data_assd _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H40 O12' _chemical_formula_weight 616.64 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' '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 12.6576(12) _cell_length_b 12.9646(12) _cell_length_c 14.7179(14) _cell_angle_alpha 64.575(2) _cell_angle_beta 80.253(2) _cell_angle_gamma 80.547(2) _cell_volume 2138.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.958 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19988 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.1594 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.06 _reflns_number_total 10122 _reflns_number_gt 4120 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0709P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10122 _refine_ls_number_parameters 548 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1939 _refine_ls_R_factor_gt 0.0740 _refine_ls_wR_factor_ref 0.1933 _refine_ls_wR_factor_gt 0.1439 _refine_ls_goodness_of_fit_ref 0.925 _refine_ls_restrained_S_all 0.925 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3853(3) 0.4649(3) 0.2712(2) 0.0265(8) Uani 1 1 d . . . H1 H 0.4510 0.4994 0.2324 0.032 Uiso 1 1 calc R . . C1A C 0.3810(3) 0.4616(3) 0.3769(3) 0.0359(9) Uani 1 1 d . . . H1A1 H 0.3669 0.5392 0.3727 0.043 Uiso 1 1 calc R . . H1A2 H 0.3222 0.4188 0.4206 0.043 Uiso 1 1 calc R . . C1B C 0.4861(3) 0.4059(4) 0.4227(3) 0.0605(13) Uani 1 1 d . . . H1B1 H 0.4970 0.3269 0.4326 0.091 Uiso 1 1 calc R . . H1B2 H 0.4828 0.4102 0.4867 0.091 Uiso 1 1 calc R . . H1B3 H 0.5449 0.4455 0.3778 0.091 Uiso 1 1 calc R . . C2 C 0.3961(3) 0.3442(3) 0.2738(2) 0.0259(8) Uani 1 1 d . . . C3 C 0.4765(3) 0.3096(3) 0.2125(2) 0.0264(8) Uani 1 1 d . . . C4 C 0.4926(3) 0.1982(3) 0.2206(2) 0.0275(8) Uani 1 1 d . . . C5 C 0.4230(3) 0.1200(3) 0.2880(3) 0.0283(8) Uani 1 1 d . . . C6 C 0.3384(3) 0.1518(3) 0.3467(2) 0.0260(8) Uani 1 1 d . . . C7 C 0.3269(3) 0.2634(3) 0.3380(2) 0.0282(8) Uani 1 1 d . . . H7 H 0.2700 0.2856 0.3770 0.034 Uiso 1 1 calc . . . C8 C 0.2578(3) 0.0668(3) 0.4164(2) 0.0283(8) Uani 1 1 d . . . H8 H 0.2882 -0.0087 0.4186 0.034 Uiso 1 1 calc R . . C8A C 0.2454(3) 0.0562(3) 0.5249(3) 0.0363(9) Uani 1 1 d . . . H8A1 H 0.2250 0.1317 0.5247 0.044 Uiso 1 1 calc R . . H8A2 H 0.1881 0.0087 0.5642 0.044 Uiso 1 1 calc R . . C8B C 0.3483(3) 0.0044(4) 0.5748(3) 0.0626(14) Uani 1 1 d . . . H8B1 H 0.3695 -0.0699 0.5741 0.094 Uiso 1 1 calc R . . H8B2 H 0.3361 -0.0032 0.6434 0.094 Uiso 1 1 calc R . . H8B3 H 0.4043 0.0535 0.5383 0.094 Uiso 1 1 calc R . . C9 C 0.1525(3) 0.0960(3) 0.3694(2) 0.0270(8) Uani 1 1 d . . . C10 C 0.1455(3) 0.0704(3) 0.2886(3) 0.0312(9) Uani 1 1 d . . . C11 C 0.0507(3) 0.0964(3) 0.2445(3) 0.0353(9) Uani 1 1 d . . . C12 C -0.0387(3) 0.1521(3) 0.2787(3) 0.0304(8) Uani 1 1 d . . . C13 C -0.0352(3) 0.1792(3) 0.3598(2) 0.0263(8) Uani 1 1 d . . . C14 C 0.0605(3) 0.1503(3) 0.4032(2) 0.0278(8) Uani 1 1 d . . . H14 H 0.0633 0.1682 0.4575 0.033 Uiso 1 1 calc . . . C15 C -0.1337(3) 0.2421(3) 0.3964(2) 0.0277(8) Uani 1 1 d . . . H15 H -0.1969 0.2099 0.3927 0.033 Uiso 1 1 calc R . . C15A C -0.1374(3) 0.2254(3) 0.5061(3) 0.0352(9) Uani 1 1 d . . . H15A H -0.1252 0.1440 0.5487 0.042 Uiso 1 1 calc R . . H15B H -0.0797 0.2627 0.5114 0.042 Uiso 1 1 calc R . . C15B C -0.2446(3) 0.2740(4) 0.5444(3) 0.0569(12) Uani 1 1 d . . . H15C H -0.2557 0.3551 0.5042 0.085 Uiso 1 1 calc R . . H15D H -0.2437 0.2601 0.6138 0.085 Uiso 1 1 calc R . . H15E H -0.3020 0.2373 0.5393 0.085 Uiso 1 1 calc R . . C16 C -0.1445(3) 0.3687(3) 0.3243(2) 0.0262(8) Uani 1 1 d . . . C17 C -0.2207(3) 0.4129(3) 0.2559(3) 0.0309(8) Uani 1 1 d . . . C18 C -0.2287(3) 0.5272(3) 0.1882(3) 0.0335(9) Uani 1 1 d . . . C19 C -0.1614(3) 0.6001(3) 0.1900(3) 0.0318(9) Uani 1 1 d . . . C20 C -0.0827(3) 0.5591(3) 0.2569(3) 0.0268(8) Uani 1 1 d . . . C21 C -0.0759(3) 0.4433(3) 0.3213(3) 0.0302(8) Uani 1 1 d . . . H21 H -0.0224 0.4142 0.3648 0.036 Uiso 1 1 calc . . . C22 C -0.0088(3) 0.6396(3) 0.2584(3) 0.0279(8) Uani 1 1 d . . . H22 H -0.0387 0.7179 0.2178 0.034 Uiso 1 1 calc R . . C22A C -0.0068(3) 0.6320(3) 0.3647(3) 0.0367(9) Uani 1 1 d . . . H22A H 0.0207 0.5547 0.4078 0.044 Uiso 1 1 calc R . . H22B H 0.0420 0.6842 0.3614 0.044 Uiso 1 1 calc R . . C22B C -0.1175(3) 0.6614(4) 0.4118(3) 0.0561(12) Uani 1 1 d . . . H22C H -0.1462 0.7368 0.3685 0.084 Uiso 1 1 calc R . . H22D H -0.1114 0.6594 0.4767 0.084 Uiso 1 1 calc R . . H22E H -0.1648 0.6064 0.4201 0.084 Uiso 1 1 calc R . . C23 C 0.1032(3) 0.6219(3) 0.2063(3) 0.0264(8) Uani 1 1 d . . . C24 C 0.1218(3) 0.6714(3) 0.1015(3) 0.0311(9) Uani 1 1 d . . . C25 C 0.2236(3) 0.6590(3) 0.0529(3) 0.0310(9) Uani 1 1 d . . . C26 C 0.3069(3) 0.5927(3) 0.1084(3) 0.0297(8) Uani 1 1 d . . . C27 C 0.2918(3) 0.5393(3) 0.2130(2) 0.0255(8) Uani 1 1 d . . . C28 C 0.1895(3) 0.5564(3) 0.2592(3) 0.0295(8) Uani 1 1 d . . . H28 H 0.1779 0.5221 0.3295 0.035 Uiso 1 1 calc . . . C29 C 0.2807(4) 0.8696(4) 0.1169(4) 0.0783(16) Uani 1 1 d . . . H29A H 0.3294 0.8871 0.1505 0.117 Uiso 1 1 calc R . . H29B H 0.3212 0.8421 0.0689 0.117 Uiso 1 1 calc R . . H29C H 0.2375 0.8115 0.1659 0.117 Uiso 1 1 calc R . . C30 C 0.5913(4) 0.8420(4) -0.0206(4) 0.0724(15) Uani 1 1 d . . . H30A H 0.5488 0.7798 0.0210 0.109 Uiso 1 1 calc R . . H30B H 0.6310 0.8273 -0.0762 0.109 Uiso 1 1 calc R . . H30C H 0.5448 0.9122 -0.0462 0.109 Uiso 1 1 calc R . . C31 C 0.8197(5) -0.0379(4) 0.1799(4) 0.0898(18) Uani 1 1 d . . . H31A H 0.8531 -0.0435 0.2360 0.135 Uiso 1 1 calc R . . H31B H 0.8293 -0.1113 0.1768 0.135 Uiso 1 1 calc R . . H31C H 0.7441 -0.0142 0.1887 0.135 Uiso 1 1 calc R . . C32 C 0.5547(6) -0.2320(5) 0.2810(5) 0.144(3) Uani 1 1 d . . . H32A H 0.6268 -0.2697 0.2839 0.215 Uiso 1 1 calc R . . H32B H 0.5096 -0.2724 0.2640 0.215 Uiso 1 1 calc R . . H32C H 0.5273 -0.2314 0.3458 0.215 Uiso 1 1 calc R . . C33 C 0.1178(7) 0.3870(7) 0.1027(7) 0.163(4) Uani 1 1 d . . . H33A H 0.1095 0.3540 0.1753 0.244 Uiso 1 1 calc R . . H33B H 0.0666 0.3595 0.0793 0.244 Uiso 1 1 calc R . . H33C H 0.1056 0.4691 0.0775 0.244 Uiso 1 1 calc R . . O1 O 0.54671(18) 0.3852(2) 0.14084(17) 0.0327(6) Uani 1 1 d . . . H1 H 0.5147 0.4497 0.1169 0.049 Uiso 1 1 calc R . . O2 O 0.57225(19) 0.1597(2) 0.1633(2) 0.0393(7) Uani 1 1 d . . . H2 H 0.6136 0.2092 0.1318 0.059 Uiso 1 1 calc R . . O3 O 0.43350(19) 0.0093(2) 0.29546(19) 0.0371(6) Uani 1 1 d . . . H3 H 0.4800 0.0030 0.2515 0.056 Uiso 1 1 calc R . . O4 O 0.2289(2) 0.0158(3) 0.2469(2) 0.0472(7) Uani 1 1 d . . . H4 H 0.2818 0.0012 0.2775 0.071 Uiso 1 1 calc R . . O5 O 0.0491(2) 0.0702(3) 0.1633(2) 0.0577(9) Uani 1 1 d . . . H5 H -0.0131 0.0784 0.1507 0.087 Uiso 1 1 calc R . . O6 O -0.12806(19) 0.1759(2) 0.2285(2) 0.0453(7) Uani 1 1 d . . . H6 H -0.1730 0.2194 0.2455 0.068 Uiso 1 1 calc R . . O7 O -0.28794(18) 0.3403(2) 0.25398(18) 0.0375(6) Uani 1 1 d . . . O8 O -0.3071(2) 0.5666(2) 0.1226(2) 0.0508(8) Uani 1 1 d . . . H8 H -0.2784 0.5917 0.0640 0.076 Uiso 1 1 calc R . . O9 O -0.1654(2) 0.7136(2) 0.1226(2) 0.0467(7) Uani 1 1 d . . . H9 H -0.2235 0.7333 0.0991 0.070 Uiso 1 1 calc R . . O10 O 0.04722(19) 0.7389(2) 0.03702(18) 0.0472(7) Uani 1 1 d . . . H10 H -0.0131 0.7337 0.0684 0.071 Uiso 1 1 calc R . . O11 O 0.24607(19) 0.7103(2) -0.05118(18) 0.0460(7) Uani 1 1 d . . . H11 H 0.1953 0.7570 -0.0756 0.069 Uiso 1 1 calc R . . O12 O 0.40893(18) 0.5793(2) 0.05991(17) 0.0404(7) Uani 1 1 d . . . H12 H 0.4060 0.6054 -0.0013 0.061 Uiso 1 1 calc R . . O13 O 0.2125(2) 0.9707(3) 0.0653(2) 0.0576(8) Uani 1 1 d . . . H13 H 0.1701 0.9874 0.1068 0.086 Uiso 1 1 calc R . . O14 O 0.6645(2) 0.8520(2) 0.0383(2) 0.0533(8) Uani 1 1 d . . . H14 H 0.6995 0.9063 0.0032 0.080 Uiso 1 1 calc R . . O15 O 0.5555(3) -0.1209(3) 0.2086(3) 0.0867(11) Uani 1 1 d . . . H15 H 0.5866 -0.1210 0.1550 0.130 Uiso 1 1 calc R . . O16 O 0.8662(3) 0.0412(3) 0.0919(3) 0.0935(12) Uani 1 1 d . . . H16 H 0.9056 0.0079 0.0604 0.140 Uiso 1 1 calc R . . O20 O 0.2115(7) 0.3586(7) 0.0711(4) 0.211(4) Uani 1 1 d . . . H20 H 0.2350 0.4142 0.0229 0.317 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 0.0226(19) 0.031(2) 0.0254(19) -0.0115(16) -0.0015(15) -0.0030(16) C1A 0.035(2) 0.039(2) 0.038(2) -0.0214(19) -0.0050(18) -0.0015(18) C1B 0.056(3) 0.081(4) 0.055(3) -0.036(3) -0.028(2) 0.010(3) C2 0.0253(19) 0.026(2) 0.0254(19) -0.0099(16) -0.0061(15) 0.0009(16) C3 0.0186(18) 0.032(2) 0.0253(19) -0.0083(17) -0.0023(15) -0.0044(16) C4 0.0223(19) 0.033(2) 0.0268(19) -0.0138(17) 0.0005(15) -0.0015(16) C5 0.0234(19) 0.029(2) 0.034(2) -0.0156(17) -0.0058(16) 0.0022(16) C6 0.0202(18) 0.026(2) 0.0270(19) -0.0069(16) -0.0028(15) -0.0001(15) C7 0.0225(19) 0.031(2) 0.0264(19) -0.0095(17) -0.0003(15) 0.0011(16) C8 0.0260(19) 0.028(2) 0.030(2) -0.0113(17) -0.0046(16) -0.0021(16) C8A 0.027(2) 0.041(2) 0.034(2) -0.0096(19) -0.0029(17) -0.0050(18) C8B 0.045(3) 0.093(4) 0.041(3) -0.020(3) -0.015(2) 0.003(3) C9 0.0254(19) 0.026(2) 0.028(2) -0.0093(16) -0.0020(16) -0.0038(16) C10 0.028(2) 0.034(2) 0.034(2) -0.0177(18) -0.0037(17) 0.0021(17) C11 0.034(2) 0.047(3) 0.032(2) -0.0218(19) -0.0069(17) -0.0028(19) C12 0.024(2) 0.034(2) 0.032(2) -0.0121(18) -0.0081(16) 0.0020(16) C13 0.0262(19) 0.021(2) 0.0285(19) -0.0073(16) -0.0046(16) 0.0003(15) C14 0.029(2) 0.027(2) 0.0271(19) -0.0108(16) -0.0034(16) -0.0053(16) C15 0.0231(19) 0.028(2) 0.031(2) -0.0112(17) -0.0030(16) -0.0020(15) C15A 0.036(2) 0.032(2) 0.033(2) -0.0108(18) 0.0022(17) -0.0032(18) C15B 0.054(3) 0.063(3) 0.049(3) -0.026(2) 0.005(2) 0.005(2) C16 0.0229(19) 0.027(2) 0.0250(19) -0.0079(16) 0.0001(15) -0.0042(15) C17 0.026(2) 0.030(2) 0.036(2) -0.0144(18) -0.0013(17) -0.0040(16) C18 0.024(2) 0.036(2) 0.037(2) -0.0111(19) -0.0108(17) 0.0002(17) C19 0.027(2) 0.024(2) 0.037(2) -0.0053(17) -0.0055(17) 0.0000(16) C20 0.0223(19) 0.026(2) 0.031(2) -0.0113(17) -0.0012(15) -0.0006(15) C21 0.0248(19) 0.036(2) 0.030(2) -0.0137(18) -0.0053(16) 0.0000(17) C22 0.0260(19) 0.025(2) 0.030(2) -0.0102(16) -0.0006(16) -0.0015(15) C22A 0.031(2) 0.043(2) 0.042(2) -0.025(2) 0.0039(18) -0.0052(18) C22B 0.051(3) 0.066(3) 0.051(3) -0.032(2) 0.003(2) 0.008(2) C23 0.0219(19) 0.028(2) 0.032(2) -0.0143(17) 