# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_08ap27_0m _database_code_depnum_ccdc_archive 'CCDC 735891' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H58' _chemical_formula_weight 707.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 12.8863(6) _cell_length_b 37.2568(17) _cell_length_c 11.0722(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5315.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2906 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description Columnar _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 'not measured' _exptl_crystal_density_diffrn 0.883 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.049 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.69263 _exptl_absorpt_correction_T_max 0.96328 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53591 _diffrn_reflns_av_R_equivalents 0.1639 _diffrn_reflns_av_sigmaI/netI 0.2119 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -49 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 28.41 _reflns_number_total 12957 _reflns_number_gt 3886 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII' _computing_cell_refinement 'Bruker APEXII' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'Shelxtl-97 (Sheldrick, 1990)' _computing_structure_refinement 'Shelxtl-97 (Sheldrick, 2000)' _computing_molecular_graphics 'Bruker Shelxtl' _computing_publication_material 'Bruker Shelxtl' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1291P)^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 SHELXL _refine_ls_extinction_coef 0.126(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 0(10) _refine_ls_number_reflns 12957 _refine_ls_number_parameters 500 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.2209 _refine_ls_R_factor_gt 0.0983 _refine_ls_wR_factor_ref 0.2631 _refine_ls_wR_factor_gt 0.2004 _refine_ls_goodness_of_fit_ref 0.810 _refine_ls_restrained_S_all 0.811 _refine_ls_shift/su_max 7.081 _refine_ls_shift/su_mean 0.229 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 0.6229(3) 0.13084(11) 0.3554(4) 0.0579(12) Uani 1 1 d . . . C2 C 0.5812(3) 0.09992(12) 0.2942(4) 0.0571(11) Uani 1 1 d . . . C3 C 0.6420(3) 0.07013(12) 0.2874(4) 0.0581(11) Uani 1 1 d . . . H3 H 0.6163 0.0503 0.2458 0.070 Uiso 1 1 calc R . . C4 C 0.7425(3) 0.06740(11) 0.3400(4) 0.0507(10) Uani 1 1 d . . . C5 C 0.8022(3) 0.03650(11) 0.3350(4) 0.0527(11) Uani 1 1 d . . . H5 H 0.7760 0.0163 0.2961 0.063 Uiso 1 1 calc R . . C6 C 0.8998(3) 0.03494(10) 0.3863(4) 0.0484(10) Uani 1 1 d . . . C7 C 0.9634(3) 0.00458(11) 0.3768(4) 0.0563(11) Uani 1 1 d . . . H7 H 0.9380 -0.0150 0.3342 0.068 Uiso 1 1 calc R . . C8 C 1.0617(3) 0.00185(11) 0.4268(4) 0.0535(11) Uani 1 1 d . . . C9 C 1.1009(3) 0.03280(11) 0.4912(4) 0.0515(10) Uani 1 1 d . . . C10 C 1.0399(3) 0.06280(11) 0.4992(4) 0.0523(11) Uani 1 1 d . . . H10 H 1.0662 0.0827 0.5398 0.063 Uiso 1 1 calc R . . C11 C 0.9389(3) 0.06522(11) 0.4491(4) 0.0509(11) Uani 1 1 d . . . C12 C 0.8795(3) 0.09595(11) 0.4546(4) 0.0540(11) Uani 1 1 d . . . H12 H 0.9058 0.1160 0.4943 0.065 Uiso 1 1 calc R . . C13 C 0.7812(3) 0.09795(11) 0.4024(4) 0.0517(10) Uani 1 1 d . . . C14 C 0.7188(3) 0.12902(11) 0.4072(4) 0.0593(12) Uani 1 1 d . . . H14 H 0.7442 0.1491 0.4473 0.071 Uiso 1 1 calc R . . C15 C 0.5632(3) 0.16538(12) 0.3632(5) 0.0672(13) Uani 1 1 d . . . C16 C 0.5504(4) 0.18297(14) 0.4712(5) 0.0868(16) Uani 1 1 d . . . H16 H 0.5770 0.1727 0.5412 0.104 Uiso 1 1 calc R . . C17 C 0.4992(5) 0.21544(16) 0.4790(6) 0.107(2) Uani 1 1 d . . . H17 H 0.4924 0.2267 0.5536 0.128 Uiso 1 1 calc R . . C18 C 0.4584(5) 0.23114(17) 0.3781(8) 0.114(2) Uani 1 1 d . . . C19 C 0.4715(5) 0.21412(17) 0.2687(7) 0.111(2) Uani 1 1 d . . . H19 H 0.4451 0.2246 0.1990 0.133 Uiso 1 1 calc R . . C20 C 0.5229(4) 0.18206(14) 0.2613(5) 0.0879(16) Uani 1 1 d . . . H20 H 0.5311 0.1712 0.1863 0.105 Uiso 1 1 calc R . . C22 C 0.4741(3) 0.09902(11) 0.2450(4) 0.0596(12) Uani 1 1 d . . . C23 C 0.3890(4) 0.10646(13) 0.3158(4) 0.0756(14) Uani 1 1 d . . . H23 H 0.3991 0.1135 0.3955 0.091 Uiso 1 1 calc R . . C24 C 0.2889(4) 0.10377(15) 0.2718(5) 0.0793(15) Uani 1 1 d . . . H24 H 0.2338 0.1090 0.3231 0.095 Uiso 1 1 calc R . . C25 C 0.2682(4) 0.09368(13) 0.1559(5) 0.0665(13) Uani 1 1 d . . . C26 C 0.3537(4) 0.08568(16) 0.0869(4) 0.0860(17) Uani 1 1 d . . . H26 H 0.3433 0.0781 0.0078 0.103 Uiso 1 1 calc R . . C27 C 0.4532(4) 0.08830(14) 0.1286(4) 0.0753(14) Uani 1 1 d . . . H27 H 0.5079 0.0827 0.0772 0.090 Uiso 1 1 calc R . . C28 C 0.1586(4) 0.08813(16) 0.1095(5) 0.0848(16) Uani 1 1 d D . . C29 C 1.1162(3) -0.03310(10) 0.4181(4) 0.0513(10) Uani 1 1 d . . . C30 C 1.1179(3) -0.05173(12) 0.3093(4) 0.0620(12) Uani 1 1 d . . . H30 H 1.0932 -0.0405 0.2400 0.074 Uiso 1 1 calc R . . C31 C 1.1549(4) -0.08610(13) 0.3008(4) 0.0686(13) Uani 1 1 d . . . H31 H 1.1560 -0.0974 0.2259 0.082 Uiso 1 1 calc R . . C32 C 1.1911(3) -0.10473(12) 0.4031(5) 0.0658(12) Uani 1 1 d . . . C33 C 1.1919(4) -0.08455(14) 0.5107(5) 0.0711(14) Uani 1 1 d . . . H33 H 1.2187 -0.0951 0.5801 0.085 Uiso 1 1 calc R . . C34 C 1.1552(3) -0.05016(12) 0.5179(4) 0.0598(12) Uani 1 1 d . . . H34 H 1.1568 -0.0382 0.5916 0.072 Uiso 1 1 calc R . . C35 C 1.2261(4) -0.14350(13) 0.3999(6) 0.0874(16) Uani 1 1 d D . . C36 C 1.2077(3) 0.03439(10) 0.5425(4) 0.0502(11) Uani 1 1 d . . . C37 C 1.2936(4) 0.02307(12) 0.4793(4) 0.0699(13) Uani 1 1 d . . . H37 H 1.2847 0.0126 0.4039 0.084 Uiso 1 1 calc R . . C38 C 1.3923(3) 0.02684(13) 0.5245(4) 0.0690(13) Uani 1 1 d . . . H38 H 1.4482 0.0193 0.4779 0.083 Uiso 1 1 calc R . . C39 C 1.4108(3) 0.04132(11) 0.6359(4) 0.0568(11) Uani 1 1 d . . . C40 C 1.3245(3) 0.05283(12) 0.6994(4) 0.0600(12) Uani 1 1 d . . . H40 H 1.3333 0.0629 0.7755 0.072 Uiso 1 1 calc R . . C41 C 1.2264(3) 0.04974(11) 0.6530(4) 0.0575(11) Uani 1 1 d . . . H41 H 1.1706 0.0583 0.6979 0.069 Uiso 1 1 calc R . . C42 C 1.5212(3) 0.04622(13) 0.6836(4) 0.0668(13) Uani 1 1 d D . . C46 C 0.0823(5) 0.1115(2) 0.1748(7) 0.158(3) Uani 1 1 d D . . H46A H 0.0987 0.1363 0.1605 0.237 Uiso 1 1 calc R . . H46B H 0.0858 0.1066 0.2599 0.237 Uiso 1 1 calc R . . H46C H 0.0135 0.1065 0.1460 0.237 Uiso 1 1 calc R . . C47 C 0.1492(5) 0.0923(2) -0.0247(5) 0.125(3) Uani 1 1 d D . . H47A H 0.0780 0.0893 -0.0482 0.187 Uiso 1 1 calc R . . H47B H 0.1911 0.0745 -0.0641 0.187 Uiso 1 1 calc R . . H47C H 0.1725 0.1158 -0.0478 0.187 Uiso 1 1 calc R . . C48 C 0.1252(5) 0.05071(19) 0.1428(7) 0.138(3) Uani 1 1 d D . . H48A H 0.1366 0.0469 0.2275 0.207 Uiso 1 1 calc R . . H48B H 0.1649 0.0336 0.0973 0.207 Uiso 1 1 calc R . . H48C H 0.0528 0.0478 0.1249 0.207 Uiso 1 1 calc R . . C49 C 1.1568(10) -0.16480(19) 0.4774(14) 0.297(9) Uani 1 1 d D . . H49A H 1.1947 -0.1846 0.5112 0.446 Uiso 1 1 calc R . . H49B H 1.1000 -0.1737 0.4302 0.446 Uiso 1 1 calc R . . H49C H 1.1306 -0.1500 0.5414 0.446 Uiso 1 1 calc R . . C50 C 1.2333(9) -0.1585(2) 0.2740(7) 0.198(5) Uani 1 1 d D . . H50A H 1.3008 -0.1535 0.2413 0.297 Uiso 1 1 calc R . . H50B H 1.1813 -0.1476 0.2241 0.297 Uiso 1 1 calc R . . H50C H 1.2225 -0.1840 0.2764 0.297 Uiso 1 1 calc R . . C51 C 1.3273(8) -0.1477(2) 0.4567(14) 0.262(8) Uani 1 1 d D . . H51A H 1.3204 -0.1450 0.5426 0.394 Uiso 1 1 calc R . . H51B H 1.3739 -0.1298 0.4262 0.394 Uiso 1 1 calc R . . H51C H 1.3543 -0.1711 0.4389 0.394 Uiso 1 1 calc R . . C52 C 1.5233(5) 0.0521(2) 0.8207(5) 0.120(2) Uani 1 1 d D . . H52A H 1.4954 0.0754 0.8392 0.180 Uiso 1 1 calc R . . H52B H 1.5936 0.0507 0.8491 0.180 Uiso 1 1 calc R . . H52C H 1.4823 0.0340 0.8596 0.180 Uiso 1 1 calc R . . C53 C 1.5891(5) 0.0138(2) 0.6526(9) 0.161(4) Uani 1 1 d D . . H53A H 1.5600 -0.0074 0.6886 0.241 Uiso 1 1 calc R . . H53B H 1.6579 0.0175 0.6833 0.241 Uiso 1 1 calc R . . H53C H 1.5919 0.0108 0.5665 0.241 Uiso 1 1 calc R . . C54 C 1.5678(5) 0.0792(2) 0.6254(7) 0.139(3) Uani 1 1 d D . . H54A H 1.5673 0.0765 0.5392 0.209 Uiso 1 1 calc R . . H54B H 1.6379 0.0823 