data_nan2 (Compound 1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H24.67 B0.67' _chemical_formula_weight 296.29 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' 'B' 'B' 0.0013 0.0007 '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 12.395(2) _cell_length_b 14.662(2) _cell_length_c 15.449(3) _cell_angle_alpha 83.122(4) _cell_angle_beta 81.769(3) _cell_angle_gamma 86.749(4) _cell_volume 2756.4(8) _cell_formula_units_Z 6 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1849 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.98 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.071 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 0.059 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9824 _exptl_absorpt_correction_T_max 0.9824 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5223 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.12 _reflns_number_total 5223 _reflns_number_gt 3697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1300P)^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 5223 _refine_ls_number_parameters 621 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1923 _refine_ls_wR_factor_gt 0.1705 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 C1A C 0.4416(3) 0.09980(18) 0.8568(3) 0.0421(12) Uani 1 1 d . . . C1 C 0.4777(4) 0.35750(19) 0.1545(4) 0.0645(16) Uani 1 1 d . . . C2A C 0.3709(3) 0.13177(18) 0.9265(3) 0.0477(13) Uani 1 1 d . . . H2AA H 0.3628 0.0955 0.9821 0.057 Uiso 1 1 calc R . . C2 C 0.4707(3) 0.38208(19) 0.2394(3) 0.0579(14) Uani 1 1 d . . . H2A H 0.5074 0.3446 0.2815 0.069 Uiso 1 1 calc R . . C3A C 0.3119(3) 0.21572(17) 0.9169(3) 0.0373(11) Uani 1 1 d . . . C3 C 0.4107(3) 0.46088(17) 0.2642(3) 0.0461(13) Uani 1 1 d . . . C4A C 0.3269(3) 0.26826(16) 0.8340(3) 0.0349(11) Uani 1 1 d . . . C4 C 0.3580(3) 0.51592(16) 0.2009(3) 0.0408(12) Uani 1 1 d . . . C5 C 0.3632(3) 0.49199(19) 0.1168(3) 0.0477(13) Uani 1 1 d . . . C5A C 0.3964(3) 0.23683(17) 0.7626(2) 0.0367(11) Uani 1 1 d . . . C6 C 0.4258(4) 0.4121(2) 0.0954(3) 0.0627(16) Uani 1 1 d . . . H6A H 0.4315 0.3962 0.0370 0.075 Uiso 1 1 calc R . . C6A C 0.4530(3) 0.15200(17) 0.7778(3) 0.0388(12) Uani 1 1 d . . . H6AA H 0.5014 0.1303 0.7306 0.047 Uiso 1 1 calc R . . C7A C 0.2386(4) 0.2478(2) 0.9930(3) 0.0580(14) Uani 1 1 d . . . H7AA H 0.2446 0.2044 1.0456 0.087 Uiso 1 1 calc R . . H7AB H 0.1631 0.2516 0.9804 0.087 Uiso 1 1 calc R . . H7AC H 0.2597 0.3087 1.0031 0.087 Uiso 1 1 calc R . . C7 C 0.4079(5) 0.4853(2) 0.3559(3) 0.0750(17) Uani 1 1 d . . . H7A H 0.4309 0.5485 0.3536 0.113 Uiso 1 1 calc R . . H7B H 0.4573 0.4431 0.3870 0.113 Uiso 1 1 calc R . . H7C H 0.3334 0.4803 0.3871 0.113 Uiso 1 1 calc R . . C8A C 0.4106(4) 0.29072(19) 0.6730(3) 0.0506(13) Uani 1 1 d . . . H8AA H 0.4211 0.3553 0.6788 0.076 Uiso 1 1 calc R . . H8AB H 0.3454 0.2862 0.6448 0.076 Uiso 1 1 calc R . . H8AC H 0.4745 0.2658 0.6369 0.076 Uiso 1 1 calc R . . C8 C 0.3057(4) 0.5480(2) 0.0487(3) 0.0704(16) Uani 1 1 d . . . H8A H 0.2281 0.5555 0.0713 0.106 Uiso 1 1 calc R . . H8B H 0.3137 0.5167 -0.0046 0.106 Uiso 1 1 calc R . . H8C H 0.3376 0.6086 0.0347 0.106 Uiso 1 1 calc R . . C9A C 0.5042(4) 0.0078(2) 0.8688(3) 0.0750(16) Uani 1 1 d . . . H9AA H 0.5157 -0.0194 0.8131 0.112 Uiso 1 1 calc R . . H9AB H 0.4623 -0.0337 0.9141 0.112 Uiso 1 1 calc R . . H9AC H 0.5750 0.0172 0.8869 0.112 Uiso 1 1 calc R . . C9 C 0.5445(4) 0.2707(2) 0.1289(4) 0.101(2) Uani 1 1 d . . . H9A H 0.5533 0.2289 0.1821 0.151 Uiso 1 1 calc R . . H9B H 0.6164 0.2881 0.0982 0.151 Uiso 1 1 calc R . . H9C H 0.5062 0.2399 0.0900 0.151 Uiso 1 1 calc R . . C10A C 0.2649(3) 0.35942(16) 0.8190(2) 0.0360(11) Uani 1 1 d . . . C10 C 0.2945(3) 0.60236(17) 0.2259(3) 0.0385(12) Uani 1 1 d . . . C11A C 0.1683(3) 0.36501(16) 0.7865(3) 0.0414(11) Uani 1 1 d . . . H11A H 0.1380 0.3102 0.7752 0.050 Uiso 1 1 calc R . . C11 C 0.3442(3) 0.68715(17) 0.2000(3) 0.0435(12) Uani 1 1 d . . . H11B H 0.4144 0.6897 0.1660 0.052 Uiso 1 1 calc R . . C12A C 0.1119(3) 0.44962(16) 0.7690(3) 0.0438(12) Uani 1 1 d . . . H12A H 0.0446 0.4519 0.7460 0.053 Uiso 1 1 calc R . . C12 C 0.2887(3) 0.76742(17) 0.2251(3) 0.0411(12) Uani 1 1 d . . . H12B H 0.3232 0.8243 0.2086 0.049 Uiso 1 1 calc R . . C13A C 0.1565(3) 0.53133(15) 0.7861(3) 0.0400(11) Uani 1 1 d . . . C13 C 0.1855(3) 0.76742(16) 0.2729(3) 0.0365(12) Uani 1 1 d . . . C14A C 0.2533(3) 0.52424(16) 0.8197(2) 0.0376(11) Uani 1 1 d . . . H14A H 0.2828 0.5785 0.8329 0.045 Uiso 1 1 calc R . . C14 C 0.1344(3) 0.68195(16) 0.2942(3) 0.0430(12) Uani 1 1 d . . . H14B H 0.0619 0.6795 0.3240 0.052 Uiso 1 1 calc R . . C15A C 0.3108(3) 0.43982(16) 0.8356(3) 0.0408(12) Uani 1 1 d . . . H15A H 0.3792 0.4373 0.8570 0.049 Uiso 1 1 calc R . . C15 C 0.1914(4) 0.60112(17) 0.2709(3) 0.0422(12) Uani 1 1 d . . . H15B H 0.1573 0.5440 0.2869 0.051 Uiso 1 1 calc R . . C16A C 0.1139(3) 0.70778(15) 0.8197(3) 0.0402(12) Uani 1 1 d . . . C16 C 0.0026(3) 0.87021(16) 0.3314(2) 0.0370(11) Uani 1 1 d . . . C17 C -0.0659(3) 0.87216(17) 0.2657(2) 0.0331(7) Uiso 1 1 d . . . C17A C 0.1571(3) 0.79189(17) 0.7763(3) 0.0436(13) Uani 1 1 d . . . C18 C -0.1756(3) 0.89684(17) 0.2816(3) 0.0429(11) Uani 1 1 d . . . H18A H -0.2190 0.8997 0.2353 0.051 Uiso 1 1 calc R . . C18A C 0.1812(4) 0.85831(18) 0.8280(3) 0.0477(13) Uani 1 1 d . . . H18B H 0.2108 0.9141 0.7992 0.057 Uiso 1 1 calc R . . C19 C -0.2241(3) 0.91782(17) 0.3654(3) 0.0419(11) Uani 1 1 d . . . C19A C 0.1641(4) 0.8465(2) 0.9176(3) 0.0604(15) Uani 1 1 d . . . C20 C -0.1580(3) 0.91206(16) 0.4311(3) 0.0363(11) Uani 1 1 d . . . H20A H -0.1897 0.9249 0.4883 0.044 Uiso 1 1 calc R . . C20A C 0.1198(3) 0.7650(2) 0.9602(3) 0.0462(13) Uani 1 1 d . . . H20B H 0.1072 0.7558 1.0227 0.055 Uiso 1 1 calc R . . C21 C -0.0466(3) 0.88814(15) 0.4168(2) 0.0346(10) Uani 1 1 d . . . C21A C 0.0936(3) 0.69642(17) 0.9114(3) 0.0416(12) Uani 1 1 d . . . C22 C 0.0160(3) 0.87966(18) 0.4937(3) 0.0405(11) Uani 1 1 d . . . H22A H 0.0458 0.8165 0.5038 0.061 Uiso 1 1 calc R . . H22B H -0.0328 0.8947 0.5463 0.061 Uiso 1 1 calc R . . H22C H 0.0759 0.9222 0.4814 0.061 Uiso 1 1 calc R . . C22A C 0.1821(5) 0.8113(2) 0.6790(3) 0.0590(14) Uani 1 1 d . . . H22D H 0.1961 0.8767 0.6631 0.089 Uiso 1 1 calc R . . H22E H 0.1198 0.7956 0.6518 0.089 Uiso 1 1 calc R . . H22F H 0.2468 0.7743 0.6579 0.089 Uiso 1 1 calc R . . C23 C -0.0184(4) 0.8568(2) 0.1709(3) 0.0547(13) Uani 1 1 d . . . H23A H -0.0775 0.8446 0.1385 0.082 Uiso 1 1 calc R . . H23B H 0.0340 0.8042 0.1718 0.082 Uiso 1 1 calc R . . H23C H 0.0187 0.9119 0.1419 0.082 Uiso 1 1 calc R . . C23A C 0.0415(3) 0.61173(17) 0.9639(3) 0.0473(12) Uani 1 1 d . . . H23D H 0.0181 0.6241 1.0249 