0.0025(16) -0.0081(16) C24 0.025(2) 0.028(2) 0.037(2) -0.0112(18) -0.0021(17) -0.0015(16) C25 0.031(2) 0.032(2) 0.0229(19) -0.0048(17) -0.0034(16) -0.0039(17) C26 0.024(2) 0.031(2) 0.034(2) -0.0142(18) 0.0007(16) -0.0054(16) C27 0.027(2) 0.021(2) 0.0276(19) -0.0095(16) -0.0023(16) -0.0038(15) C28 0.033(2) 0.028(2) 0.0271(19) -0.0112(17) -0.0007(16) -0.0063(17) C29 0.090(4) 0.055(4) 0.104(4) -0.045(3) -0.020(4) -0.001(3) C30 0.066(3) 0.078(4) 0.075(4) -0.023(3) -0.033(3) -0.009(3) C31 0.131(5) 0.058(4) 0.077(4) -0.025(3) 0.004(4) -0.029(4) C32 0.184(8) 0.072(5) 0.111(6) -0.004(4) 0.045(5) 0.000(5) C33 0.202(10) 0.129(7) 0.168(9) -0.090(6) 0.081(7) -0.070(7) O1 0.0262(13) 0.0325(15) 0.0318(14) -0.0078(12) 0.0018(11) -0.0032(11) O2 0.0320(15) 0.0396(17) 0.0458(17) -0.0224(14) 0.0097(12) -0.0033(12) O3 0.0345(16) 0.0327(16) 0.0448(17) -0.0202(13) 0.0046(12) -0.0028(12) O4 0.0322(15) 0.071(2) 0.0530(18) -0.0422(17) -0.0111(13) 0.0089(15) O5 0.0370(16) 0.099(3) 0.0610(19) -0.0570(19) -0.0168(15) 0.0103(17) O6 0.0343(16) 0.065(2) 0.0474(17) -0.0336(15) -0.0167(14) 0.0087(14) O7 0.0319(14) 0.0333(16) 0.0483(16) -0.0134(13) -0.0123(12) -0.0078(12) O8 0.0422(16) 0.0460(19) 0.0520(18) 0.0000(16) -0.0246(14) -0.0092(14) O9 0.0382(16) 0.0313(16) 0.0573(18) 0.0002(14) -0.0179(14) -0.0076(13) O10 0.0272(15) 0.061(2) 0.0349(15) -0.0059(14) -0.0055(12) 0.0063(14) O11 0.0298(15) 0.060(2) 0.0284(14) -0.0038(14) -0.0028(12) 0.0079(13) O12 0.0293(14) 0.0529(18) 0.0263(14) -0.0095(14) 0.0023(11) 0.0043(13) O13 0.055(2) 0.070(2) 0.0566(19) -0.0380(18) 0.0013(16) -0.0030(17) O14 0.0517(19) 0.051(2) 0.0538(19) -0.0144(15) -0.0187(16) -0.0022(15) O15 0.104(3) 0.066(3) 0.078(3) -0.035(2) 0.027(2) -0.001(2) O16 0.090(3) 0.123(3) 0.070(3) -0.031(2) -0.008(2) -0.047(3) O20 0.231(8) 0.239(8) 0.097(5) -0.049(4) 0.031(5) 0.044(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 C1 C27 1.523(4) . ? C1 C1A 1.530(4) . ? C1 C2 1.531(5) . ? C1A C1B 1.522(5) . ? C2 C3 1.393(4) . ? C2 C7 1.388(5) . ? C3 C4 1.380(5) . ? C3 O1 1.394(4) . ? C4 O2 1.372(4) . ? C4 C5 1.387(5) . ? C5 O3 1.378(4) . ? C5 C6 1.382(4) . ? C6 C7 1.382(5) . ? C6 C8 1.533(5) . ? C8 C9 1.523(4) . ? C8 C8A 1.526(5) . ? C8A C8B 1.516(5) . ? C9 C10 1.384(4) . ? C9 C14 1.391(5) . ? C10 O4 1.379(4) . ? C10 C11 1.385(5) . ? C11 O5 1.379(4) . ? C11 C12 1.380(5) . ? C12 O6 1.376(4) . ? C12 C13 1.389(4) . ? C13 C14 1.387(4) . ? C13 C15 1.525(5) . ? C15 C16 1.523(4) . ? C15 C15A 1.527(4) . ? C15A C15B 1.524(5) . ? C16 C21 1.384(4) . ? C16 C17 1.388(4) . ? C17 O7 1.380(4) . ? C17 C18 1.384(5) . ? C18 O8 1.383(4) . ? C18 C19 1.383(5) . ? C19 O9 1.375(4) . ? C19 C20 1.398(4) . ? C20 C21 1.387(5) . ? C20 C22 1.521(4) . ? C22 C23 1.526(4) . ? C22 C22A 1.529(5) . ? C22A C22B 1.520(5) . ? C23 C24 1.386(5) . ? C23 C28 1.392(4) . ? C24 O10 1.371(4) . ? C24 C25 1.384(5) . ? C25 O11 1.381(4) . ? C25 C26 1.382(4) . ? C26 C27 1.384(5) . ? C26 O12 1.389(4) . ? C27 C28 1.387(5) . ? C29 O13 1.428(5) . ? C30 O14 1.426(4) . ? C31 O16 1.370(5) . ? C32 O15 1.377(6) . ? C33 O20 1.254(8) . ? 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 C27 C1 C1A 114.1(3) . . ? C27 C1 C2 110.5(3) . . ? C1A C1 C2 112.0(3) . . ? C1B C1A C1 111.5(3) . . ? C3 C2 C7 116.5(3) . . ? C3 C2 C1 121.7(3) . . ? C7 C2 C1 121.8(3) . . ? C4 C3 C2 122.0(3) . . ? C4 C3 O1 116.3(3) . . ? C2 C3 O1 121.7(3) . . ? O2 C4 C3 124.0(3) . . ? O2 C4 C5 117.0(3) . . ? C3 C4 C5 118.9(3) . . ? O3 C5 C6 117.9(3) . . ? O3 C5 C4 120.8(3) . . ? C6 C5 C4 121.2(3) . . ? C5 C6 C7 117.8(3) . . ? C5 C6 C8 120.8(3) . . ? C7 C6 C8 121.3(3) . . ? C6 C7 C2 123.3(3) . . ? C9 C8 C8A 114.6(3) . . ? C9 C8 C6 109.8(3) . . ? C8A C8 C6 112.1(3) . . ? C8B C8A C8 112.3(3) . . ? C10 C9 C14 116.9(3) . . ? C10 C9 C8 120.3(3) . . ? C14 C9 C8 122.7(3) . . ? O4 C10 C9 124.1(3) . . ? O4 C10 C11 114.5(3) . . ? C9 C10 C11 121.4(3) . . ? O5 C11 C12 121.0(3) . . ? O5 C11 C10 118.6(3) . . ? C12 C11 C10 120.3(3) . . ? O6 C12 C11 115.6(3) . . ? O6 C12 C13 124.2(3) . . ? C11 C12 C13 120.2(3) . . ? C12 C13 C14 118.0(3) . . ? C12 C13 C15 120.0(3) . . ? C14 C13 C15 121.9(3) . . ? C9 C14 C13 123.2(3) . . ? C13 C15 C16 110.2(3) . . ? C13 C15 C15A 114.3(3) . . ? C16 C15 C15A 111.7(3) . . ? C15B C15A C15 112.5(3) . . ? C21 C16 C17 117.3(3) . . ? C21 C16 C15 121.5(3) . . ? C17 C16 C15 121.1(3) . . ? O7 C17 C18 119.6(3) . . ? O7 C17 C16 119.0(3) . . ? C18 C17 C16 121.3(3) . . ? O8 C18 C19 121.6(3) . . ? O8 C18 C17 118.7(3) . . ? C19 C18 C17 119.7(3) . . ? O9 C19 C18 121.4(3) . . ? O9 C19 C20 117.6(3) . . ? C18 C19 C20 120.9(3) . . ? C21 C20 C19 117.2(3) . . ? C21 C20 C22 122.1(3) . . ? C19 C20 C22 120.7(3) . . ? C16 C21 C20 123.5(3) . . ? C20 C22 C23 110.5(3) . . ? C20 C22 C22A 112.6(3) . . ? C23 C22 C22A 113.2(3) . . ? C22B C22A C22 112.7(3) . . ? C24 C23 C28 117.2(3) . . ? C24 C23 C22 119.8(3) . . ? C28 C23 C22 122.9(3) . . ? O10 C24 C25 113.7(3) . . ? O10 C24 C23 125.5(3) . . ? C25 C24 C23 120.7(3) . . ? O11 C25 C26 117.6(3) . . ? O11 C25 C24 122.3(3) . . ? C26 C25 C24 120.1(3) . . ? C25 C26 C27 121.5(3) . . ? C25 C26 O12 120.3(3) . . ? C27 C26 O12 118.2(3) . . ? C28 C27 C26 116.7(3) . . ? C28 C27 C1 123.6(3) . . ? C26 C27 C1 119.7(3) . . ? C27 C28 C23 123.8(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.400 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.054 #######END data_lsas1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common resorcinarene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H63 O10' _chemical_formula_weight 968.12 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.663(3) _cell_length_b 14.711(3) _cell_length_c 15.699(3) _cell_angle_alpha 98.691(4) _cell_angle_beta 91.894(4) _cell_angle_gamma 102.227(4) _cell_volume 2596.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1030 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24139 _diffrn_reflns_av_R_equivalents 0.0776 _diffrn_reflns_av_sigmaI/netI 0.1713 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 28.03 _reflns_number_total 12264 _reflns_number_gt 4117 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12264 _refine_ls_number_parameters 660 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2287 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1644 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 0.926 _refine_ls_restrained_S_all 0.926 _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 0.3921(3) 0.4431(2) 0.1282(2) 0.0418(9) Uani 1 1 d . . . H1 H 0.4466 0.4730 0.0892 0.050 Uiso 1 1 calc R . . C1A C 0.4582(3) 0.4633(2) 0.2182(2) 0.0478(9) Uani 1 1 d . . . H1A1 H 0.4052 0.4375 0.2592 0.057 Uiso 1 1 calc R . . H1A2 H 0.5230 0.4313 0.2158 0.057 Uiso 1 1 calc R . . C1B C 0.5065(3) 0.5683(2) 0.2507(2) 0.0617(11) Uani 1 1 d . . . H1B1 H 0.5539 0.5955 0.2074 0.074 Uiso 1 1 calc R . . H1B2 H 0.4413 0.5995 0.2585 0.074 Uiso 1 1 calc R . . C1C C 0.5799(3) 0.5860(2) 0.3346(2) 0.0512(10) Uani 1 1 d . . . C1D C 0.5323(4) 0.5987(3) 0.4128(3) 0.0840(14) Uani 1 1 d . . . H1D H 0.4521 0.5962 0.4146 0.101 Uiso 1 1 calc . . . C1E C 0.6006(6) 0.6149(4) 0.4889(3) 0.1090(19) Uani 1 1 d . . . H1E H 0.5664 0.6239 0.5413 0.131 Uiso 1 1 calc . . . C1F C 0.7159(6) 0.6179(4) 0.4882(4) 0.102(2) Uani 1 1 d . . . H1F H 0.7619 0.6285 0.5398 0.122 Uiso 1 1 calc . . . C1G C 0.7650(4) 0.6054(4) 0.4115(4) 0.1045(18) Uani 1 1 d . . . H1G H 0.8451 0.6072 0.4104 0.125 Uiso 1 1 calc . . . C1H C 0.6975(4) 0.5902(3) 0.3354(3) 0.0812(14) Uani 1 1 d . . . H1H H 0.7329 0.5826 0.2834 0.097 Uiso 1 1 calc . . . C2 C 0.3586(3) 0.3382(2) 0.0916(2) 0.0423(9) Uani 1 1 d . . . C3 C 0.3519(3) 0.3061(3) 0.0024(2) 0.0467(9) Uani 1 1 d . . . C4 C 0.3263(3) 0.2118(3) -0.0297(2) 0.0492(9) Uani 1 1 d . . . H4 H 0.3233 0.1917 -0.0890 0.059 Uiso 1 1 calc . . . C5 C 0.3049(3) 0.1468(2) 0.0253(2) 0.0440(9) Uani 1 1 d . . . C6 C 0.3063(3) 0.1733(2) 0.1143(2) 0.0388(8) Uani 1 1 d . . . C7 C 0.3339(3) 0.2695(2) 0.1442(2) 0.0417(9) Uani 1 1 d . . . H7 H 0.3362 0.2894 0.2035 0.050 Uiso 1 1 calc . . . C8 C 0.2740(3) 0.0996(2) 0.1732(2) 0.0418(9) Uani 1 1 d . . . H8 H 0.2984 0.0430 0.1457 0.050 Uiso 1 1 calc R . . C8A C 0.3407(3) 0.1288(2) 0.2631(2) 0.0486(9) Uani 1 1 d . . . H8A1 H 0.4243 0.1462 0.2556 0.058 Uiso 1 1 calc R . . H8A2 H 0.3173 0.1840 0.2928 0.058 Uiso 1 1 calc R . . C8B C 0.3185(3) 0.0513(3) 0.3193(2) 0.0557(10) Uani 1 1 d . . . H8B1 H 0.3577 0.0766 0.3760 0.067 Uiso 1 1 calc R . . H8B2 H 0.2348 0.0342 0.3265 0.067 Uiso 1 1 calc R . . C8C C 0.3597(3) -0.0365(3) 0.2842(2) 0.0514(10) Uani 1 1 d . . . C8D C 0.2818(4) -0.1171(3) 0.2472(3) 0.0745(13) Uani 1 1 d . . . H8D H 0.2018 -0.1183 0.2432 0.089 Uiso 1 1 calc . . . C8E C 0.3219(7) -0.1971(4) 0.2157(4) 0.109(2) Uani 1 1 d . . . H8E H 0.2685 -0.2518 0.1908 0.131 Uiso 1 1 calc . . . C8F C 0.4380(8) -0.1964(5) 0.2208(4) 0.122(3) Uani 1 1 d . . . H8F H 0.4643 -0.2505 0.2000 0.147 Uiso 1 1 calc . . . C8G C 0.5162(5) -0.1159(5) 0.2568(4) 0.1049(19) Uani 1 1 d . . . H8G H 0.5961 -0.1151 0.2601 0.126 Uiso 1 1 calc . . . C8H C 0.4782(4) -0.0361(3) 0.2880(3) 0.0750(13) Uani 1 1 d . . . H8H H 0.5324 0.0185 0.3119 0.090 Uiso 1 1 calc . . . C9 C 0.1427(3) 0.0726(2) 0.1780(2) 0.0391(8) Uani 1 1 d . . . C10 C 0.0736(3) -0.0078(2) 0.1272(2) 0.0431(9) Uani 1 1 d . . . C11 C -0.0456(3) -0.0321(2) 0.1307(2) 0.0460(9) Uani 1 1 d . . . H11 H -0.0890 -0.0863 0.0962 0.055 Uiso 1 1 calc . . . C12 C -0.1012(3) 0.0241(2) 0.1856(2) 0.0417(9) Uani 1 1 d . . . C13 C -0.0391(3) 0.1043(2) 0.23933(19) 0.0390(8) Uani 1 1 d . . . C14 C 0.0817(3) 0.1265(2) 0.2327(2) 0.0408(9) Uani 1 1 d . . . H14 H 0.1248 0.1810 0.2670 0.049 Uiso 1 1 calc . . . C15 C -0.0985(3) 0.1648(2) 0.30400(19) 0.0383(8) Uani 1 1 d . . . H15 H -0.1756 0.1258 0.3116 0.046 Uiso 1 1 calc R . . C15A C -0.0336(3) 0.1918(2) 0.39313(18) 0.0408(9) Uani 1 1 d . . . H15A H 0.0475 0.2224 0.3875 0.049 Uiso 1 1 calc R . . H15B H -0.0695 0.2365 0.4287 0.049 Uiso 1 1 calc R . . C15B C -0.0361(3) 0.1064(2) 0.4374(2) 0.0619(11) Uani 1 1 d . . . H15C H -0.1171 0.0784 0.4461 0.074 Uiso 1 1 calc R . . H15D H -0.0056 0.0599 0.3995 0.074 Uiso 1 1 calc R . . C15C C 0.0337(4) 