0.6529 0.209 Uiso 1 1 calc R . . H54C H 1.5277 0.1000 0.6472 0.209 Uiso 1 1 calc R . . C21 C 0.3943(10) 0.2678(2) 0.3830(9) 0.196(5) Uani 1 1 d D . . C43 C 0.3718(16) 0.2780(4) 0.5070(11) 0.411(15) Uani 1 1 d D . . H43A H 0.4170 0.2651 0.5606 0.616 Uiso 1 1 calc R . . H43B H 0.3009 0.2722 0.5255 0.616 Uiso 1 1 calc R . . H43C H 0.3825 0.3033 0.5168 0.616 Uiso 1 1 calc R . . C45 C 0.2933(10) 0.2649(4) 0.3128(15) 0.310(10) Uani 1 1 d D . . H45A H 0.2599 0.2879 0.3104 0.465 Uiso 1 1 calc R . . H45B H 0.2485 0.2478 0.3517 0.465 Uiso 1 1 calc R . . H45C H 0.3077 0.2570 0.2319 0.465 Uiso 1 1 calc R . . C44 C 0.4542(14) 0.2956(3) 0.3172(18) 0.367(13) Uani 1 1 d D . . H44A H 0.4651 0.2880 0.2353 0.550 Uiso 1 1 calc R . . H44B H 0.5201 0.2990 0.3560 0.550 Uiso 1 1 calc R . . H44C H 0.4163 0.3178 0.3176 0.550 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.052(3) 0.054(3) 0.068(3) 0.004(2) 0.000(2) 0.004(2) C2 0.050(3) 0.061(3) 0.060(3) 0.000(2) -0.002(2) 0.004(2) C3 0.057(3) 0.059(3) 0.059(3) -0.005(2) -0.004(2) -0.003(2) C4 0.044(3) 0.055(3) 0.053(3) -0.001(2) -0.002(2) -0.003(2) C5 0.054(3) 0.050(3) 0.054(3) -0.004(2) -0.001(2) -0.001(2) C6 0.042(2) 0.047(2) 0.057(3) 0.000(2) -0.001(2) 0.006(2) C7 0.056(3) 0.056(3) 0.057(3) -0.005(2) -0.006(2) -0.008(2) C8 0.051(3) 0.060(3) 0.050(3) -0.002(2) -0.001(2) -0.003(2) C9 0.045(3) 0.057(3) 0.053(3) -0.001(2) -0.001(2) -0.005(2) C10 0.046(3) 0.051(3) 0.060(3) -0.008(2) -0.005(2) -0.002(2) C11 0.048(3) 0.052(3) 0.052(3) -0.001(2) 0.001(2) 0.002(2) C12 0.046(3) 0.052(3) 0.064(3) -0.009(2) -0.004(2) -0.006(2) C13 0.045(3) 0.050(2) 0.060(3) 0.000(2) -0.004(2) -0.002(2) C14 0.053(3) 0.052(3) 0.073(3) -0.004(2) -0.002(2) -0.003(2) C15 0.060(3) 0.062(3) 0.080(4) 0.003(3) -0.003(3) 0.001(2) C16 0.101(4) 0.078(4) 0.082(4) -0.003(3) -0.012(3) 0.017(3) C17 0.136(5) 0.083(4) 0.102(5) -0.019(3) -0.009(4) 0.047(4) C18 0.124(5) 0.085(4) 0.134(6) 0.005(4) -0.005(5) 0.047(4) C19 0.131(5) 0.096(5) 0.106(5) 0.006(4) -0.013(4) 0.050(4) C20 0.093(4) 0.081(4) 0.090(4) 0.004(3) -0.013(3) 0.019(3) C22 0.051(3) 0.060(3) 0.068(3) 0.001(2) -0.002(3) 0.005(2) C23 0.062(3) 0.101(4) 0.063(3) -0.010(3) -0.005(3) 0.006(3) C24 0.048(3) 0.118(4) 0.072(4) -0.007(3) 0.002(3) 0.001(3) C25 0.051(3) 0.085(3) 0.064(3) 0.003(3) -0.007(3) 0.003(2) C26 0.061(4) 0.137(5) 0.060(3) -0.017(3) -0.010(3) -0.002(3) C27 0.056(3) 0.109(4) 0.061(3) -0.015(3) -0.003(2) 0.004(3) C28 0.050(3) 0.121(5) 0.084(4) -0.007(3) -0.011(3) 0.009(3) C29 0.047(2) 0.048(2) 0.059(3) -0.005(2) -0.003(2) 0.004(2) C30 0.064(3) 0.062(3) 0.059(3) 0.001(2) -0.004(2) 0.012(2) C31 0.072(3) 0.067(3) 0.067(3) -0.015(3) 0.001(3) 0.002(3) C32 0.057(3) 0.059(3) 0.082(3) -0.003(3) 0.000(3) 0.004(2) C33 0.059(3) 0.084(4) 0.070(3) 0.008(3) -0.008(3) 0.002(3) C34 0.060(3) 0.055(3) 0.064(3) -0.005(2) -0.007(2) 0.009(2) C35 0.089(4) 0.058(3) 0.115(4) 0.002(3) 0.003(4) 0.010(3) C36 0.041(3) 0.055(3) 0.054(3) -0.001(2) -0.006(2) 0.002(2) C37 0.059(3) 0.088(4) 0.063(3) -0.019(3) -0.006(3) 0.005(3) C38 0.045(3) 0.091(4) 0.071(3) -0.015(3) 0.001(2) 0.006(2) C39 0.052(3) 0.057(3) 0.061(3) 0.003(2) -0.005(2) -0.006(2) C40 0.046(3) 0.074(3) 0.060(3) -0.008(2) -0.003(2) -0.004(2) C41 0.049(3) 0.065(3) 0.059(3) -0.004(2) 0.004(2) 0.002(2) C42 0.053(3) 0.083(3) 0.064(3) 0.003(2) -0.005(2) -0.001(3) C46 0.068(4) 0.240(9) 0.166(7) -0.071(7) -0.040(5) 0.044(5) C47 0.076(4) 0.219(8) 0.079(4) 0.021(5) -0.028(3) -0.015(4) C48 0.106(5) 0.158(7) 0.150(6) 0.035(5) -0.048(5) -0.064(5) C49 0.354(16) 0.070(5) 0.47(2) 0.078(8) 0.263(16) 0.050(7) C50 0.355(15) 0.091(5) 0.148(8) -0.030(5) 0.007(8) 0.086(7) C51 0.226(11) 0.122(7) 0.44(2) -0.091(10) -0.165(14) 0.108(8) C52 0.075(4) 0.205(7) 0.080(4) 0.023(4) -0.031(3) -0.023(4) C53 0.081(5) 0.164(7) 0.237(9) -0.087(7) -0.070(5) 0.049(5) C54 0.101(5) 0.176(7) 0.141(6) 0.065(5) -0.050(4) -0.075(5) C21 0.320(15) 0.111(6) 0.158(8) 0.013(6) 0.016(9) 0.137(9) C43 0.76(4) 0.288(15) 0.185(11) -0.026(11) 0.020(17) 0.42(2) C45 0.239(14) 0.308(18) 0.38(2) -0.039(16) -0.145(15) 0.180(14) C44 0.51(3) 0.098(7) 0.49(3) 0.090(12) 0.23(2) 0.108(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C14 1.365(6) . ? C1 C2 1.440(6) . ? C1 C15 1.502(6) . ? C2 C3 1.360(5) . ? C2 C22 1.485(6) . ? C3 C4 1.424(5) . ? C3 H3 0.9300 . ? C4 C5 1.386(6) . ? C4 C13 1.422(5) . ? C5 C6 1.381(5) . ? C5 H5 0.9300 . ? C6 C7 1.401(5) . ? C6 C11 1.417(5) . ? C7 C8 1.385(5) . ? C7 H7 0.9300 . ? C8 C9 1.447(6) . ? C8 C29 1.483(6) . ? C9 C10 1.369(5) . ? C9 C36 1.491(5) . ? C10 C11 1.418(5) . ? C10 H10 0.9300 . ? C11 C12 1.378(5) . ? C12 C13 1.394(5) . ? C12 H12 0.9300 . ? C13 C14 1.410(6) . ? C14 H14 0.9300 . ? C15 C16 1.374(7) . ? C15 C20 1.389(7) . ? C16 C17 1.381(7) . ? C16 H16 0.9300 . ? C17 C18 1.366(8) . ? C17 H17 0.9300 . ? C18 C19 1.378(9) . ? C18 C21 1.597(9) . ? C19 C20 1.368(7) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C23 1.377(6) . ? C22 C27 1.376(6) . ? C23 C24 1.381(6) . ? C23 H23 0.9300 . ? C24 C25 1.364(7) . ? C24 H24 0.9300 . ? C25 C26 1.374(6) . ? C25 C28 1.516(7) . ? C26 C27 1.366(6) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C47 1.499(7) . ? C28 C46 1.500(7) . ? C28 C48 1.505(7) . ? C29 C34 1.370(6) . ? C29 C30 1.391(6) . ? C30 C31 1.370(6) . ? C30 H30 0.9300 . ? C31 C32 1.409(6) . ? C31 H31 0.9300 . ? C32 C33 1.408(7) . ? C32 C35 1.514(7) . ? C33 C34 1.368(6) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C51 1.456(9) . ? C35 C49 1.471(9) . ? C35 C50 1.505(9) . ? C36 C41 1.372(6) . ? C36 C37 1.376(6) . ? C37 C38 1.373(6) . ? C37 H37 0.9300 . ? C38 C39 1.368(6) . ? C38 H38 0.9300 . ? C39 C40 1.384(6) . ? C39 C42 1.528(6) . ? C40 C41 1.369(5) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? C42 C54 1.513(7) . ? C42 C53 1.532(7) . ? C42 C52 1.534(7) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C48 H48A 0.9601 . ? C48 H48B 0.9601 . ? C48 H48C 0.9601 . ? C49 H49A 0.9706 . ? C49 H49B 0.9705 . ? C49 H49C 0.9714 . ? C50 H50A 0.9601 . ? C50 H50B 0.9601 . ? C50 H50C 0.9601 . ? C51 H51A 0.9608 . ? C51 H51B 0.9608 . ? C51 H51C 0.9608 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C21 C43 1.454(12) . ? C21 C44 1.483(13) . ? C21 C45 1.520(12) . ? C43 H43A 1.0658 . ? C43 H43B 1.0868 . ? C43 H43C 1.0730 . ? C45 H45A 0.9683 . ? C45 H45B 0.9685 . ? C45 H45C 0.9681 . ? C44 H44A 0.9601 . ? C44 H44B 0.9601 . ? C44 H44C 0.9601 . ? 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 C14 C1 C2 119.7(4) . . ? C14 C1 C15 118.8(4) . . ? C2 C1 C15 121.5(4) . . ? C3 C2 C1 117.7(4) . . ? C3 C2 C22 119.8(4) . . ? C1 C2 C22 122.5(4) . . ? C2 C3 C4 124.0(4) . . ? C2 C3 H3 118.0 . . ? C4 C3 H3 118.0 . . ? C5 C4 C13 119.3(4) . . ? C5 C4 C3 123.2(4) . . ? C13 C4 C3 117.4(4) . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 122.4(4) . . ? C5 C6 C11 119.4(4) . . ? C7 C6 C11 118.2(4) . . ? C8 C7 C6 124.3(4) . . ? C8 C7 H7 117.9 . . ? C6 C7 H7 117.8 . . ? C7 C8 C9 117.2(4) . . ? C7 C8 C29 118.1(4) . . ? C9 C8 C29 124.5(4) . . ? C10 C9 C8 118.8(4) . . ? C10 C9 C36 118.2(4) . . ? C8 C9 C36 122.8(4) . . ? C9 C10 C11 123.6(4) . . ? C9 C10 H10 118.3 . . ? C11 C10 H10 118.2 . . ? C12 C11 C6 119.0(4) . . ? C12 C11 C10 123.1(4) . . ? C6 C11 C10 117.8(4) . . ? C11 C12 C13 122.0(4) . . ? C11 C12 H12 119.0 . . ? C13 C12 H12 119.0 . . ? C12 C13 C14 123.1(4) . . ? C12 C13 C4 118.5(4) . . ? C14 C13 C4 118.4(4) . . ? C1 C14 C13 122.8(4) . . ? C1 C14 H14 118.6 . . ? C13 C14 H14 118.6 . . ? C16 C15 C20 116.7(5) . . ? C16 C15 C1 121.4(4) . . ? C20 C15 C1 121.9(5) . . ? C15 C16 C17 122.0(5) . . ? C15 C16 H16 119.1 . . ? C17 C16 H16 118.9 . . ? C18 C17 C16 120.5(6) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 118.3(5) . . ? C17 C18 C21 122.5(7) . . ? C19 C18 C21 119.1(7) . . ? C20 C19 C18 121.0(6) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.5 . . ? C19 C20 C15 121.5(6) . . ? C19 C20 H20 119.2 . . ? C15 C20 H20 119.3 . . ? C23 C22 