# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Katagiri, Kosuke' _publ_contact_author_email azumayai@kph.bunri-u.ac.jp _publ_section_title ; Polymorphism or Pseudopolymorphism of a Macrocyclic Compound: Helical Structure, Layered Structure, and Pseudorotaxane Constructed by Weak Intermolecular Interactions ; loop_ _publ_author_name T.Tohaya K.Katagiri J.Katoh H.Masu M.Tominaga I.Azumaya data_a0904243mas _database_code_depnum_ccdc_archive 'CCDC 748361' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H42' _chemical_formula_weight 618.82 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 0.0000 '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 Hexagonal _symmetry_space_group_name_H-M 'P6(1) ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z+1/3' '-x+y, -x, z+2/3' '-x, -y, z+1/2' 'y, -x+y, z+5/6' 'x-y, x, z+1/6' _cell_length_a 15.071(17) _cell_length_b 15.071(17) _cell_length_c 28.95(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 5695(12) _cell_formula_units_Z 6 _cell_measurement_temperature 100 _cell_measurement_reflns_used 138 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 18.57 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.083 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 0.061 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9760 _exptl_absorpt_correction_T_max 0.9879 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16750 _diffrn_reflns_av_R_equivalents 0.0940 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 20.67 _reflns_number_total 1989 _reflns_number_gt 1430 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.0983P)^2^+4.2306P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -10(10) _refine_ls_number_reflns 1989 _refine_ls_number_parameters 440 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_ref 0.1885 _refine_ls_wR_factor_gt 0.1447 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.166 _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 -0.1204(7) -0.0275(8) 0.0794(3) 0.048(3) Uani 1 1 d . . . C2 C -0.0558(7) -0.0772(8) 0.0846(4) 0.051(3) Uani 1 1 d . . . C3 C -0.0579(8) -0.1315(8) 0.1244(4) 0.058(3) Uani 1 1 d . . . H3 H -0.1022 -0.1378 0.1491 0.069 Uiso 1 1 calc R . . C4 C 0.0028(8) -0.1763(8) 0.1287(4) 0.056(3) Uani 1 1 d . . . H4 H 0.0007 -0.2105 0.1566 0.067 Uiso 1 1 calc R . . C5 C 0.0674(8) -0.1721(8) 0.0927(4) 0.053(3) Uani 1 1 d . . . C6 C 0.0700(10) -0.1179(11) 0.0538(4) 0.087(4) Uani 1 1 d . . . H6 H 0.1135 -0.1127 0.0289 0.104 Uiso 1 1 calc R . . C7 C 0.0106(10) -0.0703(10) 0.0498(4) 0.084(4) Uani 1 1 d . . . H7 H 0.0161 -0.0325 0.0227 0.100 Uiso 1 1 calc R . . C8 C 0.1327(7) -0.2202(8) 0.0973(4) 0.049(3) Uani 1 1 d . . . C9 C 0.1897(7) -0.2083(7) 0.1378(4) 0.051(3) Uani 1 1 d . . . H9 H 0.1872 -0.1685 0.1627 0.061 Uiso 1 1 calc R . . C10 C 0.2498(8) -0.2544(8) 0.1417(4) 0.054(3) Uani 1 1 d . . . H10 H 0.2886 -0.2438 0.1690 0.065 Uiso 1 1 calc R . . C11 C 0.2550(7) -0.3165(7) 0.1062(4) 0.049(3) Uani 1 1 d . . . C12 C 0.1992(8) -0.3266(9) 0.0672(4) 0.059(3) Uani 1 1 d . . . H12 H 0.2011 -0.3667 0.0423 0.070 Uiso 1 1 calc R . . C13 C 0.1396(8) -0.2799(9) 0.0627(4) 0.062(3) Uani 1 1 d . . . H13 H 0.1024 -0.2895 0.0349 0.075 Uiso 1 1 calc R . . C14 C 0.3187(9) -0.3664(8) 0.1122(4) 0.050(3) Uani 1 1 d . . . C15 C 0.4217(9) -0.3132(8) 0.1179(3) 0.048(3) Uani 1 1 d . . . C16 C 0.4775(7) -0.1989(7) 0.1159(3) 0.046(3) Uani 1 1 d . . . C17 C 0.4946(7) -0.1464(8) 0.0738(3) 0.046(3) Uani 1 1 d . . . H17 H 0.4724 -0.1843 0.0459 0.055 Uiso 1 1 calc R . . C18 C 0.5430(7) -0.0409(7) 0.0724(3) 0.044(2) Uani 1 1 d . . . H18 H 0.5516 -0.0084 0.0433 0.053 Uiso 1 1 calc R . . C19 C 0.5802(7) 0.0208(7) 0.1121(3) 0.041(2) Uani 1 1 d . . . C20 C 0.5663(7) -0.0312(8) 0.1546(3) 0.048(3) Uani 1 1 d . . . H20 H 0.5905 0.0072 0.1824 0.058 Uiso 1 1 calc R . . C21 C 0.5175(7) -0.1380(8) 0.1562(3) 0.051(3) Uani 1 1 d . . . H21 H 0.5108 -0.1707 0.1851 0.061 Uiso 1 1 calc R . . C22 C 0.6274(7) 0.1340(8) 0.1099(3) 0.044(2) Uani 1 1 d . . . C23 C 0.5967(7) 0.1807(8) 0.0770(3) 0.045(3) Uani 1 1 d . . . H23 H 0.5465 0.1394 0.0548 0.054 Uiso 1 1 calc R . . C24 C 0.6378(7) 0.2855(8) 0.0759(3) 0.046(3) Uani 1 1 d . . . H24 H 0.6153 0.3146 0.0527 0.055 Uiso 1 1 calc R . . C25 C 0.7119(7) 0.3508(8) 0.1080(3) 0.046(3) Uani 1 1 d . . . C26 C 0.7441(8) 0.3046(8) 0.1399(4) 0.051(3) Uani 1 1 d . . . H26 H 0.7956 0.3466 0.1615 0.061 Uiso 1 1 calc R . . C27 C 0.7042(7) 0.1993(8) 0.1417(3) 0.051(3) Uani 1 1 d . . . H27 H 0.7284 0.1708 0.1643 0.061 Uiso 1 1 calc R . . C28 C 0.7552(8) 0.4650(8) 0.1071(3) 0.051(3) Uani 1 1 d . . . C29 C 0.6980(7) 0.5089(8) 0.0987(4) 0.051(3) Uani 1 1 d . . . C30 C 0.5842(8) 0.4501(7) 0.0930(4) 0.053(3) Uani 1 1 d . . . C31 C 0.5220(8) 0.3818(8) 0.1280(4) 0.057(3) Uani 1 1 d . . . H31 H 0.5529 0.3731 0.1549 0.069 Uiso 1 1 calc R . . C32 C 0.4152(8) 0.3268(8) 0.1231(4) 0.057(3) Uani 1 1 d . . . H32 H 0.3747 0.2814 0.1470 0.069 Uiso 1 1 calc R . . C33 C 0.3659(8) 0.3376(8) 0.0831(4) 0.050(3) Uani 1 1 d . . . C34 C 0.4285(9) 0.4058(8) 0.0492(4) 0.058(3) Uani 1 1 d . . . H34 H 0.3984 0.4151 0.0221 0.069 Uiso 1 1 calc R . . C35 C 0.5354(9) 0.4611(8) 0.0545(4) 0.060(3) Uani 1 1 d . . . H35 H 0.5758 0.5077 0.0309 0.072 Uiso 1 1 calc R . . C36 C 0.2533(7) 0.2759(8) 0.0786(4) 0.050(3) Uani 1 1 d . . . C37 C 0.1898(10) 0.2340(10) 0.1188(5) 0.093(4) Uani 1 1 d . . . H37 H 0.2203 0.2505 0.1486 0.111 Uiso 1 1 calc R . . C38 C 0.0842(10) 0.1695(11) 0.1149(5) 0.094(4) Uani 1 1 d . . . H38 H 0.0450 0.1406 0.1421 0.113 Uiso 1 1 calc R . . C39 C 0.0347(8) 0.1464(8) 0.0728(4) 0.056(3) Uani 1 1 d . . . C40 C 0.0939(9) 0.2062(10) 0.0372(4) 0.074(4) Uani 1 1 d . . . H40 H 0.0609 0.2061 0.0093 0.088 Uiso 1 1 calc R . . C41 C 0.1987(8) 0.2666(9) 0.0397(4) 0.073(4) Uani 1 1 d . . . H41 H 0.2347 0.3037 0.0130 0.088 Uiso 1 1 calc R . . C42 C -0.0790(8) 0.0721(9) 0.0710(3) 0.055(3) Uani 1 1 d . . . C43 C -0.2341(8) -0.0995(9) 0.0838(4) 0.064(3) Uani 1 1 d . . . H43A H -0.2668 -0.0621 0.0958 0.095 Uiso 1 1 calc R . . H43B H -0.2468 -0.1554 0.1049 0.095 Uiso 1 1 calc R . . H43C H -0.2628 -0.1279 0.0533 0.095 Uiso 1 1 calc R . . C44 C 0.2553(9) -0.4821(8) 0.1127(4) 0.066(3) Uani 1 1 d . . . H44A H 0.2998 -0.5109 0.1188 0.099 Uiso 1 1 calc R . . H44B H 0.2218 -0.5064 0.0826 0.099 Uiso 1 1 calc R . . H44C H 0.2031 -0.5041 0.1369 0.099 Uiso 1 1 calc R . . C45 C 0.4905(8) -0.3582(8) 0.1253(4) 0.060(3) Uani 1 1 d . . . H45A H 0.4484 -0.4324 0.1296 0.090 Uiso 1 1 calc R . . H45B H 0.5328 -0.3274 0.1528 0.090 Uiso 1 1 calc R . . H45C H 0.5348 -0.3438 0.0983 0.090 Uiso 1 1 calc R . . C46 C 0.8702(8) 0.5272(8) 0.1175(5) 0.074(4) Uani 1 1 d . . . H46A H 0.8997 0.5943 0.1025 0.110 Uiso 1 1 calc R . . H46B H 0.9039 0.4905 0.1058 0.110 Uiso 1 1 calc R . . H46C H 0.8806 0.5365 0.1510 0.110 Uiso 1 1 calc R . . C47 C 0.7428(8) 0.6245(8) 0.0972(5) 0.075(4) Uani 1 1 d . . . H47A H 0.7287 0.6477 0.1265 0.113 Uiso 1 1 calc R . . H47B H 0.7117 0.6422 0.0718 0.113 Uiso 1 1 calc R . . H47C H 0.8171 0.6580 0.0925 0.113 Uiso 1 1 calc R . . C48 C -0.1425(8) 0.1236(9) 0.0599(4) 0.065(3) Uani 1 1 d . . . H48A H -0.2135 0.0710 0.0534 0.098 Uiso 1 1 calc R . . H48B H -0.1135 0.1679 0.0327 0.098 Uiso 1 1 calc R . . H48C H -0.1409 0.1649 0.0863 0.098 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 0.036(6) 0.053(8) 0.053(7) -0.002(5) -0.006(5) 0.020(6) C2 0.042(6) 0.059(7) 0.050(7) -0.002(6) 0.004(5) 0.022(6) C3 0.068(8) 0.065(7) 0.038(7) -0.002(6) -0.002(6) 0.031(6) C4 0.064(7) 0.064(7) 0.049(7) 0.002(6) 0.001(6) 0.039(6) C5 0.048(6) 0.068(7) 0.044(7) 0.001(6) -0.003(6) 0.030(6) C6 0.090(10) 0.154(13) 0.050(8) 0.031(8) 0.032(7) 0.087(10) C7 0.078(9) 0.133(12) 0.063(9) 0.037(8) 0.019(7) 0.071(9) C8 0.048(6) 0.057(7) 0.042(7) -0.003(5) 0.002(5) 0.026(6) C9 0.056(6) 0.055(7) 0.048(7) -0.004(5) -0.004(6) 0.032(6) C10 0.062(7) 0.053(7) 0.047(7) 0.000(6) -0.011(5) 0.029(6) C11 0.052(7) 0.041(6) 0.042(7) -0.003(5) 0.003(6) 0.015(5) C12 0.057(7) 0.073(8) 0.047(8) -0.023(6) -0.007(6) 0.034(7) C13 0.055(7) 0.085(8) 0.043(7) -0.011(6) -0.013(5) 0.032(7) C14 0.070(8) 0.050(7) 0.042(6) -0.002(5) 0.005(5) 0.038(7) C15 0.066(8) 0.049(7) 0.035(6) 0.006(5) 0.002(5) 0.033(6) C16 0.050(6) 0.051(7) 0.044(7) -0.006(6) -0.007(5) 0.030(5) C17 0.057(7) 0.051(8) 0.030(6) 0.005(5) 0.001(5) 0.028(6) C18 0.053(6) 0.044(7) 0.035(6) 0.002(5) -0.004(5) 0.024(5) C19 0.043(6) 0.054(7) 0.028(6) -0.002(5) 0.000(5) 0.027(5) C20 0.055(6) 0.052(7) 0.031(6) -0.005(5) -0.001(5) 0.021(6) C21 0.054(6) 0.060(8) 0.042(7) 0.007(6) 0.005(5) 0.030(6) C22 0.047(6) 0.049(7) 0.033(6) -0.006(5) 0.000(5) 0.023(6) C23 0.054(6) 0.049(7) 0.036(6) -0.005(5) -0.007(5) 0.027(6) C24 0.052(7) 0.059(8) 0.033(6) -0.004(5) -0.008(5) 0.032(6) C25 0.040(6) 0.051(7) 0.048(7) -0.001(6) 0.003(5) 0.024(5) C26 0.046(6) 0.054(8) 0.043(7) -0.010(6) -0.002(5) 0.018(6) C27 0.051(6) 0.067(8) 0.039(6) 0.006(6) 0.009(5) 0.033(6) C28 0.044(7) 0.052(7) 0.045(7) -0.009(5) -0.001(5) 0.015(6) C29 0.042(6) 0.047(7) 0.061(7) -0.013(5) -0.009(5) 0.022(6) C30 0.058(7) 0.044(6) 0.054(7) -0.002(6) 0.002(6) 0.023(6) C31 0.052(7) 0.074(7) 0.046(7) -0.019(6) -0.017(6) 0.032(6) C32 0.059(8) 0.061(7) 0.052(8) -0.008(6) 0.001(6) 0.030(6) C33 0.052(7) 0.046(6) 0.051(7) -0.004(6) -0.006(6) 0.023(6) C34 0.059(8) 0.054(7) 0.062(8) 0.005(6) -0.010(6) 0.030(6) C35 0.067(8) 0.047(7) 0.067(8) 0.015(6) 0.006(6) 0.029(6) C36 0.045(7) 0.053(7) 0.048(7) 0.007(5) 0.002(6) 0.022(6) C37 0.067(10) 0.109(11) 0.074(10) 0.015(9) -0.020(8) 0.023(8) C38 0.068(10) 0.116(11) 0.072(10) 0.018(8) -0.004(8) 0.027(8) C39 0.051(7) 0.057(7) 0.052(8) -0.002(6) -0.013(6) 0.020(6) C40 0.050(8) 0.108(10) 0.047(7) 0.012(7) -0.011(6) 0.028(7) C41 0.045(8) 0.109(10) 0.049(8) 0.021(7) -0.001(6) 0.026(7) C42 0.041(7) 0.071(9) 0.048(7) -0.004(6) 0.002(5) 0.025(7) C43 0.059(7) 0.080(8) 0.061(7) -0.003(6) 0.001(6) 0.042(7) C44 0.076(8) 0.068(8) 0.059(8) -0.012(6) -0.003(6) 0.039(7) C45 0.065(7) 0.077(8) 0.047(7) 0.016(6) 0.014(6) 0.043(7) C46 0.061(8) 0.057(7) 0.098(10) -0.006(7) -0.010(7) 0.026(6) C47 0.064(8) 0.053(7) 0.106(10) -0.014(7) -0.012(7) 0.027(6) C48 0.064(7) 0.071(8) 0.065(8) 0.001(6) -0.001(6) 0.037(7) _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 C42 1.329(14) . ? C1 C2 1.503(14) . ? C1 C43 1.507(14) . ? C2 C7 1.387(15) . ? C2 C3 1.405(14) . ? C3 C4 1.387(14) . ? C3 H3 0.9500 . ? C4 C5 1.407(15) . ? C4 H4 0.9500 . ? C5 C6 1.378(16) . ? C5 C8 1.491(15) . ? C6 C7 1.405(16) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C13 1.384(15) . ? C8 C9 1.413(14) . ? C9 C10 1.394(13) . ? C9 H9 0.9500 . ? C10 C11 1.418(13) . ? C10 H10 0.9500 . ? C11 C12 1.370(14) . ? C11 C14 1.498(14) . ? C12 C13 1.397(15) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 C15 1.354(14) . ? C14 C44 1.513(14) . ? C15 C16 1.493(14) . ? C15 C45 1.511(13) . ? C16 C17 1.404(13) . ? C16 C21 1.420(14) . ? C17 C18 1.380(12) . ? C17 H17 0.9500 . ? C18 C19 1.407(13) . ? C18 H18 0.9500 . ? C19 C20 1.416(13) . ? C19 C22 1.486(14) . ? C20 C21 1.397(13) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.395(13) . ? C22 C27 1.419(14) . ? C23 C24 1.379(13) . ? C23 H23 0.9500 . ? C24 C25 1.407(13) . ? C24 H24 0.9500 . ? C25 C26 1.384(14) . ? C25 C28 1.506(14) . ? C26 C27 1.389(14) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C29 1.346(14) . ? C28 C46 1.533(14) . ? C29 C30 1.494(14) . ? C29 C47 1.522(15) . ? C30 C35 1.392(16) . ? C30 C31 1.413(15) . ? C31 C32 1.401(14) . ? C31 H31 0.9500 . ? C32 C33 1.430(15) . ? C32 H32 0.9500 . ? C33 C34 1.393(14) . ? C33 C36 1.478(14) . ? C34 C35 1.404(15) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C41 1.360(14) . ? C36 C37 1.437(17) . ? C37 C38 1.394(17) . ? C37 H37 0.9500 . ? C38 C39 1.379(16) . ? C38 H38 0.9500 . ? C39 C40 1.366(15) . ? C39 C42 1.508(15) . ? C40 C41 1.375(15) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C48 1.538(15) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? 