0.071 Uiso 1 1 calc R . . H23E H 0.0947 0.5597 0.9630 0.071 Uiso 1 1 calc R . . H23F H -0.0219 0.5969 0.9377 0.071 Uiso 1 1 calc R . . C24A C 0.1931(5) 0.9197(3) 0.9711(3) 0.087(2) Uani 1 1 d . . . H24A H 0.2366 0.9658 0.9323 0.131 Uiso 1 1 calc R . . H24B H 0.2353 0.8912 1.0169 0.131 Uiso 1 1 calc R . . H24C H 0.1260 0.9492 0.9985 0.131 Uiso 1 1 calc R . . C24 C -0.3414(4) 0.9492(2) 0.3809(3) 0.0608(14) Uani 1 1 d . . . H24D H -0.3501 0.9969 0.4210 0.091 Uiso 1 1 calc R . . H24E H -0.3856 0.8970 0.4072 0.091 Uiso 1 1 calc R . . H24F H -0.3653 0.9743 0.3248 0.091 Uiso 1 1 calc R . . C25A C 0.1926(4) 0.5940(2) 0.5788(3) 0.0595(14) Uani 1 1 d . . . H25A H 0.2111 0.5919 0.5152 0.089 Uiso 1 1 calc R . . H25B H 0.2108 0.5341 0.6099 0.089 Uiso 1 1 calc R . . H25C H 0.2342 0.6415 0.5972 0.089 Uiso 1 1 calc R . . C25 C 0.3056(3) 0.81649(18) 0.4324(3) 0.0487(12) Uani 1 1 d . . . H25D H 0.2346 0.7944 0.4609 0.073 Uiso 1 1 calc R . . H25E H 0.3528 0.8213 0.4773 0.073 Uiso 1 1 calc R . . H25F H 0.3395 0.7732 0.3919 0.073 Uiso 1 1 calc R . . C26A C -0.1459(3) 0.66848(19) 0.7933(3) 0.0489(13) Uani 1 1 d . . . H26A H -0.2212 0.6911 0.7898 0.073 Uiso 1 1 calc R . . H26B H -0.1075 0.7129 0.8191 0.073 Uiso 1 1 calc R . . H26C H -0.1460 0.6093 0.8303 0.073 Uiso 1 1 calc R . . C26 C 0.1140(4) 1.05386(19) 0.2270(3) 0.0692(15) Uani 1 1 d . . . H26D H 0.1170 1.1203 0.2096 0.104 Uiso 1 1 calc R . . H26E H 0.0412 1.0393 0.2578 0.104 Uiso 1 1 calc R . . H26F H 0.1290 1.0214 0.1744 0.104 Uiso 1 1 calc R . . C27A C -0.1710(5) 0.6551(3) 0.4734(3) 0.0861(19) Uani 1 1 d . . . H27A H -0.2488 0.6512 0.4960 0.129 Uiso 1 1 calc R . . H27B H -0.1487 0.6058 0.4362 0.129 Uiso 1 1 calc R . . H27C H -0.1579 0.7148 0.4386 0.129 Uiso 1 1 calc R . . C27 C 0.4275(4) 1.1407(2) 0.3692(3) 0.0747(17) Uani 1 1 d . . . H27D H 0.5025 1.1149 0.3626 0.112 Uiso 1 1 calc R . . H27E H 0.4079 1.1588 0.4286 0.112 Uiso 1 1 calc R . . H27F H 0.4220 1.1947 0.3258 0.112 Uiso 1 1 calc R . . C28A C 0.0253(3) 0.63523(15) 0.6865(2) 0.0340(10) Uani 1 1 d . . . C28 C 0.2086(3) 0.93233(17) 0.3277(2) 0.0325(7) Uiso 1 1 d . . . C29A C -0.0880(3) 0.65611(15) 0.7011(2) 0.0370(11) Uani 1 1 d . . . C29 C 0.1976(3) 1.02416(17) 0.2868(3) 0.0475(12) Uani 1 1 d . . . C30A C -0.1514(3) 0.66111(17) 0.6331(3) 0.0452(12) Uani 1 1 d . . . H30A H -0.2274 0.6757 0.6450 0.054 Uiso 1 1 calc R . . C30 C 0.2706(3) 1.08891(17) 0.3009(3) 0.0477(12) Uani 1 1 d . . . H30B H 0.2650 1.1496 0.2722 0.057 Uiso 1 1 calc R . . C31A C -0.1066(4) 0.6453(2) 0.5483(3) 0.0578(14) Uani 1 1 d . . . C31 C 0.3492(3) 1.06805(18) 0.3542(3) 0.0447(13) Uani 1 1 d . . . C32A C 0.0056(4) 0.62158(19) 0.5352(3) 0.0578(14) Uani 1 1 d . . . H32A H 0.0380 0.6084 0.4783 0.069 Uiso 1 1 calc R . . C32 C 0.3601(3) 0.97834(18) 0.3944(3) 0.0414(12) Uani 1 1 d . . . H32B H 0.4154 0.9626 0.4309 0.050 Uiso 1 1 calc R . . C33A C 0.0710(3) 0.61649(16) 0.6007(3) 0.0449(12) Uani 1 1 d . . . C33 C 0.2897(3) 0.91116(17) 0.3810(2) 0.0365(11) Uani 1 1 d . . . B1A B 0.0956(4) 0.62715(18) 0.7628(3) 0.0399(13) Uani 1 1 d . . . B1 B 0.1283(4) 0.85616(19) 0.3109(3) 0.0369(12) 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 C1A 0.041(3) 0.0314(14) 0.051(3) -0.0046(15) -0.006(3) 0.0137(14) C1 0.048(3) 0.0253(14) 0.112(5) -0.0048(19) 0.014(3) 0.0063(14) C2A 0.060(3) 0.0340(14) 0.044(3) -0.0002(15) -0.001(3) 0.0154(15) C2 0.043(3) 0.0304(15) 0.094(4) 0.0083(18) -0.006(3) 0.0064(14) C3A 0.035(3) 0.0297(13) 0.041(3) 0.0006(14) 0.008(2) 0.0042(13) C3 0.044(3) 0.0276(13) 0.061(3) 0.0086(15) 0.002(3) -0.0053(13) C4A 0.033(3) 0.0240(12) 0.047(3) -0.0056(14) -0.004(2) 0.0052(12) C4 0.037(3) 0.0241(12) 0.060(3) -0.0049(14) -0.002(2) 0.0025(12) C5 0.046(3) 0.0348(14) 0.061(3) -0.0102(16) -0.004(3) 0.0066(14) C5A 0.035(3) 0.0281(13) 0.044(3) -0.0031(14) 0.002(2) 0.0030(13) C6 0.061(4) 0.0386(16) 0.086(4) -0.0233(19) 0.011(3) 0.0047(17) C6A 0.030(3) 0.0367(14) 0.049(3) -0.0115(15) -0.002(2) 0.0097(14) C7A 0.071(4) 0.0418(16) 0.053(3) -0.0006(16) 0.009(3) 0.0175(17) C7 0.100(5) 0.0511(19) 0.077(4) 0.002(2) -0.033(3) 0.004(2) C8A 0.056(3) 0.0473(17) 0.041(3) 0.0050(16) 0.006(3) 0.0088(16) C8 0.081(4) 0.068(2) 0.066(4) -0.019(2) -0.023(3) 0.024(2) C9A 0.092(4) 0.0480(18) 0.078(4) -0.0047(18) -0.010(3) 0.043(2) C9 0.100(5) 0.0319(16) 0.148(6) -0.004(2) 0.045(4) 0.0233(19) C10A 0.034(3) 0.0250(12) 0.047(3) -0.0043(13) -0.002(2) 0.0066(12) C10 0.040(3) 0.0256(13) 0.048(3) -0.0059(14) -0.001(3) 0.0037(14) C11A 0.038(3) 0.0201(11) 0.066(3) -0.0022(13) -0.009(2) -0.0003(12) C11 0.042(3) 0.0320(13) 0.054(3) -0.0068(15) 0.003(3) 0.0022(13) C12A 0.043(3) 0.0254(12) 0.065(3) -0.0043(14) -0.016(2) 0.0072(12) C12 0.034(3) 0.0256(13) 0.061(3) -0.0062(15) 0.003(3) -0.0026(13) C13A 0.050(3) 0.0206(12) 0.046(3) 0.0009(13) 0.000(2) 0.0028(12) C13 0.028(3) 0.0263(13) 0.051(3) -0.0034(14) 0.005(3) -0.0023(13) C14A 0.040(3) 0.0233(12) 0.050(3) -0.0052(13) -0.008(2) 0.0036(12) C14 0.041(3) 0.0274(13) 0.060(3) -0.0058(14) -0.004(2) 0.0029(12) C15A 0.039(3) 0.0287(13) 0.055(3) -0.0055(14) -0.010(2) 0.0068(13) C15 0.045(3) 0.0254(13) 0.055(3) -0.0045(14) -0.003(3) 0.0013(14) C16A 0.055(3) 0.0215(12) 0.042(3) 0.0003(13) -0.007(3) 0.0117(12) C16 0.039(3) 0.0218(11) 0.048(3) -0.0060(13) 0.004(2) 0.0036(12) C17A 0.050(3) 0.0240(13) 0.053(4) 0.0011(15) 0.001(3) 0.0031(13) C18 0.049(3) 0.0286(13) 0.051(3) -0.0051(14) -0.009(2) 0.0023(13) C18A 0.057(3) 0.0278(13) 0.055(4) -0.0024(15) 0.002(3) -0.0037(14) C19 0.036(3) 0.0306(13) 0.059(3) -0.0105(15) -0.001(3) 0.0030(13) C19A 0.076(4) 0.0361(15) 0.070(4) -0.018(2) -0.005(3) 0.0001(17) C20 0.031(3) 0.0311(13) 0.044(3) -0.0080(14) 0.006(2) -0.0010(12) C20A 0.054(3) 0.0439(16) 0.037(3) -0.0077(17) 0.011(3) -0.0027(16) C21 0.035(3) 0.0222(11) 0.045(3) -0.0033(13) 0.000(2) 0.0022(12) C21A 0.046(3) 0.0258(13) 0.048(4) -0.0012(14) 0.006(3) 0.0081(12) C22 0.040(3) 0.0357(13) 0.043(3) -0.0052(14) 0.002(2) 0.0052(13) C22A 0.088(4) 0.0375(16) 0.050(4) 0.0110(16) -0.011(3) -0.0163(17) C23 0.060(4) 0.0509(17) 0.051(3) -0.0058(18) -0.001(3) -0.0050(17) C23A 0.062(3) 0.0321(14) 0.041(3) 0.0043(14) 0.007(3) 0.0036(14) C24A 0.140(6) 0.060(2) 0.061(4) -0.023(2) 0.010(4) -0.035(3) C24 0.042(3) 0.062(2) 0.080(4) -0.025(2) -0.007(3) 0.0129(17) C25A 0.064(4) 0.0452(17) 0.059(3) -0.0049(18) 0.022(3) 0.0015(17) C25 0.045(3) 0.0380(15) 0.059(3) -0.0021(15) -0.003(3) 0.0105(14) C26A 0.048(3) 0.0391(15) 0.057(3) -0.0019(16) -0.008(3) 0.0074(14) C26 0.081(4) 0.0320(15) 0.095(4) 0.0146(17) -0.029(3) -0.0028(16) C27A 0.137(6) 0.061(2) 0.070(4) 0.011(2) -0.052(4) -0.028(3) C27 0.073(4) 0.0460(18) 0.108(5) -0.018(2) -0.012(4) -0.0103(18) C28A 