C27 115.8(4) . . ? C23 C22 C2 121.8(4) . . ? C27 C22 C2 122.2(4) . . ? C22 C23 C24 121.9(5) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.1 . . ? C25 C24 C23 122.3(5) . . ? C25 C24 H24 118.8 . . ? C23 C24 H24 118.9 . . ? C24 C25 C26 115.2(4) . . ? C24 C25 C28 122.6(5) . . ? C26 C25 C28 121.9(5) . . ? C27 C26 C25 123.3(5) . . ? C27 C26 H26 118.3 . . ? C25 C26 H26 118.3 . . ? C26 C27 C22 121.4(5) . . ? C26 C27 H27 119.4 . . ? C22 C27 H27 119.2 . . ? C47 C28 C46 111.4(6) . . ? C47 C28 C48 108.4(5) . . ? C46 C28 C48 103.4(6) . . ? C47 C28 C25 113.4(5) . . ? C46 C28 C25 111.6(5) . . ? C48 C28 C25 108.0(4) . . ? C34 C29 C30 117.5(4) . . ? C34 C29 C8 121.9(4) . . ? C30 C29 C8 120.1(4) . . ? C31 C30 C29 122.1(4) . . ? C31 C30 H30 118.9 . . ? C29 C30 H30 119.0 . . ? C30 C31 C32 121.4(4) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C31 C32 C33 114.8(4) . . ? C31 C32 C35 123.4(5) . . ? C33 C32 C35 121.8(5) . . ? C34 C33 C32 123.1(4) . . ? C34 C33 H33 118.4 . . ? C32 C33 H33 118.5 . . ? C33 C34 C29 121.0(4) . . ? C33 C34 H34 119.6 . . ? C29 C34 H34 119.5 . . ? C51 C35 C49 103.5(10) . . ? C51 C35 C50 107.8(8) . . ? C49 C35 C50 112.2(8) . . ? C51 C35 C32 111.1(5) . . ? C49 C35 C32 108.7(5) . . ? C50 C35 C32 113.2(5) . . ? C41 C36 C37 116.1(4) . . ? C41 C36 C9 121.2(4) . . ? C37 C36 C9 122.5(4) . . ? C38 C37 C36 121.9(4) . . ? C38 C37 H37 119.0 . . ? C36 C37 H37 119.1 . . ? C39 C38 C37 122.1(4) . . ? C39 C38 H38 118.9 . . ? C37 C38 H38 119.0 . . ? C38 C39 C40 116.1(4) . . ? C38 C39 C42 121.4(4) . . ? C40 C39 C42 122.4(4) . . ? C41 C40 C39 121.7(4) . . ? C41 C40 H40 119.2 . . ? C39 C40 H40 119.1 . . ? C40 C41 C36 122.1(4) . . ? C40 C41 H41 118.9 . . ? C36 C41 H41 119.0 . . ? C54 C42 C39 108.6(4) . . ? C54 C42 C53 108.7(6) . . ? C39 C42 C53 111.1(4) . . ? C54 C42 C52 107.3(5) . . ? C39 C42 C52 112.1(4) . . ? C53 C42 C52 108.9(6) . . ? C28 C46 H46A 109.6 . . ? C28 C46 H46B 109.3 . . ? H46A C46 H46B 109.5 . . ? C28 C46 H46C 109.4 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C28 C47 H47A 109.4 . . ? C28 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C28 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C28 C48 H48A 109.3 . . ? C28 C48 H48B 109.8 . . ? H48A C48 H48B 109.5 . . ? C28 C48 H48C 109.4 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C35 C49 H49A 110.4 . . ? C35 C49 H49B 110.3 . . ? H49A C49 H49B 108.4 . . ? C35 C49 H49C 111.1 . . ? H49A C49 H49C 108.2 . . ? H49B C49 H49C 108.4 . . ? C35 C50 H50A 109.4 . . ? C35 C50 H50B 109.6 . . ? H50A C50 H50B 109.5 . . ? C35 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C35 C51 H51A 109.4 . . ? C35 C51 H51B 109.7 . . ? H51A C51 H51B 109.4 . . ? C35 C51 H51C 109.5 . . ? H51A C51 H51C 109.4 . . ? H51B C51 H51C 109.4 . . ? C42 C52 H52A 109.5 . . ? C42 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C42 C52 H52C 109.4 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C42 C53 H53A 109.4 . . ? C42 C53 H53B 109.3 . . ? H53A C53 H53B 109.5 . . ? C42 C53 H53C 109.6 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C42 C54 H54A 109.5 . . ? C42 C54 H54B 109.4 . . ? H54A C54 H54B 109.5 . . ? C42 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C43 C21 C44 112.7(13) . . ? C43 C21 C45 109.3(12) . . ? C44 C21 C45 104.2(11) . . ? C43 C21 C18 110.9(7) . . ? C44 C21 C18 108.2(9) . . ? C45 C21 C18 111.3(9) . . ? C21 C43 H43A 120.3 . . ? C21 C43 H43B 122.9 . . ? H43A C43 H43B 94.6 . . ? C21 C43 H43C 121.2 . . ? H43A C43 H43C 96.0 . . ? H43B C43 H43C 95.1 . . ? C21 C45 H45A 110.3 . . ? C21 C45 H45B 110.5 . . ? H45A C45 H45B 108.6 . . ? C21 C45 H45C 110.1 . . ? H45A C45 H45C 108.7 . . ? H45B C45 H45C 108.6 . . ? C21 C44 H44A 109.5 . . ? C21 C44 H44B 109.2 . . ? H44A C44 H44B 109.5 . . ? C21 C44 H44C 109.8 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.41 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.858 _refine_diff_density_min -0.880 _refine_diff_density_rms 0.307 data_08dc38lts _database_code_depnum_ccdc_archive 'CCDC 735892' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H49 Si' _chemical_formula_weight 533.86 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' Si Si 0.0817 0.0704 '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 8.3308(2) _cell_length_b 14.4923(4) _cell_length_c 16.8856(4) _cell_angle_alpha 64.9740(10) _cell_angle_beta 81.5660(10) _cell_angle_gamma 75.5150(10) _cell_volume 1786.59(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9990 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description Columnar _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.992 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 582 _exptl_absorpt_coefficient_mu 0.087 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7043 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33607 _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.33 _reflns_number_total 8871 _reflns_number_gt 7384 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'Shelxtl-97 (Sheldrick, 2008)' _computing_structure_refinement 'Shelxtl-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker APEX2' _computing_publication_material 'Bruker APEX2' _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^)+(0.0647P)^2^+0.6726P] 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 8871 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0508 _refine_ls_R_factor_gt 0.0425 _refine_ls_wR_factor_ref 0.1284 _refine_ls_wR_factor_gt 0.1229 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _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 Si1 Si 0.80158(4) 0.55602(2) 0.18466(2) 0.01783(9) Uani 1 1 d . . . C1 C 0.56777(14) 0.89417(9) 0.05086(7) 0.0149(2) Uani 1 1 d . . . C2 C 0.40359(14) 0.93852(9) 0.07014(7) 0.0148(2) Uani 1 1 d . . . C3 C 0.30182(14) 0.88022(9) 0.13953(7) 0.0160(2) Uani 1 1 d . . . H3 H 0.3462 0.8092 0.1742 0.019 Uiso 1 1 calc R . . C4 C 0.14187(14) 0.92314(9) 0.15806(7) 0.0159(2) Uani 1 1 d . . . C5 C 0.07376(14) 1.03103(9) 0.10620(7) 0.0157(2) Uani 1 1 d . . . C6 C 0.16855(14) 1.08767(9) 0.03813(7) 0.0155(2) Uani 1 1 d . . . H6 H 0.1216 1.1581 0.0031 0.019 Uiso 1 1 calc R . . C7 C 0.66554(14) 0.95490(9) -0.01784(7) 0.0147(2) Uani 1 1 d . . . C8 C 0.63604(14) 0.78590(9) 0.09837(7) 0.0157(2) Uani 1 1 d . . . C9 C 0.69881(14) 0.69459(9) 0.13354(8) 0.0175(2) Uani 1 1 d . . . C10 C 1.03241(16) 0.54823(10) 0.16533(10) 0.0259(3) Uani 1 1 d . . . H10 H 1.0887 0.4733 0.1937 0.031 Uiso 1 1 calc R . . C11 C 1.09296(19) 0.60786(16) 0.20739(14) 0.0466(5) Uani 1 1 d . . . H11A H 1.2134 0.6010 0.1971 0.070 Uiso 1 1 calc R . . H11B H 1.0659 0.5791 0.2705 0.070 Uiso 1 1 calc R . . H11C H 1.0383 0.6816 0.1815 0.070 Uiso 1 1 calc R . . C12 C 1.08362(18) 0.58722(13) 0.06749(11) 0.0343(3) Uani 1 1 d . . . H12A H 1.0271 0.6600 0.0375 0.051 Uiso 1 1 calc R . . H12B H 1.0525 0.5445 0.0425 0.051 Uiso 1 1 calc R . . H12C H 1.2040 0.5820 0.0599 0.051 Uiso 1 1 calc R . . C13 C 0.73195(16) 0.48635(10) 0.12802(9) 0.0225(3) Uani 1 1 d . . . H13 H 0.7878 0.5090 0.0683 0.027 Uiso 1 1 calc R . . C14 C 0.79145(19) 0.36773(11) 0.17159(11) 0.0321(3) Uani 1 1 d . . . H14A H 0.7296 0.3401 0.2276 0.048 Uiso 1 1 calc R . . H14B H 0.9102 0.3508 0.1817 0.048 Uiso 1 1 calc R . . H14C H 0.7726 0.3365 0.1333 0.048 Uiso 1 1 calc R . . C15 C 0.54564(17) 0.51509(11) 0.11388(10) 0.0283(3) Uani 1 1 d . . . H15A H 0.5220 0.4811 0.0789 0.042 Uiso 1 1 calc R . . H15B H 0.5110 0.5908 0.0830 0.042 Uiso 1 1 calc R . . H15C H 0.4847 0.4918 0.1707 0.042 Uiso 1 1 calc R . . C16 C 0.74291(19) 0.51309(11) 0.30483(9) 0.0282(3) Uani 1 1 d . . . H16 H 0.7691 0.5652 0.3225 0.034 Uiso 1 1 calc R . . C17 C 0.8458(3) 0.40699(13) 0.36220(11) 0.0509(5) Uani 1 1 d . . . H17A H 0.8201 0.3941 0.4240 0.076 Uiso 1 1 calc R . . H17B H 0.9643 0.4072 0.3486 0.076 Uiso 1 1 calc R . . H17C H 0.8188 0.3520 0.3505 0.076 Uiso 1 1 calc R . . C18 C 0.5577(2) 0.51596(15) 0.32642(10) 