Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_2 _database_code_CSD 166842 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Anslyn, Eric' 'Hennrich, Gunther' 'Lynch, Vincent' _publ_contact_author_name 'Prof Eric Anslyn' _publ_contact_author_address ; Department of Chemistry University of Texas at Austin Austin TX 78712 USA ; _publ_contact_author_email 'ANSLYN@CCWF.CC.UTEXAS.EDU' _publ_section_title ; A cascade of reactions involving anchimeric assistance leads to a highly "crowded" hexa-(alkylcarboxy) benzene ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H120 O12' _chemical_formula_weight 1465.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5161(5) _cell_length_b 11.3542(7) _cell_length_c 18.823(2) _cell_angle_alpha 82.191(4) _cell_angle_beta 79.886(3) _cell_angle_gamma 63.025(2) _cell_volume 1967.8(3) _cell_formula_units_Z 1 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description lathes _exptl_crystal_colour colorless _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11370 _diffrn_reflns_av_R_equivalents 0.0785 _diffrn_reflns_av_sigmaI/netI 0.1550 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.08 _diffrn_reflns_theta_max 27.45 _reflns_number_total 7389 _reflns_number_gt 3523 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius BV, 2000' _computing_cell_refinement 'HKL Scalepak (Otwinoski and Minor, 1997)' _computing_data_reduction 'Denzo and Scalepak (Otwinoski and Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL-Plus 5.1, XP, Bruker-AXS, 1998' _computing_publication_material 'SHELXTL-Plus, XCIF, Bruker-AXS, 1998' _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^)+(0.0371P)^2^+4.0544P] 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 calc _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0066(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7389 _refine_ls_number_parameters 488 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2235 _refine_ls_R_factor_gt 0.1093 _refine_ls_wR_factor_ref 0.2334 _refine_ls_wR_factor_gt 0.1838 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _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 0.5828(6) 0.3625(5) 0.5065(3) 0.0323(12) Uani 1 1 d . . . C2 C 0.4510(6) 0.4152(5) 0.4783(3) 0.0328(13) Uani 1 1 d . . . C3 C 0.3681(5) 0.5539(5) 0.4708(2) 0.0302(12) Uani 1 1 d . . . C4 C 0.6782(5) 0.2120(5) 0.5108(3) 0.0354(13) Uani 1 1 d . . . H4A H 0.6324 0.1686 0.4920 0.043 Uiso 1 1 d R . . H4B H 0.6907 0.1798 0.5602 0.043 Uiso 1 1 d R . . O5 O 0.8168(4) 0.1837(3) 0.46771(18) 0.0373(9) Uani 1 1 d . . . C6 C 0.8185(6) 0.1936(5) 0.3951(3) 0.0320(12) Uani 1 1 d . . . O7 O 0.7144(4) 0.2110(4) 0.36837(19) 