0.040(3) 0.0198(11) 0.040(3) 0.0012(12) -0.004(2) 0.0032(12) C29A 0.045(3) 0.0181(11) 0.045(3) 0.0067(12) -0.005(2) -0.0039(12) C29 0.050(3) 0.0265(13) 0.065(3) -0.0064(14) -0.008(3) 0.0068(13) C30A 0.046(3) 0.0292(13) 0.060(3) 0.0085(16) -0.016(3) -0.0090(13) C30 0.050(3) 0.0254(13) 0.063(3) 0.0003(14) 0.005(3) -0.0019(13) C31A 0.088(4) 0.0304(14) 0.059(4) 0.0063(17) -0.028(3) -0.0147(18) C31 0.043(3) 0.0341(14) 0.054(3) -0.0112(16) 0.010(3) -0.0032(14) C32A 0.096(4) 0.0327(15) 0.045(3) -0.0011(15) -0.012(3) -0.0067(18) C32 0.039(3) 0.0365(14) 0.046(3) -0.0115(15) 0.006(2) 0.0070(13) C33A 0.058(3) 0.0242(12) 0.050(3) -0.0014(14) -0.001(3) -0.0001(14) C33 0.038(3) 0.0309(13) 0.036(3) -0.0071(13) 0.010(2) 0.0069(12) B1A 0.046(3) 0.0233(13) 0.047(3) -0.0021(15) 0.002(3) 0.0065(14) B1 0.044(3) 0.0261(14) 0.036(3) 0.0019(14) 0.002(3) 0.0040(14) _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 C1A C6A 1.354(5) . ? C1A C2A 1.398(5) . ? C1A C9A 1.523(4) . ? C1 C6 1.351(7) . ? C1 C2 1.391(7) . ? C1 C9 1.539(4) . ? C2A C3A 1.399(4) . ? C2A H2AA 0.9500 . ? C2 C3 1.401(4) . ? C2 H2A 0.9500 . ? C3A C4A 1.406(5) . ? C3A C7A 1.486(5) . ? C3 C4 1.402(5) . ? C3 C7 1.498(6) . ? C4A C5A 1.407(5) . ? C4A C10A 1.513(4) . ? C4 C5 1.378(5) . ? C4 C10 1.514(4) . ? C5 C6 1.414(4) . ? C5 C8 1.494(6) . ? C5A C6A 1.404(4) . ? C5A C8A 1.501(5) . ? C6 H6A 0.9500 . ? C6A H6AA 0.9500 . ? C7A H7AA 0.9800 . ? C7A H7AB 0.9800 . ? C7A H7AC 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8A H8AA 0.9800 . ? C8A H8AB 0.9800 . ? C8A H8AC 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9A H9AA 0.9800 . ? C9A H9AB 0.9800 . ? C9A H9AC 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10A C11A 1.358(5) . ? C10A C15A 1.403(4) . ? C10 C15 1.364(5) . ? C10 C11 1.408(5) . ? C11A C12A 1.406(4) . ? C11A H11A 0.9500 . ? C11 C12 1.397(4) . ? C11 H11B 0.9500 . ? C12A C13A 1.415(4) . ? C12A H12A 0.9500 . ? C12 C13 1.382(5) . ? C12 H12B 0.9500 . ? C13A C14A 1.367(5) . ? C13A B1A 1.584(4) . ? C13 C14 1.419(4) . ? C13 B1 1.581(4) . ? C14A C15A 1.407(4) . ? C14A H14A 0.9500 . ? C14 C15 1.402(4) . ? C14 H14B 0.9500 . ? C15A H15A 0.9500 . ? C15 H15B 0.9500 . ? C16A C21A 1.395(5) . ? C16A C17A 1.425(5) . ? C16A B1A 1.599(4) . ? C16 C17 1.411(5) . ? C16 C21 1.420(5) . ? C16 B1 1.552(6) . ? C17 C18 1.382(5) . ? C17 C23 1.535(5) . ? C17A C18A 1.401(5) . ? C17A C22A 1.487(5) . ? C18 C19 1.409(5) . ? C18 H18A 0.9500 . ? C18A C19A 1.362(6) . ? C18A H18B 0.9500 . ? C19 C20 1.384(5) . ? C19 C24 1.495(5) . ? C19A C20A 1.394(6) . ? C19A C24A 1.517(5) . ? C20 C21 1.398(5) . ? C20 H20A 0.9500 . ? C20A C21A 1.405(5) . ? C20A H20B 0.9500 . ? C21 C22 1.499(5) . ? C21A C23A 1.522(5) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A H24A 0.9800 . ? C24A H24B 0.9800 . ? C24A H24C 0.9800 . ? C24 H24D 0.9800 . ? C24 H24E 0.9800 . ? C24 H24F 0.9800 . ? C25A C33A 1.523(5) . ? C25A H25A 0.9800 . ? C25A H25B 0.9800 . ? C25A H25C 0.9800 . ? C25 C33 1.531(5) . ? C25 H25D 0.9800 . ? C25 H25E 0.9800 . ? C25 H25F 0.9800 . ? C26A C29A 1.527(5) . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C26 C29 1.499(6) . ? C26 H26D 0.9800 . ? C26 H26E 0.9800 . ? C26 H26F 0.9800 . ? C27A C31A 1.485(6) . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C27 C31 1.540(5) . ? C27 H27D 0.9800 . ? C27 H27E 0.9800 . ? C27 H27F 0.9800 . ? C28A C29A 1.412(5) . ? C28A C33A 1.418(5) . ? C28A B1A 1.553(6) . ? C28 C33 1.387(5) . ? C28 C29 1.424(4) . ? C28 B1 1.605(5) . ? C29A C30A 1.393(5) . ? C29 C30 1.403(5) . ? C30A C31A 1.389(6) . ? C30A H30A 0.9500 . ? C30 C31 1.362(6) . ? C30 H30B 0.9500 . ? C31A C32A 1.406(6) . ? C31 C32 1.394(5) . ? C32A C33A 1.377(6) . ? C32A H32A 0.9500 . ? C32 C33 1.405(5) . ? C32 H32B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6A C1A C2A 118.7(3) . . ? C6A C1A C9A 120.5(3) . . ? C2A C1A C9A 120.8(4) . . ? C6 C1 C2 118.4(3) . . ? C6 C1 C9 121.2(5) . . ? C2 C1 C9 120.4(4) . . ? C1A C2A C3A 121.9(4) . . ? C1A C2A H2AA 119.1 . . ? C3A C2A H2AA 119.1 . . ? C1 C2 C3 121.5(4) . . ? C1 C2 H2A 119.3 . . ? C3 C2 H2A 119.3 . . ? C2A C3A C4A 117.6(3) . . ? C2A C3A C7A 120.2(3) . . ? C4A C3A C7A 122.1(3) . . ? C2 C3 C4 118.5(4) . . ? C2 C3 C7 119.2(4) . . ? C4 C3 C7 122.2(3) . . ? C3A C4A C5A 121.5(3) . . ? C3A C4A C10A 120.3(3) . . ? C5A C4A C10A 118.2(3) . . ? C5 C4 C3 120.8(3) . . ? C5 C4 C10 119.9(3) . . ? C3 C4 C10 119.3(3) . . ? C4 C5 C6 118.2(4) . . ? C4 C5 C8 122.0(3) . . ? C6 C5 C8 119.8(3) . . ? C6A C5A C4A 117.4(3) . . ? C6A C5A C8A 120.5(3) . . ? C4A C5A C8A 122.1(3) . . ? C1 C6 C5 122.7(4) . . ? C1 C6 H6A 118.6 . . ? C5 C6 H6A 118.6 . . ? C1A C6A C5A 123.0(3) . . ? C1A C6A H6AA 118.5 . . ? C5A C6A H6AA 118.5 . . ? C3A C7A H7AA 109.5 . . ? C3A C7A H7AB 109.5 . . ? H7AA C7A H7AB 109.5 . . ? C3A C7A H7AC 109.5 . . ? H7AA C7A H7AC 109.5 . . ? H7AB C7A H7AC 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5A C8A H8AA 109.5 . . ? C5A C8A H8AB 109.5 . . ? H8AA C8A H8AB 109.5 . . ? C5A C8A H8AC 109.5 . . ? H8AA C8A H8AC 109.5 . . ? H8AB C8A H8AC 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1A C9A H9AA 109.5 . . ? C1A C9A H9AB 109.5 . . ? H9AA C9A H9AB 109.5 . . ? C1A C9A H9AC 109.5 . . ? H9AA C9A H9AC 109.5 . . ? H9AB C9A H9AC 109.5 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11A C10A C15A 119.7(3) . . ? C11A C10A C4A 121.2(2) . . ? C15A C10A C4A 119.1(3) . . ? C15 C10 C11 119.3(3) . . ? C15 C10 C4 122.7(3) . . ? C11 C10 C4 118.0(4) . . ? C10A C11A C12A 121.8(3) . . ? C10A C11A H11A 119.1 . . ? C12A C11A H11A 119.1 . . ? C12 C11 C10 118.9(4) . . ? C12 C11 H11B 120.5 . . ? C10 C11 H11B 120.5 . . ? C11A C12A C13A 119.3(4) . . ? C11A C12A H12A 120.4 . . ? C13A C12A H12A 120.4 . . ? C13 C12 C11 122.7(3) . . ? C13 C12 H12B 118.7 . . ? C11 C12 H12B 118.7 . . ? C14A C13A C12A 118.1(3) . . ? C14A C13A B1A 122.5(3) . . ? C12A C13A B1A 119.3(4) . . ? C12 C13 C14 117.5(3) . . ? C12 C13 B1 122.7(3) . . ? C14 C13 B1 119.6(4) . . ? C13A C14A C15A 122.7(3) . . ? C13A C14A H14A 118.7 . . ? C15A C14A H14A 118.7 . . ? C15 C14 C13 119.7(4) . . ? C15 C14 H14B 120.2 . . ? C13 C14 H14B 120.2 . . ? C10A C15A C14A 118.4(4) . . ? C10A C15A H15A 120.8 . . ? C14A C15A H15A 120.8 . . ? C10 C15 C14 121.8(3) . . ? C10 C15 H15B 119.1 . . ? C14 C15 H15B 119.1 . . ? C21A C16A C17A 118.8(3) . . ? C21A C16A B1A 121.6(3) . . ? C17A C16A B1A 119.5(4) . . ? C17 C16 C21 117.6(3) . . ? C17 C16 B1 121.9(3) . . ? C21 C16 B1 120.3(3) . . ? C18 C17 C16 121.5(3) . . ? C18 C17 C23 117.4(3) . . ? C16 C17 C23 120.8(3) . . ? C18A C17A C16A 118.4(4) . . ? C18A C17A C22A 118.3(3) . . ? C16A C17A C22A 123.3(3) . . ? C17 C18 C19 