0.0410(4) Uani 1 1 d . . . H18A H 0.5286 0.4584 0.3195 0.061 Uiso 1 1 calc R . . H18B H 0.4939 0.5823 0.2867 0.061 Uiso 1 1 calc R . . H18C H 0.5317 0.5090 0.3869 0.061 Uiso 1 1 calc R . . C19 C 0.03940(15) 0.85923(9) 0.23049(8) 0.0168(2) Uani 1 1 d . . . C20 C 0.09720(16) 0.80444(10) 0.31488(8) 0.0229(3) Uani 1 1 d . . . H20 H 0.2076 0.8019 0.3252 0.027 Uiso 1 1 calc R . . C21 C -0.00520(17) 0.75352(11) 0.38395(8) 0.0261(3) Uani 1 1 d . . . H21 H 0.0366 0.7168 0.4409 0.031 Uiso 1 1 calc R . . C22 C -0.16846(16) 0.75488(10) 0.37174(8) 0.0216(3) Uani 1 1 d . . . C23 C -0.22146(15) 0.80474(10) 0.28646(8) 0.0196(2) Uani 1 1 d . . . H23 H -0.3293 0.8035 0.2754 0.023 Uiso 1 1 calc R . . C24 C -0.11983(15) 0.85630(9) 0.21727(8) 0.0180(2) Uani 1 1 d . . . H24 H -0.1598 0.8902 0.1598 0.022 Uiso 1 1 calc R . . C25 C -0.28193(17) 0.70509(11) 0.45109(9) 0.0270(3) Uani 1 1 d . . . C26 C -0.2071(2) 0.58869(12) 0.49826(9) 0.0337(3) Uani 1 1 d . . . H26A H -0.0959 0.5799 0.5165 0.051 Uiso 1 1 calc R . . H26B H -0.1997 0.5541 0.4586 0.051 Uiso 1 1 calc R . . H26C H -0.2780 0.5577 0.5499 0.051 Uiso 1 1 calc R . . C27 C -0.45688(18) 0.71778(13) 0.42459(10) 0.0348(3) Uani 1 1 d . . . H27A H -0.5258 0.6864 0.4770 0.052 Uiso 1 1 calc R . . H27B H -0.4508 0.6831 0.3851 0.052 Uiso 1 1 calc R . . H27C H -0.5060 0.7920 0.3947 0.052 Uiso 1 1 calc R . . C28 C -0.2949(2) 0.75757(15) 0.51440(11) 0.0399(4) Uani 1 1 d . . . H28A H -0.3414 0.8322 0.4847 0.060 Uiso 1 1 calc R . . H28B H -0.1843 0.7476 0.5339 0.060 Uiso 1 1 calc R . . H28C H -0.3674 0.7265 0.5652 0.060 Uiso 1 1 calc R . . C29 C -0.09587(14) 1.08235(9) 0.12672(8) 0.0159(2) Uani 1 1 d . . . C30 C -0.14698(15) 1.07402(9) 0.21156(8) 0.0183(2) Uani 1 1 d . . . H30 H -0.0694 1.0399 0.2564 0.022 Uiso 1 1 calc R . . C31 C -0.30899(15) 1.11463(9) 0.23141(8) 0.0187(2) Uani 1 1 d . . . H31 H -0.3404 1.1074 0.2898 0.022 Uiso 1 1 calc R . . C32 C -0.42771(15) 1.16617(9) 0.16750(8) 0.0174(2) Uani 1 1 d . . . C33 C -0.37375(15) 1.17860(10) 0.08214(8) 0.0190(2) Uani 1 1 d . . . H33 H -0.4497 1.2160 0.0367 0.023 Uiso 1 1 calc R . . C34 C -0.21119(15) 1.13754(9) 0.06186(8) 0.0179(2) Uani 1 1 d . . . H34 H -0.1784 1.1472 0.0030 0.021 Uiso 1 1 calc R . . C35 C -0.61074(15) 1.19909(11) 0.19295(9) 0.0224(3) Uani 1 1 d . . . C36 C -0.68420(18) 1.10070(13) 0.23398(11) 0.0339(3) Uani 1 1 d . . . H36A H -0.6718 1.0689 0.1918 0.051 Uiso 1 1 calc R . . H36B H -0.8022 1.1195 0.2495 0.051 Uiso 1 1 calc R . . H36C H -0.6254 1.0510 0.2867 0.051 Uiso 1 1 calc R . . C37 C -0.62899(18) 1.24705(12) 0.26007(10) 0.0304(3) Uani 1 1 d . . . H37A H -0.5725 1.1958 0.3131 0.046 Uiso 1 1 calc R . . H37B H -0.7470 1.2674 0.2748 0.046 Uiso 1 1 calc R . . H37C H -0.5792 1.3086 0.2352 0.046 Uiso 1 1 calc R . . C38 C -0.70919(17) 1.27876(13) 0.11335(10) 0.0343(3) Uani 1 1 d . . . H38A H -0.6598 1.3404 0.0854 0.051 Uiso 1 1 calc R . . H38B H -0.8246 1.2991 0.1323 0.051 Uiso 1 1 calc R . . H38C H -0.7062 1.2477 0.0715 0.051 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 Si1 0.01695(17) 0.01333(16) 0.02006(17) -0.00432(12) -0.00279(12) -0.00102(12) C1 0.0150(5) 0.0142(5) 0.0149(5) -0.0053(4) -0.0014(4) -0.0026(4) C2 0.0146(5) 0.0150(5) 0.0149(5) -0.0060(4) -0.0006(4) -0.0034(4) C3 0.0161(5) 0.0138(5) 0.0162(5) -0.0042(4) -0.0011(4) -0.0031(4) C4 0.0163(6) 0.0167(5) 0.0149(5) -0.0059(4) 0.0002(4) -0.0051(4) C5 0.0142(5) 0.0172(5) 0.0164(5) -0.0079(4) -0.0012(4) -0.0025(4) C6 0.0147(5) 0.0139(5) 0.0166(5) -0.0059(4) -0.0013(4) -0.0012(4) C7 0.0141(5) 0.0149(5) 0.0155(5) -0.0063(4) -0.0006(4) -0.0033(4) C8 0.0136(5) 0.0187(5) 0.0154(5) -0.0075(4) 0.0015(4) -0.0046(4) C9 0.0146(5) 0.0191(5) 0.0170(5) -0.0063(4) 0.0016(4) -0.0039(4) C10 0.0180(6) 0.0222(6) 0.0392(8) -0.0162(6) -0.0062(5) 0.0023(5) C11 0.0199(7) 0.0640(12) 0.0812(13) -0.0546(11) -0.0021(8) -0.0065(7) C12 0.0191(7) 0.0372(8) 0.0459(9) -0.0184(7) 0.0053(6) -0.0060(6) C13 0.0207(6) 0.0211(6) 0.0270(6) -0.0111(5) 0.0011(5) -0.0055(5) C14 0.0259(7) 0.0220(7) 0.0508(9) -0.0176(6) -0.0008(6) -0.0044(5) C15 0.0256(7) 0.0277(7) 0.0336(7) -0.0124(6) -0.0055(5) -0.0068(6) C16 0.0385(8) 0.0221(6) 0.0194(6) -0.0023(5) -0.0058(5) -0.0072(6) C17 0.0820(14) 0.0282(8) 0.0301(8) 0.0021(6) -0.0232(9) -0.0036(8) C18 0.0481(10) 0.0530(10) 0.0241(7) -0.0113(7) 0.0090(7) -0.0284(8) C19 0.0156(5) 0.0159(5) 0.0174(5) -0.0064(4) 0.0016(4) -0.0027(4) C20 0.0162(6) 0.0268(6) 0.0207(6) -0.0041(5) -0.0017(5) -0.0053(5) C21 0.0232(7) 0.0303(7) 0.0175(6) -0.0018(5) -0.0020(5) -0.0067(5) C22 0.0210(6) 0.0222(6) 0.0194(6) -0.0065(5) 0.0045(5) -0.0070(5) C23 0.0166(6) 0.0220(6) 0.0215(6) -0.0096(5) 0.0016(4) -0.0064(5) C24 0.0191(6) 0.0176(5) 0.0175(5) -0.0069(4) -0.0006(4) -0.0048(5) C25 0.0243(7) 0.0342(7) 0.0203(6) -0.0085(5) 0.0074(5) -0.0116(6) C26 0.0367(8) 0.0353(8) 0.0228(7) -0.0034(6) 0.0045(6) -0.0153(7) C27 0.0247(7) 0.0456(9) 0.0306(7) -0.0109(7) 0.0096(6) -0.0157(6) C28 0.0402(9) 0.0530(10) 0.0309(8) -0.0221(7) 0.0112(7) -0.0152(8) C29 0.0142(5) 0.0148(5) 0.0188(5) -0.0068(4) 0.0008(4) -0.0038(4) C30 0.0171(6) 0.0190(6) 0.0183(5) -0.0074(4) -0.0020(4) -0.0026(5) C31 0.0193(6) 0.0213(6) 0.0167(5) -0.0096(5) 0.0020(4) -0.0044(5) C32 0.0145(5) 0.0176(5) 0.0221(6) -0.0102(5) 0.0015(4) -0.0043(4) C33 0.0150(6) 0.0216(6) 0.0199(6) -0.0084(5) -0.0023(4) -0.0018(5) C34 0.0176(6) 0.0204(6) 0.0156(5) -0.0079(4) 0.0012(4) -0.0040(5) C35 0.0146(6) 0.0297(7) 0.0254(6) -0.0150(5) 0.0023(5) -0.0038(5) C36 0.0233(7) 0.0448(9) 0.0405(8) -0.0218(7) 0.0086(6) -0.0167(6) C37 0.0216(7) 0.0409(8) 0.0356(8) -0.0264(7) 0.0048(6) -0.0021(6) C38 0.0168(6) 0.0487(9) 0.0329(8) -0.0195(7) -0.0009(5) 0.0062(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C9 1.8441(12) . ? Si1 C16 1.8806(14) . ? Si1 C13 1.8825(13) . ? Si1 C10 1.8857(14) . ? C1 C2 1.4130(16) . ? C1 C7 1.4147(16) . ? C1 C8 1.4323(16) . ? C2 C3 1.4265(16) . ? C2 C7 1.4309(15) 2_675 ? C3 C4 1.3741(17) . ? C3 H3 0.9500 . ? C4 C5 1.4412(16) . ? C4 C19 1.4877(16) . ? C5 C6 1.3705(16) . ? C5 C29 1.4896(16) . ? C6 C7 1.4219(16) 2_675 ? C6 H6 0.9500 . ? C7 C6 1.4219(16) 2_675 ? C7 C2 1.4309(15) 2_675 ? C8 C9 1.2072(17) . ? C10 C11 1.532(2) . ? C10 C12 1.535(2) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.5299(18) . ? C13 C14 1.5339(18) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.527(2) . ? C16 C17 1.537(2) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.3908(17) . ? C19 C20 1.3949(16) . ? C20 C21 1.3883(18) . ? C20 H20 0.9500 . ? C21 C22 1.3993(18) . ? C21 H21 0.9500 . ? C22 C23 1.3919(17) . ? C22 C25 1.5366(17) . ? C23 C24 1.3886(17) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C28 1.532(2) . ? C25 C27 1.532(2) . ? C25 C26 1.533(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C34 1.3947(16) . ? C29 C30 1.3959(17) . ? C30 C31 1.3846(17) . ? C30 H30 0.9500 . ? C31 C32 1.4008(16) . ? C31 H31 0.9500 . ? C32 C33 1.3938(17) . ? C32 C35 1.5345(17) . ? C33 C34 1.3924(17) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C38 1.5327(19) . ? C35 C37 1.5341(18) . ? C35 C36 1.538(2) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 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 C9 Si1 C16 105.67(6) . . ? C9 Si1 C13 107.28(6) . . ? C16 Si1 C13 115.69(6) . . ? C9 Si1 C10 107.39(6) . . ? C16 Si1 C10 110.34(7) . . ? C13 Si1 C10 110.03(6) . . ? C2 C1 C7 120.64(10) . . ? C2 C1 C8 120.55(10) . . ? C7 C1 C8 118.76(10) . . ? C1 C2 C3 122.31(10) . . ? C1 C2 C7 119.46(10) . 2_675 ? C3 C2 C7 118.22(10) . 2_675 ? C4 C3 C2 122.36(10) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 119.22(10) . . ? C3 C4 C19 120.61(10) . . ? C5 C4 C19 120.16(10) . . ? C6 C5 C4 119.22(10) . . ? C6 C5 C29 119.65(10) . . ? C4 C5 C29 121.11(10) . . ? C5 C6 C7 122.57(10) . 2_675 ? C5 C6 H6 118.7 . . ? C7 C6 H6 118.7 2_675 . ? C1 C7 C6 121.73(10) . 2_675 ? C1 C7 C2 119.88(10) . 