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 C42 C1 C2 121.7(9) . . ? C42 C1 C43 123.5(9) . . ? C2 C1 C43 114.8(9) . . ? C7 C2 C3 116.4(10) . . ? C7 C2 C1 120.8(10) . . ? C3 C2 C1 122.8(9) . . ? C4 C3 C2 122.0(10) . . ? C4 C3 H3 119.0 . . ? C2 C3 H3 119.0 . . ? C3 C4 C5 121.4(10) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 116.5(10) . . ? C6 C5 C8 122.0(10) . . ? C4 C5 C8 121.5(10) . . ? C5 C6 C7 122.2(11) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C2 C7 C6 121.5(11) . . ? C2 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C13 C8 C9 116.4(9) . . ? C13 C8 C5 122.3(10) . . ? C9 C8 C5 121.3(9) . . ? C10 C9 C8 120.6(9) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C9 C10 C11 122.3(9) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C12 C11 C10 115.9(9) . . ? C12 C11 C14 123.6(9) . . ? C10 C11 C14 120.5(9) . . ? C11 C12 C13 122.3(10) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C8 C13 C12 122.5(10) . . ? C8 C13 H13 118.8 . . ? C12 C13 H13 118.8 . . ? C15 C14 C11 123.3(9) . . ? C15 C14 C44 123.9(9) . . ? C11 C14 C44 112.7(9) . . ? C14 C15 C16 119.7(9) . . ? C14 C15 C45 126.3(9) . . ? C16 C15 C45 113.9(9) . . ? C17 C16 C21 116.7(9) . . ? C17 C16 C15 121.5(9) . . ? C21 C16 C15 121.8(9) . . ? C18 C17 C16 121.2(9) . . ? C18 C17 H17 119.4 . . ? C16 C17 H17 119.4 . . ? C17 C18 C19 122.8(9) . . ? C17 C18 H18 118.6 . . ? C19 C18 H18 118.6 . . ? C18 C19 C20 116.5(9) . . ? C18 C19 C22 121.8(9) . . ? C20 C19 C22 121.6(9) . . ? C21 C20 C19 120.8(9) . . ? C21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C20 C21 C16 121.8(9) . . ? C20 C21 H21 119.1 . . ? C16 C21 H21 119.1 . . ? C23 C22 C27 117.0(9) . . ? C23 C22 C19 121.3(9) . . ? C27 C22 C19 121.7(9) . . ? C24 C23 C22 121.4(9) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 122.0(9) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C26 C25 C24 116.5(9) . . ? C26 C25 C28 121.7(9) . . ? C24 C25 C28 121.8(9) . . ? C25 C26 C27 122.6(10) . . ? C25 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C26 C27 C22 120.4(10) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C29 C28 C25 123.1(9) . . ? C29 C28 C46 122.9(9) . . ? C25 C28 C46 114.0(9) . . ? C28 C29 C30 123.8(9) . . ? C28 C29 C47 122.7(9) . . ? C30 C29 C47 113.4(9) . . ? C35 C30 C31 117.6(9) . . ? C35 C30 C29 122.4(10) . . ? C31 C30 C29 120.0(10) . . ? C32 C31 C30 120.4(10) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C33 121.5(10) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C34 C33 C32 117.2(9) . . ? C34 C33 C36 122.9(10) . . ? C32 C33 C36 119.9(9) . . ? C33 C34 C35 120.9(10) . . ? C33 C34 H34 119.6 . . ? C35 C34 H34 119.6 . . ? C30 C35 C34 122.4(10) . . ? C30 C35 H35 118.8 . . ? C34 C35 H35 118.8 . . ? C41 C36 C37 113.0(9) . . ? C41 C36 C33 125.6(10) . . ? C37 C36 C33 120.6(10) . . ? C38 C37 C36 121.1(12) . . ? C38 C37 H37 119.4 . . ? C36 C37 H37 119.4 . . ? C39 C38 C37 122.2(13) . . ? C39 C38 H38 118.9 . . ? C37 C38 H38 118.9 . . ? C40 C39 C38 114.0(10) . . ? C40 C39 C42 126.0(10) . . ? C38 C39 C42 119.3(10) . . ? C39 C40 C41 123.5(10) . . ? C39 C40 H40 118.3 . . ? C41 C40 H40 118.3 . . ? C36 C41 C40 123.1(10) . . ? C36 C41 H41 118.4 . . ? C40 C41 H41 118.4 . . ? C1 C42 C39 123.3(10) . . ? C1 C42 C48 123.4(10) . . ? C39 C42 C48 113.3(10) . . ? C1 C43 H43A 109.5 . . ? C1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C14 C44 H44A 109.5 . . ? C14 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C14 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C15 C45 H45A 109.5 . . ? C15 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C15 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C28 C46 H46A 109.5 . . ? C28 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C28 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C29 C47 H47A 109.5 . . ? C29 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C29 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C42 C48 H48A 109.5 . . ? C42 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C42 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 20.67 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.456 _refine_diff_density_min -0.233 _refine_diff_density_rms 0.056 data_compound1b _database_code_depnum_ccdc_archive 'CCDC 748362' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H42' _chemical_formula_weight 618.82 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)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.9511(13) _cell_length_b 24.458(3) _cell_length_c 13.2818(14) _cell_angle_alpha 90.00 _cell_angle_beta 113.4000(10) _cell_angle_gamma 90.00 _cell_volume 3562.9(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 3536 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.12 _exptl_crystal_description prismatic _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1320 _exptl_absorpt_coefficient_mu 0.065 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9745 _exptl_absorpt_correction_T_max 0.9871 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16772 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.02 _reflns_number_total 7073 _reflns_number_gt 3985 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.0721P)^2^+1.3827P] 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 7073 _refine_ls_number_parameters 439 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1742 _refine_ls_wR_factor_gt 0.1388 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.004 _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 0.0669(3) -0.03490(11) 0.4046(3) 0.0681(9) Uani 1 1 d . . . H1A H 0.0515 -0.0706 0.3683 0.102 Uiso 1 1 calc R . . H1B H -0.0103 -0.0152 0.3848 0.102 Uiso 1 1 calc R . . H1C H 0.1046 -0.0400 0.4843 0.102 Uiso 1 1 calc R . . C2 C 0.1522(3) -0.00211(10) 0.3683(2) 0.0500(7) Uani 1 1 d . . . C3 C 0.1377(2) 0.05854(9) 0.3703(2) 0.0443(6) Uani 1 1 d . . . C4 C 0.1205(2) 0.08333(10) 0.4567(2) 0.0480(7) Uani 1 1 d . . . H4 H 0.1165 0.0610 0.5138 0.058 Uiso 1 1 calc R . . C5 C 0.1089(2) 0.13940(9) 0.4630(2) 0.0482(7) Uani 1 1 d . . . H5 H 0.0983 0.1548 0.5243 0.058 Uiso 1 1 calc R . . C6 C 0.1125(2) 0.17335(9) 0.3802(2) 0.0414(6) Uani 1 1 d . . . C7 C 0.1270(2) 0.14865(10) 0.2923(2) 0.0500(7) Uani 1 1 d . . . H7 H 0.1287 0.1708 0.2341 0.060 Uiso 1 1 calc R . . C8 C 0.1389(3) 0.09255(10) 0.2869(2) 0.0535(7) Uani 1 1 d . . . H8 H 0.1481 0.0770 0.2251 0.064 Uiso 1 1 calc R . . C9 C 0.1048(2) 0.23382(9) 0.3871(2) 0.0422(6) Uani 1 1 d . . . C10 C 0.1570(3) 0.26132(10) 0.4860(2) 0.0487(7) Uani 1 1 d . . . H10 H 0.1913 0.2411 0.5523 0.058 Uiso 1 1 calc R . . C11 C 0.1599(3) 0.31821(10) 0.4896(2) 0.0497(7) Uani 1 1 d . . . H11 H 0.1947 0.3361 0.5586 0.060 Uiso 1 1 calc R . . C12 C 0.1132(2) 0.34916(9) 0.3946(2) 0.0425(6) Uani 1 1 d . . . C13 C 0.0522(2) 0.32171(10) 0.2963(2) 0.0495(7) Uani 1 1 d . . . H13 H 0.0128 0.3421 0.2307 0.059 Uiso 1 1 calc R . . C14 C 0.0482(2) 0.26493(10) 0.2925(2) 0.0508(7) Uani 1 1 d . . . H14 H 0.0060 0.2471 0.2243 0.061 Uiso 1 1 calc R . . C15 C 0.1325(2) 0.40937(9) 0.3970(2) 0.0436(6) Uani 1 1 d . . . C16 C 0.0613(3) 0.44128(10) 0.4495(3) 0.0613(8) Uani 1 1 d . . . H16A H 0.1163 0.4530 0.5231 0.092 Uiso 1 1 calc R . . H16B H -0.0029 0.4180 0.4548 0.092 Uiso 1 1 calc R . . H16C H 0.0244 0.4735 0.4046 0.092 Uiso 1 1 calc R . . C17 C 0.2221(3) 0.49461(10) 0.3612(3) 0.0590(8) Uani 1 1 d . . . H17A H 0.1711 0.5105 0.2899 0.088 Uiso 1 1 calc R . . H17B H 0.3077 0.5038 0.3792 0.088 Uiso 1 1 calc R . . H17C H 0.1972 0.5094 0.4177 0.088 Uiso 1 1 calc R . . C18 C 0.2072(2) 0.43329(9) 0.3562(2) 0.0423(6) Uani 1 1 d . . . C19 C 0.2797(2) 0.40321(9) 0.3038(2) 0.0390(6) Uani 1 1 d . . . C20 C 0.3187(2) 0.34886(10) 0.3286(2) 0.0448(6) Uani 1 1 d . . . H20 H 0.2974 0.3292 0.3801 0.054 Uiso 1 1 calc R . . C21 C 0.3876(2) 0.32327(10) 0.2797(2) 0.0444(6) Uani 1 1 d . . . H21 H 0.4110 0.2862 0.2974 0.053 Uiso 1 1 calc R . . C22 C 0.4236(2) 0.35029(9) 0.20537(19) 0.0376(5) Uani 1 1 d . . . C23 C 0.3859(2) 0.40410(10) 0.1816(2) 0.0494(7) Uani 1 1 d . . . H23 H 0.4082 0.4239 0.1309 0.059 Uiso 1 1 calc R . . C24 C 0.3168(2) 0.42949(10) 0.2301(2) 0.0486(7) Uani 1 1 d . . . H24 H 0.2938 0.4666 0.2120 0.058 Uiso 1 1 calc R . . C25 C 0.5056(2) 0.32252(9) 0.16159(19) 0.0370(6) Uani 1 1 d . . . C26 C 0.6095(2) 0.29621(9) 0.2330(2) 0.0412(6) Uani 1 1 d . . . H26 H 0.6264 0.2956 0.3092 0.049 Uiso 1 1 calc R . . C27 C 0.6890(2) 0.27086(9) 0.1955(2) 0.0400(6) Uani 1 1 d . . . H27 H 0.7605 0.2539 0.2466 0.048 Uiso 1 1 calc R . . C28 C 0.6666(2) 0.26974(9) 0.08457(19) 0.0358(5) Uani 1 1 d . . . C29 C 0.5626(2) 0.29615(9) 0.0133(2) 0.0428(6) Uani 1 1 d . . . H29 H 0.5456 0.2965 -0.0629 0.051 Uiso 1 1 calc R . . C30 C 0.4825(2) 0.32212(10) 0.0503(2) 0.0426(6) Uani 1 1 d . . . H30 H 0.4117 0.3397 -0.0006 0.051 Uiso 1 1 calc R . . C31 C 0.8112(3) 0.27797(10) -0.0111(2) 0.0512(7) Uani 1 1 d . . . H31A H 0.8630 0.2561 -0.0373 0.077 Uiso 1 1 calc R . . H31B H 0.8610 0.3057 0.0406 0.077 Uiso 1 1 calc R . . H31C H 0.7474 0.2960 -0.0735 0.077 Uiso 1 1 calc R . . C32 C 0.7533(2) 0.24125(9) 0.04570(19) 0.0386(6) Uani 1 1 d . . . C33 C 0.7773(2) 0.18792(10) 0.0642(2) 0.0437(6) Uani 1 1 d . . . C34 C 0.8624(3) 0.15565(11) 0.0279(3) 