121.0(4) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C19A C18A C17A 123.0(3) . . ? C19A C18A H18B 118.5 . . ? C17A C18A H18B 118.5 . . ? C20 C19 C18 117.6(3) . . ? C20 C19 C24 121.7(3) . . ? C18 C19 C24 120.7(4) . . ? C18A C19A C20A 118.7(3) . . ? C18A C19A C24A 121.2(4) . . ? C20A C19A C24A 120.1(5) . . ? C19 C20 C21 122.7(3) . . ? C19 C20 H20A 118.6 . . ? C21 C20 H20A 118.6 . . ? C19A C20A C21A 120.6(4) . . ? C19A C20A H20B 119.7 . . ? C21A C20A H20B 119.7 . . ? C20 C21 C16 119.4(3) . . ? C20 C21 C22 118.2(3) . . ? C16 C21 C22 122.3(3) . . ? C16A C21A C20A 120.5(3) . . ? C16A C21A C23A 123.0(3) . . ? C20A C21A C23A 116.5(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C17A C22A H22D 109.5 . . ? C17A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C17A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21A C23A H23D 109.5 . . ? C21A C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C21A C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? C19A C24A H24A 109.5 . . ? C19A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C19A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? C19 C24 H24D 109.5 . . ? C19 C24 H24E 109.5 . . ? H24D C24 H24E 109.5 . . ? C19 C24 H24F 109.5 . . ? H24D C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? C33A C25A H25A 109.5 . . ? C33A C25A H25B 109.5 . . ? H25A C25A H25B 109.5 . . ? C33A C25A H25C 109.5 . . ? H25A C25A H25C 109.5 . . ? H25B C25A H25C 109.5 . . ? C33 C25 H25D 109.5 . . ? C33 C25 H25E 109.5 . . ? H25D C25 H25E 109.5 . . ? C33 C25 H25F 109.5 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? C29A C26A H26A 109.5 . . ? C29A C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? C29A C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? C29 C26 H26D 109.5 . . ? C29 C26 H26E 109.5 . . ? H26D C26 H26E 109.5 . . ? C29 C26 H26F 109.5 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? C31A C27A H27A 109.5 . . ? C31A C27A H27B 109.5 . . ? H27A C27A H27B 109.5 . . ? C31A C27A H27C 109.5 . . ? H27A C27A H27C 109.5 . . ? H27B C27A H27C 109.5 . . ? C31 C27 H27D 109.5 . . ? C31 C27 H27E 109.5 . . ? H27D C27 H27E 109.5 . . ? C31 C27 H27F 109.5 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? C29A C28A C33A 117.3(3) . . ? C29A C28A B1A 121.3(3) . . ? C33A C28A B1A 121.3(3) . . ? C33 C28 C29 118.6(3) . . ? C33 C28 B1 121.6(3) . . ? C29 C28 B1 119.8(3) . . ? C30A C29A C28A 121.2(4) . . ? C30A C29A C26A 117.9(4) . . ? C28A C29A C26A 120.8(3) . . ? C30 C29 C28 118.6(4) . . ? C30 C29 C26 118.5(3) . . ? C28 C29 C26 122.8(3) . . ? C31A C30A C29A 121.8(4) . . ? C31A C30A H30A 119.1 . . ? C29A C30A H30A 119.1 . . ? C31 C30 C29 122.6(3) . . ? C31 C30 H30B 118.7 . . ? C29 C30 H30B 118.7 . . ? C30A C31A C32A 116.5(4) . . ? C30A C31A C27A 122.9(5) . . ? C32A C31A C27A 120.5(5) . . ? C30 C31 C32 119.0(3) . . ? C30 C31 C27 121.5(3) . . ? C32 C31 C27 119.5(4) . . ? C33A C32A C31A 123.4(4) . . ? C33A C32A H32A 118.3 . . ? C31A C32A H32A 118.3 . . ? C31 C32 C33 120.2(4) . . ? C31 C32 H32B 119.9 . . ? C33 C32 H32B 119.9 . . ? C32A C33A C28A 119.8(4) . . ? C32A C33A C25A 119.3(4) . . ? C28A C33A C25A 120.9(4) . . ? C28 C33 C32 121.0(3) . . ? C28 C33 C25 123.4(3) . . ? C32 C33 C25 115.5(4) . . ? C28A B1A C13A 117.7(3) . . ? C28A B1A C16A 125.8(2) . . ? C13A B1A C16A 116.5(3) . . ? C16 B1 C13 123.0(3) . . ? C16 B1 C28 121.2(2) . . ? C13 B1 C28 115.8(3) . . ? _diffrn_measured_fraction_theta_max 0.429 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.429 _refine_diff_density_max 0.269 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.051 data_nan3 (Compound 2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H41 B' _chemical_formula_weight 520.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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 18.0451(9) _cell_length_b 8.3350(4) _cell_length_c 20.4276(10) _cell_angle_alpha 90.00 _cell_angle_beta 93.244(4) _cell_angle_gamma 90.00 _cell_volume 3067.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1015 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 21.98 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1120 _exptl_absorpt_coefficient_mu 0.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9845 _exptl_absorpt_correction_T_max 0.9938 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13293 _diffrn_reflns_av_R_equivalents 0.0658 _diffrn_reflns_av_sigmaI/netI 0.1001 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6005 _reflns_number_gt 2978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0750P)^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 6005 _refine_ls_number_parameters 370 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1431 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1795 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.997 _refine_ls_shift/su_max 0.134 _refine_ls_shift/su_mean 0.002 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 B1 B 0.69192(17) 0.7061(4) 0.50384(16) 0.0339(8) Uani 1 1 d . . . C1 C 1.21162(15) 1.5743(4) 0.71604(14) 0.0385(8) Uani 1 1 d . . . H1A H 1.2574 1.5465 0.7384 0.046 Uiso 1 1 calc R . . C2 C 1.19582(15) 1.7349(4) 0.70429(14) 0.0364(7) Uani 1 1 d . . . C3 C 1.12834(15) 1.7724(4) 0.67264(13) 0.0377(7) Uani 1 1 d . . . H3A H 1.1167 1.8816 0.6637 0.045 Uiso 1 1 calc R . . C4 C 1.07729(15) 1.6555(4) 0.65364(13) 0.0354(7) Uani 1 1 d . . . C5 C 1.09462(15) 1.4934(3) 0.66481(13) 0.0323(7) Uani 1 1 d . . . C6 C 1.16275(15) 1.4529(4) 0.69628(13) 0.0345(7) Uani 1 1 d . . . C7 C 1.00306(17) 1.7030(4) 0.62171(17) 0.0560(9) Uani 1 1 d . . . H7A H 1.0019 1.8193 0.6147 0.084 Uiso 1 1 calc R . . H7B H 0.9635 1.6726 0.6503 0.084 Uiso 1 1 calc R . . H7C H 0.9955 1.6480 0.5795 0.084 Uiso 1 1 calc R . . C8 C 1.18373(16) 1.2794(4) 0.70816(16) 0.0469(8) Uani 1 1 d . . . H8A H 1.2310 1.2741 0.7341 0.070 Uiso 1 1 calc R . . H8B H 1.1888 1.2254 0.6660 0.070 Uiso 1 1 calc R . . H8C H 1.1450 1.2263 0.7320 0.070 Uiso 1 1 calc R . . C9 C 1.25072(18) 1.8634(4) 0.72544(16) 0.0519(9) Uani 1 1 d . . . H9A H 1.2579 1.9362 0.6886 0.078 Uiso 1 1 calc R . . H9B H 1.2982 1.8137 0.7394 0.078 Uiso 1 1 calc R . . H9C H 1.2318 1.9240 0.7621 0.078 Uiso 1 1 calc R . . C10 C 1.04169(15) 1.2986(4) 0.58098(15) 0.0421(8) Uani 1 1 d . . . H10A H 1.0794 1.3294 0.5529 0.051 Uiso 1 1 calc R . . C11 C 0.98941(15) 1.1869(4) 0.55933(14) 0.0401(8) Uani 1 1 d . . . H11A H 0.9918 1.1425 0.5167 0.048 Uiso 1 1 calc R . . C12 C 0.93309(14) 1.1379(3) 0.59896(13) 0.0327(7) Uani 1 1 d . . . C13 C 0.93329(15) 1.2026(4) 0.66156(14) 0.0404(8) Uani 1 1 d . . . H13A H 0.8968 1.1690 0.6904 0.048 Uiso 1 1 calc R . . C14 C 0.98562(16) 1.3152(4) 0.68277(14) 0.0425(8) Uani 1 1 