2_675 ? C6 C7 C2 118.37(10) 2_675 2_675 ? C9 C8 C1 175.85(12) . . ? C8 C9 Si1 177.90(11) . . ? C11 C10 C12 110.37(13) . . ? C11 C10 Si1 111.64(10) . . ? C12 C10 Si1 111.70(9) . . ? C11 C10 H10 107.6 . . ? C12 C10 H10 107.6 . . ? Si1 C10 H10 107.6 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 110.55(11) . . ? C15 C13 Si1 114.87(9) . . ? C14 C13 Si1 112.78(10) . . ? C15 C13 H13 106.0 . . ? C14 C13 H13 106.0 . . ? Si1 C13 H13 106.0 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C18 C16 C17 110.58(14) . . ? C18 C16 Si1 113.77(10) . . ? C17 C16 Si1 113.85(12) . . ? C18 C16 H16 106.0 . . ? C17 C16 H16 106.0 . . ? Si1 C16 H16 106.0 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 117.92(11) . . ? C24 C19 C4 121.16(10) . . ? C20 C19 C4 120.84(11) . . ? C21 C20 C19 120.58(12) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 121.65(12) . . ? C20 C21 H21 119.2 . . ? C22 C21 H21 119.2 . . ? C23 C22 C21 117.17(11) . . ? C23 C22 C25 122.93(12) . . ? C21 C22 C25 119.89(11) . . ? C24 C23 C22 121.28(11) . . ? C24 C23 H23 119.4 . . ? C22 C23 H23 119.4 . . ? C23 C24 C19 121.22(11) . . ? C23 C24 H24 119.4 . . ? C19 C24 H24 119.4 . . ? C28 C25 C27 108.52(13) . . ? C28 C25 C26 108.79(12) . . ? C27 C25 C26 108.91(12) . . ? C28 C25 C22 108.87(12) . . ? C27 C25 C22 111.99(11) . . ? C26 C25 C22 109.70(11) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 117.71(11) . . ? C34 C29 C5 120.75(10) . . ? C30 C29 C5 121.50(10) . . ? C31 C30 C29 121.05(11) . . ? C31 C30 H30 119.5 . . ? C29 C30 H30 119.5 . . ? C30 C31 C32 121.63(11) . . ? C30 C31 H31 119.2 . . ? C32 C31 H31 119.2 . . ? C33 C32 C31 116.96(11) . . ? C33 C32 C35 122.26(11) . . ? C31 C32 C35 120.61(11) . . ? C34 C33 C32 121.60(11) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C33 C34 C29 120.91(11) . . ? C33 C34 H34 119.5 . . ? C29 C34 H34 119.5 . . ? C38 C35 C37 108.11(12) . . ? C38 C35 C32 111.79(11) . . ? C37 C35 C32 111.41(10) . . ? C38 C35 C36 109.15(12) . . ? C37 C35 C36 108.85(12) . . ? C32 C35 C36 107.47(11) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.348 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.050 data_090226lts _database_code_depnum_ccdc_archive 'CCDC 735893' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H98' _chemical_formula_weight 1131.64 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 16.8988(11) _cell_length_b 18.7150(12) _cell_length_c 24.6740(17) _cell_angle_alpha 90.00 _cell_angle_beta 96.852(2) _cell_angle_gamma 90.00 _cell_volume 7747.7(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7601 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description Lump _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 0.970 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 0.054 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7141 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 64327 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 26.43 _reflns_number_total 15902 _reflns_number_gt 9125 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker Saint' _computing_structure_solution 'Shelxtl-97 (Sheldrick, 2008)' _computing_structure_refinement 'Shelxtl-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker APEX2' _computing_publication_material 'Bruker APEX2' _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^)+(0.1332P)^2^+7.1049P] 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 15902 _refine_ls_number_parameters 808 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1318 _refine_ls_R_factor_gt 0.0881 _refine_ls_wR_factor_ref 0.2799 _refine_ls_wR_factor_gt 0.2587 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.17560(17) -0.05546(16) 0.93071(12) 0.0157(6) Uani 1 1 d . . . C2 C 0.15503(17) 0.01086(16) 0.90297(12) 0.0147(6) Uani 1 1 d . . . C3 C 0.09065(17) 0.04832(16) 0.91697(12) 0.0152(6) Uani 1 1 d . . . H3 H 0.0769 0.0919 0.8985 0.018 Uiso 1 1 calc R . . C4 C 0.04351(17) 0.02520(15) 0.95771(12) 0.0129(6) Uani 1 1 d . . . C5 C 0.06472(17) -0.04071(15) 0.98569(12) 0.0138(6) Uani 1 1 d . . . C6 C 0.13113(17) -0.07936(16) 0.97041(12) 0.0165(6) Uani 1 1 d . . . H6 H 0.1454 -0.1233 0.9883 0.020 Uiso 1 1 calc R . . C7 C -0.02084(17) 0.06589(16) 0.97269(12) 0.0150(6) Uani 1 1 d . . . C8 C -0.04134(17) 0.13341(16) 0.94916(12) 0.0149(6) Uani 1 1 d . . . C9 C -0.06441(17) 0.19234(16) 0.93433(12) 0.0148(6) Uani 1 1 d . . . C10 C 0.24247(17) -0.10205(16) 0.91765(12) 0.0159(6) Uani 1 1 d . . . C11 C 0.30247(18) -0.12116(16) 0.95861(13) 0.0177(7) Uani 1 1 d . . . H11 H 0.2992 -0.1061 0.9950 0.021 Uiso 1 1 calc R . . C12 C 0.36726(19) -0.16208(17) 0.94708(13) 0.0205(7) Uani 1 1 d . . . H12 H 0.4073 -0.1746 0.9759 0.025 Uiso 1 1 calc R . . C13 C 0.37450(19) -0.18475(17) 0.89498(13) 0.0219(7) Uani 1 1 d . . . C14 C 0.31350(18) -0.16668(18) 0.85393(13) 0.0215(7) Uani 1 1 d . . . H14 H 0.3166 -0.1828 0.8177 0.026 Uiso 1 1 calc R . . C15 C 0.24857(18) -0.12595(17) 0.86443(13) 0.0189(7) Uani 1 1 d . . . H15 H 0.2082 -0.1142 0.8356 0.023 Uiso 1 1 calc R . . C16 C 0.44726(19) -0.22651(19) 0.87968(14) 0.0261(8) Uani 1 1 d . . . C17 C 0.5056(2) -0.2437(3) 0.93000(17) 0.0445(11) Uani 1 1 d . . . H17A H 0.5516 -0.2693 0.9189 0.067 Uiso 1 1 calc R . . H17B H 0.4790 -0.2736 0.9550 0.067 Uiso 1 1 calc R . . H17C H 0.5235 -0.1991 0.9484 0.067 Uiso 1 1 calc R . . C18 C 0.4212(2) -0.2957(2) 0.85103(16) 0.0352(9) Uani 1 1 d . . . H18A H 0.4682 -0.3221 0.8425 0.053 Uiso 1 1 calc R . . H18B H 0.3867 -0.2849 0.8172 0.053 Uiso 1 1 calc R . . H18C H 0.3917 -0.3247 0.8749 0.053 Uiso 1 1 calc R . . C19 C 0.4914(2) -0.1807(2) 0.84277(19) 0.0447(11) Uani 1 1 d . . . H19A H 0.5083 -0.1361 0.8616 0.067 Uiso 1 1 calc R . . H19B H 0.4563 -0.1696 0.8093 0.067 Uiso 1 1 calc R . . H19C H 0.5384 -0.2065 0.8335 0.067 Uiso 1 1 calc R . . C20 C 0.20515(17) 0.04121(15) 0.86313(12) 0.0133(6) Uani 1 1 d . . . C21 C 0.17118(18) 0.07382(17) 0.81487(12) 0.0177(7) Uani 1 1 d . . . H21 H 0.1148 0.0755 0.8066 0.021 Uiso 1 1 calc R . . C22 C 0.21896(18) 0.10365(16) 0.77919(12) 0.0181(7) Uani 1 1 d . . . H22 H 0.1944 0.1256 0.7467 0.022 Uiso 1 1 calc R . . C23 C 0.30211(18) 0.10272(17) 0.78912(12) 0.0181(7) Uani 1 1 d . . . C24 C 0.33506(19) 0.06999(17) 0.83663(13) 0.0222(7) Uani 1 1 d . . . H24 H 0.3914 0.0678 0.8444 0.027 Uiso 1 1 calc R . . C25 C 0.28828(17) 0.04000(16) 0.87358(12) 0.0165(6) Uani 1 1 d . . . H25 H 0.3131 0.0185 0.9061 0.020 Uiso 1 1 calc R . . C26 C 0.35323(19) 0.13729(18) 0.74868(13) 0.0232(7) Uani 1 1 d . . . C27 C 0.4425(2) 0.1301(3) 0.76800(17) 0.0448(11) Uani 1 1 d . . . H27A H 0.4545 0.1528 0.8038 0.067 Uiso 1 1 calc R . . H27B H 0.4731 0.1535 0.7417 0.067 Uiso 1 1 calc R . . H27C H 0.4568 0.0794 0.7708 0.067 Uiso 1 1 calc R . . C28 C 0.3363(3) 0.1005(3) 0.69286(16) 0.0447(11) Uani 1 1 d . . . H28A H 0.3483 0.0495 0.6968 0.067 Uiso 1 1 calc R . . H28B H 0.3697 0.1219 0.6673 0.067 Uiso 1 1 calc R . . H28C H 0.2800 0.1068 0.6788 0.067 Uiso 1 1 calc R . . C29 C 0.3322(2) 0.2165(2) 0.74300(17) 0.0400(10) Uani 1 1 d . . . H29A H 0.2768 0.2216 0.7266 0.060 Uiso 1 1 calc R . . H29B H 0.3675 0.2397 0.7196 0.060 Uiso 1 1 calc R . . H29C H 0.3389 0.2390 0.7791 0.060 Uiso 1 1 calc R . . C30 C -0.09893(18) 0.26255(16) 0.92545(13) 0.0178(7) Uani 1 1 d . . . C31 C -0.09150(19) 0.30421(17) 0.87927(13) 0.0212(7) Uani 1 1 d . . . H31 H -0.0616 0.2867 0.8519 0.025 Uiso 1 1 calc R . . C32 C -0.12746(19) 0.37107(17) 0.87305(14) 0.0226(7) Uani 1 1 d . . . C33 C -0.1697(2) 0.39570(18) 0.91524(14) 0.0266(8) Uani 1 1 d . . . H33 H -0.1936 0.4416 0.9117 0.032 Uiso 1 1 calc R . . C34 C -0.1779(2) 0.35630(18) 0.96155(14) 0.0245(7) Uani 1 1 d . . . C35 C -0.14251(19) 0.28932(18) 0.96638(13) 0.0226(7) Uani 1 1 d . . . H35 H -0.1477 0.2611 0.9977 0.027 Uiso 1 1 calc R . . C36 C -0.1265(2) 0.41718(19) 0.82206(15) 0.0300(8) Uani 1 1 d . . . C37 C -0.0732(2) 0.3868(2) 0.78147(16) 0.0384(10) Uani 1 1 d . . . H37A H -0.0185 0.3821 0.7994 0.058 Uiso 1 1 calc R . . H37B H -0.0739 