0.1286(2) 0.5228(2) 0.0535(10) Uani 1 1 d . . . C15D C -0.0177(4) 0.1426(3) 0.5993(3) 0.0684(12) Uani 1 1 d . . . H15E H -0.0985 0.1378 0.5990 0.082 Uiso 1 1 calc . . . C15E C 0.0494(5) 0.1641(3) 0.6780(3) 0.0878(15) Uani 1 1 d . . . H15F H 0.0132 0.1739 0.7294 0.105 Uiso 1 1 calc . . . C15F C 0.1661(5) 0.1704(3) 0.6795(3) 0.0925(16) Uani 1 1 d . . . H15G H 0.2106 0.1842 0.7319 0.111 Uiso 1 1 calc . . . C15G C 0.2196(4) 0.1567(4) 0.6039(4) 0.0914(15) Uani 1 1 d . . . H15H H 0.3004 0.1614 0.6045 0.110 Uiso 1 1 calc . . . C15H C 0.1524(4) 0.1358(3) 0.5268(3) 0.0765(13) Uani 1 1 d . . . H15I H 0.1893 0.1263 0.4756 0.092 Uiso 1 1 calc . . . C16 C -0.1223(3) 0.2491(2) 0.26617(19) 0.0367(8) Uani 1 1 d . . . C17 C -0.2235(3) 0.2407(2) 0.2140(2) 0.0448(9) Uani 1 1 d . . . C18 C -0.2467(3) 0.3151(3) 0.1774(2) 0.0485(9) Uani 1 1 d . . . H18 H -0.3155 0.3077 0.1430 0.058 Uiso 1 1 calc . . . C19 C -0.1673(3) 0.4002(2) 0.1924(2) 0.0427(9) Uani 1 1 d . . . C20 C -0.0651(3) 0.4153(2) 0.24575(19) 0.0387(8) Uani 1 1 d . . . C21 C -0.0463(3) 0.3369(2) 0.28072(19) 0.0391(8) Uani 1 1 d . . . H21 H 0.0217 0.3444 0.3161 0.047 Uiso 1 1 calc . . . C22 C 0.0206(3) 0.5093(2) 0.2630(2) 0.0427(9) Uani 1 1 d . . . H22 H -0.0261 0.5568 0.2593 0.051 Uiso 1 1 calc R . . C22A C 0.0851(3) 0.5349(2) 0.35268(19) 0.0477(9) Uani 1 1 d . . . H22A H 0.0292 0.5223 0.3961 0.057 Uiso 1 1 calc R . . H22B H 0.1422 0.4962 0.3566 0.057 Uiso 1 1 calc R . . C22B C 0.1470(4) 0.6379(3) 0.3697(2) 0.0694(12) Uani 1 1 d . . . H22C H 0.1923 0.6509 0.3205 0.083 Uiso 1 1 calc R . . H22D H 0.0873 0.6750 0.3718 0.083 Uiso 1 1 calc R . . C22C C 0.2276(3) 0.6730(3) 0.4496(2) 0.0590(11) Uani 1 1 d . . . C22D C 0.2288(4) 0.6234(3) 0.5161(3) 0.0685(12) Uani 1 1 d . . . H22E H 0.1774 0.5649 0.5122 0.082 Uiso 1 1 calc . . . C22E C 0.3043(4) 0.6573(4) 0.5898(3) 0.0873(15) Uani 1 1 d . . . H22F H 0.3049 0.6217 0.6339 0.105 Uiso 1 1 calc . . . C22F C 0.3768(5) 0.7431(5) 0.5958(3) 0.115(2) Uani 1 1 d . . . H22G H 0.4267 0.7676 0.6451 0.138 Uiso 1 1 calc . . . C22G C 0.3773(5) 0.7943(4) 0.5299(4) 0.123(2) Uani 1 1 d . . . H22H H 0.4278 0.8533 0.5347 0.148 Uiso 1 1 calc . . . C22H C 0.3041(4) 0.7595(3) 0.4568(3) 0.0888(15) Uani 1 1 d . . . H22I H 0.3060 0.7945 0.4120 0.107 Uiso 1 1 calc . . . C23 C 0.1059(3) 0.5185(2) 0.1916(2) 0.0398(8) Uani 1 1 d . . . C24 C 0.0880(3) 0.5676(2) 0.1245(2) 0.0445(9) Uani 1 1 d . . . C25 C 0.1653(3) 0.5760(2) 0.0596(2) 0.0479(9) Uani 1 1 d . . . H25 H 0.1520 0.6086 0.0152 0.057 Uiso 1 1 calc . . . C26 C 0.2615(3) 0.5364(2) 0.0608(2) 0.0434(9) Uani 1 1 d . . . C27 C 0.2854(3) 0.4872(2) 0.1271(2) 0.0402(9) Uani 1 1 d . . . C28 C 0.2040(3) 0.4801(2) 0.1896(2) 0.0434(9) Uani 1 1 d . . . H28 H 0.2166 0.4469 0.2337 0.052 Uiso 1 1 calc . . . C29 C 0.3936(5) -0.1469(4) 0.0163(3) 0.1129(18) Uani 1 1 d . . . H29A H 0.4289 -0.0994 0.0641 0.169 Uiso 1 1 calc R . . H29B H 0.4107 -0.2062 0.0244 0.169 Uiso 1 1 calc R . . H29C H 0.3100 -0.1525 0.0128 0.169 Uiso 1 1 calc R . . C30 C -0.0297(4) 0.7343(3) -0.0518(2) 0.0773(13) Uani 1 1 d . . . H30A H -0.0822 0.7766 -0.0516 0.116 Uiso 1 1 calc R . . H30B H -0.0732 0.6707 -0.0694 0.116 Uiso 1 1 calc R . . H30C H 0.0298 0.7493 -0.0913 0.116 Uiso 1 1 calc R . . O1 O 0.3717(2) 0.36541(17) -0.05735(14) 0.0640(7) Uani 1 1 d . . . H1A H 0.3654 0.4182 -0.0354 0.096 Uiso 1 1 calc R . . O2 O 0.2836(2) 0.05104(16) -0.00624(14) 0.0579(7) Uani 1 1 d . . . H2 H 0.2628 0.0418 -0.0578 0.087 Uiso 1 1 calc R . . O3 O 0.1233(2) -0.06874(15) 0.07133(16) 0.0562(7) Uani 1 1 d . . . H3 H 0.1704 -0.0383 0.0431 0.084 Uiso 1 1 calc R . . O4 O -0.2229(2) -0.00424(15) 0.18186(15) 0.0526(7) Uani 1 1 d . . . H4A H -0.2509 0.0404 0.2021 0.079 Uiso 1 1 calc R . . O5 O -0.3027(2) 0.15416(16) 0.20119(16) 0.0596(7) Uani 1 1 d . . . H5 H -0.3476 0.1506 0.1589 0.089 Uiso 1 1 calc R . . O6 O -0.1971(2) 0.47039(16) 0.15227(15) 0.0525(7) Uani 1 1 d . . . H6 H -0.1380 0.5113 0.1497 0.079 Uiso 1 1 calc R . . O7 O -0.0086(2) 0.60706(17) 0.12594(15) 0.0580(7) Uani 1 1 d . . . H7A H -0.0017 0.6456 0.0927 0.087 Uiso 1 1 calc R . . O8 O 0.3365(2) 0.54301(16) -0.00610(14) 0.0520(6) Uani 1 1 d . . . O9 O 0.0231(2) 0.7437(2) 0.03119(17) 0.0785(9) Uani 1 1 d . . . H9 H -0.0276 0.7400 0.0662 0.118 Uiso 1 1 calc R . . O10 O 0.4390(3) -0.1219(3) -0.0599(2) 0.1182(13) Uani 1 1 d . . . H10 H 0.4894 -0.1515 -0.0741 0.177 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 0.046(2) 0.043(2) 0.037(2) 0.0079(16) -0.0029(17) 0.0099(17) C1A 0.051(2) 0.040(2) 0.049(2) 0.0083(17) -0.0074(18) 0.0042(18) C1B 0.073(3) 0.046(3) 0.061(3) 0.012(2) -0.013(2) 0.001(2) C1C 0.057(3) 0.039(2) 0.052(2) 0.0039(19) -0.009(2) 0.0017(19) C1D 0.066(3) 0.118(4) 0.065(3) 0.012(3) 0.006(3) 0.017(3) C1E 0.136(5) 0.136(5) 0.051(3) -0.003(3) -0.008(4) 0.034(4) C1F 0.125(5) 0.085(4) 0.087(4) 0.001(3) -0.055(4) 0.026(4) C1G 0.078(4) 0.111(4) 0.118(5) -0.008(4) -0.027(4) 0.030(3) C1H 0.067(3) 0.092(4) 0.080(3) -0.006(3) -0.004(3) 0.022(3) C2 0.045(2) 0.042(2) 0.040(2) 0.0050(18) -0.0028(17) 0.0139(17) C3 0.050(2) 0.050(3) 0.043(2) 0.018(2) 0.0018(18) 0.0111(19) C4 0.060(3) 0.049(3) 0.037(2) 0.0035(19) -0.0003(18) 0.013(2) C5 0.051(2) 0.037(2) 0.042(2) -0.0017(18) -0.0064(18) 0.0136(18) C6 0.038(2) 0.038(2) 0.041(2) 0.0050(17) -0.0031(16) 0.0123(16) C7 0.045(2) 0.046(2) 0.036(2) 0.0064(18) 0.0002(16) 0.0147(18) C8 0.051(2) 0.036(2) 0.040(2) 0.0044(16) -0.0045(17) 0.0153(17) C8A 0.056(2) 0.043(2) 0.048(2) 0.0035(18) -0.0088(18) 0.0187(18) C8B 0.063(3) 0.064(3) 0.047(2) 0.014(2) -0.0008(19) 0.027(2) C8C 0.059(3) 0.055(3) 0.046(2) 0.018(2) 0.002(2) 0.018(2) C8D 0.086(3) 0.062(3) 0.069(3) 0.015(3) 0.003(2) -0.001(3) C8E 0.177(7) 0.050(4) 0.088(4) 0.014(3) 0.032(5) -0.002(4) C8F 0.221(9) 0.075(4) 0.103(5) 0.042(4) 0.054(6) 0.076(6) C8G 0.120(5) 0.113(5) 0.118(5) 0.052(4) 0.031(4) 0.080(4) C8H 0.070(3) 0.072(3) 0.091(3) 0.023(3) -0.007(3) 0.026(3) C9 0.048(2) 0.036(2) 0.0346(19) 0.0055(16) -0.0058(17) 0.0148(18) C10 0.058(3) 0.041(2) 0.034(2) 0.0029(17) -0.0016(18) 0.0204(19) C11 0.054(3) 0.037(2) 0.042(2) -0.0032(17) -0.0084(18) 0.0082(18) C12 0.046(2) 0.038(2) 0.042(2) 0.0085(17) 0.0010(18) 0.0099(18) C13 0.054(2) 0.032(2) 0.0314(19) 0.0087(16) -0.0046(17) 0.0083(17) C14 0.056(2) 0.030(2) 0.037(2) 0.0073(16) -0.0061(18) 0.0103(18) C15 0.046(2) 0.033(2) 0.0353(19) 0.0045(16) -0.0013(16) 0.0091(16) C15A 0.059(2) 0.035(2) 0.0309(18) 0.0058(16) 0.0000(17) 0.0167(17) C15B 0.096(3) 0.047(3) 0.045(2) 0.0155(19) -0.009(2) 0.018(2) C15C 0.081(3) 0.042(2) 0.041(2) 0.0129(18) -0.002(2) 0.018(2) C15D 0.079(3) 0.082(3) 0.051(3) 0.021(2) 0.002(2) 0.026(2) C15E 0.117(4) 0.114(4) 0.041(3) 0.022(3) 0.000(3) 0.039(3) C15F 0.106(4) 0.108(4) 0.068(3) 0.028(3) -0.028(3) 0.027(3) C15G 0.079(4) 0.122(4) 0.083(4) 0.038(3) -0.003(3) 0.029(3) C15H 0.091(4) 0.087(3) 0.062(3) 0.025(3) 0.009(3) 0.033(3) C16 0.048(2) 0.037(2) 0.0293(18) 0.0060(16) 0.0045(16) 0.0163(17) C17 0.049(2) 0.042(2) 0.041(2) 0.0013(18) 0.0001(18) 0.0095(19) C18 0.055(2) 0.048(2) 0.044(2) 0.0081(19) -0.0124(18) 0.017(2) C19 0.058(2) 0.041(2) 0.036(2) 0.0121(17) 0.0033(18) 0.0207(19) C20 0.049(2) 0.040(2) 0.0318(19) 0.0082(16) 0.0032(16) 0.0163(17) C21 0.045(2) 0.041(2) 0.0330(19) 0.0063(16) -0.0002(16) 0.0136(17) C22 0.055(2) 0.037(2) 0.039(2) 0.0085(16) -0.0024(18) 0.0171(18) C22A 0.062(2) 0.044(2) 0.035(2) 0.0017(17) -0.0019(18) 0.0120(19) C22B 0.096(3) 0.046(3) 0.058(3) 0.000(2) -0.013(2) 0.007(2) C22C 0.070(3) 0.052(3) 0.051(3) -0.001(2) 0.002(2) 0.012(2) C22D 0.075(3) 0.073(3) 0.051(3) -0.003(2) -0.001(2) 0.012(2) C22E 0.095(4) 0.112(4) 0.047(3) -0.002(3) -0.007(3) 0.017(3) C22F 0.098(4) 0.147(6) 0.070(4) -0.025(4) -0.026(3) -0.006(4) C22G 0.117(5) 0.118(5) 0.099(4) -0.014(4) -0.028(4) -0.026(4) C22H 0.092(4) 0.072(3) 0.085(3) -0.002(3) -0.010(3) -0.008(3) C23 0.052(2) 0.034(2) 0.035(2) 0.0071(16) 0.0006(17) 0.0134(17) C24 0.055(2) 0.041(2) 0.042(2) 0.0095(18) -0.0054(19) 0.0197(19) C25 0.063(3) 0.044(2) 0.041(2) 0.0177(18) 0.000(2) 0.014(2) C26 0.049(2) 0.040(2) 0.041(2) 0.0090(17) -0.0004(18) 0.0081(18) C27 0.049(2) 0.037(2) 0.0334(19) 0.0090(16) -0.0016(17) 0.0057(17) C28 0.057(2) 0.036(2) 0.036(2) 0.0103(16) -0.0069(18) 0.0060(18) C29 0.124(5) 0.152(5) 0.076(4) 0.018(4) 0.014(3) 0.059(4) C30 0.089(3) 0.084(3) 0.057(3) 0.005(2) -0.011(2) 0.023(3) O1 0.090(2) 0.0588(18) 0.0436(15) 0.0155(13) 0.0083(14) 0.0127(17) O2 0.0822(19) 0.0470(17) 0.0433(15) -0.0001(12) -0.0035(14) 0.0178(14) O3 0.0603(19) 0.0469(16) 0.0589(17) -0.0062(13) 0.0068(13) 0.0160(13) O4 0.0499(16) 0.0482(16) 0.0532(16) -0.0051(13) 0.0031(13) 0.0058(12) O5 0.0613(18) 0.0483(17) 0.0655(18) 0.0101(13) -0.0176(13) 0.0062(13) O6 0.0671(17) 0.0477(17) 0.0493(15) 0.0175(13) -0.0059(14) 0.0221(13) O7 0.0730(18) 0.0577(18) 0.0570(17) 0.0287(13) 0.0089(14) 0.0303(14) O8 0.0535(16) 0.0617(17) 0.0471(15) 0.0231(13) 0.0138(13) 0.0149(13) O9 0.116(2) 0.0616(19) 0.0632(18) 0.0267(16) -0.0070(17) 0.0210(19) O10 0.065(2) 0.209(4) 0.084(2) 0.037(3) -0.0169(19) 0.031(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 C27 1.521(4) . ? C1 C2 1.526(4) . ? C1 C1A 1.544(4) . ? C1A C1B 1.528(4) . ? C1B C1C 1.504(4) . ? C1C C1H 1.360(5) . ? C1C C1D 1.368(5) . ? C1D C1E 1.374(6) . ? C1E C1F 1.337(7) . ? C1F C1G 1.354(7) . ? C1G C1H 1.370(6) . ? C2 C7 1.390(4) . ? C2 C3 1.402(4) . ? C3 C4 1.367(4) . ? C3 O1 1.368(4) . ? C4 C5 1.373(4) . ? C5 O2 1.388(3) . ? C5 C6 1.391(4) . ? C6 C7 1.386(4) . ? C6 C8 1.525(4) . ? C8 C9 1.506(4) . ? C8 C8A 1.543(4) . ? C8A C8B 1.530(4) . ? C8B C8C 1.506(5) . ? C8C C8D 1.367(5) . ? C8C C8H 1.380(5) . ? C8D C8E 1.386(7) . ? C8E C8F 1.351(8) . ? C8F C8G 1.364(8) . ? C8G C8H 1.369(6) . ? C9 C10 1.396(4) . ? C9 C14 1.396(4) . ? C10 C11 1.365(4) . ? C10 O3 1.388(3) . ? C11 C12 1.377(4) . ? C12 C13 1.387(4) . ? C12 O4 1.388(4) . ? C13 C14 1.388(4) . ? C13 C15 1.529(4) . ? C15 C16 1.524(4) . ? C15 C15A 1.524(4) . ? C15A C15B 1.521(4) . ? C15B C15C 1.500(4) . ? C15C C15H 1.364(5) . ? C15C C15D 1.368(5) . ? C15D C15E 1.396(5) . ? C15E C15F 1.345(6) . ? C15F C15G 1.367(6) . ? C15G C15H 1.378(6) . ? C16 C21 1.385(4) . ? C16 C17 1.388(4) . ? C17 C18 1.380(4) . ? C17 O5 1.388(4) . ? C18 C19 1.373(4) . ? C19 O6 1.384(3) . ? C19 C20 1.392(4) . ? C20 C21 1.403(4) . ? C20 C22 1.506(4) . ? C22 C23 1.525(4) . ? C22 C22A 1.530(4) . ? C22A C22B 1.513(4) . ? C22B C22C 1.497(5) . ? C22C C22D 1.363(5) . ? C22C C22H 1.378(5) . ? C22D C22E 1.390(5) . ? C22E C22F 1.350(7) . ? C22F C22G 1.369(7) . ? C22G C22H 1.371(6) . ? C23 C28 1.378(4) . ? C23 C24 1.398(4) . ? C24 O7 1.372(4) . ? C24 C25 1.385(4) . ? C25 C26 1.371(4) . ? C26 O8 1.390(4) . ? C26 C27 1.406(4) . ? C27 C28 1.388(4) . ? C29 O10 1.392(5) . ? C30 O9 1.397(4) . ? 