0.0588(8) Uani 1 1 d . . . H34A H 0.8146 0.1337 -0.0366 0.088 Uiso 1 1 calc R . . H34B H 0.9127 0.1315 0.0875 0.088 Uiso 1 1 calc R . . H34C H 0.9150 0.1808 0.0093 0.088 Uiso 1 1 calc R . . C35 C 0.7085(2) 0.15326(9) 0.1140(2) 0.0422(6) Uani 1 1 d . . . C36 C 0.5912(3) 0.13796(12) 0.0491(3) 0.0633(8) Uani 1 1 d . . . H36 H 0.5568 0.1486 -0.0258 0.076 Uiso 1 1 calc R . . C37 C 0.5223(3) 0.10715(12) 0.0914(3) 0.0636(8) Uani 1 1 d . . . H37 H 0.4413 0.0975 0.0445 0.076 Uiso 1 1 calc R . . C38 C 0.5674(2) 0.09031(9) 0.1984(2) 0.0446(6) Uani 1 1 d . . . C39 C 0.6871(3) 0.10507(10) 0.2638(2) 0.0486(7) Uani 1 1 d . . . H39 H 0.7217 0.0942 0.3386 0.058 Uiso 1 1 calc R . . C40 C 0.7566(2) 0.13548(9) 0.2214(2) 0.0470(6) Uani 1 1 d . . . H40 H 0.8386 0.1442 0.2671 0.056 Uiso 1 1 calc R . . C41 C 0.4892(2) 0.05828(9) 0.2398(2) 0.0464(6) Uani 1 1 d . . . C42 C 0.4902(3) 0.06631(10) 0.3434(2) 0.0560(7) Uani 1 1 d . . . H42 H 0.5470 0.0911 0.3926 0.067 Uiso 1 1 calc R . . C43 C 0.4088(3) 0.03843(10) 0.3764(3) 0.0586(8) Uani 1 1 d . . . H43 H 0.4108 0.0447 0.4477 0.070 Uiso 1 1 calc R . . C44 C 0.3250(3) 0.00169(9) 0.3073(2) 0.0506(7) Uani 1 1 d . . . C45 C 0.3295(3) -0.00858(10) 0.2071(3) 0.0574(8) Uani 1 1 d . . . H45 H 0.2771 -0.0355 0.1605 0.069 Uiso 1 1 calc R . . C46 C 0.4082(3) 0.01934(11) 0.1728(3) 0.0557(7) Uani 1 1 d . . . H46 H 0.4074 0.0120 0.1023 0.067 Uiso 1 1 calc R . . C47 C 0.2339(3) -0.02738(9) 0.3398(2) 0.0541(7) Uani 1 1 d . . . C48 C 0.2409(3) -0.08919(10) 0.3352(3) 0.0763(10) Uani 1 1 d . . . H48A H 0.2340 -0.1050 0.4003 0.114 Uiso 1 1 calc R . . H48B H 0.3192 -0.0998 0.3334 0.114 Uiso 1 1 calc R . . H48C H 0.1742 -0.1027 0.2691 0.114 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 0.075(2) 0.0425(15) 0.099(3) 0.0021(15) 0.048(2) -0.0084(15) C2 0.0537(17) 0.0355(13) 0.0665(19) 0.0029(12) 0.0297(15) -0.0049(12) C3 0.0407(15) 0.0367(13) 0.0578(17) 0.0020(12) 0.0221(13) -0.0017(11) C4 0.0511(16) 0.0393(13) 0.0612(18) 0.0083(12) 0.0302(15) -0.0029(12) C5 0.0537(17) 0.0396(13) 0.0608(18) 0.0022(12) 0.0329(15) -0.0007(12) C6 0.0357(14) 0.0351(12) 0.0545(17) 0.0023(11) 0.0188(13) 0.0010(11) C7 0.0624(18) 0.0378(13) 0.0517(17) 0.0087(12) 0.0246(15) 0.0065(13) C8 0.070(2) 0.0388(14) 0.0567(18) 0.0013(12) 0.0309(16) 0.0050(13) C9 0.0382(14) 0.0362(12) 0.0551(17) 0.0026(12) 0.0216(13) 0.0002(11) C10 0.0600(18) 0.0434(14) 0.0538(18) 0.0039(13) 0.0343(15) -0.0002(13) C11 0.0606(18) 0.0436(14) 0.0566(18) -0.0061(13) 0.0357(15) -0.0033(13) C12 0.0419(15) 0.0356(12) 0.0588(17) -0.0016(12) 0.0292(14) 0.0025(11) C13 0.0449(16) 0.0367(13) 0.0629(19) 0.0038(13) 0.0171(14) 0.0050(12) C14 0.0454(16) 0.0367(13) 0.0608(19) -0.0035(13) 0.0111(14) 0.0019(12) C15 0.0449(15) 0.0351(12) 0.0576(17) -0.0055(11) 0.0276(14) 0.0031(11) C16 0.070(2) 0.0425(14) 0.094(2) -0.0119(15) 0.0565(19) -0.0034(14) C17 0.073(2) 0.0365(13) 0.085(2) -0.0069(14) 0.0495(19) -0.0049(13) C18 0.0452(15) 0.0329(12) 0.0538(16) -0.0016(11) 0.0249(13) 0.0006(11) C19 0.0378(14) 0.0370(12) 0.0455(15) -0.0003(11) 0.0201(12) 0.0001(11) C20 0.0438(15) 0.0418(13) 0.0587(17) 0.0053(12) 0.0309(14) 0.0018(11) C21 0.0454(15) 0.0372(13) 0.0591(17) 0.0033(12) 0.0299(14) 0.0012(11) C22 0.0333(13) 0.0416(13) 0.0382(14) 0.0008(11) 0.0145(11) 0.0022(10) C23 0.0582(18) 0.0474(14) 0.0519(17) 0.0088(12) 0.0316(15) 0.0058(13) C24 0.0561(17) 0.0382(13) 0.0592(18) 0.0079(12) 0.0312(15) 0.0073(12) C25 0.0373(14) 0.0379(12) 0.0395(15) 0.0000(10) 0.0190(12) 0.0008(11) C26 0.0446(15) 0.0451(14) 0.0389(15) 0.0028(11) 0.0217(13) 0.0057(12) C27 0.0388(14) 0.0436(13) 0.0400(15) 0.0033(11) 0.0182(12) 0.0057(11) C28 0.0404(14) 0.0328(11) 0.0388(14) -0.0024(10) 0.0205(12) -0.0049(10) C29 0.0501(16) 0.0456(14) 0.0349(14) -0.0020(11) 0.0191(13) -0.0007(12) C30 0.0406(14) 0.0456(14) 0.0408(15) 0.0028(11) 0.0153(12) 0.0037(12) C31 0.0615(18) 0.0521(15) 0.0532(18) -0.0040(13) 0.0367(15) -0.0043(13) C32 0.0398(14) 0.0437(13) 0.0369(14) -0.0047(11) 0.0201(12) -0.0025(11) C33 0.0414(15) 0.0435(14) 0.0539(17) -0.0049(12) 0.0271(13) -0.0007(11) C34 0.0545(18) 0.0572(16) 0.077(2) -0.0030(15) 0.0394(17) 0.0066(14) C35 0.0410(15) 0.0356(12) 0.0542(17) -0.0031(12) 0.0235(13) 0.0023(11) C36 0.0466(17) 0.081(2) 0.0570(19) 0.0197(16) 0.0148(15) -0.0097(15) C37 0.0414(17) 0.077(2) 0.067(2) 0.0115(16) 0.0153(15) -0.0117(15) C38 0.0487(16) 0.0338(12) 0.0566(18) -0.0014(12) 0.0265(14) 0.0002(11) C39 0.0586(18) 0.0380(13) 0.0505(17) -0.0052(12) 0.0229(15) -0.0052(12) C40 0.0426(15) 0.0410(13) 0.0551(18) -0.0069(12) 0.0171(14) -0.0072(12) C41 0.0504(16) 0.0327(12) 0.0634(18) 0.0011(12) 0.0303(15) 0.0003(11) C42 0.070(2) 0.0376(14) 0.070(2) -0.0087(13) 0.0379(17) -0.0117(13) C43 0.079(2) 0.0415(14) 0.069(2) -0.0059(14) 0.0439(18) -0.0055(14) C44 0.0568(17) 0.0272(12) 0.076(2) 0.0042(12) 0.0345(16) 0.0016(12) C45 0.0601(19) 0.0424(14) 0.074(2) -0.0088(14) 0.0315(17) -0.0140(13) C46 0.0579(18) 0.0503(15) 0.064(2) -0.0060(14) 0.0294(16) -0.0092(14) C47 0.0589(18) 0.0309(13) 0.078(2) 0.0063(13) 0.0329(17) -0.0014(12) C48 0.084(2) 0.0345(14) 0.127(3) 0.0082(17) 0.060(2) -0.0001(15) _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 1.518(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C47 1.332(4) . ? C2 C3 1.495(3) . ? C3 C4 1.384(3) . ? C3 C8 1.389(3) . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 C6 1.392(3) . ? C5 H5 0.9500 . ? C6 C7 1.386(3) . ? C6 C9 1.487(3) . ? C7 C8 1.384(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.384(3) . ? C9 C14 1.393(3) . ? C10 C11 1.392(3) . ? C10 H10 0.9500 . ? C11 C12 1.385(4) . ? C11 H11 0.9500 . ? C12 C13 1.390(4) . ? C12 C15 1.489(3) . ? C13 C14 1.390(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C18 1.349(3) . ? C15 C16 1.513(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.509(3) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.501(3) . ? C19 C24 1.384(3) . ? C19 C20 1.404(3) . ? C20 C21 1.384(3) . ? C20 H20 0.9500 . ? C21 C22 1.390(3) . ? C21 H21 0.9500 . ? C22 C23 1.386(3) . ? C22 C25 1.488(3) . ? C23 C24 1.380(3) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.386(3) . ? C25 C30 1.392(3) . ? C26 C27 1.383(3) . ? C26 H26 0.9500 . ? C27 C28 1.389(3) . ? C27 H27 0.9500 . ? C28 C29 1.387(3) . ? C28 C32 1.501(3) . ? C29 C30 1.392(3) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.507(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C33 1.337(3) . ? C33 C35 1.505(3) . ? C33 C34 1.509(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.374(4) . ? C35 C40 1.379(3) . ? C36 C37 1.389(4) . ? C36 H36 0.9500 . ? C37 C38 1.368(4) . ? C37 H37 0.9500 . ? C38 C39 1.394(4) . ? C38 C41 1.483(3) . ? C39 C40 1.390(3) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.386(4) . ? C41 C46 1.397(4) . ? C42 C43 1.393(4) . ? C42 H42 0.9500 . ? C43 C44 1.387(4) . ? C43 H43 0.9500 . ? C44 C45 1.376(4) . ? C44 C47 1.500(3) . ? C45 C46 1.378(4) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.516(3) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? 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 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C47 C2 C3 124.6(2) . . ? C47 C2 C1 120.4(2) . . ? C3 C2 C1 114.9(2) . . ? C4 C3 C8 116.8(2) . . ? C4 C3 C2 120.4(2) . . ? C8 C3 C2 122.8(2) . . ? C5 C4 C3 122.4(2) . . ? C5 C4 H4 118.8 . . ? C3 C4 H4 118.8 . . ? C4 C5 C6 120.5(2) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C7 C6 C5 117.4(2) . . ? C7 C6 C9 121.1(2) . . ? C5 C6 C9 121.5(2) . . ? C8 C7 C6 121.7(2) . . ? C8 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C7 C8 C3 121.3(2) . . ? C7 C8 H8 119.4 . . ? C3 C8 H8 119.4 . . ? C10 C9 C14 117.7(2) . . ? C10 C9 C6 121.7(2) . . ? C14 C9 C6 120.5(2) . . ? C9 C10 C11 121.0(2) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C12 C11 C10 121.3(3) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 117.6(2) . . ? C11 C12 C15 121.2(2) . . ? C13 C12 C15 121.1(2) . . ? C14 C13 C12 120.9(3) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C9 121.1(3) . . ? C13 C14 H14 119.5 . . ? C9 C14 H14 119.5 . . ? C18 C15 C12 122.8(2) . . ? C18 C15 C16 123.0(2) . . ? C12 C15 C16 114.2(2) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 C19 124.7(2) . . ? C15 C18 C17 119.9(2) . . ? C19 C18 C17 115.4(2) . . ? C24 C19 C20 115.8(2) . . ? C24 C19 C18 120.4(2) . . ? C20 C19 C18 123.7(2) . . ? C21 C20 C19 121.5(2) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 121.8(2) . . ? C20 C21 H21 119.1 . . ? C22 C21 H21 119.1 . . ? C23 C22 C21 116.7(2) . . ? C23 C22 C25 123.3(2) . . ? C21 C22 C25 119.9(2) . . ? C24 C23 C22 121.4(2) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C19 122.7(2) . . ? C23 C24 H24 118.6 . . ? C19 C24 H24 118.6 . . ? C26 C25 C30 118.0(2) . . ? C26 C25 C22 119.7(2) . . ? C30 C25 C22 122.3(2) . . ? C27 C26 C25 121.3(2) . . ? C27 C26 H26 119.4 . . ? C25 C26 H26 119.4 . . ? C26 C27 C28 121.3(2) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C29 C28 C27 117.3(2) . . ? C29 C28 C32 122.4(2) . . ? C27 C28 C32 120.3(2) . . ? C28 C29 C30 121.8(2) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C29 C30 C25 120.3(2) . . ? C29 C30 H30 119.9 . . ? C25 C30 H30 119.9 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C28 121.1(2) . . ? C33 C32 C31 124.5(2) . . ? C28 C32 C31 114.4(2) . . ? C32 C33 C35 121.0(2) . . ? C32 C33 C34 125.0(2) . . ? C35 C33 C34 113.6(2) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 117.7(2) . . ? C36 C35 C33 118.4(2) . . ? C40 C35 C33 123.8(2) . . ? C35 C36 C37 121.0(3) . . ? C35 C36 H36 119.5 . . ? C37 C36 H36 119.5 . . ? C38 C37 C36 122.1(3) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? C37 C38 C39 116.9(2) . . ? C37 C38 C41 119.9(2) . . ? C39 C38 C41 123.2(2) . . ? C40 C39 C38 121.1(3) . . ? C40 C39 H39 119.5 . . ? C38 C39 H39 119.5 . . ? C35 C40 C39 121.1(2) . . ? C35 C40 H40 119.4 . . ? C39 C40 H40 119.4 . . ? C42 C41 C46 117.4(2) . . ? C42 C41 C38 122.4(2) . . ? C46 C41 C38 120.2(2) . . ? C41 C42 C43 120.7(3) . . ? C41 C42 H42 119.6 . . ? C43 C42 H42 119.6 . . ? C44 C43 C42 121.4(3) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C45 C44 C43 117.6(2) . . ? C45 C44 C47 120.2(2) . . ? C43 C44 C47 122.2(3) . . ? C44 C45 C46 121.5(3) . . ? C44 C45 H45 119.2 . . ? C46 C45 H45 119.2 . . ? C45 C46 C41 121.2(3) . . ? C45 C46 H46 119.4 . . ? C41 C46 H46 119.4 . . ? C2 C47 C44 124.0(2) . . ? C2 C47 C48 122.2(2) . . ? C44 C47 C48 113.8(2) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.344 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.043 #===END data_compound1c _database_code_depnum_ccdc_archive 'CCDC 