0.4191 0.7502 0.058 Uiso 1 1 calc R . . H37C H -0.0931 0.3397 0.7689 0.058 Uiso 1 1 calc R . . C38 C -0.0959(3) 0.4929(2) 0.83909(18) 0.0451(11) Uani 1 1 d . . . H38A H -0.1321 0.5150 0.8625 0.068 Uiso 1 1 calc R . . H38B H -0.0939 0.5223 0.8064 0.068 Uiso 1 1 calc R . . H38C H -0.0424 0.4894 0.8592 0.068 Uiso 1 1 calc R . . C39 C -0.2121(2) 0.4222(2) 0.79230(16) 0.0375(9) Uani 1 1 d . . . H39A H -0.2315 0.3741 0.7820 0.056 Uiso 1 1 calc R . . H39B H -0.2120 0.4515 0.7594 0.056 Uiso 1 1 calc R . . H39C H -0.2471 0.4440 0.8166 0.056 Uiso 1 1 calc R . . C40 C -0.2227(2) 0.3869(2) 1.00675(15) 0.0325(9) Uani 1 1 d . . . C41 C -0.1786(3) 0.4524(2) 1.03138(18) 0.0537(12) Uani 1 1 d . . . H41A H -0.2078 0.4727 1.0597 0.081 Uiso 1 1 calc R . . H41B H -0.1746 0.4881 1.0028 0.081 Uiso 1 1 calc R . . H41C H -0.1250 0.4385 1.0475 0.081 Uiso 1 1 calc R . . C42 C -0.3083(3) 0.4099(3) 0.9827(2) 0.0611(14) Uani 1 1 d . . . H42A H -0.3358 0.3693 0.9638 0.092 Uiso 1 1 calc R . . H42B H -0.3050 0.4492 0.9569 0.092 Uiso 1 1 calc R . . H42C H -0.3379 0.4257 1.0124 0.092 Uiso 1 1 calc R . . C43 C -0.2326(2) 0.3339(2) 1.05165(17) 0.0402(10) Uani 1 1 d . . . H43A H -0.2599 0.2912 1.0359 0.060 Uiso 1 1 calc R . . H43B H -0.2642 0.3556 1.0781 0.060 Uiso 1 1 calc R . . H43C H -0.1800 0.3206 1.0700 0.060 Uiso 1 1 calc R . . C44 C 0.65547(17) 0.00757(17) 0.90420(12) 0.0174(7) Uani 1 1 d . . . C45 C 0.67618(18) -0.05874(16) 0.93298(12) 0.0176(7) Uani 1 1 d . . . C46 C 0.63305(17) -0.07911(16) 0.97314(12) 0.0163(6) Uani 1 1 d . . . H46 H 0.6485 -0.1213 0.9930 0.020 Uiso 1 1 calc R . . C47 C 0.56602(18) -0.04071(16) 0.98713(12) 0.0166(6) Uani 1 1 d . . . C48 C 0.54452(17) 0.02302(16) 0.95771(12) 0.0168(6) Uani 1 1 d . . . C49 C 0.59006(17) 0.04499(17) 0.91604(12) 0.0170(6) Uani 1 1 d . . . H49 H 0.5748 0.0869 0.8957 0.020 Uiso 1 1 calc R . . C50 C 0.47922(17) 0.06431(16) 0.97134(12) 0.0165(6) Uani 1 1 d . . . C51 C 0.45767(17) 0.12948(17) 0.94412(12) 0.0178(7) Uani 1 1 d . . . C52 C 0.43286(18) 0.18548(17) 0.92465(13) 0.0188(7) Uani 1 1 d . . . C53 C 0.70619(18) 0.03649(16) 0.86352(12) 0.0176(7) Uani 1 1 d . . . C54 C 0.67352(19) 0.06021(17) 0.81239(13) 0.0194(7) Uani 1 1 d . . . H54 H 0.6174 0.0588 0.8029 0.023 Uiso 1 1 calc R . . C55 C 0.72128(19) 0.08580(18) 0.77523(13) 0.0213(7) Uani 1 1 d . . . H55 H 0.6971 0.1016 0.7405 0.026 Uiso 1 1 calc R . . C56 C 0.80434(19) 0.08931(17) 0.78703(13) 0.0208(7) Uani 1 1 d . . . C57 C 0.83621(18) 0.06803(18) 0.83880(13) 0.0206(7) Uani 1 1 d . . . H57 H 0.8921 0.0715 0.8489 0.025 Uiso 1 1 calc R . . C58 C 0.78829(18) 0.04157(17) 0.87651(13) 0.0212(7) Uani 1 1 d . . . H58 H 0.8121 0.0268 0.9115 0.025 Uiso 1 1 calc R . . C59 C 0.8561(2) 0.1165(2) 0.74446(14) 0.0282(8) Uani 1 1 d . . . C60 C 0.8497(3) 0.0658(3) 0.69709(17) 0.0501(12) Uani 1 1 d . . . H60A H 0.8845 0.0819 0.6705 0.075 Uiso 1 1 calc R . . H60B H 0.7945 0.0643 0.6798 0.075 Uiso 1 1 calc R . . H60C H 0.8660 0.0179 0.7101 0.075 Uiso 1 1 calc R . . C61 C 0.8261(3) 0.1908(3) 0.7247(2) 0.0596(13) Uani 1 1 d . . . H61A H 0.8370 0.2253 0.7545 0.089 Uiso 1 1 calc R . . H61B H 0.7685 0.1887 0.7133 0.089 Uiso 1 1 calc R . . H61C H 0.8535 0.2056 0.6938 0.089 Uiso 1 1 calc R . . C62 C 0.9424(3) 0.1250(3) 0.76811(19) 0.0591(14) Uani 1 1 d . . . H62A H 0.9631 0.0790 0.7826 0.089 Uiso 1 1 calc R . . H62B H 0.9464 0.1604 0.7976 0.089 Uiso 1 1 calc R . . H62C H 0.9738 0.1410 0.7395 0.089 Uiso 1 1 calc R . . C63 C 0.74341(17) -0.10417(16) 0.91968(12) 0.0175(6) Uani 1 1 d . . . C64 C 0.75051(19) -0.12637(19) 0.86713(14) 0.0259(8) Uani 1 1 d . . . H64 H 0.7119 -0.1114 0.8382 0.031 Uiso 1 1 calc R . . C65 C 0.8117(2) -0.1692(2) 0.85568(16) 0.0362(9) Uani 1 1 d . . . H65 H 0.8142 -0.1836 0.8190 0.043 Uiso 1 1 calc R . . C66 C 0.8710(2) -0.1928(2) 0.89651(15) 0.0337(9) Uani 1 1 d . A . C67 C 0.8638(2) -0.17025(19) 0.94926(15) 0.0284(8) Uani 1 1 d . . . H67 H 0.9026 -0.1851 0.9781 0.034 Uiso 1 1 calc R . . C68 C 0.80133(19) -0.12642(18) 0.96118(14) 0.0235(7) Uani 1 1 d . . . H68 H 0.7983 -0.1117 0.9977 0.028 Uiso 1 1 calc R . . C69 C 0.9390(3) -0.2407(3) 0.8828(2) 0.0687(18) Uani 1 1 d . . . C70 C 0.9138(3) -0.2956(3) 0.84283(18) 0.0508(12) Uani 1 1 d . A . H70A H 0.8944 -0.2731 0.8079 0.076 Uiso 1 1 calc R . . H70B H 0.8709 -0.3240 0.8556 0.076 Uiso 1 1 calc R . . H70C H 0.9590 -0.3268 0.8380 0.076 Uiso 1 1 calc R . . C71 C 0.9857(8) -0.1970(9) 0.8501(9) 0.128(6) Uani 0.539(7) 1 d P A 1 H71A H 1.0295 -0.1746 0.8737 0.191 Uiso 0.539(7) 1 calc PR A 1 H71B H 0.9517 -0.1599 0.8315 0.191 Uiso 0.539(7) 1 calc PR A 1 H71C H 1.0075 -0.2270 0.8229 0.191 Uiso 0.539(7) 1 calc PR A 1 C72 C 0.9946(6) -0.2622(5) 0.9281(4) 0.0514(18) Uani 0.539(7) 1 d P A 1 H72A H 1.0412 -0.2841 0.9147 0.077 Uiso 0.539(7) 1 calc PR A 1 H72B H 0.9693 -0.2968 0.9503 0.077 Uiso 0.539(7) 1 calc PR A 1 H72C H 1.0115 -0.2202 0.9504 0.077 Uiso 0.539(7) 1 calc PR A 1 C71' C 1.0142(9) -0.2161(11) 0.9014(11) 0.128(6) Uani 0.461(7) 1 d P A 2 H71D H 1.0263 -0.2269 0.9403 0.191 Uiso 0.461(7) 1 calc PR A 2 H71E H 1.0163 -0.1643 0.8959 0.191 Uiso 0.461(7) 1 calc PR A 2 H71F H 1.0534 -0.2395 0.8811 0.191 Uiso 0.461(7) 1 calc PR A 2 C72' C 0.9496(6) -0.3068(6) 0.9376(4) 0.0514(18) Uani 0.461(7) 1 d P A 2 H72D H 0.9964 -0.3367 0.9343 0.077 Uiso 0.461(7) 1 calc PR A 2 H72E H 0.9018 -0.3368 0.9350 0.077 Uiso 0.461(7) 1 calc PR A 2 H72F H 0.9563 -0.2823 0.9730 0.077 Uiso 0.461(7) 1 calc PR A 2 C73 C 0.39265(19) 0.24812(17) 0.90245(13) 0.0195(7) Uani 1 1 d . . . C74 C 0.30963(19) 0.24926(17) 0.89804(13) 0.0211(7) Uani 1 1 d . . . H74 H 0.2816 0.2096 0.9103 0.025 Uiso 1 1 calc R . . C75 C 0.26807(19) 0.30812(18) 0.87578(14) 0.0238(7) Uani 1 1 d . . . C76 C 0.31145(19) 0.36542(17) 0.85803(14) 0.0230(7) Uani 1 1 d . . . H76 H 0.2831 0.4058 0.8427 0.028 Uiso 1 1 calc R . . C77 C 0.3942(2) 0.36592(18) 0.86182(14) 0.0244(7) Uani 1 1 d . . . C78 C 0.43476(19) 0.30589(17) 0.88425(13) 0.0225(7) Uani 1 1 d . . . H78 H 0.4913 0.3043 0.8872 0.027 Uiso 1 1 calc R . . C79 C 0.17606(19) 0.30971(18) 0.86851(14) 0.0256(8) Uani 1 1 d . . . C80 C 0.1415(2) 0.2468(2) 0.89699(19) 0.0411(10) Uani 1 1 d . . . H80A H 0.1638 0.2462 0.9355 0.062 Uiso 1 1 calc R . . H80B H 0.1552 0.2022 0.8795 0.062 Uiso 1 1 calc R . . H80C H 0.0835 0.2516 0.8942 0.062 Uiso 1 1 calc R . . C81 C 0.1469(2) 0.3049(2) 0.80768(17) 0.0423(10) Uani 1 1 d . . . H81A H 0.0885 0.3055 0.8023 0.063 Uiso 1 1 calc R . . H81B H 0.1662 0.2604 0.7929 0.063 Uiso 1 1 calc R . . H81C H 0.1674 0.3457 0.7887 0.063 Uiso 1 1 calc R . . C82 C 0.1459(2) 0.3791(2) 0.89125(17) 0.0343(9) Uani 1 1 d . . . H82A H 0.0876 0.3780 0.8884 0.052 Uiso 1 1 calc R . . H82B H 0.1629 0.4196 0.8703 0.052 Uiso 1 1 calc R . . H82C H 0.1678 0.3841 0.9297 0.052 Uiso 1 1 calc R . . C83 C 0.4386(2) 0.4289(2) 0.84024(17) 0.0347(9) Uani 1 1 d . . . C84 C 0.4314(4) 0.4225(3) 0.7777(2) 0.0752(17) Uani 1 1 d . . . H84A H 0.4595 0.3796 0.7678 0.113 Uiso 1 1 calc R . . H84B H 0.4551 0.4648 0.7626 0.113 Uiso 1 1 calc R . . H84C H 0.3751 0.4192 0.7630 0.113 Uiso 1 1 calc R . . C85 C 0.4025(3) 0.5000(2) 0.8560(3) 0.0709(17) Uani 1 1 d . . . H85A H 0.3462 0.5018 0.8411 0.106 Uiso 1 1 calc R . . H85B H 0.4311 0.5396 0.8412 0.106 Uiso 1 1 calc R . . H85C H 0.4073 0.5039 0.8959 0.106 Uiso 1 1 calc R . . C86 C 0.5267(3) 0.4295(2) 0.8628(2) 0.0583(14) Uani 1 1 d . . . H86A H 0.5320 0.4359 0.9025 0.088 Uiso 1 1 calc R . . H86B H 0.5536 0.4689 0.8462 0.088 Uiso 1 1 calc R . . H86C H 0.5512 0.3841 0.8542 0.088 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 0.0129(14) 0.0161(16) 0.0177(15) -0.0027(12) 0.0005(12) -0.0020(12) C2 0.0137(15) 0.0177(16) 0.0129(14) 0.0000(12) 0.0029(11) -0.0001(12) C3 0.0158(15) 0.0151(15) 0.0148(15) -0.0004(12) 0.0025(12) -0.0020(12) C4 0.0135(14) 0.0113(15) 0.0139(14) 0.0003(11) 0.0012(11) -0.0008(11) C5 0.0123(14) 0.0144(15) 0.0146(14) -0.0014(12) 0.0017(11) -0.0002(12) C6 