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 C27 C1 C2 111.0(3) . . ? C27 C1 C1A 112.5(3) . . ? C2 C1 C1A 112.7(3) . . ? C1B C1A C1 113.3(3) . . ? C1C C1B C1A 112.5(3) . . ? C1H C1C C1D 117.1(4) . . ? C1H C1C C1B 120.9(4) . . ? C1D C1C C1B 122.0(4) . . ? C1C C1D C1E 121.3(4) . . ? C1F C1E C1D 120.6(5) . . ? C1E C1F C1G 119.2(5) . . ? C1F C1G C1H 120.5(5) . . ? C1C C1H C1G 121.3(4) . . ? C7 C2 C3 116.5(3) . . ? C7 C2 C1 122.2(3) . . ? C3 C2 C1 121.3(3) . . ? C4 C3 O1 115.9(3) . . ? C4 C3 C2 121.0(3) . . ? O1 C3 C2 123.1(3) . . ? C3 C4 C5 120.2(3) . . ? C4 C5 O2 120.7(3) . . ? C4 C5 C6 122.1(3) . . ? O2 C5 C6 117.2(3) . . ? C7 C6 C5 115.8(3) . . ? C7 C6 C8 123.2(3) . . ? C5 C6 C8 120.9(3) . . ? C6 C7 C2 124.4(3) . . ? C9 C8 C6 110.6(2) . . ? C9 C8 C8A 112.9(3) . . ? C6 C8 C8A 113.1(3) . . ? C8B C8A C8 113.5(3) . . ? C8C C8B C8A 114.7(3) . . ? C8D C8C C8H 118.8(4) . . ? C8D C8C C8B 121.3(4) . . ? C8H C8C C8B 119.9(4) . . ? C8C C8D C8E 120.2(5) . . ? C8F C8E C8D 120.6(6) . . ? C8E C8F C8G 119.5(6) . . ? C8F C8G C8H 120.7(6) . . ? C8G C8H C8C 120.2(4) . . ? C10 C9 C14 115.5(3) . . ? C10 C9 C8 122.2(3) . . ? C14 C9 C8 122.3(3) . . ? C11 C10 O3 116.1(3) . . ? C11 C10 C9 122.4(3) . . ? O3 C10 C9 121.5(3) . . ? C10 C11 C12 119.6(3) . . ? C11 C12 C13 121.8(3) . . ? C11 C12 O4 115.3(3) . . ? C13 C12 O4 122.9(3) . . ? C12 C13 C14 116.4(3) . . ? C12 C13 C15 122.6(3) . . ? C14 C13 C15 121.0(3) . . ? C13 C14 C9 124.3(3) . . ? C16 C15 C15A 113.4(3) . . ? C16 C15 C13 110.4(2) . . ? C15A C15 C13 113.3(3) . . ? C15B C15A C15 111.9(3) . . ? C15C C15B C15A 113.7(3) . . ? C15H C15C C15D 117.3(4) . . ? C15H C15C C15B 120.7(4) . . ? C15D C15C C15B 122.1(4) . . ? C15C C15D C15E 121.0(4) . . ? C15F C15E C15D 120.1(4) . . ? C15E C15F C15G 120.0(4) . . ? C15F C15G C15H 119.2(5) . . ? C15C C15H C15G 122.4(4) . . ? C21 C16 C17 116.2(3) . . ? C21 C16 C15 123.2(3) . . ? C17 C16 C15 120.6(3) . . ? C18 C17 C16 122.1(3) . . ? C18 C17 O5 120.9(3) . . ? C16 C17 O5 117.0(3) . . ? C19 C18 C17 119.4(3) . . ? C18 C19 O6 115.4(3) . . ? C18 C19 C20 122.2(3) . . ? O6 C19 C20 122.4(3) . . ? C19 C20 C21 115.7(3) . . ? C19 C20 C22 121.8(3) . . ? C21 C20 C22 122.5(3) . . ? C16 C21 C20 124.4(3) . . ? C20 C22 C23 110.8(3) . . ? C20 C22 C22A 115.5(3) . . ? C23 C22 C22A 111.7(3) . . ? C22B C22A C22 110.6(3) . . ? C22C C22B C22A 118.1(3) . . ? C22D C22C C22H 118.1(4) . . ? C22D C22C C22B 123.1(4) . . ? C22H C22C C22B 118.8(4) . . ? C22C C22D C22E 122.1(4) . . ? C22F C22E C22D 118.5(5) . . ? C22E C22F C22G 120.5(5) . . ? C22F C22G C22H 120.6(5) . . ? C22G C22H C22C 120.2(5) . . ? C28 C23 C24 116.5(3) . . ? C28 C23 C22 122.6(3) . . ? C24 C23 C22 120.9(3) . . ? O7 C24 C25 121.7(3) . . ? O7 C24 C23 117.3(3) . . ? C25 C24 C23 121.0(3) . . ? C26 C25 C24 120.0(3) . . ? C25 C26 O8 119.3(3) . . ? C25 C26 C27 121.8(3) . . ? O8 C26 C27 118.8(3) . . ? C28 C27 C26 115.5(3) . . ? C28 C27 C1 122.8(3) . . ? C26 C27 C1 121.7(3) . . ? C23 C28 C27 125.2(3) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 28.03 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.291 _refine_diff_density_min -0.197 _refine_diff_density_rms 0.041 ######END data_als500 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'resorcinarene' _chemical_melting_point ? _chemical_formula_moiety 'C46 H59 N3 O17' _chemical_formula_sum 'C46 H59 N3 O17' _chemical_formula_weight 925.96 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4558(10) _cell_length_b 11.6273(10) _cell_length_c 18.6627(16) _cell_angle_alpha 102.785(2) _cell_angle_beta 90.042(2) _cell_angle_gamma 102.881(2) _cell_volume 2360.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.100 _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 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21800 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_sigmaI/netI 0.0641 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.12 _diffrn_reflns_theta_max 28.06 _reflns_number_total 11082 _reflns_number_gt 7603 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1159P)^2^+0.2774P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11082 _refine_ls_number_parameters 639 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0909 _refine_ls_R_factor_gt 0.0620 _refine_ls_wR_factor_ref 0.2055 _refine_ls_wR_factor_gt 0.1786 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.40566(19) 1.0746(2) 0.21298(11) 0.0186(4) Uani 1 1 d . . . H1 H 0.4003 0.9968 0.2286 0.022 Uiso 1 1 calc R . . C1A C 0.41017(19) 1.0460(2) 0.12897(12) 0.0207(5) Uani 1 1 d . . . H1A1 H 0.4087 1.1200 0.1114 0.025 Uiso 1 1 calc R . . H1A2 H 0.4868 1.0233 0.1153 0.025 Uiso 1 1 calc R . . C1B C 0.3074(2) 0.9446(2) 0.09032(14) 0.0310(6) Uani 1 1 d . . . H1B1 H 0.2305 0.9658 0.1051 0.037 Uiso 1 1 calc R . . H1B2 H 0.3105 0.8695 0.1063 0.037 Uiso 1 1 calc R . . C1C C 0.3114(3) 0.9209(3) 0.00709(15) 0.0467(8) Uani 1 1 d . . . H1C1 H 0.3053 0.9940 -0.0092 0.070 Uiso 1 1 calc R . . H1C2 H 0.2442 0.8541 -0.0153 0.070 Uiso 1 1 calc R . . H1C3 H 0.3871 0.8994 -0.0079 0.070 Uiso 1 1 calc R . . C2 C 0.51755(19) 1.1625(2) 0.25175(12) 0.0194(4) Uani 1 1 d . . . C3 C 0.55371(19) 1.15827(19) 0.32256(12) 0.0190(4) Uani 1 1 d . . . C4 C 0.6519(2) 1.2411(2) 0.35988(11) 0.0192(4) Uani 1 1 d . . . C5 C 0.71726(19) 1.3312(2) 0.32818(12) 0.0192(4) Uani 1 1 d . . . C6 C 0.68494(19) 1.3372(2) 0.25723(12) 0.0180(4) Uani 1 1 d . . . C7 C 0.5855(2) 1.2530(2) 0.22108(12) 0.0201(4) Uani 1 1 d . . . H7 H 0.5625 1.2572 0.1730 0.024 Uiso 1 1 calc R . . C8 C 0.76029(19) 1.4345(2) 0.22289(12) 0.0193(4) Uani 1 1 d . . . H8 H 0.8456 1.4446 0.2398 0.023 Uiso 1 1 calc R . . C8A C 0.7543(2) 1.3980(2) 0.13844(12) 0.0234(5) Uani 1 1 d . . . H8A1 H 0.7702 1.3160 0.1229 0.028 Uiso 1 1 calc R . . H8A2 H 0.6722 1.3938 0.1198 0.028 Uiso 1 1 calc R . . C8B C 0.8433(2) 1.4850(2) 0.10359(14) 0.0308(6) Uani 1 1 d . . . H8B1 H 0.8307 1.5679 0.1210 0.037 Uiso 1 1 calc R . . H8B2 H 0.9259 1.4855 0.1196 0.037 Uiso 1 1 calc R . . C8C C 0.8305(3) 1.4506(3) 0.02075(15) 0.0481(8) Uani 1 1 d . . . H8C1 H 0.8468 1.3701 0.0031 0.072 Uiso 1 1 calc R . . H8C2 H 0.8876 1.5100 0.0006 0.072 Uiso 1 1 calc R . . H8C3 H 0.7486 1.4492 0.0046 0.072 Uiso 1 1 calc R . . C9 C 0.72813(19) 1.5565(2) 0.25075(12) 0.0196(4) Uani 1 1 d . . . C10 C 0.80370(19) 1.6510(2) 0.30058(12) 0.0201(4) Uani 1 1 d . . . C11 C 0.7734(2) 1.7631(2) 0.32201(12) 0.0213(5) Uani 1 1 d . . . C12 C 0.6697(2) 1.7825(2) 0.29321(12) 0.0216(5) Uani 1 1 d . . . C13 C 0.59220(19) 1.6896(2) 0.24318(12) 0.0194(4) Uani 1 1 d . . . C14 C 0.6228(2) 1.5779(2) 0.22456(12) 0.0215(5) Uani 1 1 d . . . H14 H 0.5691 1.5128 0.1923 0.026 Uiso 1 1 calc R . . C15 C 0.4796(2) 1.7087(2) 0.20858(12) 0.0212(5) Uani 1 1 d . . . H15 H 0.4825 1.7975 0.2226 0.025 Uiso 1 1 calc R . . C15A C 0.4769(2) 1.6728(2) 0.12463(13) 0.0253(5) Uani 1 1 d . . . H15A H 0.4800 1.5865 0.1092 0.030 Uiso 1 1 calc R . . H15B H 0.4000 1.6813 0.1046 0.030 Uiso 1 1 calc R . . C15B C 0.5799(2) 1.7485(3) 0.09158(15) 0.0336(6) Uani 1 1 d . . . H15C H 0.5752 1.8346 0.1053 0.040 Uiso 1 1 calc R . . H15D H 0.6569 1.7422 0.1126 0.040 Uiso 1 1 calc R . . C15C C 0.5775(3) 1.7085(3) 0.00865(16) 0.0476(8) Uani 1 1 d . . . H15E H 0.5838 1.6239 -0.0052 0.071 Uiso 1 1 calc R . . H15F H 0.6450 1.7597 -0.0100 0.071 Uiso 1 1 calc R . . H15G H 0.5020 1.7161 -0.0125 0.071 Uiso 1 1 calc R . . C16 C 0.36870(19) 1.64465(19) 0.24131(12) 0.0190(4) Uani 1 1 d . . . C17 C 0.3394(2) 1.6977(2) 0.31188(12) 0.0212(5) Uani 1 1 d . . . C18 C 0.2405(2) 1.6432(2) 0.34442(12) 0.0206(5) Uani 1 1 d . . . C19 C 0.17006(19) 1.5314(2) 0.30863(12) 0.0205(5) Uani 1 1 d . . . C20 C 0.19640(19) 1.4741(2) 0.23847(12) 0.0186(4) Uani 1 1 d . . . C21 C 0.2953(2) 1.5339(2) 0.20642(12) 0.0194(4) Uani 1 1 d . . . H21 H 0.3132 1.4969 0.1583 0.023 Uiso 1 1 calc R . . C22 C 0.12121(19) 1.3499(2) 0.20110(12) 0.0196(4) Uani 1 1 d . . . H22 H 0.0364 1.3497 0.2140 0.024 Uiso 1 1 calc R . . C22A C 0.1218(2) 1.3211(2) 0.11722(13) 0.0250(5) Uani 1 1 d . . . H22A H 0.1019 1.3886 0.0991 0.030 Uiso 1 1 calc R . . H22B H 0.2035 1.3149 0.1023 0.030 Uiso 1 1 calc R . . C22B C 0.0333(2) 1.2038(3) 0.08132(15) 0.0359(6) Uani 1 1 d . . . H22C H 0.0532 1.1363 0.0994 0.043 Uiso 1 1 calc R . . H22D H -0.0484 1.2099 0.0963 0.043 Uiso 1 1 calc R . . C22C C 0.0337(3) 1.1752(3) -0.00128(16) 0.0476(8) Uani 1 1 d . . . H22E H 0.0106 1.2400 -0.0198 0.071 Uiso 1 1 calc R . . H22F H -0.0236 1.0983 -0.0214 0.071 Uiso 1 1 calc R . . H22G H 0.1142 1.1687 -0.0166 0.071 Uiso 1 1 calc R . . C23 C 0.1573(2) 1.2522(2) 0.23314(12) 0.0223(5) Uani 1 1 d . . . C24 C 0.0896(2) 1.2033(2) 0.28533(13) 0.0248(5) Uani 1 1 d . . . C25 C 0.1239(2) 1.1151(2) 0.31522(13) 0.0249(5) Uani 1 1 d . . . C26 C 0.2248(2) 1.0746(2) 0.29177(12) 0.0217(5) Uani 1 1 d . . . C27 C 0.2942(2) 1.1203(2) 0.23916(12) 0.0205(4) Uani 1 1 d . . . C28 C 0.2607(2) 1.2115(2) 0.21202(12) 0.0204(4) Uani 1 1 d . . . H28 H 0.3099 1.2470 0.1781 0.025 Uiso 1 1 calc R . . CN1 C 0.4416(3) 1.4434(3) 0.36170(16) 0.0551(9) Uani 1 1 d . . . HN1A H 0.3688 1.3832 0.3404 0.083 Uiso 1 1 calc R . . HN1B H 0.5025 1.4021 0.3734 0.083 Uiso 1 1 calc R . . HN1C H 0.4722 1.4922 0.3263 0.083 Uiso 1 1 calc R . . CN2 C 0.4140(3) 1.5212(3) 0.42808(15) 0.0411(7) Uani 1 1 d . . . O1 O 0.49466(14) 1.07141(15) 0.35725(9) 0.0246(4) Uani 1 1 d . . . H1A H 0.4223 1.0496 0.3422 0.037 Uiso 1 1 calc R . . O2 O 0.68657(15) 1.23056(15) 0.42900(8) 0.0237(4) Uani 1 1 d . . . H2 H 0.6692 1.2862 0.4613 0.036 Uiso 1 1 calc R . . O03 O 0.92966(17) 