748363' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H56' _chemical_formula_weight 704.99 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 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.762(9) _cell_length_b 15.100(9) _cell_length_c 22.115(13) _cell_angle_alpha 77.181(12) _cell_angle_beta 74.946(11) _cell_angle_gamma 62.186(9) _cell_volume 4181(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150 _cell_measurement_reflns_used 1115 _cell_measurement_theta_min 2.64 _cell_measurement_theta_max 27.50 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9814 _exptl_absorpt_correction_T_max 0.9876 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150 _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 APEXII CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25347 _diffrn_reflns_av_R_equivalents 0.0912 _diffrn_reflns_av_sigmaI/netI 0.4129 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 27.69 _reflns_number_total 18414 _reflns_number_gt 4012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2006)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2006)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.0687P)^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 18414 _refine_ls_number_parameters 989 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2878 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.2262 _refine_ls_wR_factor_gt 0.1836 _refine_ls_goodness_of_fit_ref 0.802 _refine_ls_restrained_S_all 0.802 _refine_ls_shift/su_max 0.002 _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 0.4535(3) 0.6096(3) 0.1609(2) 0.0493(15) Uani 1 1 d . . . H1A H 0.4311 0.5572 0.1627 0.074 Uiso 1 1 calc R . . H1B H 0.4326 0.6599 0.1245 0.074 Uiso 1 1 calc R . . H1C H 0.4209 0.6423 0.1996 0.074 Uiso 1 1 calc R . . C2 C 0.5719(3) 0.5619(4) 0.1546(2) 0.0370(13) Uani 1 1 d . . . C3 C 0.6153(3) 0.6332(3) 0.1494(2) 0.0312(12) Uani 1 1 d . . . C4 C 0.5923(3) 0.7182(4) 0.1067(3) 0.0453(15) Uani 1 1 d . . . H4 H 0.5443 0.7326 0.0804 0.054 Uiso 1 1 calc R . . C5 C 0.6363(4) 0.7838(4) 0.1001(2) 0.0431(14) Uani 1 1 d . . . H5 H 0.6212 0.8395 0.0681 0.052 Uiso 1 1 calc R . . C6 C 0.7031(3) 0.7691(3) 0.1403(2) 0.0347(13) Uani 1 1 d . . . C7 C 0.7221(3) 0.6860(3) 0.1858(2) 0.0400(14) Uani 1 1 d . . . H7 H 0.7658 0.6742 0.2144 0.048 Uiso 1 1 calc R . . C8 C 0.6799(4) 0.6206(4) 0.1907(2) 0.0431(14) Uani 1 1 d . . . H8 H 0.6945 0.5650 0.2229 0.052 Uiso 1 1 calc R . . C9 C 0.7540(3) 0.8361(3) 0.1332(3) 0.0341(13) Uani 1 1 d . . . C10 C 0.7758(4) 0.8880(4) 0.0752(3) 0.0462(15) Uani 1 1 d . . . H10 H 0.7564 0.8818 0.0392 0.055 Uiso 1 1 calc R . . C11 C 0.8261(4) 0.9491(4) 0.0696(3) 0.0469(15) Uani 1 1 d . . . H11 H 0.8396 0.9843 0.0296 0.056 Uiso 1 1 calc R . . C12 C 0.8567(3) 0.9597(3) 0.1211(3) 0.0365(13) Uani 1 1 d . . . C13 C 0.8341(4) 0.9087(4) 0.1782(3) 0.0472(15) Uani 1 1 d . . . H13 H 0.8543 0.9137 0.2143 0.057 Uiso 1 1 calc R . . C14 C 0.7818(4) 0.8496(3) 0.1840(3) 0.0417(14) Uani 1 1 d . . . H14 H 0.7647 0.8176 0.2244 0.050 Uiso 1 1 calc R . . C15 C 0.9082(4) 1.0257(3) 0.1170(2) 0.0385(14) Uani 1 1 d . . . C16 C 0.8338(4) 1.1342(3) 0.1226(3) 0.0575(17) Uani 1 1 d . . . H16A H 0.7911 1.1407 0.1649 0.086 Uiso 1 1 calc R . . H16B H 0.7887 1.1589 0.0911 0.086 Uiso 1 1 calc R . . H16C H 0.8731 1.1742 0.1153 0.086 Uiso 1 1 calc R . . C17 C 1.0674(4) 1.0489(3) 0.1152(3) 0.0591(17) Uani 1 1 d . . . H17A H 1.0256 1.1204 0.1023 0.089 Uiso 1 1 calc R . . H17B H 1.1346 1.0247 0.0864 0.089 Uiso 1 1 calc R . . H17C H 1.0789 1.0406 0.1582 0.089 Uiso 1 1 calc R . . C18 C 1.0097(4) 0.9882(3) 0.1133(2) 0.0386(14) Uani 1 1 d . . . C19 C 1.0806(3) 0.8794(4) 0.1063(3) 0.0386(14) Uani 1 1 d . . . C20 C 1.1312(3) 0.8146(3) 0.1551(2) 0.0434(14) Uani 1 1 d . . . H20 H 1.1212 0.8397 0.1933 0.052 Uiso 1 1 calc R . . C21 C 1.1961(3) 0.7140(3) 0.1483(2) 0.0390(14) Uani 1 1 d . . . H21 H 1.2282 0.6708 0.1825 0.047 Uiso 1 1 calc R . . C22 C 1.2154(3) 0.6745(3) 0.0924(2) 0.0339(13) Uani 1 1 d . . . C23 C 1.1653(3) 0.7406(3) 0.0440(2) 0.0420(14) Uani 1 1 d . . . H23 H 1.1769 0.7164 0.0052 0.050 Uiso 1 1 calc R . . C24 C 1.0995(4) 0.8401(3) 0.0510(3) 0.0443(15) Uani 1 1 d . . . H24 H 1.0662 0.8829 0.0171 0.053 Uiso 1 1 calc R . . C25 C 1.2827(3) 0.5673(3) 0.0861(3) 0.0355(13) Uani 1 1 d . . . C26 C 1.3500(3) 0.5375(3) 0.0286(2) 0.0397(14) Uani 1 1 d . . . H26 H 1.3546 0.5876 -0.0051 0.048 Uiso 1 1 calc R . . C27 C 1.4094(3) 0.4369(3) 0.0201(2) 0.0412(14) Uani 1 1 d . . . H27 H 1.4546 0.4191 -0.0190 0.049 Uiso 1 1 calc R . . C28 C 1.4040(3) 0.3622(3) 0.0674(3) 0.0370(14) Uani 1 1 d . . . C29 C 1.3409(3) 0.3902(3) 0.1252(2) 0.0383(14) Uani 1 1 d . . . H29 H 1.3391 0.3396 0.1591 0.046 Uiso 1 1 calc R . . C30 C 1.2810(3) 0.4906(3) 0.1340(2) 0.0377(14) Uani 1 1 d . . . H30 H 1.2376 0.5076 0.1737 0.045 Uiso 1 1 calc R . . C31 C 1.5809(3) 0.2187(3) 0.0346(2) 0.0527(16) Uani 1 1 d . . . H31A H 1.6104 0.1549 0.0168 0.079 Uiso 1 1 calc R . . H31B H 1.6136 0.2088 0.0703 0.079 Uiso 1 1 calc R . . H31C H 1.5937 0.2696 0.0023 0.079 Uiso 1 1 calc R . . C32 C 1.4624(3) 0.2546(3) 0.0573(2) 0.0340(13) Uani 1 1 d . . . C33 C 1.4779(3) 0.0812(3) 0.0602(2) 0.0516(16) Uani 1 1 d . . . H33A H 1.5034 0.0715 0.0155 0.077 Uiso 1 1 calc R . . H33B H 1.4326 0.0474 0.0789 0.077 Uiso 1 1 calc R . . H33C H 1.5371 0.0525 0.0821 0.077 Uiso 1 1 calc R . . C34 C 1.4173(3) 0.1922(3) 0.0664(2) 0.0330(13) Uani 1 1 d . . . C35 C 1.3021(3) 0.2310(3) 0.0808(2) 0.0366(13) Uani 1 1 d . . . C36 C 1.2388(3) 0.3104(3) 0.0436(2) 0.0415(14) Uani 1 1 d . . . H36 H 1.2696 0.3427 0.0084 0.050 Uiso 1 1 calc R . . C37 C 1.1320(3) 0.3444(3) 0.0560(2) 0.0391(14) Uani 1 1 d . . . H37 H 1.0914 0.4000 0.0294 0.047 Uiso 1 1 calc R . . C38 C 1.0819(3) 0.2997(3) 0.1060(2) 0.0346(13) Uani 1 1 d . . . C39 C 1.1453(3) 0.2187(3) 0.1428(2) 0.0443(15) Uani 1 1 d . . . H39 H 1.1145 0.1861 0.1777 0.053 Uiso 1 1 calc R . . C40 C 1.2523(4) 0.1840(3) 0.1300(2) 0.0430(14) Uani 1 1 d . . . H40 H 1.2932 0.1267 0.1554 0.052 Uiso 1 1 calc R . . C41 C 0.9678(4) 0.3375(3) 0.1185(2) 0.0346(13) Uani 1 1 d . . . C42 C 0.9128(4) 0.3158(3) 0.1768(2) 0.0429(14) Uani 1 1 d . . . H42 H 0.9498 0.2740 0.2096 0.051 Uiso 1 1 calc R . . C43 C 0.8046(3) 0.3542(3) 0.1880(2) 0.0388(14) Uani 1 1 d . . . H43 H 0.7697 0.3359 0.2276 0.047 Uiso 1 1 calc R . . C44 C 0.7469(3) 0.4186(3) 0.1424(2) 0.0349(13) Uani 1 1 d . . . C45 C 0.8008(3) 0.4395(3) 0.0838(2) 0.0424(14) Uani 1 1 d . . . H45 H 0.7635 0.4821 0.0514 0.051 Uiso 1 1 calc R . . C46 C 0.9087(3) 0.3989(3) 0.0722(2) 0.0411(14) Uani 1 1 d . . . H46 H 0.9436 0.4133 0.0315 0.049 Uiso 1 1 calc R . . C47 C 0.6310(3) 0.4625(4) 0.1544(2) 0.0389(14) Uani 1 1 d . . . C48 C 0.5864(3) 0.3870(3) 0.1637(3) 0.0524(16) Uani 1 1 d . . . H48A H 0.5221 0.4074 0.1952 0.079 Uiso 1 1 calc R . . H48B H 0.6371 0.3201 0.1784 0.079 Uiso 1 1 calc R . . H48C H 0.5713 0.3847 0.1237 0.079 Uiso 1 1 calc R . . C49 C -0.0048(4) 0.3953(4) 0.3907(3) 0.0705(19) Uani 1 1 d . . . H49A H 0.0577 0.3971 0.3969 0.106 Uiso 1 1 calc R . . H49B H -0.0085 0.3331 0.4132 0.106 Uiso 1 1 calc R . . H49C H -0.0668 0.4536 0.4069 0.106 Uiso 1 1 calc R . . C50 C 0.0003(4) 0.3985(4) 0.3211(3) 0.0546(17) Uani 1 1 d . . . H50A H -0.0621 0.3951 0.3151 0.066 Uiso 1 1 calc R . . H50B H 0.0623 0.3387 0.3051 0.066 Uiso 1 1 calc R . . C51 C 0.0061(4) 0.4928(4) 0.2830(3) 0.0569(16) Uani 1 1 d . . . H51A H 0.0698 0.4949 0.2880 0.068 Uiso 1 1 calc R . . H51B H -0.0545 0.5525 0.3002 0.068 Uiso 1 1 calc R . . C52 C 0.0077(4) 0.4993(4) 0.2129(3) 0.0533(16) Uani 1 1 d . . . H52A H 0.0725 0.4439 0.1947 0.064 Uiso 1 1 calc R . . H52B H -0.0518 0.4896 0.2081 0.064 Uiso 1 1 calc R . . C53 C 0.0015(4) 0.5997(3) 0.1760(3) 0.0500(16) Uani 1 1 d . . . H53A H -0.0629 0.6550 0.1947 0.060 Uiso 1 1 calc R . . H53B H 0.0613 0.6090 0.1807 0.060 Uiso 1 1 calc R . . C54 C 0.0020(4) 0.6078(4) 0.1063(3) 0.0679(19) Uani 1 1 d . . . H54A H 0.0697 0.5599 0.0861 0.102 Uiso 1 1 calc R . . H54B H -0.0107 0.6765 0.0866 0.102 Uiso 1 1 calc R . . H54C H -0.0529 0.5923 0.1011 0.102 Uiso 1 1 calc R . . C55 C 0.3765(6) 0.7984(5) 0.3041(4) 0.125(3) Uani 1 1 d . . . H55A H 0.4375 0.7389 0.3167 0.187 Uiso 1 1 calc R . . H55B H 0.3364 0.7773 0.2863 0.187 Uiso 1 1 calc R . . H55C H 0.3328 0.8333 0.3410 0.187 Uiso 1 1 calc R . . C56 C 0.4117(6) 0.8687(6) 0.2551(4) 0.130(3) Uani 1 1 d . . . H56A H 0.3506 0.9211 0.2371 0.156 Uiso 1 1 calc R . . H56B H 0.4623 0.8297 0.2206 0.156 Uiso 1 1 calc R . . C57 C 0.4615(5) 0.9215(5) 0.2773(3) 0.090(3) Uani 1 1 d . . . H57A H 0.4125 0.9556 0.3140 0.108 Uiso 1 1 calc R . . H57B H 0.5247 0.8683 0.2930 0.108 Uiso 1 1 calc R . . C58 C 0.4916(5) 0.9948(6) 0.2345(3) 0.102(3) Uani 1 1 d . . . H58A H 0.4284 1.0490 0.2194 0.123 Uiso 1 1 calc R . . H58B H 0.5399 0.9614 0.1974 0.123 Uiso 1 1 calc R . . C59 C 0.5429(4) 1.0448(6) 0.2579(3) 0.102(3) Uani 1 1 d . . . H59A H 0.4956 1.0797 0.2947 0.123 Uiso 1 1 calc R . . H59B H 0.6078 0.9922 0.2719 0.123 Uiso 1 1 calc R . . C60 C 0.5685(5) 1.1202(5) 0.2074(3) 0.115(3) Uani 1 1 d . . . H60A H 0.6174 1.0855 0.1715 0.172 Uiso 1 1 calc R . . H60B H 0.6001 1.1513 0.2247 0.172 Uiso 1 1 calc R . . H60C H 0.5045 1.1726 0.1934 0.172 Uiso 1 1 calc R . . C61 C -0.4088(3) 0.9543(3) 0.4211(2) 0.0532(16) Uani 1 1 d . . . H61A H -0.4837 0.9883 0.4206 0.080 Uiso 1 1 calc R . . H61B H -0.3721 0.9804 0.3835 0.080 Uiso 1 1 calc R . . H61C H -0.3958 0.9669 0.4589 0.080 Uiso 1 1 calc R . . C62 C -0.3699(3) 0.8426(3) 0.4214(2) 0.0395(14) Uani 1 1 d . . . C63 C -0.2543(4) 0.7873(3) 0.4094(2) 0.0381(14) Uani 1 1 d . . . C64 C -0.1923(3) 0.8066(3) 0.3542(2) 0.0385(13) Uani 1 1 d . . . H64 H -0.2251 0.8578 0.3227 0.046 Uiso 1 1 calc R . . C65 C -0.0843(3) 0.7544(3) 0.3427(2) 0.0405(14) Uani 1 1 d . . . H65 H -0.0454 0.7682 0.3033 0.049 Uiso 1 1 calc R . . C66 C -0.0328(3) 0.6821(3) 0.3887(2) 0.0338(13) Uani 1 1 d . . . C67 C -0.0943(4) 0.6647(4) 0.4439(2) 0.0538(17) Uani 1 1 d . . . H67 H -0.0615 0.6172 0.4767 0.065 Uiso 1 1 calc R . . C68 C -0.2025(3) 0.7135(3) 0.4539(2) 0.0515(16) Uani 1 1 d . . . H68 H -0.2414 0.6958 0.4920 0.062 Uiso 1 1 calc R . . C69 C 0.0824(3) 0.6242(3) 0.3778(2) 0.0343(13) Uani 1 1 d . . . C70 C 0.1449(4) 0.6369(4) 0.3231(3) 0.070(2) Uani 1 1 d . . . H70 H 0.1139 0.6857 0.2902 0.084 Uiso 1 1 calc R . . C71 C 0.2520(4) 0.5817(4) 0.3131(3) 0.084(2) Uani 1 1 d . . . H71 H 0.2921 0.5952 0.2742 0.101 Uiso 1 1 calc R . . C72 C 0.3015(3) 0.5081(3) 0.3576(2) 0.0346(13) Uani 1 1 d . . . C73 C 0.2386(4) 0.4979(4) 0.4131(3) 0.070(2) Uani 1 1 d . . . H73 H 0.2694 0.4501 0.4464 0.084 Uiso 