116.0(4) . . ? C23 C18 C4 121.2(4) . . ? C19 C18 C4 122.8(4) . . ? C20 C19 C18 121.8(4) . . ? C20 C19 H19A 119.1 . . ? C18 C19 H19A 119.1 . . ? C19 C20 C21 120.8(3) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C22 C21 C20 117.5(3) . . ? C22 C21 C24 121.3(4) . . ? C20 C21 C24 121.3(4) . . ? C21 C22 C23 121.3(4) . . ? C21 C22 H22A 119.3 . . ? C23 C22 H22A 119.3 . . ? C22 C23 C18 122.6(4) . . ? C22 C23 H23A 118.7 . . ? C18 C23 H23A 118.7 . . ? C29 C24 C25 117.4(4) . . ? C29 C24 C21 121.4(4) . . ? C25 C24 C21 121.2(4) . . ? C26 C25 C24 120.7(4) . . ? C26 C25 H25A 119.6 . . ? C24 C25 H25A 119.6 . . ? C27 C26 C25 120.5(4) . . ? C27 C26 H26A 119.8 . . ? C25 C26 H26A 119.8 . . ? C28 C27 C26 119.6(4) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C29 120.0(4) . . ? C27 C28 H28A 120.0 . . ? C29 C28 H28A 120.0 . . ? C24 C29 C28 121.9(4) . . ? C24 C29 H29A 119.1 . . ? C28 C29 H29A 119.1 . . ? C60 C59 C64 130.3(3) . . ? C60 C59 C63 108.9(3) . . ? C64 C59 C63 120.8(3) . . ? C59 C60 C61 108.5(3) . . ? C59 C60 C70 130.2(3) . . ? C61 C60 C70 121.3(3) . . ? C62 C61 C60 109.5(3) . . ? C62 C61 H61 125.3 . . ? C60 C61 H61 125.3 . . ? C61 C62 C76 126.4(4) . . ? C61 C62 C63 107.7(3) . . ? C76 C62 C63 125.8(4) . . ? C62 C63 C59 105.4(3) . . ? C62 C63 H63A 110.7 . . ? C59 C63 H63A 110.7 . . ? C62 C63 H63B 110.7 . . ? C59 C63 H63B 110.7 . . ? H63A C63 H63B 108.8 . . ? C69 C64 C65 117.0(4) . . ? C69 C64 C59 122.7(3) . . ? C65 C64 C59 120.3(3) . . ? C66 C65 C64 121.6(4) . . ? C66 C65 H65A 119.2 . . ? C64 C65 H65A 119.2 . . ? C67 C66 C65 120.1(4) . . ? C67 C66 H66A 120.0 . . ? C65 C66 H66A 120.0 . . ? C66 C67 C68 119.3(4) . . ? C66 C67 H67A 120.3 . . ? C68 C67 H67A 120.3 . . ? C67 C68 C69 121.1(4) . . ? C67 C68 H68A 119.4 . . ? C69 C68 H68A 119.4 . . ? C68 C69 C64 120.7(4) . . ? C68 C69 H69A 119.6 . . ? C64 C69 H69A 119.6 . . ? C71 C70 C75 117.1(4) . . ? C71 C70 C60 122.8(3) . . ? C75 C70 C60 120.0(3) . . ? C70 C71 C72 121.5(4) . . ? C70 C71 H71A 119.3 . . ? C72 C71 H71A 119.3 . . ? C73 C72 C71 120.2(4) . . ? C73 C72 H72A 119.9 . . ? C71 C72 H72A 119.9 . . ? C72 C73 C74 120.3(4) . . ? C72 C73 H73A 119.9 . . ? C74 C73 H73A 119.9 . . ? C73 C74 C75 118.6(4) . . ? C73 C74 H74A 120.7 . . ? C75 C74 H74A 120.7 . . ? C74 C75 C70 122.3(4) . . ? C74 C75 H75A 118.9 . . ? C70 C75 H75A 118.9 . . ? C81 C76 C77 116.5(3) . . ? C81 C76 C62 121.3(4) . . ? C77 C76 C62 122.1(4) . . ? C76 C77 C78 121.6(3) . . ? C76 C77 H77A 119.2 . . ? C78 C77 H77A 119.2 . . ? C77 C78 C79 121.2(3) . . ? C77 C78 H78A 119.4 . . ? C79 C78 H78A 119.4 . . ? C80 C79 C78 116.9(3) . . ? C80 C79 C82 122.0(4) . . ? C78 C79 C82 121.1(4) . . ? C79 C80 C81 121.5(4) . . ? C79 C80 H80A 119.2 . . ? C81 C80 H80A 119.2 . . ? C76 C81 C80 122.2(4) . . ? C76 