1.38867(19) 0.48405(10) 0.0398(5) Uani 1 1 d . . . O3 O 0.81309(14) 1.41579(15) 0.36497(9) 0.0235(4) Uani 1 1 d . . . H3 H 0.8366 1.3917 0.4005 0.035 Uiso 1 1 calc R . . O4 O 0.91135(14) 1.64368(15) 0.32972(9) 0.0254(4) Uani 1 1 d . . . H4 H 0.9050 1.5747 0.3384 0.038 Uiso 1 1 calc R . . O5 O 0.85030(15) 1.85170(15) 0.37120(9) 0.0268(4) Uani 1 1 d . . . H5 H 0.8266 1.9164 0.3777 0.040 Uiso 1 1 calc R . . O6 O 0.65151(15) 1.89819(14) 0.31534(10) 0.0271(4) Uani 1 1 d . . . H6 H 0.5808 1.8947 0.3282 0.041 Uiso 1 1 calc R . . O7 O 0.41143(15) 1.80587(15) 0.34792(9) 0.0283(4) Uani 1 1 d . . . H7A H 0.3898 1.8245 0.3911 0.042 Uiso 1 1 calc R . . O8 O 0.21592(15) 1.69931(15) 0.41335(8) 0.0251(4) Uani 1 1 d . . . H8A H 0.1783 1.7524 0.4102 0.038 Uiso 1 1 calc R . . O9 O 0.07526(15) 1.48558(15) 0.34714(9) 0.0260(4) Uani 1 1 d . . . H9 H 0.0526 1.4104 0.3306 0.039 Uiso 1 1 calc R . . O10 O -0.01194(15) 1.24206(16) 0.31093(10) 0.0306(4) Uani 1 1 d . . . H10 H -0.0734 1.1904 0.2912 0.046 Uiso 1 1 calc R . . O010 O -0.14280(15) 1.09060(15) 0.43307(9) 0.0261(4) Uani 1 1 d . . . O11 O 0.06161(17) 1.06732(17) 0.36744(11) 0.0343(4) Uani 1 1 d . . . H11 H 0.0009 1.0965 0.3760 0.051 Uiso 1 1 calc R . . O12 O 0.25185(14) 0.98463(15) 0.32188(9) 0.0257(4) Uani 1 1 d . . . H12 H 0.3067 0.9578 0.2988 0.039 Uiso 1 1 calc R . . O012 O 0.09079(17) 0.86820(17) 0.41648(10) 0.0357(4) Uani 1 1 d . . . O020 O -0.18545(19) 1.0637(2) 0.24004(12) 0.0477(5) Uani 1 1 d . . . N1 N 0.3905(3) 1.5816(3) 0.47976(14) 0.0572(8) Uani 1 1 d . . . N3 N -0.0569(3) 0.8789(3) 0.18897(16) 0.0578(8) Uani 1 1 d . . . CN5 C 0.0085(3) 0.8193(3) 0.19399(15) 0.0406(7) Uani 1 1 d . . . CN6 C 0.0911(3) 0.7449(3) 0.20027(18) 0.0455(7) Uani 1 1 d . . . HN6A H 0.1661 0.7960 0.2254 0.068 Uiso 1 1 calc R . . HN6B H 0.1073 0.7027 0.1511 0.068 Uiso 1 1 calc R . . HN6C H 0.0560 0.6853 0.2287 0.068 Uiso 1 1 calc R . . N2 N 0.6478(18) 1.8287(15) 0.5116(8) 0.099(5) Uani 0.482(12) 1 d P A 1 CN3 C 0.7865(16) 1.6841(11) 0.4953(8) 0.055(3) Uani 0.482(12) 1 d P A 1 HN3A H 0.8057 1.6686 0.5429 0.082 Uiso 0.482(12) 1 calc PR A 1 HN3B H 0.8605 1.7207 0.4746 0.082 Uiso 0.482(12) 1 calc PR A 1 HN3C H 0.7477 1.6075 0.4616 0.082 Uiso 0.482(12) 1 calc PR A 1 CN4 C 0.6995(9) 1.7728(11) 0.5058(5) 0.037(2) Uani 0.482(12) 1 d P A 1 N4 N 0.8619(8) 1.6855(7) 0.5121(4) 0.065(2) Uani 0.518(12) 1 d P A 2 CN7 C 0.7833(11) 1.7305(10) 0.5101(5) 0.046(3) Uani 0.518(12) 1 d P A 2 CN8 C 0.6689(6) 1.7871(5) 0.5006(4) 0.148(19) Uani 0.518(12) 1 d P A 2 HN8A H 0.6962 1.8743 0.5037 0.221 Uiso 0.518(12) 1 calc PR A 2 HN8B H 0.6140 1.7738 0.5398 0.221 Uiso 0.518(12) 1 calc PR A 2 HN8C H 0.6272 1.7476 0.4527 0.221 Uiso 0.518(12) 1 calc PR A 2 H1X H -0.2138 1.1277 0.4454 0.097(15) Uiso 1 1 d R . . H1Y H -0.1431 1.0919 0.4876 0.091(14) Uiso 1 1 d R . . O07 O 0.3872(5) 1.9330(4) 0.4816(2) 0.0631(13) Uiso 0.50 1 d PR . . O07A O 0.4618(5) 1.9654(5) 0.4850(3) 0.0523(19) Uiso 0.30 1 d PR . . 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 0.0185(10) 0.0168(11) 0.0194(10) 0.0036(8) -0.0005(8) 0.0020(8) C1A 0.0185(11) 0.0186(11) 0.0228(11) 0.0026(9) 0.0006(8) 0.0021(9) C1B 0.0283(13) 0.0305(14) 0.0263(12) -0.0032(10) 0.0010(10) 0.0002(11) C1C 0.0451(17) 0.0520(19) 0.0272(14) -0.0084(13) -0.0008(12) -0.0041(14) C2 0.0174(10) 0.0203(11) 0.0202(10) 0.0031(8) -0.0012(8) 0.0052(9) C3 0.0192(11) 0.0160(10) 0.0238(11) 0.0077(8) 0.0030(8) 0.0052(8) C4 0.0214(11) 0.0230(11) 0.0154(10) 0.0045(8) -0.0007(8) 0.0096(9) C5 0.0177(10) 0.0191(11) 0.0208(10) 0.0025(8) -0.0016(8) 0.0063(9) C6 0.0178(10) 0.0171(11) 0.0197(10) 0.0039(8) 0.0020(8) 0.0056(8) C7 0.0223(11) 0.0213(11) 0.0187(10) 0.0059(8) -0.0011(8) 0.0076(9) C8 0.0174(10) 0.0188(11) 0.0209(10) 0.0030(8) -0.0006(8) 0.0041(9) C8A 0.0255(12) 0.0209(12) 0.0228(11) 0.0044(9) 0.0016(9) 0.0034(9) C8B 0.0300(13) 0.0327(14) 0.0303(13) 0.0124(11) 0.0039(10) 0.0032(11) C8C 0.057(2) 0.057(2) 0.0303(15) 0.0196(14) 0.0098(13) 0.0031(16) C9 0.0201(11) 0.0204(11) 0.0189(10) 0.0060(8) 0.0032(8) 0.0046(9) C10 0.0170(10) 0.0214(11) 0.0222(11) 0.0066(9) 0.0010(8) 0.0035(9) C11 0.0215(11) 0.0162(11) 0.0238(11) 0.0033(9) 0.0006(9) 0.0008(9) C12 0.0223(11) 0.0182(11) 0.0248(11) 0.0054(9) 0.0042(9) 0.0051(9) C13 0.0185(10) 0.0186(11) 0.0224(11) 0.0076(9) 0.0034(8) 0.0042(9) C14 0.0210(11) 0.0182(11) 0.0237(11) 0.0045(9) -0.0003(8) 0.0012(9) C15 0.0205(11) 0.0192(11) 0.0249(11) 0.0072(9) 0.0015(9) 0.0046(9) C15A 0.0249(12) 0.0293(13) 0.0246(12) 0.0118(10) 0.0039(9) 0.0068(10) C15B 0.0310(14) 0.0355(15) 0.0372(14) 0.0173(12) 0.0069(11) 0.0046(11) C15C 0.0479(18) 0.064(2) 0.0372(16) 0.0262(15) 0.0162(13) 0.0107(16) C16 0.0197(11) 0.0155(11) 0.0241(11) 0.0072(8) 0.0004(8) 0.0059(9) C17 0.0194(11) 0.0202(11) 0.0239(11) 0.0037(9) -0.0006(8) 0.0055(9) C18 0.0235(11) 0.0222(12) 0.0178(10) 0.0024(9) 0.0023(8) 0.0110(9) C19 0.0196(11) 0.0222(11) 0.0235(11) 0.0100(9) 0.0031(8) 0.0075(9) C20 0.0190(10) 0.0184(11) 0.0198(10) 0.0057(8) 0.0001(8) 0.0058(9) C21 0.0235(11) 0.0191(11) 0.0178(10) 0.0053(8) 0.0022(8) 0.0083(9) C22 0.0163(10) 0.0198(11) 0.0227(11) 0.0054(9) 0.0028(8) 0.0035(9) C22A 0.0224(11) 0.0263(13) 0.0256(12) 0.0044(9) -0.0036(9) 0.0056(10) C22B 0.0326(14) 0.0341(15) 0.0338(14) -0.0018(11) -0.0073(11) 0.0017(12) C22C 0.0479(18) 0.0505(19) 0.0355(15) -0.0055(13) -0.0128(13) 0.0081(15) C23 0.0217(11) 0.0187(11) 0.0246(11) 0.0030(9) 0.0001(9) 0.0027(9) C24 0.0235(12) 0.0202(12) 0.0295(12) 0.0039(9) 0.0058(9) 0.0041(9) C25 0.0250(12) 0.0221(12) 0.0264(12) 0.0068(9) 0.0078(9) 0.0013(9) C26 0.0238(11) 0.0190(11) 0.0208(11) 0.0053(9) 0.0002(9) 0.0009(9) C27 0.0208(11) 0.0179(11) 0.0201(10) 0.0009(8) -0.0013(8) 0.0027(9) C28 0.0203(11) 0.0204(11) 0.0197(10) 0.0054(8) 0.0023(8) 0.0019(9) CN1 0.081(2) 0.068(2) 0.0295(15) 0.0044(15) 0.0027(15) 0.052(2) CN2 0.0514(18) 0.0489(18) 0.0315(14) 0.0071(13) -0.0052(12) 0.0313(15) O1 0.0186(8) 0.0241(9) 0.0310(9) 0.0120(7) -0.0021(7) -0.0007(7) O2 0.0291(9) 0.0268(9) 0.0167(7) 0.0059(6) -0.0022(6) 0.0087(7) O03 0.0351(10) 0.0496(12) 0.0307(10) 0.0153(9) -0.0033(8) -0.0046(9) O3 0.0216(8) 0.0242(9) 0.0220(8) 0.0061(6) -0.0057(6) -0.0008(7) O4 0.0208(8) 0.0203(8) 0.0344(9) 0.0059(7) -0.0062(7) 0.0035(7) O5 0.0242(8) 0.0186(8) 0.0334(9) -0.0016(7) -0.0062(7) 0.0036(7) O6 0.0230(8) 0.0170(8) 0.0396(10) 0.0020(7) 0.0000(7) 0.0053(7) O7 0.0271(9) 0.0230(9) 0.0291(9) -0.0028(7) 0.0021(7) 0.0025(7) O8 0.0288(9) 0.0267(9) 0.0208(8) 0.0025(7) 0.0040(6) 0.0111(7) O9 0.0275(9) 0.0213(9) 0.0287(9) 0.0067(7) 0.0097(7) 0.0037(7) O10 0.0249(9) 0.0235(9) 0.0440(11) 0.0087(8) 0.0144(8) 0.0058(7) O010 0.0288(9) 0.0284(9) 0.0230(8) 0.0056(7) 0.0040(7) 0.0109(7) O11 0.0338(10) 0.0347(11) 0.0437(11) 0.0223(9) 0.0216(8) 0.0136(8) O12 0.0225(9) 0.0271(9) 0.0328(9) 0.0148(7) 0.0064(7) 0.0084(7) O012 0.0411(11) 0.0364(11) 0.0316(9) 0.0022(8) -0.0094(8) 0.0187(9) O020 0.0378(11) 0.0469(13) 0.0555(13) 0.0056(10) 0.0062(10) 0.0096(10) N1 0.082(2) 0.072(2) 0.0292(13) -0.0019(13) -0.0067(13) 0.0535(18) N3 0.0643(19) 0.065(2) 0.0471(16) 0.0084(14) 0.0096(14) 0.0243(17) CN5 0.0448(17) 0.0451(18) 0.0271(13) 0.0053(12) 0.0025(12) 0.0034(14) CN6 0.0410(17) 0.0464(18) 0.0488(18) 0.0171(14) -0.0041(13) 0.0032(14) N2 0.165(12) 0.066(7) 0.060(7) -0.020(5) -0.013(7) 0.049(8) CN3 0.062(7) 0.057(8) 0.040(7) -0.003(5) 0.002(5) 0.019(7) CN4 0.021(4) 0.062(7) 0.023(4) 0.009(4) 0.003(3) 0.001(3) N4 0.066(5) 0.076(5) 0.055(4) 0.010(3) 0.000(3) 0.026(4) CN7 0.051(6) 0.058(7) 0.018(4) 0.001(4) 0.012(3) -0.001(6) CN8 0.19(4) 0.12(3) 0.082(14) -0.015(15) 0.006(16) -0.04(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.516(3) . ? C1 C27 1.529(3) . ? C1 C1A 1.533(3) . ? C1A C1B 1.517(3) . ? C1B C1C 1.519(4) . ? C2 C7 1.394(3) . ? C2 C3 1.399(3) . ? C3 O1 1.372(3) . ? C3 C4 1.377(3) . ? C4 O2 1.388(2) . ? C4 C5 1.391(3) . ? C5 O3 1.365(3) . ? C5 C6 1.396(3) . ? C6 C7 1.386(3) . ? C6 C8 1.524(3) . ? C8 C9 1.525(3) . ? C8 C8A 1.536(3) . ? C8A C8B 1.522(3) . ? C8B C8C 1.507(4) . ? C9 C14 1.394(3) . ? C9 C10 1.394(3) . ? C10 O4 1.375(3) . ? C10 C11 1.397(3) . ? C11 O5 1.362(3) . ? C11 C12 1.387(3) . ? C12 O6 1.380(3) . ? C12 C13 1.397(3) . ? C13 C14 1.390(3) . ? C13 C15 1.523(3) . ? C15 C16 1.524(3) . ? C15 C15A 1.528(3) . ? C15A C15B 1.525(3) . ? C15B C15C 1.513(4) . ? C16 C21 1.391(3) . ? C16 C17 1.401(3) . ? C17 O7 1.370(3) . ? C17 C18 1.381(3) . ? C18 O8 1.368(3) . ? C18 C19 1.391(3) . ? C19 O9 1.376(3) . ? C19 C20 1.398(3) . ? C20 C21 1.399(3) . ? C20 C22 1.520(3) . ? C22 C22A 1.527(3) . ? C22 C23 1.526(3) . ? C22A C22B 1.522(3) . ? C22B C22C 1.503(4) . ? C23 C24 1.386(3) . ? C23 C28 1.397(3) . ? C24 O10 1.388(3) . ? C24 C25 1.396(3) . ? C25 O11 1.353(3) . ? C25 C26 1.379(3) . ? C26 O12 1.382(3) . ? C26 C27 1.387(3) . ? C27 C28 1.396(3) . ? CN1 CN2 1.444(4) . ? CN2 N1 1.132(4) . ? N3 CN5 1.145(4) . ? CN5 CN6 1.438(5) . ? N2 CN4 0.96(3) . ? CN3 CN4 1.571(17) . ? N4 CN7 1.143(15) . ? CN7 CN8 1.617(14) . ? O07 O07A 0.850(5) . ? O07A O07A 1.101(12) 2_696 ? 