0.0444(10) Uani 1 1 d . . . C8 C 0.9569(5) 0.1875(4) 0.3548(3) 0.0310(12) Uani 1 1 d . . . C9 C 0.9769(6) 0.3040(5) 0.3749(3) 0.0387(14) Uani 1 1 d . . . H9A H 0.9823 0.2962 0.4258 0.046 Uiso 1 1 d R . . H9B H 0.8957 0.3857 0.3641 0.046 Uiso 1 1 d R . . C10 C 1.1139(6) 0.3048(5) 0.3323(3) 0.0414(14) Uani 1 1 d . . . H10 H 1.1242 0.3789 0.3448 0.050 Uiso 1 1 d R . . C11 C 1.1073(6) 0.3150(5) 0.2508(3) 0.0470(15) Uani 1 1 d . . . H11A H 1.1935 0.3162 0.2244 0.056 Uiso 1 1 d R . . H11B H 1.0266 0.3954 0.2380 0.056 Uiso 1 1 d R . . C12 C 1.0906(6) 0.1970(5) 0.2316(3) 0.0401(14) Uani 1 1 d . . . H12 H 1.0873 0.2018 0.1806 0.048 Uiso 1 1 d R . . C13 C 0.9520(6) 0.1977(5) 0.2736(3) 0.0414(14) Uani 1 1 d . . . H13A H 0.8718 0.2785 0.2607 0.050 Uiso 1 1 d R . . H13B H 0.9390 0.1248 0.2615 0.050 Uiso 1 1 d R . . C14 C 1.0884(5) 0.0571(5) 0.3751(3) 0.0366(13) Uani 1 1 d . . . H14A H 1.0773 -0.0174 0.3639 0.044 Uiso 1 1 d R . . H14B H 1.0931 0.0506 0.4261 0.044 Uiso 1 1 d R . . C15 C 1.2257(6) 0.0574(5) 0.3325(3) 0.0408(14) Uani 1 1 d . . . H15 H 1.3064 -0.0238 0.3444 0.049 Uiso 1 1 d R . . C16 C 1.2188(6) 0.0683(5) 0.2517(3) 0.0431(14) Uani 1 1 d . . . H16A H 1.3066 0.0663 0.2253 0.052 Uiso 1 1 d R . . H16B H 1.2083 -0.0057 0.2390 0.052 Uiso 1 1 d R . . C17 C 1.2434(6) 0.1758(5) 0.3527(3) 0.0425(14) Uani 1 1 d . . . H17A H 1.2482 0.1695 0.4037 0.051 Uiso 1 1 d R . . H17B H 1.3311 0.1752 0.3271 0.051 Uiso 1 1 d R . . C18 C 0.3970(6) 0.3212(5) 0.4598(3) 0.0369(13) Uani 1 1 d . . . H18A H 0.4657 0.2628 0.4244 0.044 Uiso 1 1 d R . . H18B H 0.3070 0.3699 0.4407 0.044 Uiso 1 1 d R . . O19 O 0.3771(4) 0.2464(3) 0.52620(18) 0.0390(9) Uani 1 1 d . . . C20 C 0.2429(6) 0.2717(6) 0.5564(3) 0.0403(14) Uani 1 1 d . . . O21 O 0.1388(5) 0.3381(5) 0.5254(2) 0.0784(15) Uani 1 1 d . . . C22 C 0.2360(5) 0.2170(5) 0.6342(3) 0.0331(12) Uani 1 1 d . . . C23 C 0.1029(6) 0.1922(5) 0.6566(3) 0.0418(14) Uani 1 1 d . . . H23A H 0.1112 0.1235 0.6289 0.050 Uiso 1 1 d R . . H23B H 0.0182 0.2710 0.6463 0.050 Uiso 1 1 d R . . C24 C 0.0907(6) 0.1499(5) 0.7370(3) 0.0408(14) Uani 1 1 d . . . H24 H 0.0077 0.1333 0.7505 0.049 Uiso 1 1 d R . . C25 C 0.0785(6) 0.2588(5) 0.7807(3) 0.0452(15) Uani 1 1 d . . . H25A H 0.0669 0.2347 0.8315 0.054 Uiso 1 1 d R . . H25B H -0.0051 0.3385 0.7703 0.054 Uiso 1 1 d R . . C26 C 0.2107(6) 0.2841(5) 0.7602(3) 0.0437(14) Uani 1 1 d . . . H26 H 0.2026 0.3523 0.7882 0.052 Uiso 1 1 d R . . C27 C 0.2228(6) 0.3260(5) 0.6795(3) 0.0402(14) Uani 1 1 d . . . H27A H 0.1380 0.4053 0.6700 0.048 Uiso 1 1 d R . . H27B H 0.3047 0.3443 0.6655 0.048 Uiso 1 1 d R . . C28 C 0.3703(6) 0.0899(5) 0.6508(3) 0.0425(14) Uani 1 1 d . . . H28A H 0.4545 