d . . . H14A H 0.9839 1.3579 0.7258 0.051 Uiso 1 1 calc R . . C15 C 1.04035(15) 1.3670(3) 0.64299(14) 0.0336(7) Uani 1 1 d . . . C16 C 0.85156(15) 1.0185(3) 0.50799(14) 0.0355(7) Uani 1 1 d . . . H16A H 0.8762 1.0829 0.4776 0.043 Uiso 1 1 calc R . . C17 C 0.79404(15) 0.9197(3) 0.48566(14) 0.0363(7) Uani 1 1 d . . . H17A H 0.7798 0.9187 0.4402 0.044 Uiso 1 1 calc R . . C18 C 0.75610(14) 0.8208(3) 0.52813(13) 0.0319(7) Uani 1 1 d . . . C19 C 0.78063(15) 0.8268(3) 0.59439(13) 0.0344(7) Uani 1 1 d . . . H19A H 0.7572 0.7597 0.6247 0.041 Uiso 1 1 calc R . . C20 C 0.83751(14) 0.9264(3) 0.61743(13) 0.0334(7) Uani 1 1 d . . . H20A H 0.8518 0.9274 0.6629 0.040 Uiso 1 1 calc R . . C21 C 0.87431(14) 1.0256(3) 0.57469(13) 0.0302(7) Uani 1 1 d . . . C22 C 0.61867(19) 1.0262(4) 0.46724(16) 0.0554(9) Uani 1 1 d . . . H22A H 0.5694 1.0762 0.4640 0.083 Uiso 1 1 calc R . . H22B H 0.6564 1.1066 0.4582 0.083 Uiso 1 1 calc R . . H22C H 0.6285 0.9832 0.5115 0.083 Uiso 1 1 calc R . . C23 C 0.66493(17) 0.4452(4) 0.40100(15) 0.0481(9) Uani 1 1 d . . . H23A H 0.6534 0.3797 0.3619 0.072 Uiso 1 1 calc R . . H23B H 0.6381 0.4033 0.4377 0.072 Uiso 1 1 calc R . . H23C H 0.7184 0.4415 0.4122 0.072 Uiso 1 1 calc R . . C24 C 0.5580(2) 0.8394(5) 0.23816(16) 0.0799(13) Uani 1 1 d . . . H24A H 0.5307 0.9411 0.2379 0.120 Uiso 1 1 calc R . . H24B H 0.5246 0.7530 0.2227 0.120 Uiso 1 1 calc R . . H24C H 0.5993 0.8479 0.2091 0.120 Uiso 1 1 calc R . . C25 C 0.64975(14) 0.7382(3) 0.43553(14) 0.0337(7) Uani 1 1 d . . . C26 C 0.64158(15) 0.6170(4) 0.38739(14) 0.0381(8) Uani 1 1 d . . . C27 C 0.61236(16) 0.6511(4) 0.32471(15) 0.0459(9) Uani 1 1 d . . . H27A H 0.6089 0.5675 0.2931 0.055 Uiso 1 1 calc R . . C28 C 0.58804(16) 0.8030(5) 0.30690(16) 0.0493(9) Uani 1 1 d . . . C29 C 0.59119(16) 0.9203(4) 0.35458(16) 0.0485(9) Uani 1 1 d . . . H29A H 0.5722 1.0240 0.3440 0.058 Uiso 1 1 calc R . . C30 C 0.62134(16) 0.8918(4) 0.41794(15) 0.0388(8) Uani 1 1 d . . . C32 C 0.80549(15) 0.4494(4) 0.53859(17) 0.0501(9) Uani 1 1 d . . . H32A H 0.8201 0.3467 0.5198 0.075 Uiso 1 1 calc R . . H32B H 0.8395 0.4761 0.5761 0.075 Uiso 1 1 calc R . . H32C H 0.8075 0.5337 0.5053 0.075 Uiso 1 1 calc R . . C33 C 0.54158(15) 0.6578(4) 0.55658(14) 0.0404(8) Uani 1 1 d . . . H33A H 0.4971 0.6262 0.5788 0.061 Uiso 1 1 calc R . . H33B H 0.5293 0.6680 0.5094 0.061 Uiso 1 1 calc R . . H33C H 0.5597 0.7610 0.5740 0.061 Uiso 1 1 calc R . . C34 C 0.61650(17) 0.1207(4) 0.64856(16) 0.0504(9) Uani 1 1 d . . . H34A H 0.5725 0.0727 0.6260 0.076 Uiso 1 1 calc R . . H34B H 0.6059 0.1453 0.6940 0.076 Uiso 1 1 calc R . . H34C H 0.6581 0.0450 0.6482 0.076 Uiso 1 1 calc R . . C35 C 0.67311(14) 0.5562(3) 0.54652(13) 0.0305(7) Uani 1 1 d . . . C36 C 0.60104(14) 0.5319(3) 0.56813(13) 0.0325(7) Uani 1 1 d . . . C37 C 0.58451(15) 0.3927(3) 0.60126(13) 0.0340(7) Uani 1 1 d . . . H37A H 0.5358 0.3789 0.6158 0.041 Uiso 1 1 calc R . . C38 C 0.63656(15) 0.2726(3) 0.61401(13) 0.0352(7) Uani 1 1 d . . . C39 C 0.70764(15) 0.2981(3) 0.59361(14) 0.0381(7) Uani 1 1 d . . . H39A H 0.7443 0.2178 0.6022 0.046 Uiso 1 1 calc R . . C40 C 0.72700(14) 0.4365(4) 0.56115(14) 0.0358(7) 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 B1 0.0316(17) 0.036(2) 0.0348(19) -0.0043(16) 0.0035(14) 0.0097(16) C1 0.0301(16) 0.044(2) 0.0416(18) 0.0003(15) 0.0024(13) 0.0000(15) C2 0.0336(16) 0.0341(19) 0.0420(18) -0.0032(15) 0.0066(13) -0.0040(14) C3 0.0386(17) 0.0346(19) 0.0403(18) 0.0041(14) 0.0052(14) 0.0028(15) C4 0.0306(15) 0.041(2) 0.0349(17) 0.0009(14) 0.0034(12) -0.0008(14) C5 0.0334(16) 0.0327(19) 0.0311(16) -0.0006(13) 0.0050(12) -0.0032(13) C6 0.0317(16) 0.0352(19) 0.0371(17) -0.0024(14) 0.0063(13) 0.0013(14) C7 0.0442(19) 0.050(2) 0.073(2) 0.0133(19) -0.0072(17) 0.0047(17) C8 0.0419(18) 0.039(2) 0.060(2) -0.0007(16) -0.0024(15) 0.0015(15) C9 0.051(2) 0.040(2) 0.064(2) -0.0009(17) 0.0003(17) -0.0074(17) C10 0.0361(17) 0.045(2) 0.0464(19) -0.0052(16) 0.0132(14) -0.0095(15) C11 0.0390(17) 0.0400(19) 0.0422(18) -0.0116(15) 0.0099(14) -0.0038(15) C12 0.0269(15) 0.0364(18) 0.0346(17) 0.0025(14) 0.0002(12) 0.0036(13) C13 0.0322(16) 0.053(2) 0.0370(18) 0.0016(15) 0.0075(13) -0.0106(15) C14 0.0410(17) 0.053(2) 0.0341(17) -0.0026(15) 0.0047(13) -0.0088(16) C15 0.0295(15) 0.0340(18) 0.0371(17) 0.0027(14) 0.0009(12) 0.0007(13) C16 0.0354(16) 0.0352(19) 0.0363(17) 0.0018(14) 0.0056(13) 0.0019(14) C17 0.0353(16) 0.0373(18) 0.0361(17) -0.0028(14) -0.0001(13) -0.0006(14) C18 0.0303(15) 0.0280(17) 0.0374(17) 0.0024(14) 0.0010(12) 0.0042(13) C19 0.0314(15) 0.0371(19) 0.0343(17) 0.0049(14) 0.0003(13) 0.0004(14) C20 0.0305(15) 0.0364(18) 0.0330(16) 0.0018(14) -0.0018(12) 0.0004(14) C21 0.0263(14) 0.0281(17) 0.0365(17) -0.0015(13) 0.0032(12) 0.0023(13) C22 0.060(2) 0.038(2) 0.068(2) 0.0024(18) -0.0047(18) 0.0103(17) C23 0.059(2) 0.043(2) 0.0434(19) -0.0099(16) 0.0093(15) -0.0079(17) C24 0.078(3) 0.118(4) 0.043(2) 0.017(2) -0.0100(19) 0.008(3) C25 0.0319(15) 0.0325(18) 0.0370(17) 0.0027(14) 0.0054(13) -0.0030(13) C26 0.0356(16) 0.043(2) 0.0369(18) 0.0006(15) 0.0105(13) -0.0046(14) C27 0.0396(18) 0.064(3) 0.0346(18) -0.0047(17) 0.0049(14) -0.0064(17) C28 0.0359(17) 0.073(3) 0.039(2) 0.0091(19) -0.0012(14) -0.0016(18) C29 0.0394(18) 0.055(2) 0.051(2) 0.0212(19) 0.0012(15) 0.0018(16) C30 0.0369(17) 0.0338(19) 0.0454(19) 0.0042(15) 0.0003(14) -0.0021(14) C32 0.0301(16) 0.044(2) 0.077(2) 0.0110(18) 0.0082(15) 0.0078(15) C33 0.0304(16) 0.049(2) 0.0416(18) 0.0019(15) 0.0017(13) 0.0081(14) C34 0.0463(19) 0.047(2) 0.058(2) 0.0106(17) 0.0028(16) -0.0060(16) C35 0.0293(15) 0.0302(17) 0.0315(16) 0.0008(13) -0.0016(12) 0.0005(13) C36 0.0312(15) 0.0347(18) 0.0313(16) -0.0035(14) -0.0021(12) 0.0012(14) C37 0.0313(15) 0.0417(19) 0.0291(16) -0.0002(14) 0.0021(12) -0.0022(14) C38 0.0377(16) 0.0346(18) 0.0330(16) 0.0031(14) -0.0011(13) -0.0018(14) C39 0.0348(16) 0.0330(18) 0.0461(19) 0.0053(15) -0.0010(14) 0.0048(14) C40 0.0285(15) 0.0349(18) 0.0438(18) 0.0023(15) 0.0013(13) -0.0004(14) _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 B1 C18 1.561(4) . ? B1 C35 1.572(4) . ? B1 C25 1.574(4) . ? C1 C2 1.386(4) . ? C1 C6 1.387(4) . ? C1 H1A 0.9500 . ? C2 C3 1.382(4) . ? C2 C9 1.506(4) . ? C3 C4 1.381(4) . ? C3 H3A 0.9500 . ? C4 C5 1.402(4) . ? C4 C7 1.509(4) . ? C5 C6 1.396(4) . ? C5 C15 1.489(4) . ? C6 C8 1.511(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.380(4) . ? C10 C15 1.391(4) . ? C10 H10A 0.9500 . ? C11 C12 1.396(4) . ? C11 H11A 0.9500 . ? C12 C13 1.388(4) . ? C12 C21 1.479(4) . ? C13 C14 1.383(4) . ? C13 H13A 0.9500 . ? C14 C15 1.383(4) . ? C14 H14A 0.9500 . ? C16 C17 1.382(4) . ? C16 C21 1.402(4) . ? C16 H16A 