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 C27 110.11(17) . . ? C2 C1 C1A 113.22(18) . . ? C27 C1 C1A 112.35(17) . . ? C1B C1A C1 113.46(19) . . ? C1A C1B C1C 112.5(2) . . ? C7 C2 C3 117.11(19) . . ? C7 C2 C1 122.71(18) . . ? C3 C2 C1 120.13(19) . . ? O1 C3 C4 117.30(19) . . ? O1 C3 C2 121.87(19) . . ? C4 C3 C2 120.8(2) . . ? C3 C4 O2 118.62(19) . . ? C3 C4 C5 120.79(19) . . ? O2 C4 C5 120.57(19) . . ? O3 C5 C4 121.64(18) . . ? O3 C5 C6 118.32(19) . . ? C4 C5 C6 120.0(2) . . ? C7 C6 C5 117.9(2) . . ? C7 C6 C8 123.10(18) . . ? C5 C6 C8 118.99(19) . . ? C6 C7 C2 123.32(19) . . ? C6 C8 C9 111.29(18) . . ? C6 C8 C8A 112.73(18) . . ? C9 C8 C8A 111.75(17) . . ? C8B C8A C8 113.44(19) . . ? C8C C8B C8A 112.1(2) . . ? C14 C9 C10 117.9(2) . . ? C14 C9 C8 120.2(2) . . ? C10 C9 C8 121.82(19) . . ? O4 C10 C9 124.2(2) . . ? O4 C10 C11 115.81(19) . . ? C9 C10 C11 119.92(19) . . ? O5 C11 C12 122.0(2) . . ? O5 C11 C10 117.26(19) . . ? C12 C11 C10 120.7(2) . . ? O6 C12 C11 115.9(2) . . ? O6 C12 C13 123.4(2) . . ? C11 C12 C13 120.7(2) . . ? C14 C13 C12 117.4(2) . . ? C14 C13 C15 120.5(2) . . ? C12 C13 C15 122.11(19) . . ? C13 C14 C9 123.3(2) . . ? C16 C15 C13 109.93(17) . . ? C16 C15 C15A 113.61(19) . . ? C13 C15 C15A 111.61(19) . . ? C15B C15A C15 113.5(2) . . ? C15C C15B C15A 112.4(2) . . ? C21 C16 C17 117.0(2) . . ? C21 C16 C15 124.2(2) . . ? C17 C16 C15 118.71(19) . . ? O7 C17 C18 120.6(2) . . ? O7 C17 C16 118.2(2) . . ? C18 C17 C16 121.2(2) . . ? O8 C18 C17 118.7(2) . . ? O8 C18 C19 120.9(2) . . ? C17 C18 C19 120.4(2) . . ? O9 C19 C18 114.92(19) . . ? O9 C19 C20 124.5(2) . . ? C18 C19 C20 120.6(2) . . ? C21 C20 C19 117.3(2) . . ? C21 C20 C22 122.64(19) . . ? C19 C20 C22 120.01(19) . . ? C16 C21 C20 123.5(2) . . ? C20 C22 C22A 114.29(18) . . ? C20 C22 C23 110.14(17) . . ? C22A C22 C23 111.87(19) . . ? C22B C22A C22 112.8(2) . . ? C22C C22B C22A 113.0(2) . . ? C24 C23 C28 118.1(2) . . ? C24 C23 C22 120.9(2) . . ? C28 C23 C22 121.0(2) . . ? C23 C24 O10 121.5(2) . . ? C23 C24 C25 120.6(2) . . ? O10 C24 C25 117.8(2) . . ? O11 C25 C26 117.9(2) . . ? O11 C25 C24 122.3(2) . . ? C26 C25 C24 119.8(2) . . ? O12 C26 C25 117.0(2) . . ? O12 C26 C27 121.6(2) . . ? C25 C26 C27 121.4(2) . . ? C26 C27 C28 117.8(2) . . ? C26 C27 C1 121.26(19) . . ? C28 C27 C1 120.9(2) . . ? C23 C28 C27 122.2(2) . . ? N1 CN2 CN1 178.9(4) . . ? N3 CN5 CN6 179.7(4) . . ? N2 CN4 CN3 178(2) . . ? N4 CN7 CN8 175.3(10) . . ? O07 O07A O07A 148.8(7) . 2_696 ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.567 _refine_diff_density_min -0.621 _refine_diff_density_rms 0.098 ######END data_asd3a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common pyrrogallolarene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43.40 H49.50 Cl0.50 O16.35' _chemical_formula_weight 850.45 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.26(4) _cell_length_b 24.57(7) _cell_length_c 22.96(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.32(6) _cell_angle_gamma 90.00 _cell_volume 9155(44) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3594 _exptl_absorpt_coefficient_mu 0.122 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28006 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.1921 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 28.06 _reflns_number_total 17149 _reflns_number_gt 5106 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1500P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17149 _refine_ls_number_parameters 1111 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2701 _refine_ls_R_factor_gt 0.0943 _refine_ls_wR_factor_ref 0.3363 _refine_ls_wR_factor_gt 0.2404 _refine_ls_goodness_of_fit_ref 0.923 _refine_ls_restrained_S_all 0.923 _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 C11A C 0.0595(6) 0.8968(3) 0.2313(4) 0.062(2) Uani 1 1 d . . . H11A H 0.0557 0.9124 0.1924 0.075 Uiso 1 1 calc R A 1 H11B H 0.0406 0.9242 0.2578 0.075 Uiso 1 1 calc R A 1 C11B C 0.1366(17) 0.8867(10) 0.2453(11) 0.085(10) Uani 0.358(14) 1 d P B 1 H11C H 0.1406 0.8567 0.2721 0.128 Uiso 0.358(14) 1 calc PR B 1 H11D H 0.1618 0.9183 0.2634 0.128 Uiso 0.358(14) 1 calc PR B 1 H11E H 0.1645 0.8778 0.2108 0.128 Uiso 0.358(14) 1 calc PR B 1 C11C C 0.0554(8) 0.9360(5) 0.2799(5) 0.073(5) Uani 0.642(14) 1 d P B 2 H11F H 0.0776 0.9196 0.3153 0.109 Uiso 0.642(14) 1 calc PR B 2 H11G H -0.0009 0.9461 0.2843 0.109 Uiso 0.642(14) 1 calc PR B 2 H11H H 0.0868 0.9679 0.2715 0.109 Uiso 0.642(14) 1 calc PR B 2 C110 C -0.0347(6) 0.7750(3) -0.0537(3) 0.058(2) Uani 1 1 d . B . C12A C -0.1697(5) 1.0203(3) 0.1571(3) 0.058(2) Uani 1 1 d . . . H12A H -0.1582 1.0308 0.1975 0.069 Uiso 1 1 calc R . . H12B H -0.1184 1.0079 0.1419 0.069 Uiso 1 1 calc R . . C12B C -0.2008(5) 1.0705(3) 0.1219(4) 0.076(3) Uani 1 1 d . . . H12C H -0.2021 1.0624 0.0810 0.114 Uiso 1 1 calc R . . H12D H -0.1645 1.1007 0.1302 0.114 Uiso 1 1 calc R . . H12E H -0.2553 1.0798 0.1327 0.114 Uiso 1 1 calc R . . C15A C -0.1007(5) 0.9818(3) -0.0504(3) 0.066(2) Uani 1 1 d . . . H15A H -0.1343 1.0143 -0.0485 0.079 Uiso 1 1 calc R . . H15B H -0.0654 0.9801 -0.0149 0.079 Uiso 1 1 calc R . . C15B C -0.0491(6) 0.9857(4) -0.1010(4) 0.097(3) Uani 1 1 d . . . H15C H -0.0133 0.9547 -0.1016 0.146 Uiso 1 1 calc R . . H15D H -0.0166 1.0184 -0.0979 0.146 Uiso 1 1 calc R . . H15E H -0.0837 0.9867 -0.1363 0.146 Uiso 1 1 calc R . . C18A C 0.1329(5) 0.8546(3) 0.0265(4) 0.069(2) Uani 1 1 d . . . H18A H 0.1064 0.8849 0.0449 0.083 Uiso 1 1 calc R . . H18B H 0.1440 0.8654 -0.0129 0.083 Uiso 1 1 calc R . . C18B C 0.2146(5) 0.8420(4) 0.0604(4) 0.095(3) Uani 1 1 d . . . H18C H 0.2039 0.8289 0.0986 0.143 Uiso 1 1 calc R . . H18D H 0.2472 0.8746 0.0639 0.143 Uiso 1 1 calc R . . H18E H 0.2440 0.8148 0.0400 0.143 Uiso 1 1 calc R . . C21A C -0.3195(5) 0.4809(3) 0.1342(3) 0.055(2) Uani 1 1 d . . . H21A H -0.3207 0.4691 0.1744 0.065 Uiso 1 1 calc R . . H21B H -0.3742 0.4939 0.1221 0.065 Uiso 1 1 calc R . . C21B C -0.2995(5) 0.4322(3) 0.0968(4) 0.079(3) Uani 1 1 d . . . H21C H -0.3011 0.4429 0.0565 0.118 Uiso 1 1 calc R . . H21D H -0.3392 0.4039 0.1018 0.118 Uiso 1 1 calc R . . H21E H -0.2454 0.4189 0.1084 0.118 Uiso 1 1 calc R . . C22A C -0.5161(4) 0.5992(3) 0.2416(3) 0.057(2) Uani 1 1 d . . . H22A H -0.5246 0.5844 0.2025 0.068 Uiso 1 1 calc R . . H22B H -0.4912 0.5710 0.2664 0.068 Uiso 1 1 calc R . . C22B C -0.5983(5) 0.6142(4) 0.2639(4) 0.089(3) Uani 1 1 d . . . H22C H -0.5900 0.6348 0.2993 0.134 Uiso 1 1 calc R . . H22D H -0.6286 0.5817 0.2714 0.134 Uiso 1 1 calc R . . H22E H -0.6287 0.6358 0.2351 0.134 Uiso 1 1 calc R . . C26A C -0.6606(4) 0.6582(3) 0.0515(3) 0.0516(19) Uani 1 1 d . . . H26A H -0.6832 0.6484 0.0129 0.062 Uiso 1 1 calc R . . H26B H -0.6285 0.6275 0.0668 0.062 Uiso 1 1 calc R . . C26B C -0.7308(5) 0.6689(3) 0.0908(4) 0.078(3) Uani 1 1 d . . . H26C H -0.7087 0.6798 0.1287 0.118 Uiso 1 1 calc R . . H26D H -0.7628 0.6363 0.0942 0.118 Uiso 1 1 calc R . . H26E H -0.7652 0.6974 0.0743 0.118 Uiso 1 1 calc R . . C28A C -0.4589(4) 0.5450(3) -0.0618(3) 0.0519(19) Uani 1 1 d . . . H28A H -0.4785 0.5406 -0.0230 0.062 Uiso 1 1 calc R . . H28B H -0.5061 0.5533 -0.0881 0.062 Uiso 1 1 calc R . . C28B C -0.4201(5) 0.4911(3) -0.0808(4) 0.075(3) Uani 1 1 d . . . H28C H -0.3905 0.4971 -0.1152 0.113 Uiso 1 1 calc R . . H28D H -0.4628 0.4647 -0.0890 0.113 Uiso 1 1 calc R . . H28E H -0.3829 0.4779 -0.0500 0.113 Uiso 1 1 calc R . . C101 C 0.0012(5) 0.8485(3) 0.2322(3) 0.0502(19) Uani 1 1 d . B . H101 H 0.0131 0.8301 0.2696 0.060 Uiso 1 1 calc R . . C102 C 0.0152(4) 0.8065(3) 0.1850(3) 0.0459(18) Uani 1 1 d . . . C103 C 0.0090(4) 0.7510(3) 0.1945(3) 0.0490(19) Uani 1 1 d . B . C104 C 0.0260(5) 0.7136(3) 0.1519(3) 0.056(2) Uani 1 1 d . . . C105 C 0.0437(4) 0.7303(3) 0.0967(3) 0.0505(19) Uani 1 1 d . B . C106 C 0.0508(4) 0.7862(3) 0.0847(3) 0.0511(19) Uani 1 1 d . . . C107 C 0.0352(4) 0.8229(3) 0.1292(3) 0.0509(19) Uani 1 1 d . B . H107 H 0.0383 0.8600 0.1213 0.061 Uiso 1 1 calc . . . C108 C 0.0743(5) 0.8062(3) 0.0237(3) 0.056(2) Uani 1 1 d . B . H108 H 0.1039 0.7762 0.0062 0.067 Uiso 1 1 calc R . . C109 C -0.0018(5) 0.8170(3) -0.0163(3) 0.049(2) Uani 1 1 d . . . C111 C -0.1036(6) 0.7852(3) -0.0897(3) 0.056(2) Uani 1 1 d . . . C112 C -0.1410(5) 0.8359(3) -0.0892(3) 0.056(2) Uani 1 1 d . B . C113 C -0.1127(5) 0.8776(3) -0.0535(3) 0.0475(19) Uani 1 1 d . . . C114 C -0.0427(5) 0.8665(3) -0.0175(3) 0.053(2) Uani 1 1 d . B . H114 H -0.0222 0.8939 0.0071 0.064 Uiso 1 1 calc . . . C115 C -0.1568(5) 0.9319(3) -0.0535(3) 0.052(2) Uani 1 1 d . B . H115 H -0.1882 0.9343 -0.0912 0.062 Uiso 1 1 calc R . . C116 C -0.2195(5) 0.9338(3) -0.0077(3) 0.0477(19) Uani 1 1 d . . . C117 C -0.2996(6) 0.9190(3) -0.0204(3) 0.054(2) Uani 1 1 d . B . C118 C -0.3578(5) 0.9203(3) 0.0216(3) 0.052(2) Uani 1 1 d . . . C119 C -0.3368(5) 0.9387(3) 0.0767(3) 0.0471(19) Uani 1 1 d . B . C120 C -0.2564(5) 0.9535(3) 0.0925(3) 0.0440(18) Uani 1 1 d . . . C121 C -0.1995(4) 0.9508(3) 0.0503(3) 0.0480(19) Uani 1 1 d . B . H121 H -0.1454 0.9607 0.0605 0.058 Uiso 1 1 calc . . . C122 C -0.2320(5) 0.9726(3) 0.1548(3) 0.052(2) Uani 1 1 d . B . H122 H -0.2824 0.9862 0.1713 0.063 Uiso 1 1 calc R . . C123 C -0.2016(5) 0.9245(3) 0.1934(3) 0.0469(19) Uani 1 1 d . . . C124 C -0.2549(5) 0.8957(3) 0.2274(3) 0.0497(19) Uani 1 1 d . B . C125 C -0.2256(5) 0.8543(3) 0.2643(3) 0.0508(19) Uani 1 1 d . . . C126 C -0.1432(5) 0.8403(3) 0.2660(3) 0.0505(19) Uani 1 1 d . B . C127 C -0.0885(5) 0.8655(3) 0.2313(3) 0.0461(18) Uani 1 1 d . . . C128 C -0.1195(5) 0.9079(3) 0.1955(3) 0.0459(18) Uani 1 1 d . B . H128 H -0.0835 0.9258 0.1720 0.055 Uiso 1 1 calc . . . C201 C -0.2587(4) 0.5285(3) 0.1311(3) 0.0456(18) Uani 1 1 d . . . H201 H -0.2039 0.5138 0.1418 0.055 Uiso 1 1 calc R . . C202 C -0.2547(5) 0.5521(3) 0.0704(3) 0.0427(18) Uani 1 1 d . . . C203 C -0.1798(5) 0.5674(3) 0.0496(3) 0.0494(19) Uani 1 1 d . . . C204 C -0.1744(5) 0.5913(3) -0.0049(4) 0.053(2) Uani 1 1 d . . . C205 C -0.2453(5) 0.5997(3) -0.0399(3) 0.0476(19) Uani 1 1 d . . . C206 C -0.3223(4) 0.5850(2) -0.0206(3) 0.0412(18) Uani 1 1 d . . . C207 C -0.3247(5) 0.5612(3) 0.0348(3) 0.0466(19) Uani 1 1 d . . . H207 H -0.3755 0.5513 0.0482 0.056 Uiso 1 1 calc . . . C208 C -0.3983(4) 0.5934(2) -0.0614(3) 0.0446(19) Uani 1 1 d . . . H208 H -0.3784 0.5954 -0.1008 0.053 Uiso 1 1 calc R . . C209 C -0.4418(4) 0.6476(2) -0.0513(3) 0.0383(16) Uani 1 1 d . . . C210 C -0.4270(4) 0.6922(3) -0.0859(3) 0.0486(19) Uani 1 1 d . . . C211 C -0.4702(5) 0.7412(3) -0.0794(3) 0.0475(19) Uani 1 1 d . . . C212 C -0.5271(4) 0.7455(3) -0.0367(3) 0.0458(18) Uani 1 1 d . . . C213 C -0.5429(4) 0.7016(3) -0.0007(3) 0.0410(17) Uani 1 1 d . . . C214 C -0.4993(4) 0.6531(3) -0.0087(3) 0.0430(17) Uani 1 1 d . . . H214 H -0.5090 0.6235 0.0153 0.052 Uiso 1 1 calc . . . C215 C -0.6040(4) 0.7074(3) 0.0467(3) 0.0455(19) Uani 1 1 d . . . H215 H -0.6395 0.7385 0.0358 0.055 Uiso 1 1 calc R . . C216 C -0.5584(4) 0.7221(3) 0.1055(3) 0.0391(17) Uani 1 1 d . . . C217 C -0.5442(4) 0.7754(3) 0.1210(3) 0.0465(18) Uani 1 1 d . . . C218 C -0.5033(4) 0.7891(3) 0.1736(3) 0.049(2) Uani 1 1 d . . . C219 C -0.4751(5) 0.7488(3) 0.2114(3) 0.0484(19) Uani 1 1 d . . . C220 C -0.4874(4) 0.6940(3) 0.1980(3) 0.0449(18) Uani 1 1 d . . . C221 C -0.5278(4) 0.6823(2) 0.1438(3) 0.0406(17) Uani 1 1 d . . . H221 H -0.5343 0.6461 0.1330 0.049 Uiso 1 1 calc . . . C222 C -0.4564(4) 0.6482(3) 0.2401(3) 0.0458(18) Uani 1 1 d . . . H222 H -0.4529 0.6639 0.2794 0.055 Uiso 1 1 calc R . . C223 C -0.3695(5) 0.6308(3) 0.2269(3) 0.0428(18) Uani 1 1 d . . . C224 C -0.3047(5) 0.6550(3) 0.2571(3) 0.050(2) Uani 1 1 d . . . C225 C -0.2247(5) 0.6405(3) 0.2464(3) 0.054(2) Uani 1 1 d . . . C226 C -0.2100(5) 0.5991(3) 0.2060(3) 0.053(2) Uani 1 1 d . . . C227 C -0.2750(5) 0.5732(3) 0.1760(3) 0.0415(18) Uani 1 1 d . . . C228 C -0.3534(4) 0.5911(3) 0.1871(3) 0.0452(18) Uani 1 1 d . . . H228 H -0.3979 0.5752 0.1662 0.054 Uiso 1 1 calc . . . C301 C -0.2629(6) 0.7589(4) 0.4195(4) 0.113(4) Uani 1 1 d . . . H30A H -0.2353 0.7837 0.4463 0.170 Uiso 1 1 calc R . . H30B H -0.2861 0.7296 0.4409 0.170 Uiso 1 1 calc R . . H30C H -0.3061 0.7777 0.3974 0.170 Uiso 1 1 calc R . . C302 C -0.5701(16) 0.9848(9) 0.2078(10) 0.083(7) Uiso 0.40 1 d P . . C303 C -0.7206(13) 0.9795(8) 0.1769(9) 0.098(6) Uiso 0.50 1 d P . . C304 C 0.0943(7) 0.5579(5) 0.0168(5) 0.131(5) Uani 1 1 d . . . H30D H 0.0718 0.5720 -0.0197 0.197 Uiso 1 1 calc R . . H30E H 0.0874 0.5191 0.0175 0.197 Uiso 1 1 calc R . . H30F H 0.1519 0.5666 0.0213 0.197 Uiso 1 1 calc R . . C305 C -0.2838(6) 0.7666(5) -0.2485(4) 0.111(4) Uani 1 1 d . . . H30G H -0.2918 0.7983 -0.2726 0.167 Uiso 1 1 calc R . . H30H H -0.3127 0.7364 -0.2665 0.167 Uiso 1 1 calc R . . H30I H -0.2261 0.7583 -0.2440 0.167 Uiso 1 1 calc R . . C306 C 0.063(2) 0.6074(13) -0.1805(15) 0.131(11) Uiso 0.40 1 d P . . C307 C 0.2054(10) 0.5206(7) 0.1606(7) 0.194(7) Uiso 1 1 d . . . H30M H 0.2419 0.5365 0.1339 0.291 Uiso 1 1 calc R . . H30N H 0.1939 0.4836 0.1494 0.291 Uiso 1 1 calc R . . H30O H 0.2309 0.5214 0.1994 0.291 Uiso 1 1 calc R . . C308 C -0.6025(6) 0.9570(4) 0.0527(5) 0.118(4) Uani 1 1 d . . . H30J H -0.6561 0.9682 0.0633 0.177 Uiso 1 1 calc R . . H30K H -0.6078 0.9339 0.0189 0.177 Uiso 1 1 calc R . . H30L H -0.5704 0.9885 0.0440 0.177 Uiso 1 1 calc R . . C309 C -0.5747(8) 0.9171(5) -0.1181(5) 0.121(4) Uiso 1 1 d . . . C401 C -0.1930(14) 0.7025(8) 0.1007(10) 0.092(6) Uiso 0.50 1 d P . . C402 C -0.2630(13) 0.6992(8) 0.0719(9) 0.082(6) Uiso 0.50 1 d P . . C403 C -0.2649(15) 0.7318(10) 0.0154(11) 0.124(8) Uiso 0.50 1 d P . . C404 C -0.1723(18) 0.7292(12) 0.0570(13) 0.150(10) Uiso 0.50 1 d P . . C405 C -0.2024(13) 0.7785(8) 0.0398(8) 0.081(5) Uiso 0.50 1 d P . . C406 C -0.2762(11) 0.7803(7) 0.0156(7) 0.070(5) Uiso 0.50 1 d P . . C407 C -0.195(3) 0.747(2) 0.137(2) 0.26(2) Uiso 0.50 1 d P . . C408 C -0.2761(18) 0.7077(11) 0.1130(12) 0.120(8) Uiso 0.50 1 d P . . C409 C -0.3271(16) 0.7316(11) 0.1003(12) 0.112(8) Uiso 0.50 1 d P . . C410 C -0.3341(17) 0.7470(11) 0.0536(13) 0.138(9) Uiso 0.50 1 d P . . C411 C -0.281(2) 0.7759(14) 0.1431(15) 0.164(12) Uiso 0.50 1 d P . . C412 C -0.3179(16) 0.7939(10) 0.1106(11) 0.117(8) Uiso 0.50 1 d P . . C413 C -0.2250(17) 0.8018(10) 0.1168(12) 0.106(7) Uiso 0.50 1 d P . . C414 C -0.2448(13) 0.8082(8) 0.0734(10) 0.089(6) Uiso 0.50 1 d P . . C415 C -0.1738(17) 0.7850(11) 0.0955(13) 0.130(9) Uiso 0.50 1 d P . . O101 O -0.0090(4) 0.72751(19) 0.2472(2) 0.0678(15) Uani 1 1 d . . . H10A H -0.0044 0.7504 0.2732 0.102 Uiso 1 1 calc R B . O102 O 0.0202(4) 0.65761(19) 0.1597(2) 0.0682(15) Uani 1 1 d . B . H102 H 0.0425 0.6492 0.1914 0.102 Uiso 1 1 calc R . . O103 O 0.0570(3) 0.6936(2) 0.0525(2) 0.0628(14) Uani 1 1 d . . . H103 H 0.0629 0.6630 0.0664 0.094 Uiso 1 1 calc R B . O104 O -0.0002(4) 0.7237(2) -0.0568(2) 0.0864(19) Uani 1 1 d . . . H104 H 0.0159 0.7138 -0.0240 0.130 Uiso 1 1 calc R B . O105 O -0.1376(4) 0.7447(2) -0.1254(3) 0.090(2) Uani 1 1 d . B . H105 H -0.1039 0.7202 -0.1285 0.135 Uiso 1 1 calc R . . O106 O -0.2131(4) 0.8424(2) -0.1236(2) 0.0641(15) Uani 1 1 d . . . H106 H -0.2086 0.8688 -0.1451 0.096 Uiso 1 1 calc R B . O107 O -0.3312(3) 0.9019(2) -0.0749(2) 0.0708(16) Uani 1 1 d . . . H107 H -0.2937 0.8901 -0.0938 0.106 Uiso 1 1 calc R B . O108 O -0.4385(3) 0.9043(2) 0.0095(2) 0.0710(16) Uani 1 1 d . B . H10B H -0.4472 0.9010 -0.0258 0.106 Uiso 1 1 calc R . . O109 O -0.3941(3) 0.9394(2) 0.1192(2) 0.0615(14) Uani 1 1 d . . . H109 H -0.4393 0.9303 0.1046 0.092 Uiso 1 1 calc R B . O110 O -0.3368(3) 0.9069(2) 0.2279(3) 0.0730(16) Uani 1 1 d . . . H110 H -0.3619 0.8791 0.2356 0.109 Uiso 1 1 calc R B . O111 O -0.2765(3) 0.8256(2) 0.2985(2) 0.0719(16) Uani 1 1 d . B . H111 H -0.3246 0.8321 0.2882 0.108 Uiso 1 1 calc R . . O112 O -0.1143(3) 0.7988(2) 0.3028(2) 0.0608(14) Uani 1 1 d . . . H112 H -0.1530 0.7851 0.3189 0.091 Uiso 1 1 calc R B . O201 O -0.1082(3) 0.5594(2) 0.0838(2) 0.0682(15) Uani 1 1 d . . . H20A H -0.1059 0.5814 0.1106 0.102 Uiso 1 1 calc R . . O202 O -0.0991(3) 0.6049(2) -0.0230(3) 0.0746(17) Uani 1 1 d . . . H202 H -0.0760 0.6256 0.0008 0.112 Uiso 1 1 calc R . . O203 O -0.2331(3) 0.6242(2) -0.0928(2) 0.0679(16) Uani 1 1 d . . . H203 H -0.2753 0.6400 -0.1045 0.102 Uiso 1 1 calc R . . O204 O -0.3693(3) 0.68859(19) -0.1270(2) 0.0599(14) Uani 1 1 d . . . H204 H -0.3642 0.7183 -0.1427 0.090 Uiso 1 1 calc R . . O205 O -0.4530(4) 0.78313(19) -0.1155(2) 0.0720(16) Uani 1 1 d . . . H205 H -0.4625 0.8121 -0.0994 0.108 Uiso 1 1 calc R . . O206 O -0.5684(3) 0.79508(19) -0.0352(2) 0.0616(14) Uani 1 1 d . . . H206 H -0.5667 0.8065 -0.0016 0.092 Uiso 1 1 calc R . . O207 O -0.5714(3) 0.81642(17) 0.0818(2) 0.0562(13) Uani 1 1 d . . . H207 H -0.5652 0.8462 0.0975 0.084 Uiso 1 1 calc R . . O208 O -0.4914(4) 0.84379(19) 0.1853(2) 0.0742(16) Uani 1 1 d . . . H20B H -0.4816 0.8481 0.2205 0.111 Uiso 1 1 calc R . . O209 O -0.4367(4) 0.7681(2) 0.2618(2) 0.0749(17) Uani 1 1 d . . . H209 H -0.3958 0.7496 0.2703 0.112 Uiso 1 1 calc R . . O210 O -0.3144(3) 0.6957(2) 0.2979(2) 0.0649(15) Uani 1 1 d . . . H210 H -0.3588 0.6919 0.3127 0.097 Uiso 1 1 calc R . . O211 O -0.1612(3) 0.6666(2) 0.2770(2) 0.0758(17) Uani 1 1 d . . . H211 H -0.1195 0.6648 0.2587 0.114 Uiso 1 1 calc R . . O212 O -0.1282(3) 0.5879(3) 0.2002(3) 0.0766(17) Uani 1 1 d . . . H212 H -0.1239 0.5639 0.1757 0.115 Uiso 1 1 calc R . . OT1 O -0.2060(4) 0.7377(2) 0.3813(2) 0.0750(16) Uiso 1 1 d . . . HT1 H -0.1864 0.7094 0.3947 0.113 Uiso 1 1 calc R . . OZ1 O -0.4970(4) 0.8912(2) -0.1074(3) 0.095(2) Uani 1 1 d . . . OZ2 O 0.0523(3) 0.5817(2) 0.0634(3) 0.0772(17) Uani 1 1 d . . . HZ2 H 0.0861 0.5933 0.0883 0.116 Uiso 1 1 calc R . . OXL1 O -0.4834(14) 0.9865(9) 0.2524(10) 0.163(8) Uiso 0.40 1 d P . . OXL2 O 0.0397(18) 0.6200(12) -0.1402(13) 0.201(12) Uiso 0.40 1 d P . . OXL3 O -0.1465(15) 0.6210(10) -0.2245(10) 0.174(9) Uiso 0.40 1 d P . . OXX1 O -0.6383(8) 0.9806(4) 0.1872(5) 0.077(3) Uiso 0.50 1 d P . . OXX3 O 0.1366(6) 0.5484(4) 0.1593(4) 0.164(4) Uani 1 1 d . . . OJ3 O -0.0724(6) 0.6402(4) -0.1400(4) 0.179(4) Uiso 1 1 d . . . OZ3 O -0.5616(3) 0.9272(2) 0.1009(2) 0.0741(16) Uani 1 1 d . . . HZ3 H -0.5831 0.9348 0.1313 0.111 Uiso 1 1 calc R . . OZ4 O -0.3145(4) 0.7767(3) -0.1930(2) 0.0785(17) Uani 1 1 d . . . HZ4 H -0.3623 0.7872 -0.1970 0.118 Uiso 1 1 calc R . . Cl1 Cl 0.0986(2) 0.60331(11) 0.27701(12) 0.1297(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 C11A 0.057(6) 0.067(6) 0.063(6) -0.006(4) -0.003(5) -0.009(5) C11B 0.07(2) 0.09(2) 0.09(2) -0.003(15) 0.036(19) -0.006(15) C11C 0.107(12) 0.060(8) 0.047(8) -0.030(6) -0.023(8) -0.016(7) C110 0.076(7) 0.054(5) 0.045(5) -0.003(4) 0.009(5) 0.011(5) C12A 0.071(6) 0.047(4) 0.054(5) -0.009(4) -0.002(4) -0.013(4) C12B 0.112(8) 0.040(5) 0.076(6) -0.002(4) 0.002(6) -0.007(5) C15A 0.074(6) 0.071(6) 0.053(5) 0.009(4) 0.002(5) -0.026(4) C15B 0.114(8) 0.097(7) 0.081(7) 0.009(5) 0.015(6) -0.036(6) C18A 0.042(6) 0.091(6) 0.073(6) 0.008(5) 0.009(5) -0.011(5) C18B 0.057(7) 0.109(8) 0.120(8) -0.002(6) 0.005(6) -0.011(5) C21A 0.067(6) 0.045(4) 0.051(5) 0.010(4) 0.004(4) 0.000(4) C21B 0.104(8) 0.051(5) 0.081(6) -0.006(4) 0.009(6) 0.002(5) C22A 0.062(6) 0.052(5) 0.056(5) 0.008(4) 0.005(4) 0.004(4) C22B 0.070(7) 0.093(7) 0.106(8) 0.013(6) 0.023(6) 0.012(5) C26A 0.047(5) 0.047(4) 0.059(5) 0.001(4) -0.013(4) -0.004(4) C26B 0.049(6) 0.078(6) 0.110(7) 0.006(5) 0.011(5) -0.006(4) C28A 0.051(5) 0.044(4) 0.059(5) -0.003(4) -0.009(4) -0.001(4) C28B 0.101(7) 0.043(5) 0.082(6) -0.020(4) 0.017(5) -0.011(4) C101 0.062(6) 0.048(4) 0.040(4) 0.003(3) -0.006(4) -0.004(4) C102 0.033(5) 0.057(5) 0.047(4) 0.005(4) -0.008(4) -0.003(3) C103 0.052(5) 0.053(5) 0.042(4) 0.006(4) 0.001(4) 0.000(4) C104 0.054(5) 0.054(5) 0.059(5) 0.013(4) -0.004(4) -0.003(4) C105 0.043(5) 0.046(4) 0.061(5) 0.004(4) -0.009(4) 0.004(4) C106 0.039(5) 0.063(5) 0.050(5) 0.004(4) -0.010(4) 0.000(4) C107 0.049(5) 0.044(4) 0.058(5) 0.003(4) -0.006(4) 0.003(3) C108 0.051(6) 0.069(5) 0.047(5) 0.000(4) 0.002(5) 0.000(4) C109 0.050(6) 0.059(5) 0.040(4) 0.001(4) 0.006(4) -0.006(4) C111 0.054(6) 0.077(6) 0.037(5) -0.010(4) -0.010(5) -0.011(5) C112 0.054(6) 0.064(6) 0.049(5) 0.003(4) -0.004(5) -0.001(4) C113 0.053(6) 0.052(5) 0.037(4) 0.000(4) 0.004(4) -0.013(4) C114 0.066(6) 0.054(5) 0.041(4) 0.004(4) 0.013(5) -0.006(4) C115 0.062(5) 0.046(4) 0.047(4) -0.003(3) -0.008(4) -0.016(4) C116 0.045(5) 0.040(4) 0.056(5) 0.006(3) -0.011(5) -0.009(4) C117 0.074(7) 0.047(4) 0.038(5) 0.000(3) -0.012(5) 0.003(4) C118 0.050(6) 0.049(4) 0.057(5) -0.003(4) -0.006(5) -0.003(4) C119 0.041(5) 0.043(4) 0.056(5) 0.007(4) -0.016(5) 0.005(4) C120 0.046(5) 0.040(4) 0.045(5) 0.005(3) -0.005(4) -0.001(3) C121 0.048(5) 0.043(4) 0.051(5) 0.004(3) -0.012(4) -0.002(3) C122 0.062(6) 0.055(5) 0.038(4) -0.010(4) -0.008(4) 0.001(4) C123 0.058(6) 0.045(4) 0.036(4) -0.004(3) -0.008(4) -0.003(4) C124 0.038(5) 0.055(5) 0.056(5) -0.010(4) 0.002(4) -0.002(4) C125 0.058(6) 0.054(5) 0.040(5) -0.003(4) -0.007(4) -0.011(4) C126 0.058(6) 0.053(5) 0.039(4) 0.001(4) -0.010(4) -0.001(4) C127 0.055(5) 0.050(4) 0.032(4) -0.001(3) -0.005(4) 0.006(4) C128 0.046(5) 0.047(4) 0.044(4) -0.007(3) -0.002(4) -0.005(4) C201 0.048(5) 0.045(4) 0.044(4) 0.000(3) 0.003(4) 0.001(3) C202 0.040(5) 0.043(4) 0.045(4) -0.003(3) 0.002(4) 0.000(3) C203 0.046(6) 0.047(4) 0.055(5) -0.004(4) -0.003(5) 0.005(4) C204 0.045(6) 