0.1047 0.6374 0.051 Uiso 1 1 d R . . H28B H 0.3799 0.0205 0.6232 0.051 Uiso 1 1 d R . . C29 C 0.3572(6) 0.0485(5) 0.7312(3) 0.0428(14) Uani 1 1 d . . . H29 H 0.4409 -0.0314 0.7413 0.051 Uiso 1 1 d R . . C30 C 0.2263(6) 0.0235(5) 0.7525(3) 0.0498(16) Uani 1 1 d . . . H30A H 0.2353 -0.0461 0.7252 0.060 Uiso 1 1 d R . . H30B H 0.2187 -0.0044 0.8029 0.060 Uiso 1 1 d R . . C31 C 0.3443(6) 0.1575(6) 0.7748(3) 0.0475(15) Uani 1 1 d . . . H31A H 0.3386 0.1304 0.8254 0.057 Uiso 1 1 d R . . H31B H 0.4285 0.1726 0.7616 0.057 Uiso 1 1 d R . . C32 C 0.2355(5) 0.6075(5) 0.4341(3) 0.0350(13) Uani 1 1 d . . . H32A H 0.1900 0.7025 0.4327 0.042 Uiso 1 1 d R . . H32B H 0.1686 0.5759 0.4599 0.042 Uiso 1 1 d R . . O33 O 0.2779(4) 0.5638(3) 0.36030(17) 0.0361(9) Uani 1 1 d . . . C34 C 0.3331(6) 0.6322(6) 0.3117(3) 0.0447(15) Uani 1 1 d . . . O35 O 0.3298(5) 0.7354(4) 0.3244(2) 0.0657(14) Uani 1 1 d . . . C36 C 0.4036(6) 0.5655(5) 0.2416(3) 0.0363(13) Uani 1 1 d . . . C37 C 0.3809(7) 0.4437(5) 0.2362(3) 0.0483(16) Uani 1 1 d . . . H37A H 0.2796 0.4709 0.2384 0.058 Uiso 1 1 d R . . H37B H 0.4156 0.3809 0.2762 0.058 Uiso 1 1 d R . . C38 C 0.4598(7) 0.3823(6) 0.1639(3) 0.0563(18) Uani 1 1 d . . . H38 H 0.4444 0.3066 0.1595 0.068 Uiso 1 1 d R . . C39 C 0.6203(7) 0.3392(6) 0.1615(3) 0.0545(17) Uani 1 1 d . . . H39A H 0.6713 0.2983 0.1171 0.065 Uiso 1 1 d R . . H39B H 0.6560 0.2754 0.2009 0.065 Uiso 1 1 d R . . C40 C 0.6464(6) 0.4598(6) 0.1669(3) 0.0470(15) Uani 1 1 d . . . H40 H 0.7476 0.4327 0.1652 0.056 Uiso 1 1 d R . . C41 C 0.5665(6) 0.5227(6) 0.2383(3) 0.0453(15) Uani 1 1 d . . . H41A H 0.6025 0.4602 0.2781 0.054 Uiso 1 1 d R . . H41B H 0.5811 0.5989 0.2426 0.054 Uiso 1 1 d R . . C42 C 0.3491(7) 0.6659(6) 0.1779(3) 0.0486(15) Uani 1 1 d . . . H42A H 0.3662 0.7408 0.1819 0.058 Uiso 1 1 d R . . H42B H 0.2474 0.6958 0.1798 0.058 Uiso 1 1 d R . . C43 C 0.4294(6) 0.6018(6) 0.1071(3) 0.0486(16) Uani 1 1 d . . . H43 H 0.3942 0.6653 0.0675 0.058 Uiso 1 1 d R . . C44 C 0.5884(6) 0.5601(6) 0.1048(3) 0.0503(16) Uani 1 1 d . . . H44A H 0.6383 0.5196 0.0603 0.060 Uiso 1 1 d R . . H44B H 0.6052 0.6360 0.1066 0.060 Uiso 1 1 d R . . C45 C 0.4042(7) 0.4817(7) 0.1011(3) 0.0618(19) Uani 1 1 d . . . H45A H 0.3032 0.5089 0.1019 0.074 Uiso 1 1 d R . . H45B H 0.4530 0.4429 0.0560 0.074 Uiso 1 1 d R . . C1A C 0.0222(8) -0.0959(9) -0.0442(5) 0.078(2) Uani 1 1 d . . . H1A H 0.0356 -0.1623 -0.0751 0.094 Uiso 1 1 d R . . C2A C 0.0643(8) -0.1311(8) 0.0226(5) 0.082(2) Uani 1 1 d . . . H2A H 0.1112 -0.2234 0.0379 0.099 Uiso 1 1 d R . . C3A C 0.0421(9) -0.0359(11) 0.0670(4) 0.084(3) Uani 1 1 d . . . H3A H 0.0702 -0.0615 0.1146 0.101 Uiso 1 1 d R . . C1B C 