C81 H81A 118.9 . . ? C80 C81 H81A 118.9 . . ? C87 C82 C83 116.6(3) . . ? C87 C82 C79 121.3(4) . . ? C83 C82 C79 122.1(3) . . ? C84 C83 C82 121.4(3) . . ? C84 C83 H83A 119.3 . . ? C82 C83 H83A 119.3 . . ? C85 C84 C83 120.4(4) . . ? C85 C84 H84A 119.8 . . ? C83 C84 H84A 119.8 . . ? C86 C85 C84 119.2(4) . . ? C86 C85 H85A 120.4 . . ? C84 C85 H85A 120.4 . . ? C85 C86 C87 120.4(4) . . ? C85 C86 H86A 119.8 . . ? C87 C86 H86A 119.8 . . ? C86 C87 C82 122.0(4) . . ? C86 C87 H87A 119.0 . . ? C82 C87 H87A 119.0 . . ? C31 C30 C34 108.6(4) . . ? C31 C30 C35 129.4(4) . . ? C34 C30 C35 121.9(3) . . ? C30 C31 C41 130.7(4) . . ? C30 C31 C32 108.4(3) . . ? C41 C31 C32 120.8(3) . . ? C33 C32 C31 105.7(3) . . ? C33 C32 H32A 110.6 . . ? C31 C32 H32A 110.6 . . ? C33 C32 H32B 110.6 . . ? C31 C32 H32B 110.6 . . ? H32A C32 H32B 108.7 . . ? C34 C33 C32 107.2(3) . . ? C34 C33 C47 126.6(4) . . ? C32 C33 C47 126.2(4) . . ? C33 C34 C30 110.1(4) . . ? C33 C34 H34A 124.9 . . ? C30 C34 H34A 124.9 . . ? C40 C35 C36 116.9(4) . . ? C40 C35 C30 123.3(3) . . ? C36 C35 C30 119.8(4) . . ? C37 C36 C35 122.2(4) . . ? C37 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? C38 C37 C36 119.4(4) . . ? C38 C37 H37A 120.3 . . ? C36 C37 H37A 120.3 . . ? C39 C38 C37 119.6(4) . . ? C39 C38 H38A 120.2 . . ? C37 C38 H38A 120.2 . . ? C38 C39 C40 121.0(4) . . ? C38 C39 H39A 119.5 . . ? C40 C39 H39A 119.5 . . ? C39 C40 C35 120.9(4) . . ? C39 C40 H40A 119.5 . . ? C35 C40 H40A 119.5 . . ? C46 C41 C42 118.4(4) . . ? C46 C41 C31 120.7(3) . . ? C42 C41 C31 120.9(3) . . ? C43 C42 C41 120.5(4) . . ? C43 C42 H42A 119.8 . . ? C41 C42 H42A 119.8 . . ? C44 C43 C42 120.6(4) . . ? C44 C43 H43A 119.7 . . ? C42 C43 H43A 119.7 . . ? C43 C44 C45 120.1(4) . . ? C43 C44 H44A 119.9 . . ? C45 C44 H44A 119.9 . . ? C44 C45 C46 119.4(4) . . ? C44 C45 H45A 120.3 . . ? C46 C45 H45A 120.3 . . ? C41 C46 C45 121.0(4) . . ? C41 C46 H46A 119.5 . . ? C45 C46 H46A 119.5 . . ? C48 C47 C52 117.0(3) . . ? C48 C47 C33 121.5(4) . . ? C52 C47 C33 121.4(3) . . ? C49 C48 C47 121.4(4) . . ? C49 C48 H48A 119.3 . . ? C47 C48 H48A 119.3 . . ? C48 C49 C50 122.0(3) . . ? C48 C49 H49A 119.0 . . ? C50 C49 H49A 119.0 . . ? C51 C50 C49 116.4(3) . . ? C51 C50 C53 121.5(3) . . ? C49 C50 C53 122.1(3) . . ? C52 C51 C50 121.8(3) . . ? C52 C51 H51A 119.1 . . ? C50 C51 H51A 119.1 . . ? C51 C52 C47 121.3(3) . . ? C51 C52 H52A 119.3 . . ? C47 C52 H52A 119.3 . . ? C54 C53 C58 116.2(3) . . ? C54 C53 C50 121.6(4) . . ? C58 C53 C50 122.1(3) . . ? C55 C54 C53 122.0(3) . . ? C55 C54 H54A 119.0 . . ? C53 C54 H54A 119.0 . . ? C56 C55 C54 120.5(4) . . ? C56 C55 H55A 119.7 . . ? C54 C55 H55A 119.7 . . ? C55 C56 C57 118.9(4) . . ? C55 C56 H56A 120.6 . . ? C57 C56 H56A 120.6 . . ? C58 C57 C56 