1 1 calc R . . C74 C 0.1322(4) 0.5540(4) 0.4230(3) 0.070(2) Uani 1 1 d . . . H74 H 0.0923 0.5433 0.4627 0.084 Uiso 1 1 calc R . . C75 C 0.4166(3) 0.4460(4) 0.3467(2) 0.0356(13) Uani 1 1 d . . . C76 C 0.4801(3) 0.5029(3) 0.3403(3) 0.0550(16) Uani 1 1 d . . . H76A H 0.4514 0.5459 0.3743 0.082 Uiso 1 1 calc R . . H76B H 0.4777 0.5449 0.2995 0.082 Uiso 1 1 calc R . . H76C H 0.5524 0.4550 0.3430 0.082 Uiso 1 1 calc R . . C77 C 0.5740(3) 0.2793(3) 0.3441(2) 0.0526(16) Uani 1 1 d . . . H77A H 0.6006 0.2415 0.3076 0.079 Uiso 1 1 calc R . . H77B H 0.5853 0.2320 0.3828 0.079 Uiso 1 1 calc R . . H77C H 0.6108 0.3208 0.3398 0.079 Uiso 1 1 calc R . . C78 C 0.4582(3) 0.3468(4) 0.3474(2) 0.0385(14) Uani 1 1 d . . . C79 C 0.3945(3) 0.2927(3) 0.3503(2) 0.0373(14) Uani 1 1 d . . . C80 C 0.3412(3) 0.3100(3) 0.3028(2) 0.0423(14) Uani 1 1 d . . . H80 H 0.3462 0.3567 0.2670 0.051 Uiso 1 1 calc R . . C81 C 0.2804(3) 0.2606(4) 0.3062(2) 0.0429(15) Uani 1 1 d . . . H81 H 0.2446 0.2742 0.2728 0.051 Uiso 1 1 calc R . . C82 C 0.2712(4) 0.1917(3) 0.3579(3) 0.0389(14) Uani 1 1 d . . . C83 C 0.3271(3) 0.1730(3) 0.4044(2) 0.0415(14) Uani 1 1 d . . . H83 H 0.3232 0.1255 0.4400 0.050 Uiso 1 1 calc R . . C84 C 0.3888(4) 0.2215(4) 0.4007(3) 0.0484(15) Uani 1 1 d . . . H84 H 0.4274 0.2056 0.4331 0.058 Uiso 1 1 calc R . . C85 C 0.2015(4) 0.1423(3) 0.3647(3) 0.0381(14) Uani 1 1 d . . . C86 C 0.1425(4) 0.1277(3) 0.4230(2) 0.0461(15) Uani 1 1 d . . . H86 H 0.1470 0.1494 0.4588 0.055 Uiso 1 1 calc R . . C87 C 0.0768(4) 0.0820(4) 0.4299(3) 0.0491(15) Uani 1 1 d . . . H87 H 0.0382 0.0721 0.4703 0.059 Uiso 1 1 calc R . . C88 C 0.0672(4) 0.0509(4) 0.3784(3) 0.0457(15) Uani 1 1 d . . . C89 C 0.1273(4) 0.0659(4) 0.3209(3) 0.0490(15) Uani 1 1 d . . . H89 H 0.1235 0.0437 0.2851 0.059 Uiso 1 1 calc R . . C90 C 0.1917(4) 0.1112(4) 0.3132(3) 0.0477(15) Uani 1 1 d . . . H90 H 0.2297 0.1213 0.2726 0.057 Uiso 1 1 calc R . . C91 C -0.0025(4) 0.0020(4) 0.3876(3) 0.0484(15) Uani 1 1 d . . . C92 C 0.0535(4) -0.1077(4) 0.3765(3) 0.075(2) Uani 1 1 d . . . H92A H 0.0997 -0.1463 0.4072 0.112 Uiso 1 1 calc R . . H92B H 0.0947 -0.1138 0.3337 0.112 Uiso 1 1 calc R . . H92C H 0.0023 -0.1341 0.3813 0.112 Uiso 1 1 calc R . . C93 C -0.1804(4) 0.0039(4) 0.4186(3) 0.0615(17) Uani 1 1 d . . . H93A H -0.2255 0.0343 0.3869 0.092 Uiso 1 1 calc R . . H93B H -0.2232 0.0162 0.4607 0.092 Uiso 1 1 calc R . . H93C H -0.1413 -0.0688 0.4165 0.092 Uiso 1 1 calc R . . C94 C -0.1052(4) 0.0507(4) 0.4060(3) 0.0448(15) Uani 1 1 d . . . C95 C -0.1576(4) 0.1605(4) 0.4112(3) 0.0417(14) Uani 1 1 d . . . C96 C -0.1645(3) 0.2300(4) 0.3574(2) 0.0428(14) Uani 1 1 d . . . H96 H -0.1333 0.2062 0.3173 0.051 Uiso 1 1 calc R . . C97 C -0.2152(3) 0.3319(4) 0.3607(3) 0.0394(14) Uani 1 1 d . . . H97 H -0.2206 0.3769 0.3228 0.047 Uiso 1 1 calc R . . C98 C -0.2593(3) 0.3711(4) 0.4188(3) 0.0422(14) Uani 1 1 d . . . C99 C -0.2535(4) 0.3011(4) 0.4719(3) 0.0559(17) Uani 1 1 d . . . H99 H -0.2854 0.3247 0.5120 0.067 Uiso 1 1 calc R . . C100 C -0.2042(4) 0.1998(4) 0.4689(3) 0.0534(16) Uani 1 1 d . . . H100 H -0.2013 0.1549 0.5068 0.064 Uiso 1 1 calc R . . C101 C -0.3094(4) 0.4803(4) 0.4216(3) 0.0417(14) Uani 1 1 d . . . C102 C -0.2825(3) 0.5448(4) 0.3731(2) 0.0437(15) Uani 1 1 d . . . H102 H -0.2343 0.5178 0.3366 0.052 Uiso 1 1 calc R . . C103 C -0.3232(3) 0.6462(4) 0.3764(2) 0.0458(15) Uani 1 1 d . . . H103 H -0.3034 0.6878 0.3420 0.055 Uiso 1 1 calc R . . C104 C -0.3938(4) 0.6899(4) 0.4298(2) 0.0426(14) Uani 1 1 d . . . C105 C -0.4265(4) 0.6262(4) 0.4763(3) 0.0535(16) Uani 1 1 d . . . H105 H -0.4793 0.6541 0.5110 0.064 Uiso 1 1 calc R . . C106 C -0.3842(4) 0.5239(4) 0.4733(3) 0.0589(18) Uani 1 1 d . . . H106 H -0.4062 0.4826 0.5067 0.071 Uiso 1 1 calc R . . C107 C -0.4340(3) 0.7979(4) 0.4340(2) 0.0415(14) Uani 1 1 d . . . C108 C -0.5504(3) 0.8532(3) 0.4550(2) 0.0512(16) Uani 1 1 d . . . H10A H -0.5719 0.9261 0.4463 0.077 Uiso 1 1 calc R . . H10B H -0.5688 0.8350 0.5003 0.077 Uiso 1 1 calc R . . H10C H -0.5861 0.8345 0.4319 0.077 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 0.028(3) 0.059(4) 0.060(4) -0.024(3) 0.003(3) -0.017(3) C2 0.023(3) 0.053(3) 0.036(4) -0.010(3) 0.002(2) -0.019(3) C3 0.024(3) 0.045(3) 0.033(3) -0.006(3) -0.004(2) -0.023(2) C4 0.031(3) 0.052(4) 0.055(4) -0.011(3) -0.007(3) -0.019(3) C5 0.041(3) 0.047(3) 0.033(4) -0.001(3) -0.011(3) -0.012(3) C6 0.026(3) 0.041(3) 0.031(3) -0.010(3) 0.006(2) -0.013(2) C7 0.035(3) 0.044(3) 0.040(4) -0.003(3) -0.008(3) -0.016(3) C8 0.045(3) 0.049(3) 0.038(4) 0.003(3) -0.014(3) -0.023(3) C9 0.026(3) 0.041(3) 0.032(4) -0.008(3) -0.003(2) -0.011(2) C10 0.042(3) 0.062(4) 0.037(4) -0.005(3) -0.009(3) -0.024(3) C11 0.053(4) 0.056(4) 0.033(4) 0.000(3) -0.010(3) -0.026(3) C12 0.030(3) 0.036(3) 0.034(4) -0.006(3) -0.005(3) -0.007(2) C13 0.042(3) 0.055(4) 0.047(4) -0.010(3) -0.012(3) -0.019(3) C14 0.044(3) 0.041(3) 0.033(4) -0.004(3) -0.006(3) -0.013(3) C15 0.036(3) 0.028(3) 0.044(4) -0.006(2) 0.002(3) -0.012(2) C16 0.050(3) 0.035(3) 0.078(5) -0.005(3) -0.010(3) -0.012(3) C17 0.049(3) 0.048(3) 0.085(5) -0.017(3) -0.014(3) -0.019(3) C18 0.032(3) 0.026(3) 0.060(4) -0.010(3) -0.002(3) -0.015(2) C19 0.027(3) 0.043(3) 0.045(4) -0.008(3) -0.005(3) -0.013(2) C20 0.037(3) 0.044(3) 0.041(4) -0.013(3) 0.000(3) -0.011(3) C21 0.031(3) 0.037(3) 0.043(4) -0.010(3) -0.005(3) -0.008(2) C22 0.025(3) 0.038(3) 0.043(4) -0.008(3) -0.005(3) -0.016(2) C23 0.049(3) 0.043(3) 0.031(4) -0.004(3) -0.013(3) -0.014(3) C24 0.049(3) 0.033(3) 0.050(4) -0.003(3) -0.018(3) -0.013(3) C25 0.026(3) 0.036(3) 0.047(4) -0.011(3) -0.012(3) -0.010(2) C26 0.036(3) 0.041(3) 0.039(4) 0.007(3) -0.006(3) -0.019(3) C27 0.024(3) 0.044(3) 0.040(4) -0.008(3) 0.008(2) -0.008(2) C28 0.019(3) 0.038(3) 0.052(4) -0.009(3) -0.009(3) -0.008(2) C29 0.029(3) 0.039(3) 0.038(4) -0.001(3) -0.002(3) -0.011(2) C30 0.027(3) 0.035(3) 0.043(4) -0.005(3) -0.003(3) -0.008(2) C31 0.034(3) 0.042(3) 0.068(4) -0.018(3) -0.006(3) -0.001(2) C32 0.023(3) 0.034(3) 0.037(3) -0.017(2) 0.001(2) -0.004(2) C33 0.043(3) 0.041(3) 0.064(4) -0.015(3) -0.011(3) -0.008(3) C34 0.023(3) 0.036(3) 0.035(3) -0.009(2) 0.000(2) -0.009(2) C35 0.025(3) 0.039(3) 0.041(4) -0.004(3) -0.005(3) -0.010(2) C36 0.032(3) 0.040(3) 0.034(4) 0.002(2) -0.001(3) -0.006(2) C37 0.029(3) 0.043(3) 0.038(4) -0.003(3) -0.007(3) -0.010(2) C38 0.028(3) 0.034(3) 0.038(4) -0.006(2) -0.001(3) -0.012(2) C39 0.031(3) 0.049(3) 0.042(4) 0.009(3) -0.007(3) -0.015(3) C40 0.035(3) 0.049(3) 0.042(4) 0.001(3) -0.010(3) -0.017(3) C41 0.039(3) 0.041(3) 0.026(3) -0.009(2) -0.007(3) -0.016(2) C42 0.038(3) 0.048(3) 0.041(4) -0.006(3) -0.011(3) -0.015(3) C43 0.038(3) 0.043(3) 0.034(4) -0.006(3) 0.000(3) -0.019(3) C44 0.032(3) 0.044(3) 0.031(3) -0.009(3) -0.005(3) -0.016(2) C45 0.027(3) 0.060(3) 0.040(4) -0.004(3) -0.004(3) -0.021(3) C46 0.038(3) 0.057(3) 0.029(4) 0.002(3) -0.008(3) -0.024(3) C47 0.033(3) 0.043(3) 0.044(4) -0.007(3) 0.001(3) -0.022(3) C48 0.035(3) 0.061(4) 0.069(4) -0.009(3) -0.003(3) -0.030(3) C49 0.061(4) 0.072(4) 0.062(5) 0.000(3) -0.002(4) -0.023(3) C50 0.041(3) 0.047(4) 0.069(5) -0.003(3) -0.013(3) -0.015(3) C51 0.051(4) 0.065(4) 0.061(5) -0.016(3) -0.013(3) -0.025(3) C52 0.043(3) 0.049(4) 0.068(5) -0.013(3) -0.011(3) -0.017(3) C53 0.029(3) 0.051(4) 0.061(5) -0.014(3) 0.003(3) -0.012(3) C54 0.057(4) 0.073(4) 0.057(5) -0.001(3) -0.005(3) -0.019(3) C55 0.150(7) 0.070(5) 0.130(8) -0.027(5) 0.024(6) -0.046(5) C56 0.094(6) 0.123(8) 0.169(10) -0.065(7) 0.018(6) -0.043(6) C57 0.068(5) 0.057(5) 0.095(7) -0.005(4) 0.001(5) 0.005(4) C58 0.071(5) 0.122(7) 0.066(6) -0.033(5) -0.013(5) 0.006(5) C59 0.035(4) 0.172(8) 0.061(6) -0.047(5) -0.015(4) 0.005(4) C60 0.148(7) 0.091(5) 0.091(6) -0.033(5) 0.045(5) -0.064(5) C61 0.043(3) 0.039(3) 0.062(4) -0.006(3) -0.005(3) -0.007(3) C62 0.023(3) 0.039(3) 0.045(4) -0.013(3) 0.001(3) -0.005(2) C63 0.033(3) 0.035(3) 0.036(4) -0.006(3) -0.004(3) -0.006(2) C64 0.036(3) 0.040(3) 0.034(4) -0.008(2) -0.004(3) -0.012(2) C65 0.028(3) 0.047(3) 0.037(4) -0.001(3) 0.000(3) -0.014(2) C66 0.024(3) 0.035(3) 0.035(3) -0.015(2) 0.000(2) -0.005(2) C67 0.036(3) 0.054(4) 0.038(4) 0.003(3) 0.005(3) -0.002(3) C68 0.029(3) 0.057(4) 0.038(4) 0.003(3) 0.008(3) -0.005(3) C69 0.025(3) 0.030(3) 0.038(4) -0.007(2) -0.004(3) -0.004(2) C70 0.029(3) 0.088(4) 0.045(4) 0.015(3) 0.004(3) -0.002(3) C71 0.030(3) 0.115(5) 0.046(4) 0.021(4) -0.002(3) 0.002(3) C72 0.028(3) 0.041(3) 0.033(3) -0.010(3) 0.002(3) -0.015(2) C73 0.028(3) 0.096(5) 0.053(4) 0.024(4) -0.006(3) -0.015(3) C74 0.028(3) 0.111(5) 0.040(4) 0.021(4) 0.000(3) -0.020(3) C75 0.022(3) 0.052(3) 0.037(4) -0.008(3) 0.000(2) -0.021(3) C76 0.031(3) 0.067(4) 0.067(5) -0.007(3) -0.008(3) -0.023(3) C77 0.024(3) 0.066(4) 0.063(4) -0.019(3) -0.001(3) -0.014(3) C78 0.022(3) 0.050(3) 0.037(4) -0.005(3) -0.004(2) -0.012(3) C79 0.029(3) 0.039(3) 0.035(4) -0.009(3) -0.002(3) -0.007(2) C80 0.036(3) 0.053(3) 0.032(4) 0.005(3) -0.011(3) -0.017(3) C81 0.021(3) 0.056(3) 0.040(4) -0.001(3) -0.005(3) -0.010(3) C82 0.029(3) 0.040(3) 0.040(4) -0.009(3) -0.007(3) -0.006(2) C83 0.033(3) 0.040(3) 0.039(4) 0.006(3) -0.008(3) -0.010(3) C84 0.034(3) 0.052(3) 0.056(4) -0.005(3) -0.019(3) -0.011(3) C85 0.030(3) 0.039(3) 0.038(4) -0.003(3) -0.002(3) -0.013(2) C86 0.046(3) 0.053(3) 0.035(4) -0.012(3) -0.001(3) -0.017(3) C87 0.049(4) 0.048(3) 0.046(4) 0.001(3) -0.005(3) -0.023(3) C88 0.032(3) 0.041(3) 0.057(4) -0.007(3) -0.002(3) -0.013(3) C89 0.040(3) 0.062(4) 0.050(4) -0.015(3) -0.002(3) -0.026(3) C90 0.037(3) 0.063(4) 0.045(4) -0.012(3) 0.003(3) -0.026(3) C91 0.034(3) 0.043(3) 0.067(4) -0.011(3) 0.002(3) -0.020(3) C92 0.048(4) 0.056(4) 0.114(6) -0.031(4) 0.004(4) -0.018(3) C93 0.049(3) 0.060(4) 0.075(5) -0.003(3) -0.007(3) -0.027(3) C94 0.031(3) 0.046(3) 0.058(4) -0.009(3) 0.002(3) -0.022(3) C95 0.033(3) 0.040(3) 0.052(4) -0.002(3) -0.008(3) -0.017(3) C96 0.040(3) 0.053(4) 0.039(4) -0.002(3) -0.012(3) -0.021(3) C97 0.036(3) 0.046(3) 0.040(4) 0.000(3) -0.008(3) -0.023(3) C98 0.028(3) 0.046(3) 0.043(4) 0.005(3) -0.003(3) -0.015(3) C99 0.059(4) 0.045(4) 0.046(4) -0.009(3) 0.010(3) -0.016(3) C100 0.046(3) 0.051(4) 0.048(4) -0.004(3) -0.003(3) -0.013(3) C101 0.034(3) 0.041(3) 0.041(4) -0.005(3) -0.004(3) -0.010(3) C102 0.032(3) 0.052(4) 0.036(4) -0.006(3) -0.002(3) -0.011(3) C103 0.034(3) 0.045(3) 0.046(4) -0.006(3) 0.002(3) -0.010(3) C104 0.031(3) 0.041(3) 0.039(4) -0.003(3) 0.002(3) -0.007(3) C105 0.037(3) 0.055(4) 0.050(4) -0.008(3) 0.015(3) -0.016(3) C106 0.046(3) 0.052(4) 0.055(4) 0.001(3) 0.011(3) -0.015(3) C107 0.021(3) 0.043(3) 0.044(4) -0.008(3) 