0.6175(9) -0.0161(9) -0.0490(4) 0.086(3) Uani 1 1 d . . . H1B H 0.6998 -0.0251 -0.0836 0.103 Uiso 1 1 d R . . C2B C 0.5244(9) -0.0598(7) -0.0624(4) 0.078(2) Uani 1 1 d . . . H2B H 0.5407 -0.1005 -0.1067 0.093 Uiso 1 1 d R . . C3B C 0.4075(9) -0.0448(8) -0.0135(4) 0.081(2) Uani 1 1 d . . . H3B H 0.3427 -0.0770 -0.0234 0.097 Uiso 1 1 d R . . C1C C 1.0892(8) 0.3813(7) -0.0307(4) 0.0647(19) Uani 1 1 d . . . H1C H 1.1512 0.2985 -0.0518 0.078 Uiso 1 1 d R . . C2C C 1.1067(7) 0.4018(7) 0.0367(4) 0.0637(19) Uani 1 1 d . . . H2C H 1.1816 0.3348 0.0623 0.076 Uiso 1 1 d R . . C3C C 1.0172(8) 0.5218(7) 0.0674(4) 0.068(2) Uani 1 1 d . . . H3C H 1.0284 0.5372 0.1144 0.081 Uiso 1 1 d 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 0.031(3) 0.031(3) 0.032(3) -0.002(2) 0.000(2) -0.013(3) C2 0.036(3) 0.032(3) 0.034(3) -0.007(2) 0.000(2) -0.018(3) C3 0.019(3) 0.037(3) 0.033(3) -0.006(2) 0.000(2) -0.010(2) C4 0.026(3) 0.025(3) 0.047(3) -0.002(2) -0.001(2) -0.005(2) O5 0.030(2) 0.032(2) 0.041(2) -0.0047(16) -0.0002(17) -0.0078(17) C6 0.030(3) 0.020(3) 0.042(3) -0.008(2) -0.002(3) -0.007(2) O7 0.034(2) 0.055(3) 0.045(2) -0.0167(19) 0.0005(19) -0.019(2) C8 0.029(3) 0.016(3) 0.040(3) -0.005(2) -0.003(2) -0.002(2) C9 0.037(3) 0.020(3) 0.053(3) -0.008(2) -0.001(3) -0.008(3) C10 0.041(4) 0.026(3) 0.056(4) -0.013(3) 0.001(3) -0.013(3) C11 0.042(4) 0.035(3) 0.056(4) -0.001(3) 0.001(3) -0.012(3) C12 0.040(4) 0.044(3) 0.035(3) -0.006(3) -0.001(3) -0.018(3) C13 0.041(4) 0.036(3) 0.045(3) -0.001(3) -0.009(3) -0.014(3) C14 0.029(3) 0.024(3) 0.048(3) -0.007(2) -0.003(3) -0.003(2) C15 0.028(3) 0.030(3) 0.053(3) -0.007(3) -0.001(3) -0.004(3) C16 0.038(4) 0.038(3) 0.048(3) -0.011(3) 0.002(3) -0.013(3) C17 0.034(3) 0.049(4) 0.044(3) -0.010(3) 0.000(3) -0.017(3) C18 0.036(3) 0.032(3) 0.039(3) 0.001(2) -0.006(3) -0.012(3) O19 0.033(2) 0.036(2) 0.046(2) 0.0029(17) -0.0039(18) -0.0154(18) C20 0.022(3) 0.046(4) 0.052(4) -0.013(3) -0.001(3) -0.013(3) O21 0.034(3) 0.121(4) 0.062(3) 0.020(3) -0.008(2) -0.025(3) C22 0.028(3) 0.024(3) 0.041(3) -0.007(2) -0.002(2) -0.005(2) C23 0.030(3) 0.041(3) 0.054(4) -0.006(3) -0.005(3) -0.014(3) C24 0.034(3) 0.038(3) 0.049(3) -0.008(3) 0.003(3) -0.016(3) C25 0.041(4) 0.036(3) 0.050(3) -0.006(3) 0.006(3) -0.013(3) C26 0.046(4) 0.033(3) 0.048(3) -0.005(3) -0.004(3) -0.014(3) C27 0.037(3) 0.026(3) 0.052(3) -0.006(3) -0.002(3) -0.009(3) C28 0.036(4) 0.030(3) 0.055(4) -0.009(3) 0.002(3) -0.010(3) C29 0.034(3) 0.034(3) 0.051(3) -0.004(3) -0.005(3) -0.006(3) C30 0.052(4) 0.037(3) 0.054(4) -0.008(3) 0.002(3) -0.016(3) C31 0.042(4) 0.051(4) 0.049(3) -0.001(3) -0.007(3) -0.020(3) C32 0.030(3) 0.039(3) 0.033(3) -0.006(2) -0.002(2) -0.013(3) O33 