0.0168(15) 0.0129(15) 0.0202(16) 0.0011(12) 0.0035(12) 0.0018(12) C7 0.0157(15) 0.0141(15) 0.0151(15) -0.0004(12) 0.0016(12) -0.0016(12) C8 0.0125(14) 0.0184(16) 0.0139(14) 0.0019(12) 0.0020(11) 0.0000(12) C9 0.0157(15) 0.0138(16) 0.0157(15) 0.0006(12) 0.0044(12) -0.0010(12) C10 0.0130(14) 0.0153(15) 0.0199(16) 0.0007(12) 0.0043(12) 0.0000(12) C11 0.0178(15) 0.0186(16) 0.0176(15) -0.0003(12) 0.0060(12) 0.0021(13) C12 0.0209(16) 0.0217(17) 0.0191(16) -0.0004(13) 0.0033(13) 0.0056(13) C13 0.0184(16) 0.0195(17) 0.0291(18) -0.0024(14) 0.0074(13) 0.0024(13) C14 0.0205(16) 0.0268(18) 0.0182(16) -0.0039(13) 0.0058(13) 0.0041(14) C15 0.0164(15) 0.0206(17) 0.0200(16) 0.0002(13) 0.0038(12) -0.0003(13) C16 0.0167(17) 0.030(2) 0.0324(19) -0.0078(15) 0.0053(14) 0.0063(14) C17 0.029(2) 0.059(3) 0.045(2) -0.016(2) 0.0006(18) 0.019(2) C18 0.029(2) 0.034(2) 0.043(2) -0.0082(18) 0.0080(17) 0.0114(17) C19 0.032(2) 0.046(3) 0.061(3) -0.009(2) 0.024(2) 0.0073(19) C20 0.0137(14) 0.0115(15) 0.0157(15) -0.0002(12) 0.0054(12) -0.0019(11) C21 0.0138(15) 0.0219(17) 0.0184(15) 0.0015(13) 0.0056(12) 0.0027(13) C22 0.0223(16) 0.0176(16) 0.0150(15) 0.0015(12) 0.0044(12) -0.0002(13) C23 0.0177(16) 0.0192(16) 0.0188(16) -0.0016(13) 0.0082(12) 0.0000(13) C24 0.0176(16) 0.0228(18) 0.0267(18) -0.0015(14) 0.0048(13) -0.0008(13) C25 0.0163(15) 0.0186(16) 0.0147(15) 0.0016(12) 0.0018(12) 0.0002(12) C26 0.0209(17) 0.0267(18) 0.0237(17) 0.0021(14) 0.0096(13) -0.0043(14) C27 0.032(2) 0.065(3) 0.041(2) 0.008(2) 0.0153(18) -0.009(2) C28 0.048(2) 0.060(3) 0.029(2) -0.003(2) 0.0183(18) -0.013(2) C29 0.043(2) 0.039(2) 0.041(2) 0.0102(19) 0.0155(19) -0.0061(19) C30 0.0159(15) 0.0148(16) 0.0220(16) 0.0005(12) -0.0006(12) 0.0005(12) C31 0.0192(16) 0.0194(17) 0.0244(17) 0.0042(13) 0.0011(13) -0.0003(13) C32 0.0235(17) 0.0155(16) 0.0278(18) 0.0028(13) -0.0008(14) 0.0019(13) C33 0.0286(18) 0.0136(16) 0.036(2) -0.0005(14) -0.0035(15) 0.0057(14) C34 0.0235(17) 0.0209(18) 0.0274(18) -0.0036(14) -0.0034(14) 0.0010(14) C35 0.0236(17) 0.0216(17) 0.0220(17) 0.0016(14) -0.0001(13) 0.0031(14) C36 0.0292(19) 0.0247(19) 0.035(2) 0.0130(16) -0.0014(15) 0.0046(15) C37 0.039(2) 0.036(2) 0.041(2) 0.0177(18) 0.0062(18) 0.0060(18) C38 0.056(3) 0.027(2) 0.050(3) 0.0149(19) -0.004(2) -0.0076(19) C39 0.036(2) 0.037(2) 0.038(2) 0.0157(18) -0.0028(17) 0.0044(17) C40 0.038(2) 0.028(2) 0.031(2) -0.0074(16) 0.0012(16) 0.0108(17) C41 0.084(4) 0.040(3) 0.038(2) -0.013(2) 0.013(2) -0.007(2) C42 0.058(3) 0.070(3) 0.055(3) -0.014(3) 0.007(2) 0.030(3) C43 0.040(2) 0.034(2) 0.049(2) -0.0094(19) 0.0185(19) 0.0056(18) C44 0.0151(15) 0.0207(17) 0.0162(15) 0.0010(12) 0.0018(12) -0.0017(12) C45 0.0177(15) 0.0184(16) 0.0167(15) 0.0002(12) 0.0019(12) 0.0015(13) C46 0.0168(15) 0.0141(15) 0.0183(15) 0.0037(12) 0.0027(12) 0.0025(12) C47 0.0168(15) 0.0154(15) 0.0181(15) -0.0006(12) 0.0037(12) -0.0014(12) C48 0.0140(15) 0.0181(16) 0.0182(15) 0.0032(12) 0.0018(12) 0.0002(12) C49 0.0158(15) 0.0174(16) 0.0178(15) 0.0034(12) 0.0023(12) -0.0012(12) C50 0.0152(15) 0.0166(16) 0.0174(15) 0.0032(12) 0.0006(12) 0.0003(12) C51 0.0135(15) 0.0210(17) 0.0197(16) -0.0010(13) 0.0053(12) 0.0035(13) C52 0.0170(15) 0.0190(17) 0.0205(16) 0.0024(13) 0.0025(12) 0.0001(13) C53 0.0199(16) 0.0182(16) 0.0154(15) -0.0015(12) 0.0050(12) -0.0017(13) C54 0.0169(15) 0.0204(17) 0.0211(16) -0.0010(13) 0.0028(13) -0.0020(13) C55 0.0235(17) 0.0243(18) 0.0166(16) -0.0007(13) 0.0035(13) -0.0037(14) C56 0.0224(17) 0.0216(17) 0.0189(16) -0.0040(13) 0.0050(13) -0.0048(13) C57 0.0131(15) 0.0297(19) 0.0195(16) -0.0011(14) 0.0035(12) -0.0012(13) C58 0.0197(16) 0.0249(18) 0.0195(16) -0.0012(13) 0.0040(13) -0.0016(14) C59 0.0266(18) 0.037(2) 0.0233(18) 0.0030(15) 0.0112(14) -0.0092(16) C60 0.049(3) 0.070(3) 0.035(2) -0.009(2) 0.017(2) -0.005(2) C61 0.054(3) 0.061(3) 0.067(3) 0.018(3) 0.022(3) -0.012(2) C62 0.037(2) 0.098(4) 0.044(3) 0.008(3) 0.013(2) -0.018(3) C63 0.0147(15) 0.0174(16) 0.0210(16) -0.0024(13) 0.0047(12) -0.0026(12) C64 0.0193(17) 0.036(2) 0.0219(17) -0.0053(15) 0.0005(13) 0.0012(15) C65 0.0224(18) 0.053(3) 0.032(2) -0.0204(18) 0.0008(15) 0.0054(17) C66 0.0164(17) 0.043(2) 0.040(2) -0.0249(18) -0.0029(15) 0.0068(16) C67 0.0186(17) 0.030(2) 0.035(2) -0.0055(16) -0.0027(14) 0.0053(15) C68 0.0201(17) 0.0271(19) 0.0235(17) -0.0022(14) 0.0034(13) 0.0018(14) C69 0.026(2) 0.107(4) 0.069(3) -0.056(3) -0.009(2) 0.020(3) C70 0.051(3) 0.052(3) 0.047(3) -0.016(2) -0.002(2) 0.021(2) C71 0.039(6) 0.116(10) 0.23(2) -0.037(13) 0.025(8) 0.008(6) C72 0.050(5) 0.052(5) 0.051(4) -0.012(4) 0.000(3) 0.021(3) C71' 0.039(6) 0.116(10) 0.23(2) -0.037(13) 0.025(8) 0.008(6) C72' 0.050(5) 0.052(5) 0.051(4) -0.012(4) 0.000(3) 0.021(3) C73 0.0195(16) 0.0171(16) 0.0217(16) 0.0017(13) 0.0013(13) 0.0036(13) C74 0.0223(17) 0.0188(17) 0.0223(17) 0.0020(13) 0.0025(13) -0.0007(13) C75 0.0217(17) 0.0225(18) 0.0264(18) -0.0020(14) -0.0006(14) 0.0033(14) C76 0.0250(17) 0.0124(16) 0.0307(19) 0.0062(13) -0.0003(14) 0.0059(13) C77 0.0237(17) 0.0209(18) 0.0288(18) 0.0056(14) 0.0043(14) 0.0002(14) C78 0.0196(16) 0.0196(17) 0.0278(18) 0.0048(14) 0.0010(13) 0.0010(13) C79 0.0193(17) 0.0223(18) 0.0347(19) -0.0025(15) 0.0009(14) 0.0011(14) C80 0.0217(19) 0.034(2) 0.069(3) -0.003(2) 0.0112(19) -0.0018(16) C81 0.027(2) 0.053(3) 0.046(2) -0.008(2) -0.0027(17) 0.0110(19) C82 0.0275(19) 0.030(2) 0.045(2) -0.0028(17) 0.0043(17) 0.0048(16) C83 0.030(2) 0.024(2) 0.050(2) 0.0105(17) 0.0021(17) -0.0033(16) C84 0.100(4) 0.063(4) 0.065(3) 0.019(3) 0.019(3) -0.029(3) C85 0.053(3) 0.022(2) 0.139(5) 0.012(3) 0.021(3) 0.000(2) C86 0.038(2) 0.038(3) 0.099(4) 0.029(3) 0.007(2) -0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.378(4) . ? C1 C2 1.440(4) . ? C1 C10 1.493(4) . ? C2 C3 1.373(4) . ? C2 C20 1.485(4) . ? C3 C4 1.422(4) . ? C3 H3 0.9500 . ? C4 C7 1.412(4) . ? C4 C5 1.438(4) . ? C5 C7 1.417(4) 3_557 ? C5 C6 1.423(4) . ? C6 H6 0.9500 . ? C7 C8 1.416(4) . ? C7 C5 1.417(4) 3_557 ? C8 C9 1.212(4) . ? C9 C30 1.444(4) . ? C10 C11 1.390(4) . ? C10 C15 1.403(4) . ? C11 C12 1.393(4) . ? C11 H11 0.9500 . ? C12 C13 1.373(4) . ? C12 H12 0.9500 . ? C13 C14 1.398(5) . ? C13 C16 1.541(4) . ? C14 C15 1.386(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C19 1.512(5) . ? C16 C18 1.515(5) . ? C16 C17 1.524(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C25 1.398(4) . ? C20 C21 1.399(4) . ? C21 C22 1.382(4) . ? C21 H21 0.9500 . ? C22 C23 1.397(4) . ? C22 H22 0.9500 . ? C23 C24 1.380(5) . ? C23 C26 1.538(4) . ? C24 C25 1.394(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C29 1.527(5) . ? C26 C27 1.532(5) . ? C26 C28 1.536(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.399(4) . ? C30 C35 1.411(4) . ? C31 C32 1.392(4) . ? C31 H31 0.9500 . ? C32 C33 1.408(5) . ? C32 C36 1.527(5) . ? C33 C34 1.381(5) . ? C33 H33 0.9500 . ? C34 C35 1.388(5) . ? C34 C40 1.532(5) . ? C35 H35 0.9500 . ? C36 C37 1.534(5) . ? C36 C39 1.545(5) . ? C36 C38 1.550(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C43 1.511(6) . ? C40 C41 1.523(6) . ? C40 C42 1.556(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C49 1.369(4) . ? C44 C45 1.452(4) . ? C44 C53 1.497(4) . ? C45 C46 1.353(4) . ? C45 C63 1.487(4) . ? C46 C47 1.418(4) . ? C46 H46 0.9500 . ? C47 C50 1.420(4) 3_657 ? C47 C48 1.421(4) . ? C48 C49 1.417(4) . ? C48 C50 1.420(4) . ? C49 H49 0.9500 . ? C50 C51 1.419(4) . ? C50 C47 1.420(4) 3_657 ? C51 C52 1.207(4) . ? C52 C73 1.431(4) . ? C53 C54 1.388(4) . ? C53 C58 1.389(4) . ? C54 C55 1.378(4) . ? C54 H54 0.9500 . ? C55 C56 1.400(4) . ? C55 H55 0.9500 . ? C56 C57 1.384(4) . ? C56 C59 1.532(4) . ? C57 C58 1.395(4) . ? C57 H57 0.9500 . ? C58 H58 0.9500 . ? C59 C60 1.500(5) . ? C59 C62 1.514(6) . ? C59 C61 1.539(6) . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.380(4) . ? C63 C68 1.393(4) . ? C64 C65 1.364(5) . ? C64 H64 0.9500 . ? C65 C66 1.405(5) . ? C65 H65 0.9500 . ? C66 C67 1.387(5) . ? C66 C69 1.528(5) . ? C67 C68 1.396(5) . ? C67 H67 0.9500 . ? C68 H68 0.9500 . ? C69 C71' 1.377(18) . ? C69 C72 1.429(10) . ? C69 C71 1.447(18) . ? C69 C70 1.453(6) . ? C69 C72' 1.825(13) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C71' H71D 0.9800 . ? C71' H71E 0.9800 . ? C71' H71F 0.9800 . ? C72' H72D 0.9800 . ? C72' H72E 0.9800 . ? C72' H72F 0.9800 . ? C73 C74 1.394(4) . ? C73 C78 1.398(4) . ? C74 C75 1.384(5) . ? C74 H74 0.9500 . ? C75 C76 1.398(5) . ? C75 C79 1.544(5) . ? C76 C77 1.391(5) . ? C76 H76 0.9500 . ? C77 C78 1.395(5) . ? C77 C83 1.526(5) . ? C78 H78 0.9500 . ? C79 C80 1.522(5) . ? C79 C81 1.525(5) . ? C79 C82 1.526(5) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 C86 1.527(6) . ? C83 C85 1.532(6) . ? C83 C84 1.537(7) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 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 C6 C1 C2 119.8(3) . . ? C6 C1 C10 117.1(3) . . ? C2 C1 C10 123.2(3) . . ? C3 C2 C1 118.3(3) . . ? C3 C2 C20 120.2(3) . . ? C1 C2 C20 121.3(3) . . ? C2 C3 C4 123.4(3) . . ? C2 C3 H3 118.3 . . ? C4 C3 H3 118.3 . . ? C7 C4 C3 122.3(3) . . ? C7 C4 C5 119.5(3) . . ? C3 C4 C5 118.1(3) . . ? C7 C5 C6 121.3(3) 3_557 . ? C7 C5 C4 120.7(3) 3_557 . ? C6 C5 C4 117.9(3) . . ? C1 C6 C5 122.5(3) . . ? C1 C6 H6 118.8 . . ? C5 C6 H6 118.8 . . ? C4 C7 C8 122.1(3) . . ? C4 C7 C5 119.7(3) . 3_557 ? C8 C7 C5 118.0(3) . 3_557 ? C9 C8 C7 171.9(3) . . ? C8 C9 C30 169.7(3) . . ? C11 C10 C15 118.0(3) . . ? C11 C10 C1 119.9(3) . . ? C15 C10 C1 122.0(3) . . ? C10 C11 C12 121.1(3) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 121.4(3) . . ? C13 C12 H12 119.3 . . ? C11 C12 H12 119.3 . . ? C12 C13 C14 117.6(3) . . ? C12 C13 C16 123.3(3) . . ? C14 C13 C16 119.1(3) . . ? C15 C14 C13 122.0(3) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 C10 119.9(3) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? C19 C16 C18 109.9(3) . . ? C19 C16 C17 107.0(3) . . ? C18 C16 C17 108.9(3) . . ? C19 C16 C13 109.0(3) . . ? C18 C16 C13 110.6(3) . . ? C17 C16 C13 111.4(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C25 C20 C21 117.7(3) . . ? C25 C20 C2 120.8(3) . . ? C21 C20 C2 121.4(3) . . ? C22 C21 C20 120.5(3) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 122.3(3) . . ? C21 C22 H22 118.8 . . ? C23 C22 H22 118.8 . . ? C24 C23 C22 116.8(3) . . ? C24 C23 C26 122.5(3) . . ? C22 C23 C26 120.8(3) . . ? C23 C24 C25 122.1(3) . . ? C23 C24 H24 118.9 . . ? C25 C24 H24 118.9 . . ? C24 C25 C20 120.6(3) . . ? C24 C25 H25 119.7 . . ? C20 C25 H25 119.7 . . ? C29 C26 C27 108.9(3) . . ? C29 C26 C28 109.6(3) . . ? C27 C26 C28 108.1(3) . . ? C29 C26 C23 109.0(3) . . ? C27 C26 C23 111.7(3) . . ? C28 C26 C23 109.5(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C35 119.4(3) . . ? C31 C30 C9 123.9(3) . . ? C35 C30 C9 116.8(3) . . ? C32 C31 C30 120.7(3) . . ? C32 C31 H31 119.6 . . ? C30 C31 H31 119.6 . . ? C31 C32 C33 117.8(3) . . ? C31 C32 C36 123.5(3) . . ? C33 C32 C36 118.7(3) . . ? C34 C33 C32 123.2(3) . . ? C34 C33 H33 118.4 . . ? C32 C33 H33 118.4 . . ? C33 C34 C35 117.9(3) . . ? C33 C34 C40 120.7(3) . . ? C35 C34 C40 121.4(3) . . ? C34 C35 C30 121.1(3) . . ? C34 C35 H35 119.5 . . ? C30 C35 H35 119.5 . . ? C32 C36 C37 113.1(3) . . ? C32 C36 C39 108.9(3) . . ? C37 C36 C39 107.5(3) . . ? C32 C36 C38 109.2(3) . . ? C37 C36 C38 108.3(3) . . ? C39 C36 C38 109.7(3) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C43 C40 C41 109.1(3) . . ? C43 C40 C34 113.3(3) . . ? C41 C40 C34 109.3(3) . . ? C43 C40 C42 106.4(4) . . ? C41 C40 C42 108.5(4) . . ? C34 C40 C42 110.1(3) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C49 C44 C45 119.1(3) . . ? C49 C44 C53 120.0(3) . . ? C45 C44 C53 120.9(3) . . ? C46 C45 C44 118.7(3) . . ? C46 C45 C63 119.5(3) . . ? C44 C45 C63 121.8(3) . . ? C45 C46 C47 123.4(3) . . ? C45 C46 H46 118.3 . . ? C47 C46 H46 118.3 . . ? C46 C47 C50 122.2(3) . 3_657 ? C46 C47 C48 117.6(3) . . ? C50 C47 C48 120.2(3) 3_657 . ? C49 C48 C50 121.2(3) . . ? C49 C48 C47 119.1(3) . . ? C50 C48 C47 119.6(3) . . ? C44 C49 C48 121.9(3) . . ? C44 C49 H49 119.0 . . ? C48 C49 H49 119.0 . . ? C51 C50 C48 121.2(3) . . ? C51 C50 C47 118.6(3) . 3_657 ? C48 C50 C47 120.1(3) . 3_657 ? C52 C51 C50 172.8(3) . . ? C51 C52 C73 172.0(3) . . ? C54 C53 C58 117.8(3) . . ? C54 C53 C44 121.8(3) . . ? C58 C53 C44 120.4(3) . . ? C55 C54 C53 121.0(3) . . ? C55 C54 H54 119.5 . . ? C53 C54 H54 119.5 . . ? C54 C55 C56 122.0(3) . . ? C54 C55 H55 119.0 . . ? C56 C55 H55 119.0 . . ? C57 C56 C55 116.6(3) . . ? C57 C56 C59 122.5(3) . . ? C55 C56 C59 120.9(3) . . ? C56 C57 C58 121.6(3) . . ? C56 C57 H57 119.2 . . ? C58 C57 H57 119.2 . . ? C53 C58 C57 120.9(3) . . ? C53 C58 H58 119.6 . . ? C57 C58 H58 119.6 . . ? C60 C59 C62 110.1(3) . . ? C60 C59 C56 109.3(3) . . ? C62 C59 C56 111.9(3) . . ? C60 C59 C61 109.6(4) . . ? C62 C59 C61 107.1(4) . . ? C56 C59 C61 108.8(3) . . ? 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 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C59 C62 H62A 109.5 . . ? C59 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C59 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C64 C63 C68 117.9(3) . . ? C64 C63 C45 122.3(3) . . ? C68 C63 C45 119.8(3) . . ? C65 C64 C63 121.6(3) . . ? C65 C64 H64 119.2 . . ? C63 C64 H64 119.2 . . ? C64 C65 C66 122.0(3) . . ? C64 C65 H65 119.0 . . ? C66 C65 H65 119.0 . . ? C67 C66 C65 116.3(3) . . ? C67 C66 C69 122.6(4) . . ? C65 C66 C69 121.1(3) . . ? C66 C67 C68 122.0(3) . . ? C66 C67 H67 119.0 . . ? C68 C67 H67 119.0 . . ? C63 C68 C67 120.2(3) . . ? C63 C68 H68 119.9 . . ? C67 C68 H68 119.9 . . ? C71' C69 C72 48.7(10) . . ? C71' C69 C71 56.9(11) . . ? C72 C69 C71 104.1(8) . . ? C71' C69 C70 130.3(9) . . ? C72 C69 C70 116.4(6) . . ? C71 C69 C70 99.0(8) . . ? C71' C69 C66 114.7(8) . . ? C72 C69 C66 115.7(5) . . ? C71 C69 C66 105.4(7) . . ? C70 C69 C66 113.4(4) . . ? C71' C69 C72' 88.6(12) . . ? C72 C69 C72' 39.9(6) . . ? C71 C69 C72' 141.7(8) . . ? C70 C69 C72' 91.1(5) . . ? C66 C69 C72' 104.1(5) . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? C69 C72 H72A 109.5 . . ? C69 C72 H72B 109.5 . . ? C69 C72 H72C 109.5 . . ? C69 C71' H71D 109.5 . . ? C69 C71' H71E 109.5 . . ? H71D C71' H71E 109.5 . . ? C69 C71' H71F 109.5 . . ? H71D C71' H71F 109.5 . . ? H71E C71' H71F 109.5 . . ? C69 C72' H72D 109.5 . . ? C69 C72' H72E 109.5 . . ? H72D C72' H72E 109.5 . . ? C69 C72' H72F 109.5 . . ? H72D C72' H72F 109.5 . . ? H72E C72' H72F 109.5 . . ? C74 C73 C78 120.6(3) . . ? C74 C73 C52 118.0(3) . . ? C78 C73 C52 121.3(3) . . ? C75 C74 C73 120.1(3) . . ? C75 C74 H74 120.0 . . ? C73 C74 H74 120.0 . . ? C74 C75 C76 118.3(3) . . ? C74 C75 C79 121.2(3) . . ? C76 C75 C79 120.5(3) . . ? C77 C76 C75 123.0(3) . . ? C77 C76 H76 118.5 . . ? C75 C76 H76 118.5 . . ? C76 C77 C78 117.6(3) . . ? C76 C77 C83 120.9(3) . . ? C78 C77 C83 121.5(3) . . ? C77 C78 C73 120.4(3) . . ? C77 C78 H78 119.8 . . ? C73 C78 H78 119.8 . . ? C80 C79 C81 108.2(3) . . ? C80 C79 C82 109.0(3) . . ? C81 C79 C82 109.2(3) . . ? C80 C79 C75 111.6(3) . . ? C81 C79 C75 108.4(3) . . ? C82 C79 C75 110.5(3) . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C79 C82 H82A 109.5 . . ? C79 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C79 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C77 C83 C86 112.1(3) . . ? C77 C83 C85 110.8(3) . . ? C86 C83 C85 107.5(4) . . ? C77 C83 C84 107.9(3) . . ? C86 C83 C84 108.8(4) . . ? C85 C83 C84 109.7(4) . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C83 C85 H85A 109.5 . . ? C83 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C83 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C83 C86 H86A 109.5 . . ? C83 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C83 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.43 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.685 _refine_diff_density_min -0.569 _refine_diff_density_rms 0.085