0.9500 . ? C17 C18 1.403(4) . ? C17 H17A 0.9500 . ? C18 C19 1.401(4) . ? C19 C20 1.382(4) . ? C19 H19A 0.9500 . ? C20 C21 1.398(4) . ? C20 H20A 0.9500 . ? C22 C30 1.509(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C26 1.514(4) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C28 1.507(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.412(4) . ? C25 C30 1.418(4) . ? C26 C27 1.386(4) . ? C27 C28 1.382(4) . ? C27 H27A 0.9500 . ? C28 C29 1.379(4) . ? C29 C30 1.396(4) . ? C29 H29A 0.9500 . ? C32 C40 1.518(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C36 1.510(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C38 1.504(4) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.411(3) . ? C35 C40 1.413(4) . ? C36 C37 1.384(4) . ? C37 C38 1.387(4) . ? C37 H37A 0.9500 . ? C38 C39 1.387(4) . ? C39 C40 1.385(4) . ? C39 H39A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C18 B1 C35 119.3(3) . . ? C18 B1 C25 119.4(3) . . ? C35 B1 C25 121.2(3) . . ? C2 C1 C6 122.2(3) . . ? C2 C1 H1A 118.9 . . ? C6 C1 H1A 118.9 . . ? C3 C2 C1 117.8(3) . . ? C3 C2 C9 121.4(3) . . ? C1 C2 C9 120.8(3) . . ? C4 C3 C2 121.9(3) . . ? C4 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? C3 C4 C5 119.6(3) . . ? C3 C4 C7 119.9(3) . . ? C5 C4 C7 120.5(3) . . ? C6 C5 C4 119.4(3) . . ? C6 C5 C15 120.9(3) . . ? C4 C5 C15 119.7(3) . . ? C1 C6 C5 119.1(3) . . ? C1 C6 C8 120.1(3) . . ? C5 C6 C8 120.8(3) . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 121.4(2) . . ? C11 C10 H10A 119.3 . . ? C15 C10 H10A 119.3 . . ? C10 C11 C12 121.2(3) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C13 C12 C11 117.2(3) . . ? C13 C12 C21 121.3(2) . . ? C11 C12 C21 121.5(2) . . ? C14 C13 C12 121.2(2) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C13 C14 C15 121.7(3) . . ? C13 C14 H14A 119.1 . . ? C15 C14 H14A 119.1 . . ? C14 C15 C10 117.2(3) . . ? C14 C15 C5 121.6(3) . . ? C10 C15 C5 121.2(2) . . ? C17 C16 C21 121.3(3) . . ? C17 C16 H16A 119.4 . . ? C21 C16 H16A 119.4 . . ? C16 C17 C18 122.0(3) . . ? C16 C17 H17A 119.0 . . ? C18 C17 H17A 119.0 . . ? C19 C18 C17 116.0(3) . . ? C19 C18 B1 121.2(2) . . ? C17 C18 B1 122.9(3) . . ? C20 C19 C18 122.6(3) . . ? C20 C19 H19A 118.7 . . ? C18 C19 H19A 118.7 . . ? C19 C20 C21 120.8(3) . . ? C19 C20 H20A 119.6 . . ? C21 C20 H20A 119.6 . . ? C20 C21 C16 117.3(3) . . ? C20 C21 C12 121.5(3) . . ? C16 C21 C12 121.2(2) . . ? C30 C22 H22A 109.5 . . ? C30 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C30 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C26 C23 H23A 109.5 . . ? C26 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C26 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C28 C24 H24A 109.5 . . ? C28 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C28 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 116.6(3) . . ? C26 C25 B1 121.5(3) . . ? C30 C25 B1 121.9(3) . . ? C27 C26 C25 121.1(3) . . ? C27 C26 C23 116.8(3) . . ? C25 C26 C23 122.1(3) . . ? C28 C27 C26 122.0(3) . . ? C28 C27 H27A 119.0 . . ? C26 C27 H27A 119.0 . . ? C29 C28 C27 117.6(3) . . ? C29 C28 C24 120.9(3) . . ? C27 C28 C24 121.5(3) . . ? C28 C29 C30 122.2(3) . . ? C28 C29 H29A 118.9 . . ? C30 C29 H29A 118.9 . . ? C29 C30 C25 120.4(3) . . ? C29 C30 C22 117.8(3) . . ? C25 C30 C22 121.7(3) . . ? C40 C32 H32A 109.5 . . ? C40 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C40 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C36 C33 H33A 109.5 . . ? C36 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C36 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C38 C34 H34A 109.5 . . ? C38 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C38 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C40 117.9(2) . . ? C36 C35 B1 121.3(2) . . ? C40 C35 B1 120.7(2) . . ? C37 C36 C35 120.1(3) . . ? C37 C36 C33 119.2(2) . . ? C35 C36 C33 120.7(3) . . ? C36 C37 C38 122.3(3) . . ? C36 C37 H37A 118.9 . . ? C38 C37 H37A 118.9 . . ? C39 C38 C37 117.5(3) . . ? C39 C38 C34 121.4(3) . . ? C37 C38 C34 121.2(3) . . ? C40 C39 C38 122.3(3) . . ? C40 C39 H39A 118.9 . . ? C38 C39 H39A 118.9 . . ? C39 C40 C35 120.0(2) . . ? C39 C40 C32 118.0(3) . . ? C35 C40 C32 121.9(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.211 _refine_diff_density_min -0.229 _refine_diff_density_rms 0.051 data_nan6a (Compound 3) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H45 B' _chemical_formula_weight 596.62 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' 'B' 'B' 0.0013 0.0007 '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 10.5203(4) _cell_length_b 11.1484(4) _cell_length_c 16.2389(6) _cell_angle_alpha 90.825(3) _cell_angle_beta 101.464(3) _cell_angle_gamma 111.939(2) _cell_volume 1723.15(11) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 1367 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 20.93 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9810 _exptl_absorpt_correction_T_max 0.9873 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17235 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.1257 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7401 _reflns_number_gt 3350 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0700P)^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 7401 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1684 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_ref 0.1762 _refine_ls_wR_factor_gt 0.1340 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 2.375 _refine_ls_shift/su_mean 0.033 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 B1 B 0.2880(3) 1.1859(3) 0.13200(19) 0.0383(8) Uani 1 1 d . . . C1 C 0.2536(3) -0.0971(3) 0.6051(2) 0.0554(9) Uani 1 1 d . . . H1A H 0.2657 -0.1583 0.5693 0.066 Uiso 1 1 calc R . . C2 C 0.2383(3) -0.1256(3) 0.6862(2) 0.0551(9) Uani 1 1 d . . . C3 C 0.2271(3) -0.0322(3) 0.73824(18) 0.0515(8) Uani 1 1 d . . . H3A H 0.2180 -0.0495 0.7944 0.062 Uiso 1 1 calc R . . C4 C 0.2287(3) 0.0867(3) 0.71102(17) 0.0438(7) Uani 1 1 d . . . C5 C 0.2374(3) 0.1105(2) 0.62784(17) 0.0399(7) Uani 1 1 d . . . C6 C 0.2519(3) 0.0173(3) 0.57482(17) 0.0436(7) Uani 1 1 d . . . C7 C 0.2718(4) 0.0421(3) 0.48643(18) 0.0622(9) Uani 1 1 d . . . H7A H 0.3254 -0.0063 0.4702 0.093 Uiso 1 1 calc R . . H7B H 0.3232 0.1352 0.4842 0.093 Uiso 1 1 calc R . . H7C H 0.1799 0.0136 0.4473 0.093 Uiso 1 1 calc R . . C8 C 0.2239(3) 0.1869(3) 0.77324(17) 0.0565(8) Uani 1 1 d . . . H8A H 0.1687 0.1426 0.8137 0.085 Uiso 1 1 calc R . . H8B H 0.1803 0.2418 0.7427 0.085 Uiso 1 1 calc R . . H8C H 0.3197 0.2410 0.8035 0.085 Uiso 1 1 calc R . . C9 C 0.2360(4) -0.2527(3) 0.7173(2) 0.0784(11) Uani 1 1 d . . . H9A H 0.2963 -0.2822 