0.037(2) 0.035(2) 0.0309(19) -0.0053(16) -0.0013(16) -0.0125(18) C34 0.054(4) 0.037(4) 0.036(3) -0.003(3) -0.003(3) -0.015(3) O35 0.113(4) 0.037(2) 0.047(2) -0.013(2) 0.009(2) -0.036(3) C36 0.046(4) 0.030(3) 0.032(3) -0.002(2) -0.005(3) -0.016(3) C37 0.058(4) 0.043(4) 0.046(3) -0.011(3) 0.006(3) -0.027(3) C38 0.071(5) 0.060(4) 0.050(4) -0.025(3) 0.012(3) -0.040(4) C39 0.061(5) 0.039(4) 0.054(4) -0.015(3) 0.005(3) -0.015(3) C40 0.036(4) 0.049(4) 0.048(3) -0.002(3) -0.006(3) -0.013(3) C41 0.048(4) 0.042(4) 0.042(3) -0.001(3) -0.010(3) -0.015(3) C42 0.050(4) 0.046(4) 0.038(3) -0.001(3) -0.003(3) -0.012(3) C43 0.045(4) 0.051(4) 0.038(3) -0.001(3) -0.004(3) -0.011(3) C44 0.047(4) 0.055(4) 0.047(3) -0.004(3) 0.000(3) -0.022(3) C45 0.055(4) 0.090(5) 0.042(4) -0.022(4) 0.000(3) -0.030(4) C1A 0.063(5) 0.086(7) 0.086(6) -0.022(5) 0.002(4) -0.033(5) C2A 0.071(6) 0.057(5) 0.103(7) 0.013(5) -0.010(5) -0.021(4) C3A 0.069(6) 0.121(8) 0.065(5) 0.028(6) -0.015(4) -0.051(6) C1B 0.079(6) 0.121(7) 0.062(5) -0.032(5) 0.024(4) -0.052(6) C2B 0.084(6) 0.074(5) 0.070(5) -0.021(4) 0.001(5) -0.030(5) C3B 0.082(6) 0.091(6) 0.077(5) -0.006(5) -0.006(5) -0.045(5) C1C 0.078(6) 0.061(5) 0.058(4) -0.018(4) 0.000(4) -0.033(4) C2C 0.061(5) 0.055(4) 0.069(5) -0.006(4) -0.010(4) -0.019(4) C3C 0.080(6) 0.072(5) 0.052(4) -0.013(4) -0.004(4) -0.033(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.407(7) . ? C1 C3 1.408(7) 2_666 ? C1 C4 1.539(7) . ? C2 C3 1.413(7) . ? C2 C18 1.517(7) . ? C3 C1 1.408(7) 2_666 ? C3 C32 1.499(7) . ? C4 O5 1.455(6) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? O5 C6 1.353(6) . ? C6 O7 1.209(6) . ? C6 C8 1.495(7) . ? C8 C13 1.525(7) . ? C8 C9 1.535(7) . ? C8 C14 1.557(7) . ? C9 C10 1.524(7) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C10 C11 1.533(7) . ? C10 C17 1.539(7) . ? C10 H10 0.9600 . ? C11 C12 1.525(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C12 C13 1.529(7) . ? C12 C16 1.529(7) . ? C12 H12 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9599 . ? C14 C15 1.525(7) . ? C14 H14A 0.9600 . ? C14 H14B 0.9599 . ? C15 C16 1.521(7) . ? C15 C17 1.543(7) . ? C15 H15 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C17 H17A 0.9601 . ? C17 H17B 0.9599 . ? C18 O19 1.452(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? O19 C20 1.339(6) . ? C20 O21 1.210(6) . ? C20 C22 1.514(7) . ? C22 C23 1.529(7) . ? C22 C28 1.535(7) . ? C22 C27 1.538(7) . ? C23 C24 1.526(7) . ? C23 H23A 0.9601 . ? C23 H23B 0.9601 . ? C24 C25 1.522(7) . ? C24 C30 1.534(8) . ? C24 H24 0.9600 . ? C25 C26 1.519(7) . ? C25 H25A 0.9601 . ? C25 H25B 0.9600 . ? C26 C31 1.520(7) . ? C26 C27 1.529(7) . ? C26 