0.002(3) -0.004(2) C108 0.030(3) 0.047(3) 0.066(4) -0.016(3) 0.001(3) -0.009(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 C1 C2 1.528(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C47 1.338(6) . ? C2 C3 1.461(6) . ? C3 C4 1.371(6) . ? C3 C8 1.408(6) . ? C4 C5 1.383(6) . ? C4 H4 0.9500 . ? C5 C6 1.404(6) . ? C5 H5 0.9500 . ? C6 C7 1.387(6) . ? C6 C9 1.481(6) . ? C7 C8 1.366(6) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C14 1.375(6) . ? C9 C10 1.391(6) . ? C10 C11 1.399(6) . ? C10 H10 0.9500 . ? C11 C12 1.395(6) . ? C11 H11 0.9500 . ? C12 C13 1.373(6) . ? C12 C15 1.487(6) . ? C13 C14 1.396(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C18 1.319(6) . ? C15 C16 1.499(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.526(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.498(6) . ? C19 C24 1.384(6) . ? C19 C20 1.395(6) . ? C20 C21 1.383(6) . ? C20 H20 0.9500 . ? C21 C22 1.396(6) . ? C21 H21 0.9500 . ? C22 C23 1.392(6) . ? C22 C25 1.468(6) . ? C23 C24 1.374(6) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C30 1.391(6) . ? C25 C26 1.411(6) . ? C26 C27 1.381(6) . ? C26 H26 0.9500 . ? C27 C28 1.374(6) . ? C27 H27 0.9500 . ? C28 C29 1.391(6) . ? C28 C32 1.480(6) . ? C29 C30 1.381(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.543(6) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 C34 1.343(6) . ? C33 C34 1.505(6) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.486(6) . ? C35 C36 1.381(5) . ? C35 C40 1.398(6) . ? C36 C37 1.382(6) . ? C36 H36 0.9500 . ? C37 C38 1.391(6) . ? C37 H37 0.9500 . ? C38 C39 1.385(5) . ? C38 C41 1.473(6) . ? C39 C40 1.382(6) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.396(6) . ? C41 C46 1.397(5) . ? C42 C43 1.393(6) . ? C42 H42 0.9500 . ? C43 C44 1.389(6) . ? C43 H43 0.9500 . ? C44 C45 1.389(6) . ? C44 C47 1.489(6) . ? C45 C46 1.387(6) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 C48 1.517(6) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.512(7) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 C51 1.513(6) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.527(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.527(6) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.518(7) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.510(9) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 C57 1.524(9) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 C58 1.448(8) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.523(9) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.519(8) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.505(6) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C107 1.343(6) . ? C62 C63 1.487(6) . ? C63 C68 1.380(6) . ? C63 C64 1.388(6) . ? C64 C65 1.391(6) . ? C64 H64 0.9500 . ? C65 C66 1.392(6) . ? C65 H65 0.9500 . ? C66 C67 1.374(6) . ? C66 C69 1.486(6) . ? C67 C68 1.391(6) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C70 1.354(6) . ? C69 C74 1.359(6) . ? C70 C71 1.383(6) . ? C70 H70 0.9500 . ? C71 C72 1.368(6) . ? C71 H71 0.9500 . ? C72 C73 1.359(6) . ? C72 C75 1.491(6) . ? C73 C74 1.376(6) . ? C73 H73 0.9500 . ? C74 H74 0.9500 . ? C75 C78 1.325(6) . ? C75 C76 1.507(6) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.519(5) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C79 1.489(6) . ? C79 C80 1.381(6) . ? C79 C84 1.381(6) . ? C80 C81 1.389(6) . ? C80 H80 0.9500 . ? C81 C82 1.390(6) . ? C81 H81 0.9500 . ? C82 C83 1.383(6) . ? C82 C85 1.491(6) . ? C83 C84 1.390(6) . ? C83 H83 0.9500 . ? C84 H84 0.9500 . ? C85 C90 1.387(7) . ? C85 C86 1.392(6) . ? C86 C87 1.392(6) . ? C86 H86 0.9500 . ? C87 C88 1.387(7) . ? C87 H87 0.9500 . ? C88 C89 1.389(7) . ? C88 C91 1.475(7) . ? C89 C90 1.367(6) . ? C89 H89 0.9500 . ? C90 H90 0.9500 . ? C91 C94 1.332(6) . ? C91 C92 1.512(6) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 C94 1.514(6) . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 C95 1.485(6) . ? C95 C96 1.391(6) . ? C95 C100 1.397(7) . ? C96 C97 1.371(6) . ? C96 H96 0.9500 . ? C97 C98 1.404(6) . ? C97 H97 0.9500 . ? C98 C99 1.386(6) . ? C98 C101 1.468(6) . ? C99 C100 1.362(6) . ? C99 H99 0.9500 . ? C100 H100 0.9500 . ? C101 C102 1.390(6) . ? C101 C106 1.400(6) . ? C102 C103 1.370(6) . ? C102 H102 0.9500 . ? C103 C104 1.406(6) . ? C103 H103 0.9500 . ? C104 C105 1.397(6) . ? C104 C107 1.469(6) . ? C105 C106 1.380(6) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 C108 1.512(5) . ? C108 H10A 0.9800 . ? C108 H10B 0.9800 . ? C108 H10C 0.9800 . ? 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 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C47 C2 C3 122.7(4) . . ? C47 C2 C1 122.7(5) . . ? C3 C2 C1 114.7(4) . . ? C4 C3 C8 115.9(5) . . ? C4 C3 C2 122.7(5) . . ? C8 C3 C2 121.3(4) . . ? C3 C4 C5 122.7(5) . . ? C3 C4 H4 118.6 . . ? C5 C4 H4 118.6 . . ? C4 C5 C6 120.8(5) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C7 C6 C5 116.5(5) . . ? C7 C6 C9 121.4(5) . . ? C5 C6 C9 122.1(5) . . ? C8 C7 C6 122.0(5) . . ? C8 C7 H7 119.0 . . ? C6 C7 H7 119.0 . . ? C7 C8 C3 121.9(5) . . ? C7 C8 H8 119.1 . . ? C3 C8 H8 119.1 . . ? C14 C9 C10 117.2(5) . . ? C14 C9 C6 121.1(5) . . ? C10 C9 C6 121.8(5) . . ? C9 C10 C11 120.6(5) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C12 C11 C10 121.6(5) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C13 C12 C11 117.3(5) . . ? C13 C12 C15 119.7(5) . . ? C11 C12 C15 123.0(5) . . ? C12 C13 C14 121.0(5) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C9 C14 C13 122.3(5) . . ? C9 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C18 C15 C12 121.4(4) . . ? C18 C15 C16 124.5(5) . . ? C12 C15 C16 113.9(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 C19 122.1(4) . . ? C15 C18 C17 124.7(4) . . ? C19 C18 C17 113.1(4) . . ? C24 C19 C20 117.7(5) . . ? C24 C19 C18 121.2(5) . . ? C20 C19 C18 121.0(5) . . ? C21 C20 C19 120.5(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 121.7(5) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C23 C22 C21 117.0(5) . . ? C23 C22 C25 121.8(5) . . ? C21 C22 C25 121.2(5) . . ? C24 C23 C22 121.4(5) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C19 121.6(5) . . ? C23 C24 H24 119.2 . . ? C19 C24 H24 119.2 . . ? C30 C25 C26 116.7(4) . . ? C30 C25 C22 123.1(5) . . ? C26 C25 C22 120.1(5) . . ? C27 C26 C25 121.3(4) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C28 C27 C26 121.1(5) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 118.3(5) . . ? C27 C28 C32 121.2(5) . . ? C29 C28 C32 120.4(5) . . ? C30 C29 C28 120.9(5) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C25 121.5(5) . . ? C29 C30 H30 119.2 . . ? C25 C30 H30 119.2 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C34 C32 C28 123.5(4) . . ? C34 C32 C31 121.9(4) . . ? C28 C32 C31 114.6(4) . . ? C34 C33 H33A 109.5 . . ? C34 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C34 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 C35 120.9(4) . . ? C32 C34 C33 123.2(4) . . ? C35 C34 C33 115.8(4) . . ? C36 C35 C40 116.1(4) . . ? C36 C35 C34 121.9(4) . . ? C40 C35 C34 121.8(4) . . ? C35 C36 C37 121.9(5) . . ? C35 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C36 C37 C38 122.1(4) . . ? C36 C37 H37 118.9 . . ? C38 C37 H37 118.9 . . ? C39 C38 C37 116.2(4) . . ? C39 C38 C41 122.7(4) . . ? C37 C38 C41 121.1(4) . . ? C40 C39 C38 121.7(5) . . ? C40 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? C39 C40 C35 121.9(4) . . ? C39 C40 H40 119.1 . . ? C35 C40 H40 119.1 . . ? C42 C41 C46 116.5(4) . . ? C42 C41 C38 122.2(4) . . ? C46 C41 C38 121.2(5) . . ? C43 C42 C41 121.3(5) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C44 C43 C42 121.4(5) . . ? C44 C43 H43 119.3 . . ? C42 C43 H43 119.3 . . ? C43 C44 C45 117.7(4) . . ? C43 C44 C47 121.9(5) . . ? C45 C44 C47 120.3(4) . . ? C46 C45 C44 120.7(5) . . ? C46 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? C45 C46 C41 122.3(5) . . ? C45 C46 H46 118.9 . . ? C41 C46 H46 118.9 . . ? C2 C47 C44 121.7(4) . . ? C2 C47 C48 123.2(4) . . ? C44 C47 C48 115.0(4) . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C49 C50 C51 112.5(5) . . ? C49 C50 H50A 109.1 . . ? C51 C50 H50A 109.1 . . ? C49 C50 H50B 109.1 . . ? C51 C50 H50B 109.1 . . ? H50A C50 H50B 107.8 . . ? C50 C51 C52 113.4(5) . . ? C50 C51 H51A 108.9 . . ? C52 C51 H51A 108.9 . . ? C50 C51 H51B 108.9 . . ? C52 C51 H51B 108.9 . . ? H51A C51 H51B 107.7 . . ? C53 C52 C51 113.1(5) . . ? C53 C52 H52A 109.0 . . ? C51 C52 H52A 109.0 . . ? C53 C52 H52B 109.0 . . ? C51 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? C54 C53 C52 113.8(5) . . ? C54 C53 H53A 108.8 . . ? C52 C53 H53A 108.8 . . ? C54 C53 H53B 108.8 . . ? C52 C53 H53B 108.8 . . ? H53A C53 H53B 107.7 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 H55A 109.5 . . ? C56 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C56 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C55 C56 C57 116.8(8) . . ? C55 C56 H56A 108.1 . . ? C57 C56 H56A 108.1 . . ? C55 C56 H56B 108.1 . . ? C57 C56 H56B 108.1 . . ? H56A C56 H56B 107.3 . . ? C58 C57 C56 120.5(7) . . ? C58 C57 H57A 107.2 . . ? C56 C57 H57A 107.2 . . ? C58 C57 H57B 107.2 . . ? C56 C57 H57B 107.2 . . ? H57A C57 H57B 106.8 . . ? C57 C58 C59 119.1(7) . . ? C57 C58 H58A 107.5 . . ? C59 C58 H58A 107.5 . . ? C57 C58 H58B 107.5 . . ? C59 C58 H58B 107.5 . . ? H58A C58 H58B 107.0 . . ? C60 C59 C58 112.3(6) . . ? C60 C59 H59A 109.1 . . ? C58 C59 H59A 109.1 . . ? C60 C59 H59B 109.1 . . ? C58 C59 H59B 109.1 . . ? H59A C59 H59B 107.9 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 H61A 109.5 . . ? C62 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C62 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C107 C62 C63 124.0(4) . . ? C107 C62 C61 122.9(4) . . ? C63 C62 C61 113.1(4) . . ? C68 C63 C64 116.1(4) . . ? C68 C63 C62 121.0(5) . . ? C64 C63 C62 123.0(4) . . ? C63 C64 C65 123.0(4) . . ? C63 C64 H64 118.5 . . ? C65 C64 H64 118.5 . . ? C64 C65 C66 120.3(5) . . ? C64 C65 H65 119.8 . . ? C66 C65 H65 119.8 . . ? C67 C66 C65 116.5(4) . . ? C67 C66 C69 121.8(4) . . ? C65 C66 C69 121.7(4) . . ? C66 C67 C68 122.9(5) . . ? C66 C67 H67 118.5 . . ? C68 C67 H67 118.5 . . ? C63 C68 C67 121.1(5) . . ? C63 C68 H68 119.5 . . ? C67 C68 H68 119.5 . . ? C70 C69 C74 115.4(4) . . ? C70 C69 C66 123.2(4) . . ? C74 C69 C66 121.4(5) . . ? C69 C70 C71 122.7(5) . . ? C69 C70 H70 118.6 . . ? C71 C70 H70 118.6 . . ? C72 C71 C70 121.8(5) . . ? C72 C71 H71 119.1 . . ? C70 C71 H71 119.1 . . ? C73 C72 C71 115.1(4) . . ? C73 C72 C75 122.6(4) . . ? C71 C72 C75 122.3(5) . . ? C72 C73 C74 122.8(5) . . ? C72 C73 H73 118.6 . . ? C74 C73 H73 118.6 . . ? C69 C74 C73 122.2(5) . . ? C69 C74 H74 118.9 . . ? C73 C74 H74 118.9 . . ? C78 C75 C72 121.6(5) . . ? C78 C75 C76 123.1(4) . . ? C72 C75 C76 115.1(4) . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 H77A 109.5 . . ? C78 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C78 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C75 C78 C79 122.1(4) . . ? C75 C78 C77 123.3(5) . . ? C79 C78 C77 114.5(4) . . ? C80 C79 C84 117.8(5) . . ? C80 C79 C78 121.8(5) . . ? C84 C79 C78 120.4(5) . . ? C79 C80 C81 121.6(5) . . ? C79 C80 H80 119.2 . . ? C81 C80 H80 119.2 . . ? C80 C81 C82 120.8(5) . . ? C80 C81 H81 119.6 . . ? C82 C81 H81 119.6 . . ? C83 C82 C81 117.1(5) . . ? C83 C82 C85 120.8(5) . . ? C81 C82 C85 122.0(5) . . ? C82 C83 C84 122.1(5) . . ? C82 C83 H83 119.0 . . ? C84 C83 H83 119.0 . . ? C79 C84 C83 120.5(5) . . ? C79 C84 H84 119.8 . . ? C83 C84 H84 119.8 . . ? C90 C85 C86 117.8(5) . . ? C90 C85 C82 121.4(5) . . ? C86 C85 C82 120.9(5) . . ? C87 C86 C85 121.4(5) . . ? C87 C86 H86 119.3 . . ? C85 C86 H86 119.3 . . ? C88 C87 C86 120.8(5) . . ? C88 C87 H87 119.6 . . ? C86 C87 H87 119.6 . . ? C87 C88 C89 116.6(5) . . ? C87 C88 C91 119.2(5) . . ? C89 C88 C91 124.2(6) . . ? C90 C89 C88 123.4(6) . . ? C90 C89 H89 118.3 . . ? C88 C89 H89 118.3 . . ? C89 C90 C85 120.1(5) . . ? C89 C90 H90 120.0 . . ? C85 C90 H90 120.0 . . ? C94 C91 C88 122.2(5) . . ? C94 C91 C92 123.8(5) . . ? C88 C91 C92 114.0(4) . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C94 C93 H93A 109.5 . . ? C94 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C94 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C91 C94 C95 121.8(5) . . ? C91 C94 C93 124.8(5) . . ? C95 C94 C93 113.3(4) . . ? C96 C95 C100 116.6(5) . . ? C96 C95 C94 120.6(5) . . ? C100 C95 C94 122.8(5) . . ? C97 C96 C95 121.8(5) . . ? C97 C96 H96 119.1 . . ? C95 C96 H96 119.1 . . ? C96 C97 C98 121.4(5) . . ? C96 C97 H97 119.3 . . ? C98 C97 H97 119.3 . . ? C99 C98 C97 116.1(5) . . ? C99 C98 C101 123.2(5) . . ? C97 C98 C101 120.7(5) . . ? C100 C99 C98 122.7(5) . . ? C100 C99 H99 118.7 . . ? C98 C99 H99 118.7 . . ? C99 C100 C95 121.3(5) . . ? C99 C100 H100 119.3 . . ? C95 C100 H100 119.3 . . ? C102 C101 C106 117.1(5) . . ? C102 C101 C98 121.0(5) . . ? C106 C101 C98 121.9(5) . . ? C103 C102 C101 122.1(5) . . ? C103 C102 H102 119.0 . . ? C101 C102 H102 119.0 . . ? C102 C103 C104 121.3(5) . . ? C102 C103 H103 119.4 . . ? C104 C103 H103 119.4 . . ? C105 C104 C103 116.4(5) . . ? C105 C104 C107 122.6(5) . . ? C103 C104 C107 120.9(5) . . ? C106 C105 C104 122.0(5) . . ? C106 C105 H105 119.0 . . ? C104 C105 H105 119.0 . . ? C105 C106 C101 120.9(5) . . ? C105 C106 H106 119.6 . . ? C101 C106 H106 119.6 . . ? C62 C107 C104 121.4(4) . . ? C62 C107 C108 123.0(5) . . ? C104 C107 C108 115.6(5) . . ? C107 C108 H10A 109.5 . . ? C107 C108 H10B 109.5 . . ? H10A C108 H10B 109.5 . . ? C107 C108 H10C 109.5 . . ? H10A C108 H10C 109.5 . . ? H10B C108 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.700 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.066 #===END data_9042tto _database_code_depnum_ccdc_archive 'CCDC 748364' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H50 O2' _chemical_formula_weight 706.92 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 Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.385(3) _cell_length_b 14.405(4) _cell_length_c 14.984(4) _cell_angle_alpha 115.121(4) _cell_angle_beta 95.522(4) _cell_angle_gamma 109.930(4) _cell_volume 2006.0(9) _cell_formula_units_Z 2 _cell_measurement_temperature 120 _cell_measurement_reflns_used 2510 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 25.78 _exptl_crystal_description prismatic _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.170 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9863 _exptl_absorpt_correction_T_max 0.9863 _exptl_absorpt_process_details ; SADABS Sheldrick 1996 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120 _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 Smart1000 CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 8.333 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11995 _diffrn_reflns_av_R_equivalents 0.0279 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.56 _reflns_number_total 8724 _reflns_number_gt 5394 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Smart (Bruker AXS)' _computing_cell_refinement 'Smart (Bruker AXS)' _computing_data_reduction 'SAINT (Bruker AXS, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker AXS,2002)' _computing_publication_material 'XCIF (Bruker AXS, 2001)' _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^)+(0.1384P)^2^+1.0727P] 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 8724 _refine_ls_number_parameters 495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1252 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.2665 _refine_ls_wR_factor_gt 0.2373 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 -0.0140(4) -0.2335(3) -0.2031(2) 0.0571(10) Uani 1 1 d . . . H1A H 0.0483 -0.2570 -0.2369 0.086 Uiso 1 1 calc R . . H1B H -0.0340 -0.1839 -0.2247 0.086 Uiso 1 1 calc R . . H1C H -0.0942 -0.3005 -0.2224 0.086 Uiso 1 1 calc R . . C2 C 0.0446(3) -0.1704(2) -0.0878(2) 0.0393(7) Uani 1 1 d . . . C3 C 0.1631(3) -0.0618(2) -0.0477(2) 0.0372(7) Uani 1 1 d . . . C4 C 0.2622(3) -0.0563(3) -0.0950(2) 0.0421(7) Uani 1 1 d . . . H4 H 0.2537 -0.1225 -0.1538 0.051 Uiso 1 1 calc R . . C5 C 0.3728(3) 0.0429(3) -0.0588(2) 0.0413(7) Uani 1 1 d . . . H5 H 0.4395 0.0430 -0.0923 0.050 Uiso 1 1 calc R . . C6 C 0.3890(3) 0.1430(2) 0.0260(2) 0.0342(6) Uani 1 1 d . . . C7 C 0.2868(3) 0.1391(2) 0.0709(2) 0.0376(7) Uani 1 1 d . . . H7 H 0.2927 0.2064 0.1268 0.045 Uiso 1 1 calc R . . C8 C 0.1765(3) 0.0385(2) 0.0353(2) 0.0375(7) Uani 1 1 d . . . H8 H 0.1092 0.0381 0.0682 0.045 Uiso 1 1 calc R . . C9 C 0.5107(3) 0.2475(2) 0.0680(2) 0.0345(6) Uani 1 1 d . . . C10 C 0.6299(3) 0.2430(3) 0.0623(2) 0.0456(7) Uani 1 1 d . . . H10 H 0.6324 0.1715 0.0269 0.055 Uiso 1 1 calc R . . C11 C 0.7456(3) 0.3406(3) 0.1071(3) 0.0510(8) Uani 1 1 d . . . H11 H 0.8255 0.3345 0.1021 0.061 Uiso 1 1 calc R . . C12 C 0.7467(3) 0.4460(3) 0.1585(2) 0.0445(8) Uani 1 1 d . . . C13 C 0.6290(3) 0.4521(3) 0.1612(2) 0.0473(8) Uani 1 1 d . . . H13 H 0.6273 0.5242 0.1935 0.057 Uiso 1 1 calc R . . C14 C 0.5126(3) 0.3551(3) 0.1177(2) 0.0430(7) Uani 1 1 d . . . H14 H 0.4330 0.3621 0.1217 0.052 Uiso 1 1 calc R . . C15 C 0.9271(4) 0.5836(4) 0.1316(3) 0.0800(14) Uani 1 1 d . . . H15A H 0.8667 0.5981 0.0938 0.120 Uiso 1 1 calc R . . H15B H 0.9426 0.5203 0.0833 0.120 Uiso 1 1 calc R . . H15C H 1.0098 0.6515 0.1684 0.120 Uiso 1 1 calc R . . C16 C 0.8687(3) 0.5544(3) 0.2080(3) 0.0582(10) Uani 1 1 d . . . C17 C 0.9141(3) 0.6215(3) 0.3099(2) 0.0404(7) Uani 1 1 d . . . C18 C 1.0202(4) 0.7372(3) 0.3592(3) 0.0652(11) Uani 1 1 d . . . H18A H 1.1015 0.7366 0.3865 0.098 Uiso 1 1 calc R . . H18B H 0.9981 0.7887 0.4154 0.098 Uiso 1 1 calc R . . H18C H 1.0311 0.7628 0.3082 0.098 Uiso 1 1 calc R . . C19 C 0.8625(3) 0.5835(2) 0.3832(2) 0.0360(7) Uani 1 1 d . . . C20 C 0.8103(3) 0.6421(3) 0.4548(2) 0.0432(7) Uani 1 1 d . . . H20 H 0.8058 0.7079 0.4576 0.052 Uiso 1 1 calc R . . C21 C 0.7646(3) 0.6071(3) 0.5223(2) 0.0411(7) Uani 1 1 d . . . H21 H 0.7276 0.6482 0.5697 0.049 Uiso 1 1 calc R . . C22 C 0.7718(3) 0.5124(2) 0.5218(2) 0.0327(6) Uani 1 1 d . . . C23 C 0.8276(3) 0.4558(2) 0.4525(2) 0.0390(7) Uani 1 1 d . . . H23 H 0.8370 0.3927 0.4525 0.047 Uiso 1 1 calc R . . C24 C 0.8703(3) 0.4897(2) 0.3828(2) 0.0388(7) Uani 1 1 d . . . H24 H 0.9054 0.4477 0.3342 0.047 Uiso 1 1 calc R . . C25 C 0.7169(3) 0.4704(2) 0.5908(2) 0.0339(6) Uani 1 1 d . . . C26 C 0.5979(3) 0.4676(3) 0.6067(2) 0.0413(7) Uani 1 1 d . . . H26 H 0.5545 0.4981 0.5772 0.050 Uiso 1 1 calc R . . C27 C 0.5413(3) 0.4214(3) 0.6647(2) 0.0430(7) Uani 1 1 d . . . H27 H 0.4580 0.4178 0.6717 0.052 Uiso 1 1 calc R . . C28 C 0.6038(3) 0.3804(2) 0.7126(2) 0.0377(7) Uani 1 1 d . . . C29 C 0.7246(3) 0.3866(3) 0.6994(2) 0.0452(8) Uani 1 1 d . . . H29 H 0.7710 0.3611 0.7329 0.054 Uiso 1 1 calc R . . C30 C 0.6193(4) 0.4059(3) 0.8913(2) 0.0637(11) Uani 1 1 d . . . H30A H 0.6101 0.4773 0.9220 0.096 Uiso 1 1 calc R . . H30B H 0.7114 0.4219 0.8976 0.096 Uiso 1 1 calc R . . H30C H 0.5859 0.3637 0.9271 0.096 Uiso 1 1 calc R . . C31 C 0.5426(3) 0.3361(3) 0.7788(2) 0.0429(7) Uani 1 1 d . . . C32 C 0.4259(3) 0.2474(3) 0.7428(2) 0.0403(7) Uani 1 1 d . . . C33 C 0.3563(4) 0.2156(3) 0.8139(3) 0.0595(10) Uani 1 1 d . . . H33A H 0.3537 0.1432 0.8042 0.089 Uiso 1 1 calc R . . H33B H 0.2672 0.2087 0.7980 0.089 Uiso 1 1 calc R . . H33C H 0.4030 0.2744 0.8854 0.089 Uiso 1 1 calc R . . C34 C 0.3578(3) 0.1719(2) 0.6306(2) 0.0351(6) Uani 1 1 d . . . C35 C 0.2260(3) 0.1363(2) 0.5922(2) 0.0381(7) Uani 1 1 d . . . H35 H 0.1767 0.1585 0.6383 0.046 Uiso 1 1 calc R . . C36 C 0.1639(3) 0.0687(2) 0.4874(2) 0.0370(6) Uani 1 1 d . . . H36 H 0.0732 0.0466 0.4635 0.044 Uiso 1 1 calc R . . C37 C 0.2308(3) 0.0324(2) 0.4163(2) 0.0334(6) Uani 1 1 d . . . C38 C 0.3622(3) 0.0629(3) 0.4570(2) 0.0426(7) Uani 1 1 d . . . H38 H 0.4105 0.0362 0.4118 0.051 Uiso 1 1 calc R . . C39 C 0.4239(3) 0.1309(3) 0.5609(2) 0.0434(7) Uani 1 1 d . . . H39 H 0.5135 0.1502 0.5855 0.052 Uiso 1 1 calc R . . C40 C 0.1672(3) -0.0336(2) 0.3030(2) 0.0340(6) Uani 1 1 d . . . C41 C 0.0516(3) -0.0345(3) 0.2612(2) 0.0415(7) Uani 1 1 d . . . H41 H 0.0111 0.0054 0.3058 0.050 Uiso 1 1 calc R . . C42 C -0.0053(3) -0.0925(3) 0.1560(2) 0.0434(7) Uani 1 1 d . . . H42 H -0.0859 -0.0943 0.1299 0.052 Uiso 1 1 calc R . . C43 C 0.0533(3) -0.1481(2) 0.0877(2) 0.0367(7) Uani 1 1 d . . . C44 C 0.1668(3) -0.1492(3) 0.1288(2) 0.0417(7) Uani 1 1 d . . . H44 H 0.2077 -0.1884 0.0842 0.050 Uiso 1 1 calc R . . C45 C 0.2218(3) -0.0935(2) 0.2350(2) 0.0389(7) Uani 1 1 d . . . H45 H 0.2988 -0.0968 0.2612 0.047 Uiso 1 1 calc R . . C46 C -0.0064(3) -0.2082(2) -0.0260(2) 0.0387(7) Uani 1 1 d . . . C47 C -0.1272(3) -0.3164(3) -0.0640(3) 0.0532(9) Uani 1 1 d . . . H47A H -0.1731 -0.3424 -0.1348 0.080 Uiso 1 1 calc R . . H47B H -0.1844 -0.3026 -0.0199 0.080 Uiso 1 1 calc R . . H47C H -0.1024 -0.3745 -0.0621 0.080 Uiso 1 1 calc R . . C48 C 0.7790(3) 0.4289(3) 0.6386(2) 0.0414(7) Uani 1 1 d . . . H48 H 0.8607 0.4296 0.6294 0.050 Uiso 1 1 calc R . . C49 C 0.4812(6) 0.2472(6) 0.3319(4) 0.1075(19) Uani 1 1 d . . . H49A H 0.4992 0.2592 0.4022 0.161 Uiso 1 1 calc R . . H49B H 0.3883 0.2251 0.3053 0.161 Uiso 1 1 calc R . . H49C H 0.5327 0.3174 0.3321 0.161 Uiso 1 1 calc R . . C50 C 0.5136(5) 0.1645(5) 0.2717(4) 0.0860(14) Uani 1 1 d . . . H50A H 0.5184 0.1666 0.2069 0.103 Uiso 1 1 calc R . . H50B H 0.4446 0.0901 0.2540 0.103 Uiso 1 1 calc R . . C51 C 0.6446(5) 0.0902(4) 0.3267(3) 0.0735(12) Uani 1 1 d . . . C52 C 0.7792(6) 0.1162(5) 0.3773(5) 0.130(3) Uani 1 1 d . . . H52A H 0.7881 0.1365 0.4496 0.195 Uiso 1 1 calc R . . H52B H 0.8415 0.1797 0.3729 0.195 Uiso 1 1 calc R . . H52C H 0.7970 0.0496 0.3426 0.195 Uiso 1 1 calc R . . O1 O 0.6349(4) 0.1756(3) 0.3203(3) 0.1039(12) Uani 1 1 d . . . O2 O 0.5512(3) 0.0011(3) 0.2891(3) 0.0946(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.067(2) 0.0438(19) 0.0319(16) 0.0152(15) -0.0010(16) 0.0012(17) C2 0.0447(17) 0.0289(14) 0.0279(14) 0.0112(12) 0.0001(12) 0.0040(13) C3 0.0455(17) 0.0303(14) 0.0266(13) 0.0160(12) 0.0018(12) 0.0056(12) C4 0.058(2) 0.0315(15) 0.0283(14) 0.0119(13) 0.0113(14) 0.0130(14) C5 0.0494(18) 0.0385(16) 0.0332(15) 0.0173(13) 0.0160(13) 0.0147(14) C6 0.0411(16) 0.0318(14) 0.0259(13) 0.0165(12) 0.0064(12) 0.0090(12) C7 0.0454(17) 0.0318(15) 0.0300(14) 0.0144(12) 0.0087(13) 0.0116(13) C8 0.0421(16) 0.0321(15) 0.0297(14) 0.0155(12) 0.0088(12) 0.0061(12) C9 0.0406(16) 0.0361(15) 0.0251(13) 0.0180(12) 0.0099(12) 0.0101(13) C10 0.0472(19) 0.0439(18) 0.0418(17) 0.0209(15) 0.0116(14) 0.0154(15) C11 0.0376(17) 0.070(2) 0.0444(18) 0.0320(18) 0.0125(14) 0.0155(17) C12 0.0428(18) 0.0503(19) 0.0287(14) 0.0230(14) 0.0099(13) 0.0025(14) C13 0.057(2) 0.0335(16) 0.0383(16) 0.0154(14) 0.0157(15) 0.0063(14) C14 0.0443(18) 0.0388(16) 0.0404(16) 0.0201(14) 0.0139(14) 0.0102(14) C15 0.069(3) 0.090(3) 0.051(2) 0.044(2) 0.012(2) -0.010(2) C16 0.052(2) 0.062(2) 0.0430(18) 0.0337(18) 0.0096(16) -0.0052(17) C17 0.0401(16) 0.0373(16) 0.0386(16) 0.0245(14) 0.0094(13) 0.0033(13) C18 0.080(3) 0.044(2) 0.067(2) 0.0345(19) 0.033(2) 0.0082(18) C19 0.0332(15) 0.0317(14) 0.0304(14) 0.0179(12) 0.0020(12) -0.0017(12) C20 0.0546(19) 0.0381(16) 0.0418(17) 0.0246(14) 0.0153(15) 0.0178(15) C21 0.0496(18) 0.0375(16) 0.0370(16) 0.0204(14) 0.0150(14) 0.0157(14) C22 0.0330(14) 0.0311(14) 0.0277(13) 0.0160(12) 0.0050(11) 0.0056(12) C23 0.0444(17) 0.0339(15) 0.0404(16) 0.0215(13) 0.0157(14) 0.0131(13) C24 0.0439(17) 0.0317(15) 0.0352(15) 0.0160(13) 0.0165(13) 0.0090(13) C25 0.0376(15) 0.0317(14) 0.0260(13) 0.0149(12) 0.0064(11) 0.0073(12) C26 0.0484(18) 0.0505(18) 0.0386(16) 0.0294(15) 0.0170(14) 0.0246(15) C27 0.0423(17) 0.0530(19) 0.0396(16) 0.0278(15) 0.0179(14) 0.0181(15) C28 0.0404(16) 0.0339(15) 0.0244(13) 0.0146(12) 0.0032(12) 0.0011(12) C29 0.0425(18) 0.0507(19) 0.0452(17) 0.0346(16) 0.0061(14) 0.0100(15) C30 0.074(3) 0.058(2) 0.0302(16) 0.0236(16) 0.0041(16) -0.0030(19) C31 0.0483(18) 0.0421(17) 0.0270(14) 0.0191(13) 0.0072(13) 0.0048(14) C32 0.0468(17) 0.0396(16) 0.0275(14) 0.0189(13) 0.0100(13) 0.0077(14) C33 0.066(2) 0.059(2) 0.0373(17) 0.0264(17) 0.0161(16) 0.0048(18) C34 0.0430(16) 0.0299(14) 0.0296(14) 0.0181(12) 0.0106(12) 0.0077(12) C35 0.0469(17) 0.0361(15) 0.0316(14) 0.0186(13) 0.0155(13) 0.0140(13) C36 0.0364(15) 0.0374(15) 0.0350(15) 0.0207(13) 0.0101(12) 0.0093(13) C37 0.0361(15) 0.0276(13) 0.0290(13) 0.0151(12) 0.0078(12) 0.0039(11) C38 0.0412(17) 0.0455(17) 0.0332(15) 0.0158(14) 0.0114(13) 0.0141(14) C39 0.0383(16) 0.0444(18) 0.0359(16) 0.0177(14) 0.0047(13) 0.0090(14) C40 0.0354(15) 0.0296(14) 0.0290(14) 0.0168(12) 0.0063(12) 0.0025(12) C41 0.0460(18) 0.0465(18) 0.0322(15) 0.0216(14) 0.0129(13) 0.0161(14) C42 0.0401(17) 0.0501(18) 0.0393(16) 0.0266(15) 0.0070(14) 0.0135(14) C43 0.0371(16) 0.0300(14) 0.0315(14) 0.0171(12) 0.0058(12) 0.0002(12) C44 0.0402(17) 0.0367(16) 0.0315(15) 0.0108(13) 0.0080(13) 0.0063(13) C45 0.0343(15) 0.0394(16) 0.0314(14) 0.0153(13) 0.0050(12) 0.0068(13) C46 0.0423(17) 0.0289(14) 0.0304(14) 0.0120(12) 0.0032(12) 0.0046(12) C47 0.050(2) 0.0390(18) 0.0465(18) 0.0218(16) -0.0019(15) -0.0044(15) C48 0.0334(15) 0.0463(17) 0.0454(17) 0.0293(15) 0.0097(13) 0.0096(13) C49 0.096(4) 0.113(5) 0.070(3) 0.009(3) -0.004(3) 0.050(4) C50 0.079(3) 0.098(4) 0.078(3) 0.049(3) 0.001(3) 0.034(3) C51 0.088(3) 0.071(3) 0.065(3) 0.038(2) 0.022(2) 0.031(3) C52 0.147(5) 0.064(3) 0.129(5) 0.039(3) -0.062(4) 0.028(3) O1 0.126(3) 0.068(2) 0.099(3) 0.0363(19) -0.015(2) 0.038(2) O2 0.071(2) 0.073(2) 0.109(3) 0.028(2) 0.0329(19) 0.0158(18) _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 1.512(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C46 1.346(4) . ? C2 C3 1.495(4) . ? C3 C4 1.386(4) . ? C3 C8 1.394(4) . ? C4 C5 1.381(4) . ? C4 H4 0.9500 . ? C5 C6 1.395(4) . ? C5 H5 0.9500 . ? C6 C7 1.395(4) . ? C6 C9 1.479(4) . ? C7 C8 1.391(4) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C10 1.390(4) . ? C9 C14 1.397(4) . ? C10 C11 1.388(5) . ? C10 H10 0.9500 . ? C11 C12 1.375(5) . ? C11 H11 0.9500 . ? C12 C13 1.375(5) . ? C12 C16 1.502(4) . ? C13 C14 1.390(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.514(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.337(4) . ? C17 C18 1.481(4) . ? C17 C19 1.504(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.382(4) . ? C19 C20 1.383(4) . ? C20 C21 1.380(4) . ? C20 H20 0.9500 . ? C21 C22 1.391(4) . ? C21 H21 0.9500 . ? C22 C23 1.381(4) . ? C22 C25 1.491(4) . ? C23 C24 1.391(4) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.388(4) . ? C25 C48 1.388(4) . ? C26 C27 1.386(4) . ? C26 H26 0.9500 . ? C27 C28 1.385(4) . ? C27 H27 0.9500 . ? C28 C29 1.387(4) . ? C28 C31 1.498(4) . ? C29 C48 1.381(4) . ? C29 H29 0.9500 . ? C30 C31 1.515(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.344(4) . ? C32 C34 1.494(4) . ? C32 C33 1.516(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.380(4) . ? C34 C39 1.391(4) . ? C35 C36 1.391(4) . ? C35 H35 0.9500 . ? C36 C37 1.394(4) . ? C36 H36 0.9500 . ? C37 C38 1.397(4) . ? C37 C40 1.495(4) . ? C38 C39 1.380(4) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.382(4) . ? C40 C41 1.395(4) . ? C41 C42 1.385(4) . ? C41 H41 0.9500 . ? C42 C43 1.390(5) . ? C42 H42 0.9500 . ? C43 C44 1.385(4) . ? C43 C46 1.496(4) . ? C44 C45 1.397(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.509(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48 0.9500 . ? C49 C50 1.349(7) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 O1 1.422(5) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 O2 1.199(5) . ? C51 O1 1.313(5) . ? C51 C52 1.486(7) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? 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 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C46 C2 C3 122.5(2) . . ? C46 C2 C1 122.8(3) . . ? C3 C2 C1 114.7(2) . . ? C4 C3 C8 117.3(3) . . ? C4 C3 C2 120.7(3) . . ? C8 C3 C2 122.0(3) . . ? C5 C4 C3 121.6(3) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 121.5(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C7 117.0(3) . . ? C5 C6 C9 121.3(3) . . ? C7 C6 C9 121.7(3) . . ? C8 C7 C6 121.3(3) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C3 121.2(3) . . ? C7 C8 H8 119.4 . . ? C3 C8 H8 119.4 . . ? C10 C9 C14 116.6(3) . . ? C10 C9 C6 121.3(3) . . ? C14 C9 C6 122.1(3) . . ? C11 C10 C9 121.6(3) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C12 C11 C10 121.2(3) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C13 C12 C11 117.9(3) . . ? C13 C12 C16 118.5(3) . . ? C11 C12 C16 123.5(3) . . ? C12 C13 C14 121.4(3) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? C13 C14 C9 121.1(3) . . ? C13 C14 H14 119.4 . . ? C9 C14 H14 119.4 . . ? C16 C15 H15A 109.5 . . ? C16 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C16 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C12 122.1(3) . . ? C17 C16 C15 124.1(3) . . ? C12 C16 C15 113.6(3) . . ? C16 C17 C18 122.8(3) . . ? C16 C17 C19 122.2(3) . . ? C18 C17 C19 115.0(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 117.7(2) . . ? C24 C19 C17 120.2(3) . . ? C20 C19 C17 122.0(3) . . ? C21 C20 C19 121.5(3) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 120.9(3) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C23 C22 C21 117.8(2) . . ? C23 C22 C25 120.8(3) . . ? C21 C22 C25 121.4(3) . . ? C22 C23 C24 121.0(3) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C19 C24 C23 121.0(3) . . ? C19 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C26 C25 C48 117.2(3) . . ? C26 C25 C22 120.7(3) . . ? C48 C25 C22 122.0(3) . . ? C27 C26 C25 121.4(3) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C28 C27 C26 121.2(3) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C29 117.3(3) . . ? C27 C28 C31 119.8(3) . . ? C29 C28 C31 122.9(3) . . ? C48 C29 C28 121.5(3) . . ? C48 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C31 C30 H30A 109.5 . . ? C31 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C31 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C28 123.0(3) . . ? C32 C31 C30 123.1(3) . . ? C28 C31 C30 113.7(3) . . ? C31 C32 C34 122.5(2) . . ? C31 C32 C33 121.9(3) . . ? C34 C32 C33 115.6(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C34 C39 117.2(3) . . ? C35 C34 C32 121.5(3) . . ? C39 C34 C32 121.2(3) . . ? C34 C35 C36 121.3(3) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C35 C36 C37 121.9(3) . . ? C35 C36 H36 119.1 . . ? C37 C36 H36 119.1 . . ? C36 C37 C38 116.1(3) . . ? C36 C37 C40 122.3(3) . . ? C38 C37 C40 121.5(3) . . ? C39 C38 C37 121.8(3) . . ? C39 C38 H38 119.1 . . ? C37 C38 H38 119.1 . . ? C38 C39 C34 121.5(3) . . ? C38 C39 H39 119.2 . . ? C34 C39 H39 119.2 . . ? C45 C40 C41 117.2(3) . . ? C45 C40 C37 121.7(3) . . ? C41 C40 C37 121.1(3) . . ? C42 C41 C40 121.3(3) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C41 C42 C43 121.3(3) . . ? C41 C42 H42 119.3 . . ? C43 C42 H42 119.3 . . ? C44 C43 C42 117.6(3) . . ? C44 C43 C46 121.1(3) . . ? C42 C43 C46 121.3(3) . . ? C43 C44 C45 120.9(3) . . ? C43 C44 H44 119.5 . . ? C45 C44 H44 119.5 . . ? C40 C45 C44 121.6(3) . . ? C40 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C2 C46 C43 123.1(2) . . ? C2 C46 C47 123.7(3) . . ? C43 C46 C47 113.2(2) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C29 C48 C25 121.4(3) . . ? C29 C48 H48 119.3 . . ? C25 C48 H48 119.3 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C49 C50 O1 112.2(5) . . ? C49 C50 H50A 109.2 . . ? O1 C50 H50A 109.2 . . ? C49 C50 H50B 109.2 . . ? O1 C50 H50B 109.2 . . ? H50A C50 H50B 107.9 . . ? O2 C51 O1 119.9(5) . . ? O2 C51 C52 126.9(5) . . ? O1 C51 C52 113.2(4) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 O1 C50 120.7(4) . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.524 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.065