0.6905 0.118 Uiso 1 1 calc R . . H9B H 0.1396 -0.3178 0.7029 0.118 Uiso 1 1 calc R . . H9C H 0.2706 -0.2410 0.7787 0.118 Uiso 1 1 calc R . . C10 C 0.3344(3) 0.3538(2) 0.62051(16) 0.0448(7) Uani 1 1 d . . . H10A H 0.4078 0.3636 0.6681 0.054 Uiso 1 1 calc R . . C11 C 0.3326(3) 0.4613(3) 0.58011(16) 0.0450(7) Uani 1 1 d . . . H11A H 0.4048 0.5437 0.6007 0.054 Uiso 1 1 calc R . . C12 C 0.2278(3) 0.4522(2) 0.50998(15) 0.0365(6) Uani 1 1 d . . . C13 C 0.1205(3) 0.3305(2) 0.48443(16) 0.0404(7) Uani 1 1 d . . . H13A H 0.0452 0.3213 0.4382 0.048 Uiso 1 1 calc R . . C14 C 0.1219(3) 0.2236(3) 0.52522(16) 0.0428(7) Uani 1 1 d . . . H14A H 0.0467 0.1421 0.5068 0.051 Uiso 1 1 calc R . . C15 C 0.2305(3) 0.2312(2) 0.59269(15) 0.0361(6) Uani 1 1 d . . . C16 C 0.2343(3) 0.5638(2) 0.46058(16) 0.0367(7) Uani 1 1 d . . . C17 C 0.1143(3) 0.5826(3) 0.41969(16) 0.0384(6) Uani 1 1 d . . . H17A H 0.0250 0.5257 0.4272 0.046 Uiso 1 1 calc R . . C18 C 0.1218(3) 0.6813(2) 0.36888(16) 0.0386(7) Uani 1 1 d . . . H18A H 0.0377 0.6911 0.3423 0.046 Uiso 1 1 calc R . . C19 C 0.2493(3) 0.7674(2) 0.35530(16) 0.0368(7) Uani 1 1 d . . . C20 C 0.3695(3) 0.7507(3) 0.39804(18) 0.0479(8) Uani 1 1 d . . . H20A H 0.4590 0.8089 0.3916 0.057 Uiso 1 1 calc R . . C21 C 0.3617(3) 0.6518(3) 0.44959(18) 0.0474(8) Uani 1 1 d . . . H21A H 0.4460 0.6441 0.4781 0.057 Uiso 1 1 calc R . . C22 C 0.2591(3) 0.8723(2) 0.29893(16) 0.0355(6) Uani 1 1 d . . . C23 C 0.1498(3) 0.9150(3) 0.27621(17) 0.0443(7) Uani 1 1 d . . . H23A H 0.0668 0.8754 0.2968 0.053 Uiso 1 1 calc R . . C24 C 0.1590(3) 1.0136(3) 0.22447(17) 0.0432(7) Uani 1 1 d . . . H24A H 0.0832 1.0420 0.2122 0.052 Uiso 1 1 calc R . . C25 C 0.2755(3) 1.0729(3) 0.18960(16) 0.0380(7) Uani 1 1 d . . . C26 C 0.3843(3) 1.0278(3) 0.21192(16) 0.0413(7) Uani 1 1 d . . . H26A H 0.4657 1.0645 0.1893 0.050 Uiso 1 1 calc R . . C27 C 0.3770(3) 0.9317(3) 0.26583(16) 0.0399(7) Uani 1 1 d . . . H27A H 0.4543 0.9057 0.2805 0.048 Uiso 1 1 calc R . . C28 C 0.2964(3) 1.3260(3) 0.29743(16) 0.0562(9) Uani 1 1 d . . . H28A H 0.3366 1.4112 0.3301 0.084 Uiso 1 1 calc R . . H28B H 0.3723 1.3029 0.2850 0.084 Uiso 1 1 calc R . . H28C H 0.2422 1.2606 0.3302 0.084 Uiso 1 1 calc R . . C29 C 0.0899(3) 1.2164(3) -0.01984(15) 0.0462(7) Uani 1 1 d . . . H29A H 0.0113 1.2242 -0.0602 0.069 Uiso 1 1 calc R . . H29B H 0.0726 1.1243 -0.0153 0.069 Uiso 1 1 calc R . . H29C H 0.1769 1.2586 -0.0395 0.069 Uiso 1 1 calc R . . C30 C -0.0498(3) 1.5039(3) 0.15228(19) 0.0606(9) Uani 1 1 d . . . H30A H -0.0523 1.5207 0.2112 0.091 Uiso 1 1 calc R . . H30B H -0.1459 1.4598 0.1189 0.091 Uiso 1 1 calc R . . H30C H -0.0043 1.5865 0.1297 0.091 Uiso 1 1 calc R . . C31 C 0.1959(3) 1.2687(2) 0.13795(15) 0.0367(6) Uani 1 1 d . . . C32 C 0.1033(3) 1.2808(2) 0.06513(16) 0.0375(7) Uani 1 1 d . . . C33 C 0.0220(3) 1.3527(3) 0.07188(17) 0.0433(7) Uani 1 1 d . . . H33A H -0.0428 1.3567 0.0231 0.052 Uiso 1 1 calc R . . C34 C 0.0323(3) 1.4187(3) 0.14760(18) 0.0448(7) Uani 1 1 d . . . C35 C 0.1222(3) 1.4060(3) 0.21809(17) 0.0456(7) Uani 1 1 d . . . H35A H 0.1305 1.4505 0.2704 0.055 Uiso 1 1 calc R . . C36 C 0.2010(3) 1.3309(3) 0.21561(16) 0.0409(7) Uani 1 1 d . . . C37 C 0.2678(3) 0.9871(2) -0.00624(17) 0.0462(7) Uani 1 1 d . . . H37A H 0.3034 0.9263 -0.0281 0.069 Uiso 1 1 calc R . . H37B H 0.1845 0.9854 -0.0468 0.069 Uiso 1 1 calc R . . H37C H 0.2427 0.9614 0.0477 0.069 Uiso 1 1 calc R . . C38 C 0.5264(3) 1.4456(3) 0.14573(17) 0.0514(8) Uani 1 1 d . . . H38A H 0.5949 1.5283 0.1347 0.077 Uiso 1 1 calc R . . H38B H 0.5637 1.4199 0.1997 0.077 Uiso 1 1 calc R . . H38C H 0.4385 1.4557 0.1481 0.077 Uiso 1 1 calc R . . C39 C 0.6632(3) 1.3156(3) -0.10807(19) 0.0595(9) Uani 1 1 d . . . H39A H 0.7144 1.2578 -0.1066 0.089 Uiso 1 1 calc R . . H39B H 0.7303 1.4057 -0.0938 0.089 Uiso 1 1 calc R . . H39C H 0.6051 1.3065 -0.1648 0.089 Uiso 1 1 calc R . . C40 C 0.3913(3) 1.2168(2) 0.07074(15) 0.0348(6) Uani 1 1 d . . . C41 C 0.4986(3) 1.3420(2) 0.07553(16) 0.0381(7) Uani 1 1 d . . . C42 C 0.5830(3) 1.3703(3) 0.01821(18) 0.0446(7) Uani 1 1 d . . . H42A H 0.6526 1.4555 0.0221 0.053 Uiso 1 1 calc R . . C43 C 0.5704(3) 1.2796(3) -0.04487(17) 0.0420(7) Uani 1 1 d . . . C44 C 0.4697(3) 1.1564(3) -0.04877(17) 0.0408(7) Uani 1 1 d . . . H44A H 0.4610 1.0920 -0.0909 0.049 Uiso 1 1 calc R . . C45 C 0.3808(3) 1.1236(2) 0.00700(16) 0.0369(7) 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 B1 0.0342(16) 0.0392(18) 0.0340(17) 0.0007(15) -0.0006(15) 0.0098(14) C1 0.059(2) 0.0384(17) 0.059(2) 0.0018(16) -0.0010(17) 0.0146(15) C2 0.0500(18) 0.0409(18) 0.059(2) 0.0119(17) -0.0052(17) 0.0091(15) C3 0.0464(17) 0.0546(19) 0.0436(17) 0.0198(16) 0.0051(15) 0.0101(15) C4 0.0361(15) 0.0512(18) 0.0367(16) 0.0072(15) 0.0037(13) 0.0107(14) C5 0.0371(15) 0.0370(16) 0.0389(15) 0.0066(14) 0.0048(13) 0.0083(13) C6 0.0457(17) 0.0379(16) 0.0404(16) 0.0059(14) 0.0019(14) 0.0122(13) C7 0.082(2) 0.060(2) 0.0450(18) 0.0029(16) 0.0101(18) 0.0311(19) C8 0.0563(19) 0.068(2) 0.0425(17) 0.0134(16) 0.0097(16) 0.0217(17) C9 0.077(2) 0.051(2) 0.088(3) 0.0292(19) -0.004(2) 0.0130(18) C10 0.0442(16) 0.0407(17) 0.0425(16) 0.0054(14) -0.0019(14) 0.0143(14) C11 0.0477(17) 0.0344(15) 0.0453(16) 0.0057(14) -0.0003(14) 0.0123(13) C12 0.0408(15) 0.0369(15) 0.0335(14) 0.0049(13) 0.0087(13) 0.0166(13) C13 0.0390(15) 0.0408(16) 0.0373(15) 0.0085(13) 0.0025(13) 0.0134(13) C14 0.0389(15) 0.0399(16) 0.0440(16) 0.0076(14) 0.0039(14) 0.0114(13) C15 0.0375(15) 0.0362(15) 0.0337(14) 0.0063(12) 0.0085(13) 0.0126(12) C16 0.0401(15) 0.0364(15) 0.0352(15) 0.0062(13) 0.0103(13) 0.0153(13) C17 0.0371(15) 0.0414(15) 0.0384(15) 0.0064(13) 0.0112(13) 0.0152(13) C18 0.0379(15) 0.0423(16) 0.0388(15) 0.0089(14) 0.0069(14) 0.0195(13) C19 0.0392(15) 0.0369(15) 0.0363(15) 0.0035(13) 0.0053(13) 0.0184(13) C20 0.0381(16) 0.0445(17) 0.0593(19) 0.0199(15) 0.0113(15) 0.0130(14) C21 0.0374(16) 0.0501(18) 0.0561(18) 0.0186(16) 0.0060(15) 0.0201(14) C22 0.0390(15) 0.0352(15) 0.0332(14) 0.0064(12) 0.0060(13) 0.0163(13) C23 0.0392(16) 0.0495(17) 0.0452(17) 0.0142(15) 0.0103(14) 0.0172(14) C24 0.0412(16) 0.0518(18) 0.0427(16) 0.0144(15) 0.0090(14) 0.0245(14) C25 0.0394(15) 0.0441(16) 0.0322(14) 0.0051(13) 0.0079(13) 0.0179(13) C26 0.0425(16) 0.0477(17) 0.0380(15) 0.0101(14) 0.0118(14) 0.0203(14) C27 0.0431(16) 0.0468(17) 0.0383(15) 0.0107(14) 0.0111(14) 0.0255(14) C28 0.064(2) 0.070(2) 0.0391(16) -0.0001(15) 0.0046(16) 0.0351(18) C29 0.0479(17) 0.0477(17) 0.0401(16) 0.0035(14) 0.0016(14) 0.0193(14) C30 0.072(2) 0.070(2) 0.059(2) 0.0182(17) 0.0192(18) 0.0461(19) C31 0.0401(15) 0.0352(15) 0.0345(14) 0.0089(12) 0.0087(13) 0.0138(12) C32 0.0383(15) 