H26 0.9601 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C28 C29 1.523(7) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C29 C30 1.506(8) . ? C29 C31 1.520(7) . ? C29 H29 0.9600 . ? C30 H30A 0.9602 . ? C30 H30B 0.9600 . ? C31 H31A 0.9599 . ? C31 H31B 0.9599 . ? C32 O33 1.465(5) . ? C32 H32A 0.9600 . ? C32 H32B 0.9599 . ? O33 C34 1.345(6) . ? C34 O35 1.211(6) . ? C34 C36 1.511(7) . ? C36 C37 1.524(7) . ? C36 C42 1.531(7) . ? C36 C41 1.546(7) . ? C37 C38 1.538(7) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C38 C45 1.515(9) . ? C38 C39 1.524(8) . ? C38 H38 0.9600 . ? C39 C40 1.533(8) . ? C39 H39A 0.9600 . ? C39 H39B 0.9601 . ? C40 C44 1.515(8) . ? C40 C41 1.530(7) . ? C40 H40 0.9600 . ? C41 H41A 0.9599 . ? C41 H41B 0.9600 . ? C42 C43 1.525(7) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C43 C44 1.511(8) . ? C43 C45 1.525(8) . ? C43 H43 0.9601 . ? C44 H44A 0.9600 . ? C44 H44B 0.9599 . ? C45 H45A 0.9599 . ? C45 H45B 0.9600 . ? C1A C2A 1.356(10) . ? C1A C3A 1.375(11) 2 ? C1A H1A 0.9599 . ? C2A C3A 1.366(11) . ? C2A H2A 0.9600 . ? C3A C1A 1.375(11) 2 ? C3A H3A 0.9598 . ? C1B C2B 1.352(10) . ? C1B C3B 1.372(10) 2_655 ? C1B H1B 0.9600 . ? C2B C3B 1.357(10) . ? C2B H2B 0.9600 . ? C3B C1B 1.372(10) 2_655 ? C3B H3B 0.9599 . ? C1C C3C 1.374(9) 2_765 ? C1C C2C 1.378(8) . ? C1C H1C 0.9600 . ? C2C C3C 1.392(9) . ? C2C H2C 0.9599 . ? C3C C1C 1.374(9) 2_765 ? C3C H3C 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 C2 C1 C3 120.9(5) . 2_666 ? C2 C1 C4 120.3(4) . . ? C3 C1 C4 118.8(5) 2_666 . ? C1 C2 C3 119.8(4) . . ? C1 C2 C18 119.0(5) . . ? C3 C2 C18 121.1(5) . . ? C1 C3 C2 119.3(4) 2_666 . ? C1 C3 C32 121.9(5) 2_666 . ? C2 C3 C32 118.7(4) . . ? O5 C4 C1 109.1(4) . . ? O5 C4 H4A 109.4 . . ? C1 C4 H4A 109.3 . . ? O5 C4 H4B 110.4 . . ? C1 C4 H4B 110.1 . . ? H4A C4 H4B 108.5 . . ? C6 O5 C4 116.1(4) . . ? O7 C6 O5 121.4(5) . . ? O7 C6 C8 125.8(5) . . ? O5 C6 C8 112.7(5) . . ? C6 C8 C13 109.8(4) . . ? C6 C8 C9 108.3(4) . . ? C13 C8 C9 109.6(4) . . ? C6 C8 C14 111.9(4) . . ? C13 C8 C14 109.2(4) . . ? C9 C8 C14 107.9(4) . . ? C10 C9 C8 110.0(4) . . ? C10 C9 H9A 110.1 . . ? C8 C9 H9A 109.4 . . ? C10 C9 H9B 109.6 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 108.3 . . ? C9 C10 C11 110.4(5) . . ? C9 C10 C17 108.8(4) . . ? C11 C10 C17 109.8(4) . . ? C9 C10 H10 109.0 . . ? C11 C10 H10 109.7 . . ? C17 C10 H10 109.2 . . ? C12 C11 C10 109.2(4) . . ? C12 C11 H11A 110.0 . . ? C10 C11 H11A 109.8 . . ? C12 C11 H11B 109.3 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.5 . . ? C11 C12 C13 109.2(4) . . ? C11 C12 C16 109.7(5) . . ? C13 C12 C16 109.3(4) . . ? C11 C12 H12 110.1 . . ? C13 C12 H12 109.9 . . ? C16 C12 H12 108.7 . . ? C8 C13 C12 110.5(4) . . ? C8 C13 H13A 109.5 . . ? C12 C13 H13A 109.0 . . ? C8 C13 H13B 109.1 . . ? C12 C13 H13B 110.3 . . ? H13A C13 H13B 108.4 . . ? C15 C14 C8 109.2(4) . . ? C15 C14 H14A 110.0 . . ? C8 C14 H14A 109.4 . . ? C15 C14 H14B 110.1 . . ? C8 C14 H14B 109.7 . . ? H14A C14 H14B 108.4 . . ? C16 C15 C14 110.4(5) . . ? C16 C15 C17 109.6(4) . . ? C14 C15 C17 109.1(4) . . ? C16 C15 H15 109.0 . . ? C14 C15 H15 109.0 . . ? C17 C15 H15 109.7 . . ? C15 C16 C12 109.8(4) . . ? C15 C16 H16A 109.8 . . ? C12 C16 H16A 110.1 . . ? C15 C16 H16B 109.6 . . ? C12 C16 H16B 109.4 . . ? H16A C16 H16B 108.1 . . ? C10 C17 C15 108.7(4) . . ? C10 C17 H17A 109.9 . . ? C15 C17 H17A 110.1 . . ? C10 C17 H17B 110.1 . . ? C15 C17 H17B 109.6 . . ? H17A C17 H17B 108.4 . . ? O19 C18 C2 107.4(4) . . ? O19 C18 H18A 110.5 . . ? C2 C18 H18A 110.1 . . ? O19 C18 H18B 109.6 . . ? C2 C18 H18B 110.4 . . ? H18A C18 H18B 108.9 . . ? C20 O19 C18 118.6(4) . . ? O21 C20 O19 122.7(5) . . ? O21 C20 C22 124.4(5) . . ? O19 C20 C22 112.7(5) . . ? C20 C22 C23 111.3(4) . . ? C20 C22 C28 114.0(4) . . ? C23 C22 C28 109.1(4) . . ? C20 C22 C27 105.4(4) . . ? C23 C22 C27 108.5(4) . . ? C28 C22 C27 108.4(4) . . ? C24 C23 C22 110.2(4) . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23A 108.8 . . ? C24 C23 H23B 110.1 . . ? C22 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? C25 C24 C23 109.5(4) . . ? C25 C24 C30 108.7(5) . . ? C23 C24 C30 109.4(4) . . ? C25 C24 H24 110.0 . . ? C23 C24 H24 109.7 . . ? C30 C24 H24 109.5 . . ? C26 C25 C24 110.2(4) . . ? C26 C25 H25A 110.6 . . ? C24 C25 H25A 110.2 . . ? C26 C25 H25B 109.0 . . ? C24 C25 H25B 108.7 . . ? H25A C25 H25B 108.1 . . ? C25 C26 C31 109.5(5) . . ? C25 C26 C27 109.0(5) . . ? C31 C26 C27 109.0(4) . . ? C25 C26 H26 109.7 . . ? C31 C26 H26 109.5 . . ? C27 C26 H26 110.2 . . ? C26 C27 C22 110.5(4) . . ? C26 C27 H27A 109.2 . . ? C22 C27 H27A 108.7 . . ? C26 C27 H27B 110.4 . . ? C22 C27 H27B 109.7 . . ? H27A C27 H27B 108.3 . . ? C29 C28 C22 109.9(4) . . ? C29 C28 H28A 109.6 . . ? C22 C28 H28A 109.8 . . ? C29 C28 H28B 109.6 . . ? C22 C28 H28B 109.5 . . ? H28A C28 H28B 108.4 . . ? C30 C29 C31 109.5(5) . . ? C30 C29 C28 109.9(5) . . ? C31 C29 C28 109.6(4) . . ? C30 C29 H29 108.8 . . ? C31 C29 H29 109.3 . . ? C28 C29 H29 109.7 . . ? C29 C30 C24 109.9(5) . . ? C29 C30 H30A 109.2 . . ? C24 C30 H30A 109.6 . . ? C29 C30 H30B 110.2 . . ? C24 C30 H30B 109.9 . . ? H30A C30 H30B 108.1 . . ? C26 C31 C29 109.8(5) . . ? C26 C31 H31A 109.9 . . ? C29 C31 H31A 109.5 . . ? C26 C31 H31B 110.0 . . ? C29 C31 H31B 109.4 . . ? H31A C31 H31B 108.2 . . ? O33 C32 C3 108.3(4) . . ? O33 C32 H32A 109.7 . . ? C3 C32 H32A 109.9 . . ? O33 C32 H32B 109.9 . . ? C3 C32 H32B 110.3 . . ? H32A C32 H32B 108.7 . . ? C34 O33 C32 116.3(4) . . ? O35 C34 O33 122.6(5) . . ? O35 C34 C36 123.8(5) . . ? O33 C34 C36 113.5(5) . . ? C34 C36 C37 113.6(4) . . ? C34 C36 C42 109.5(4) . . ? C37 C36 C42 110.4(5) . . ? C34 C36 C41 106.3(4) . . ? C37 C36 C41 108.8(5) . . ? C42 C36 C41 108.0(4) . . ? C36 C37 C38 109.1(4) . . ? C36 C37 H37A 108.4 . . ? C38 C37 H37A 109.8 . . ? C36 C37 H37B 110.1 . . ? C38 C37 H37B 110.8 . . ? H37A C37 H37B 108.5 . . ? C45 C38 C39 109.4(5) . . ? C45 C38 C37 110.6(5) . . ? C39 C38 C37 109.2(5) . . ? C45 C38 H38 108.7 . . ? C39 C38 H38 109.3 . . ? C37 C38 H38 109.7 . . ? C38 C39 C40 109.7(5) . . ? C38 C39 H39A 110.1 . . ? C40 C39 H39A 109.6 . . ? C38 C39 H39B 109.5 . . ? C40 C39 H39B 109.9 . . ? H39A C39 H39B 108.1 . . ? C44 C40 C41 109.0(5) . . ? C44 C40 C39 109.3(5) . . ? C41 C40 C39 109.0(5) . . ? C44 C40 H40 110.0 . . ? C41 C40 H40 109.9 . . ? C39 C40 H40 109.7 . . ? C40 C41 C36 110.1(4) . . ? C40 C41 H41A 109.8 . . ? C36 C41 H41A 109.3 . . ? C40 C41 H41B 110.2 . . ? C36 C41 H41B 109.1 . . ? H41A C41 H41B 108.3 . . ? C43 C42 C36 109.5(5) . . ? C43 C42 H42A 109.7 . . ? C36 C42 H42A 108.9 . . ? C43 C42 H42B 111.0 . . ? C36 C42 H42B 109.3 . . ? H42A C42 H42B 108.4 . . ? C44 C43 C42 109.6(5) . . ? C44 C43 C45 109.9(5) . . ? C42 C43 C45 109.8(5) . . ? C44 C43 H43 109.1 . . ? C42 C43 H43 108.9 . . ? C45 C43 H43 109.5 . . ? C43 C44 C40 110.0(5) . . ? C43 C44 H44A 109.2 . . ? C40 C44 H44A 108.5 . . ? C43 C44 H44B 110.3 . . ? C40 C44 H44B 110.8 . . ? H44A C44 H44B 108.1 . . ? C38 C45 C43 109.1(5) . . ? C38 C45 H45A 110.0 . . ? C43 C45 H45A 109.6 . . ? C38 C45 H45B 110.4 . . ? C43 C45 H45B 109.6 . . ? H45A C45 H45B 108.2 . . ? C2A C1A C3A 119.5(7) . 2 ? C2A C1A H1A 120.4 . . ? C3A C1A H1A 120.2 2 . ? C1A C2A C3A 120.0(7) . . ? C1A C2A H2A 119.2 . . ? C3A C2A H2A 120.8 . . ? C2A C3A C1A 120.5(7) . 2 ? C2A C3A H3A 119.5 . . ? C1A C3A H3A 119.9 2 . ? C2B C1B C3B 119.8(7) . 2_655 ? C2B C1B H1B 120.6 . . ? C3B C1B H1B 119.5 2_655 . ? C1B C2B C3B 120.0(7) . . ? C1B C2B H2B 119.8 . . ? C3B C2B H2B 120.1 . . ? C2B C3B C1B 120.1(7) . 2_655 ? C2B C3B H3B 119.3 . . ? C1B C3B H3B 120.6 2_655 . ? C3C C1C C2C 120.4(6) 2_765 . ? C3C C1C H1C 119.9 2_765 . ? C2C C1C H1C 119.7 . . ? C1C C2C C3C 119.8(7) . . ? C1C C2C H2C 120.6 . . ? C3C C2C H2C 119.5 . . ? C1C C3C C2C 119.8(6) 2_765 . ? C1C C3C H3C 119.7 2_765 . ? C2C C3C H3C 120.6 . . ? _diffrn_measured_fraction_theta_max 0.821 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.821 _refine_diff_density_max 0.420 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.064 #===END