120.5(4) . . ? C58 C57 H57A 119.7 . . ? C56 C57 H57A 119.7 . . ? C57 C58 C53 121.8(3) . . ? C57 C58 H58A 119.1 . . ? C53 C58 H58A 119.1 . . ? C89 C88 C92 108.6(4) . . ? C89 C88 C93 129.9(4) . . ? C92 C88 C93 121.4(3) . . ? C88 C89 C99 130.9(4) . . ? C88 C89 C90 108.1(3) . . ? C99 C89 C90 120.8(3) . . ? C91 C90 C89 105.6(3) . . ? C91 C90 H90A 110.6 . . ? C89 C90 H90A 110.6 . . ? C91 C90 H90B 110.6 . . ? C89 C90 H90B 110.6 . . ? H90A C90 H90B 108.7 . . ? C92 C91 C90 108.2(4) . . ? C92 C91 C105 126.2(4) . . ? C90 C91 C105 125.6(4) . . ? C91 C92 C88 109.4(4) . . ? C91 C92 H92A 125.3 . . ? C88 C92 H92A 125.3 . . ? C94 C93 C98 117.4(4) . . ? C94 C93 C88 120.2(4) . . ? C98 C93 C88 122.3(4) . . ? C95 C94 C93 120.9(4) . . ? C95 C94 H94A 119.6 . . ? C93 C94 H94A 119.6 . . ? C96 C95 C94 120.7(4) . . ? C96 C95 H95A 119.7 . . ? C94 C95 H95A 119.7 . . ? C95 C96 C97 119.1(4) . . ? C95 C96 H96A 120.4 . . ? C97 C96 H96A 120.4 . . ? C96 C97 C98 121.1(4) . . ? C96 C97 H97A 119.4 . . ? C98 C97 H97A 119.4 . . ? C97 C98 C93 120.7(4) . . ? C97 C98 H98A 119.7 . . ? C93 C98 H98A 119.7 . . ? C104 C99 C100 117.4(4) . . ? C104 C99 C89 120.4(3) . . ? C100 C99 C89 122.1(3) . . ? C101 C100 C99 121.2(4) . . ? C101 C100 H10B 119.4 . . ? C99 C100 H10B 119.4 . . ? C100 C101 C102 119.4(4) . . ? C100 C101 H10C 120.3 . . ? C102 C101 H10C 120.3 . . ? C103 C102 C101 119.8(4) . . ? C103 C102 H10D 120.1 . . ? C101 C102 H10D 120.1 . . ? C104 C103 C102 120.9(4) . . ? C104 C103 H10E 119.5 . . ? C102 C103 H10E 119.5 . . ? C103 C104 C99 121.2(4) . . ? C103 C104 H10F 119.4 . . ? C99 C104 H10F 119.4 . . ? C106 C105 C110 116.7(4) . . ? C106 C105 C91 120.9(4) . . ? C110 C105 C91 122.4(4) . . ? C107 C106 C105 122.2(3) . . ? C107 C106 H10G 118.9 . . ? C105 C106 H10G 118.9 . . ? C106 C107 C108 121.4(4) . . ? C106 C107 H10H 119.3 . . ? C108 C107 H10H 119.3 . . ? C107 C108 C109 116.8(3) . . ? C107 C108 C111 120.9(4) . . ? C109 C108 C111 122.3(4) . . ? C110 C109 C108 121.4(3) . . ? C110 C109 H10I 119.3 . . ? C108 C109 H10I 119.3 . . ? C109 C110 C105 121.4(3) . . ? C109 C110 H11B 119.3 . . ? C105 C110 H11B 119.3 . . ? C112 C111 C116 117.6(3) . . ? C112 C111 C108 121.5(3) . . ? C116 C111 C108 120.9(3) . . ? C111 C112 C113 121.4(4) . . ? C111 C112 H11C 119.3 . . ? C113 C112 H11C 119.3 . . ? C114 C113 C112 120.4(4) . . ? C114 C113 H11D 119.8 . . ? C112 C113 H11D 119.8 . . ? C113 C114 C115 119.8(4) . . ? C113 C114 H11E 120.1 . . ? C115 C114 H11E 120.1 . . ? C114 C115 C116 120.0(4) . . ? C114 C115 H11F 120.0 . . ? C116 C115 H11F 120.0 . . ? C115 C116 C111 120.8(3) . . ? C115 C116 H11G 119.6 . . ? C111 C116 H11G 119.6 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.134 _refine_diff_density_min -0.159 _refine_diff_density_rms 0.032 # = = = END