0.0350(15) 0.0387(15) 0.0111(13) 0.0098(13) 0.0124(12) C33 0.0377(15) 0.0498(17) 0.0412(16) 0.0119(14) 0.0058(14) 0.0165(14) C34 0.0451(17) 0.0493(17) 0.0477(17) 0.0161(15) 0.0172(15) 0.0231(14) C35 0.0513(17) 0.0492(17) 0.0420(16) 0.0070(14) 0.0167(15) 0.0222(15) C36 0.0429(16) 0.0440(16) 0.0354(15) 0.0038(13) 0.0062(13) 0.0174(14) C37 0.0495(17) 0.0411(16) 0.0434(16) 0.0049(14) 0.0124(15) 0.0110(14) C38 0.0506(18) 0.0407(16) 0.0563(19) -0.0012(15) 0.0099(16) 0.0114(14) C39 0.059(2) 0.060(2) 0.060(2) 0.0131(17) 0.0261(18) 0.0165(17) C40 0.0404(15) 0.0348(15) 0.0306(14) 0.0091(12) 0.0056(13) 0.0170(13) C41 0.0411(15) 0.0365(15) 0.0370(15) 0.0046(13) 0.0056(14) 0.0169(13) C42 0.0423(16) 0.0378(16) 0.0486(17) 0.0065(14) 0.0093(15) 0.0101(13) C43 0.0422(16) 0.0447(17) 0.0419(16) 0.0096(15) 0.0120(15) 0.0181(14) C44 0.0440(16) 0.0410(16) 0.0393(16) 0.0048(14) 0.0090(15) 0.0184(14) C45 0.0366(14) 0.0357(15) 0.0371(15) 0.0068(13) 0.0056(13) 0.0135(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 B1 C25 1.561(4) . ? B1 C40 1.565(4) . ? B1 C31 1.583(4) . ? C1 C6 1.379(4) . ? C1 C2 1.385(4) . ? C1 H1A 0.9500 . ? C2 C3 1.385(4) . ? C2 C9 1.505(4) . ? C3 C4 1.399(4) . ? C3 H3A 0.9500 . ? C4 C5 1.394(3) . ? C4 C8 1.517(4) . ? C5 C6 1.411(4) . ? C5 C15 1.490(3) . ? C6 C7 1.506(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.379(3) . ? C10 C15 1.391(3) . ? C10 H10A 0.9500 . ? C11 C12 1.392(3) . ? C11 H11A 0.9500 . ? C12 C13 1.393(3) . ? C12 C16 1.478(3) . ? C13 C14 1.376(3) . ? C13 H13A 0.9500 . ? C14 C15 1.393(3) . ? C14 H14A 0.9500 . ? C16 C21 1.382(4) . ? C16 C17 1.395(3) . ? C17 C18 1.373(3) . ? C17 H17A 0.9500 . ? C18 C19 1.390(4) . ? C18 H18A 0.9500 . ? C19 C20 1.394(3) . ? C19 C22 1.481(3) . ? C20 C21 1.382(4) . ? C20 H20A 0.9500 . ? C21 H21A 0.9500 . ? C22 C27 1.388(3) . ? C22 C23 1.390(3) . ? C23 C24 1.379(4) . ? C23 H23A 0.9500 . ? C24 C25 1.393(4) . ? C24 H24A 0.9500 . ? C25 C26 1.402(3) . ? C26 C27 1.383(3) . ? C26 H26A 0.9500 . ? C27 H27A 0.9500 . ? C28 C36 1.513(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C32 1.503(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C34 1.513(4) . ? C30 H30A 0.9801 . ? C30 H30B 0.9801 . ? C30 H30C 0.9801 . ? C31 C36 1.412(3) . ? C31 C32 1.418(3) . ? C32 C33 1.391(3) . ? C33 C34 1.388(4) . ? C33 H33A 0.9500 . ? C34 C35 1.378(4) . ? C35 C36 1.386(3) . ? C35 H35A 0.9500 . ? C37 C45 1.521(3) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C41 1.515(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C43 1.512(4) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C45 1.414(3) . ? C40 C41 1.420(3) . ? C41 C42 1.372(3) . ? C42 C43 1.380(4) . ? C42 H42A 0.9500 . ? C43 C44 1.378(4) . ? C44 C45 1.386(3) . ? C44 H44A 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C25 B1 C40 120.2(2) . . ? C25 B1 C31 118.6(2) . . ? C40 B1 C31 121.1(2) . . ? C6 C1 C2 122.0(3) . . ? C6 C1 H1A 119.0 . . ? C2 C1 H1A 119.0 . . ? C3 C2 C1 117.7(3) . . ? C3 C2 C9 121.0(3) . . ? C1 C2 C9 121.2(3) . . ? C2 C3 C4 122.3(3) . . ? C2 C3 H3A 118.9 . . ? C4 C3 H3A 118.9 . . ? C5 C4 C3 118.9(3) . . ? C5 C4 C8 122.0(3) . . ? C3 C4 C8 119.1(3) . . ? C4 C5 C6 119.3(2) . . ? C4 C5 C15 122.0(2) . . ? C6 C5 C15 118.7(2) . . ? C1 C6 C5 119.7(3) . . ? C1 C6 C7 118.8(3) . . ? C5 C6 C7 121.4(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 121.1(2) . . ? C11 C10 H10A 119.5 . . ? C15 C10 H10A 119.5 . . ? C10 C11 C12 121.8(2) . . ? C10 C11 H11A 119.1 . . ? C12 C11 H11A 119.1 . . ? C11 C12 C13 117.1(2) . . ? C11 C12 C16 121.9(2) . . ? C13 C12 C16 120.8(2) . . ? C14 C13 C12 121.0(2) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C13 C14 C15 122.0(2) . . ? C13 C14 H14A 119.0 . . ? C15 C14 H14A 119.0 . . ? C10 C15 C14 117.0(2) . . ? C10 C15 C5 122.8(2) . . ? C14 C15 C5 120.1(2) . . ? C21 C16 C17 116.8(2) . . ? C21 C16 C12 120.5(2) . . ? C17 C16 C12 122.6(2) . . ? C18 C17 C16 121.7(3) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C17 C18 C19 121.7(2) . . ? C17 C18 H18A 119.1 . . ? C19 C18 H18A 119.2 . . ? C18 C19 C20 116.5(2) . . ? C18 C19 C22 122.4(2) . . ? C20 C19 C22 121.1(2) . . ? C21 C20 C19 121.7(3) . . ? C21 C20 H20A 119.2 . . ? C19 C20 H20A 119.2 . . ? C16 C21 C20 121.5(2) . . ? C16 C21 H21A 119.2 . . ? C20 C21 H21A 119.2 . . ? C27 C22 C23 116.9(2) . . ? C27 C22 C19 121.7(2) . . ? C23 C22 C19 121.4(3) . . ? C24 C23 C22 121.6(3) . . ? C24 C23 H23A 119.2 . . ? C22 C23 H23A 119.2 . . ? C23 C24 C25 122.3(2) . . ? C23 C24 H24A 118.9 . . ? C25 C24 H24A 118.9 . . ? C24 C25 C26 115.7(2) . . ? C24 C25 B1 122.7(2) . . ? C26 C25 B1 121.5(3) . . ? C27 C26 C25 122.1(3) . . ? C27 C26 H26A 119.0 . . ? C25 C26 H26A 119.0 . . ? C26 C27 C22 121.4(2) . . ? C26 C27 H27A 119.3 . . ? C22 C27 H27A 119.3 . . ? C36 C28 H28A 109.5 . . ? C36 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C36 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C32 C29 H29A 109.5 . . ? C32 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C32 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C34 C30 H30A 109.5 . . ? C34 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C34 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C36 C31 C32 117.8(2) . . ? C36 C31 B1 121.5(2) . . ? C32 C31 B1 120.7(2) . . ? C33 C32 C31 119.8(2) . . ? C33 C32 C29 118.8(2) . . ? C31 C32 C29 121.4(2) . . ? C34 C33 C32 122.1(2) . . ? C34 C33 H33A 119.0 . . ? C32 C33 H33A 119.0 . . ? C35 C34 C33 117.6(2) . . ? C35 C34 C30 121.1(3) . . ? C33 C34 C30 121.2(2) . . ? C34 C35 C36 122.6(2) . . ? C34 C35 H35A 118.7 . . ? C36 C35 H35A 118.7 . . ? C35 C36 C31 119.9(2) . . ? C35 C36 C28 117.3(2) . . ? C31 C36 C28 122.7(2) . . ? C45 C37 H37A 109.5 . . ? C45 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C45 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C41 C38 H38A 109.5 . . ? C41 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C41 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C43 C39 H39A 109.5 . . ? C43 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C43 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C45 C40 C41 116.8(2) . . ? C45 C40 B1 122.2(2) . . ? C41 C40 B1 121.0(2) . . ? C42 C41 C40 120.5(2) . . ? C42 C41 C38 118.5(2) . . ? C40 C41 C38 121.0(3) . . ? C41 C42 C43 122.4(3) . . ? C41 C42 H42A 118.8 . . ? C43 C42 H42A 118.8 . . ? C44 C43 C42 117.9(3) . . ? C44 C43 C39 121.3(3) . . ? C42 C43 C39 120.8(3) . . ? C43 C44 C45 121.8(3) . . ? C43 C44 H44A 119.1 . . ? C45 C44 H44A 119.1 . . ? C44 C45 C40 120.6(2) . . ? C44 C45 C37 117.4(2) . . ? C40 C45 C37 121.9(3) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.225 _refine_diff_density_min -0.218 _refine_diff_density_rms 0.045