0.054(5) 0.060(5) -0.007(4) 0.004(5) -0.003(4) C205 0.049(6) 0.050(4) 0.043(4) 0.002(3) 0.001(4) 0.002(4) C206 0.035(5) 0.038(4) 0.050(5) -0.006(3) 0.002(4) 0.004(3) C207 0.051(5) 0.045(4) 0.045(4) 0.000(3) 0.009(4) 0.002(3) C208 0.051(5) 0.037(4) 0.046(4) -0.002(3) 0.008(4) -0.006(3) C209 0.044(5) 0.035(4) 0.035(4) -0.002(3) -0.008(4) -0.004(3) C210 0.050(5) 0.053(5) 0.042(4) 0.002(4) -0.005(4) -0.003(4) C211 0.061(5) 0.041(4) 0.041(4) 0.014(3) 0.003(4) 0.001(4) C212 0.047(5) 0.035(4) 0.054(5) 0.001(3) -0.009(4) 0.001(3) C213 0.047(5) 0.040(4) 0.035(4) 0.003(3) -0.010(4) -0.004(3) C214 0.046(5) 0.036(4) 0.045(4) 0.006(3) -0.012(4) -0.009(3) C215 0.039(5) 0.038(4) 0.059(5) -0.001(3) 0.004(4) 0.000(3) C216 0.037(5) 0.042(4) 0.038(4) -0.001(3) -0.002(4) 0.004(3) C217 0.046(5) 0.036(4) 0.057(5) 0.005(4) 0.002(4) 0.004(3) C218 0.047(5) 0.038(4) 0.062(5) -0.013(4) -0.003(4) -0.003(3) C219 0.062(6) 0.045(4) 0.036(4) -0.006(4) -0.015(4) 0.004(4) C220 0.054(5) 0.038(4) 0.042(4) -0.002(3) 0.003(4) 0.003(3) C221 0.047(5) 0.032(4) 0.043(4) -0.006(3) 0.001(4) -0.002(3) C222 0.060(5) 0.046(4) 0.031(4) 0.002(3) -0.004(4) 0.002(4) C223 0.049(5) 0.038(4) 0.040(4) 0.009(3) -0.008(4) 0.001(4) C224 0.061(6) 0.044(4) 0.044(5) 0.011(4) -0.005(5) -0.003(4) C225 0.054(6) 0.060(5) 0.045(5) 0.007(4) -0.021(5) -0.021(4) C226 0.040(6) 0.066(5) 0.052(5) 0.008(4) -0.009(5) -0.012(4) C227 0.044(5) 0.042(4) 0.038(4) 0.006(3) -0.009(4) -0.006(4) C228 0.052(5) 0.046(4) 0.036(4) 0.000(3) -0.010(4) -0.002(4) C301 0.131(10) 0.154(11) 0.056(6) -0.013(6) 0.009(6) 0.019(8) C304 0.115(9) 0.163(12) 0.115(9) -0.075(8) 0.003(8) 0.019(8) C305 0.084(8) 0.180(12) 0.070(7) -0.024(7) 0.005(6) -0.012(7) C308 0.089(8) 0.106(8) 0.157(10) 0.081(8) -0.011(8) 0.014(6) O101 0.096(4) 0.053(3) 0.053(3) 0.006(3) -0.002(3) 0.003(3) O102 0.098(5) 0.049(3) 0.058(3) 0.005(3) 0.001(3) 0.004(3) O103 0.075(4) 0.054(3) 0.060(3) -0.002(3) 0.004(3) 0.008(3) O104 0.106(5) 0.084(4) 0.068(4) -0.016(3) -0.008(4) 0.019(4) O105 0.108(5) 0.079(4) 0.079(4) -0.023(4) -0.031(4) -0.002(4) O106 0.068(4) 0.073(4) 0.050(3) 0.003(3) -0.008(3) -0.007(3) O107 0.059(4) 0.093(4) 0.059(4) -0.014(3) -0.008(3) -0.002(3) O108 0.053(4) 0.094(4) 0.065(4) -0.009(3) -0.013(3) -0.003(3) O109 0.047(3) 0.068(4) 0.068(4) -0.003(3) -0.002(3) 0.001(3) O110 0.053(4) 0.089(4) 0.077(4) 0.006(3) 0.012(3) -0.007(3) O111 0.058(4) 0.089(4) 0.069(4) 0.015(3) 0.006(3) -0.015(3) O112 0.061(4) 0.063(3) 0.057(3) 0.018(3) 0.000(3) -0.003(3) O201 0.052(4) 0.086(4) 0.066(4) 0.000(3) -0.007(3) 0.007(3) O202 0.044(4) 0.095(5) 0.086(4) -0.001(3) 0.012(3) -0.012(3) O203 0.072(4) 0.083(4) 0.049(3) 0.019(3) 0.013(3) 0.006(3) O204 0.073(4) 0.054(3) 0.054(3) 0.007(3) 0.017(3) -0.001(3) O205 0.109(5) 0.047(3) 0.061(3) 0.018(3) 0.021(3) 0.007(3) O206 0.082(4) 0.047(3) 0.056(3) 0.006(2) 0.003(3) 0.016(3) O207 0.068(4) 0.036(3) 0.062(3) 0.001(2) -0.017(3) 0.002(3) O208 0.099(5) 0.041(3) 0.079(4) -0.008(3) -0.022(4) 0.005(3) O209 0.103(5) 0.052(3) 0.065(4) -0.014(3) -0.030(4) 0.006(3) O210 0.076(4) 0.059(3) 0.059(3) -0.008(3) -0.004(3) -0.001(3) O211 0.066(4) 0.091(4) 0.068(4) -0.014(3) -0.014(3) -0.026(4) O212 0.043(4) 0.106(5) 0.080(5) -0.009(3) -0.004(3) -0.001(3) OZ1 0.086(5) 0.076(4) 0.120(5) 0.017(4) -0.016(4) 0.013(3) OZ2 0.058(4) 0.079(4) 0.095(5) -0.027(3) 0.010(3) 0.003(3) OXX3 0.150(8) 0.219(10) 0.122(6) 0.016(6) 0.010(6) 0.092(7) OZ3 0.077(4) 0.052(3) 0.093(4) -0.002(3) -0.002(4) 0.009(3) OZ4 0.081(5) 0.083(4) 0.070(4) 0.013(3) -0.011(4) -0.018(4) Cl1 0.223(4) 0.0877(19) 0.0759(18) 0.0015(15) -0.014(2) 0.011(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11A C11B 1.30(3) . ? C11A C11C 1.478(12) . ? C11A C101 1.521(10) . ? C110 C111 1.375(11) . ? C110 O104 1.383(9) . ? C110 C109 1.426(11) . ? C12A C12B 1.545(10) . ? C12A C122 1.549(10) . ? C15A C15B 1.476(11) . ? C15A C115 1.525(10) . ? C18A C108 1.522(10) . ? C18A C18B 1.533(11) . ? C21A C21B 1.520(10) . ? C21A C201 1.535(9) . ? C22A C22B 1.504(10) . ? C22A C222 1.548(10) . ? C26A C26B 1.517(10) . ? C26A C215 1.528(9) . ? C28A C28B 1.541(10) . ? C28A C208 1.543(9) . ? C101 C127 1.516(10) . ? C101 C102 1.524(10) . ? C102 C103 1.384(10) . ? C102 C107 1.400(10) . ? C103 C104 1.383(10) . ? C103 O101 1.388(8) . ? C104 C105 1.378(10) . ? C104 O102 1.391(9) . ? C105 O103 1.384(8) . ? C105 C106 1.405(10) . ? C106 C107 1.396(10) . ? C106 C108 1.553(10) . ? C108 C109 1.522(11) . ? C109 C114 1.385(10) . ? C111 O105 1.382(9) . ? C111 C112 1.388(11) . ? C112 C113 1.374(10) . ? C112 O106 1.383(9) . ? C113 C114 1.394(10) . ? C113 C115 1.516(10) . ? C115 C116 1.508(10) . ? C116 C117 1.366(10) . ? C116 C121 1.417(10) . ? C117 C118 1.390(11) . ? C117 O107 1.391(9) . ? C118 C119 1.369(10) . ? C118 O108 1.382(9) . ? C119 C120 1.384(10) . ? C119 O109 1.388(9) . ? C120 C121 1.378(10) . ? C120 C122 1.536(10) . ? C122 C123 1.541(10) . ? C123 C124 1.393(10) . ? C123 C128 1.395(10) . ? C124 O110 1.360(9) . ? C124 C125 1.390(10) . ? C125 O111 1.368(8) . ? C125 C126 1.381(10) . ? C126 C127 1.375(10) . ? C126 O112 1.389(8) . ? C127 C128 1.402(10) . ? C201 C202 1.514(10) . ? C201 C227 1.539(9) . ? C202 C207 1.380(10) . ? C202 C203 1.386(10) . ? C203 O201 1.379(9) . ? C203 C204 1.389(10) . ? C204 O202 1.359(9) . ? C204 C205 1.382(10) . ? C205 O203 1.381(8) . ? C205 C206 1.400(10) . ? C206 C207 1.402(10) . ? C206 C208 1.520(10) . ? C208 C209 1.531(9) . ? C209 C210 1.384(9) . ? C209 C214 1.398(9) . ? C210 O204 1.372(8) . ? C210 C211 1.404(10) . ? C211 O205 1.362(8) . ? C211 C212 1.391(10) . ? C212 O206 1.391(8) . ? C212 C213 1.392(9) . ? C213 C214 1.405(9) . ? C213 C215 1.522(9) . ? C215 C216 1.544(10) . ? C216 C217 1.373(9) . ? C216 C221 1.387(9) . ? C217 C218 1.386(10) . ? C217 O207 1.406(8) . ? C218 C219 1.377(10) . ? C218 O208 1.383(9) . ? C219 O209 1.367(8) . ? C219 C220 1.394(10) . ? C220 C221 1.402(9) . ? C220 C222 1.548(9) . ? C222 C223 1.523(10) . ? C223 C224 1.363(10) . ? C223 C228 1.374(9) . ? C224 C225 1.384(11) . ? C224 O210 1.387(9) . ? C225 O211 1.374(8) . ? C225 C226 1.407(11) . ? C226 O212 1.371(9) . ? C226 C227 1.383(10) . ? C227 C228 1.384(10) . ? C301 OT1 1.411(10) . ? C302 OXX1 1.18(2) . ? C302 OXL1 1.69(3) . ? C303 OXX1 1.35(2) . ? C304 OZ2 1.428(10) . ? C305 OZ4 1.416(10) . ? C306 OXL2 1.06(4) . ? C307 OXX3 1.308(15) . ? C308 OZ3 1.456(10) . ? C309 OZ1 1.424(13) . ? C401 C404 1.26(3) . ? C401 C402 1.29(2) . ? C401 C407 1.37(5) . ? C401 C408 1.40(3) . ? C402 C408 1.00(3) . ? C402 C409 1.49(3) . ? C402 C403 1.52(3) . ? C402 C410 1.68(3) . ? C402 C404 1.70(3) . ? C403 C406 1.21(3) . ? C403 C410 1.51(3) . ? C403 C405 1.61(3) . ? C403 C404 1.74(4) . ? C404 C405 1.36(3) . ? C404 C415 1.63(4) . ? C404 C407 1.95(6) . ? C405 C414 1.29(2) . ? C405 C406 1.29(2) . ? C405 C415 1.34(3) . ? C405 C413 1.91(3) . ? C406 C414 1.55(3) . ? C406 C410 1.55(3) . ? C407 C415 1.41(5) . ? C407 C413 1.51(5) . ? C407 C411 1.59(5) . ? C407 C408 1.69(5) . ? C408 C409 1.04(3) . ? C408 C411 1.82(4) . ? C408 C410 1.88(4) . ? C409 C410 1.13(3) . ? C409 C412 1.56(3) . ? C409 C411 1.62(4) . ? C410 C412 1.75(4) . ? C411 C412 1.03(4) . ? C411 C413 1.29(3) . ? C411 C414 1.91(4) . ? C412 C413 1.52(4) . ? C412 C414 1.54(3) . ? C413 C414 1.04(3) . ? C413 C415 1.07(3) . ? C414 C415 1.36(3) . ? 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 C11B C11A C11C 91.3(13) . . ? C11B C11A C101 116.1(13) . . ? C11C C11A C101 116.3(8) . . ? C111 C110 O104 116.9(8) . . ? C111 C110 C109 119.7(8) . . ? O104 C110 C109 123.4(9) . . ? C12B C12A C122 113.1(7) . . ? C15B C15A C115 112.4(7) . . ? C108 C18A C18B 112.7(7) . . ? C21B C21A C201 114.6(6) . . ? C22B C22A C222 112.8(7) . . ? C26B C26A C215 112.4(6) . . ? C28B C28A C208 113.1(6) . . ? C127 C101 C11A 112.6(7) . . ? C127 C101 C102 111.1(6) . . ? C11A C101 C102 113.6(6) . . ? C103 C102 C107 116.9(6) . . ? C103 C102 C101 122.6(6) . . ? C107 C102 C101 120.5(6) . . ? C104 C103 C102 121.6(7) . . ? C104 C103 O101 113.6(7) . . ? C102 C103 O101 124.7(6) . . ? C105 C104 C103 120.9(7) . . ? C105 C104 O102 115.7(7) . . ? C103 C104 O102 123.3(7) . . ? C104 C105 O103 121.9(7) . . ? C104 C105 C106 119.7(7) . . ? O103 C105 C106 118.4(7) . . ? C107 C106 C105 117.9(7) . . ? C107 C106 C108 121.2(7) . . ? C105 C106 C108 120.9(7) . . ? C106 C107 C102 122.9(7) . . ? C109 C108 C18A 111.9(7) . . ? C109 C108 C106 111.5(6) . . ? C18A C108 C106 113.4(6) . . ? C114 C109 C110 117.4(8) . . ? C114 C109 C108 122.5(7) . . ? C110 C109 C108 120.1(7) . . ? C110 C111 O105 120.6(8) . . ? C110 C111 C112 120.0(8) . . ? O105 C111 C112 119.3(8) . . ? C113 C112 O106 119.9(8) . . ? C113 C112 C111 122.8(9) . . ? O106 C112 C111 117.2(8) . . ? C112 C113 C114 116.2(8) . . ? C112 C113 C115 121.0(8) . . ? C114 C113 C115 122.8(7) . . ? C109 C114 C113 123.9(7) . . ? C116 C115 C113 111.4(6) . . ? C116 C115 C15A 111.7(6) . . ? C113 C115 C15A 115.3(7) . . ? C117 C116 C121 116.2(7) . . ? C117 C116 C115 121.2(7) . . ? C121 C116 C115 122.5(7) . . ? C116 C117 C118 121.7(7) . . ? C116 C117 O107 124.7(7) . . ? C118 C117 O107 113.5(8) . . ? C119 C118 O108 117.6(7) . . ? C119 C118 C117 120.3(8) . . ? O108 C118 C117 122.2(7) . . ? C118 C119 C120 120.7(7) . . ? C118 C119 O109 120.8(7) . . ? C120 C119 O109 118.4(7) . . ? C121 C120 C119 117.7(7) . . ? C121 C120 C122 121.4(7) . . ? C119 C120 C122 120.9(7) . . ? C120 C121 C116 123.2(7) . . ? C120 C122 C123 111.0(6) . . ? C120 C122 C12A 113.3(6) . . ? C123 C122 C12A 111.9(6) . . ? C124 C123 C128 117.2(7) . . ? C124 C123 C122 121.5(7) . . ? C128 C123 C122 121.2(6) . . ? O110 C124 C125 116.4(7) . . ? O110 C124 C123 122.8(7) . . ? C125 C124 C123 120.7(7) . . ? O111 C125 C126 118.3(7) . . ? O111 C125 C124 121.9(8) . . ? C126 C125 C124 119.8(7) . . ? C127 C126 C125 122.0(7) . . ? C127 C126 O112 118.5(7) . . ? C125 C126 O112 119.5(7) . . ? C126 C127 C128 116.9(7) . . ? C126 C127 C101 121.4(7) . . ? C128 C127 C101 121.7(6) . . ? C123 C128 C127 123.2(6) . . ? C202 C201 C21A 113.3(6) . . ? C202 C201 C227 111.2(6) . . ? C21A C201 C227 112.1(6) . . ? C207 C202 C203 117.6(7) . . ? C207 C202 C201 122.0(6) . . ? C203 C202 C201 120.4(7) . . ? O201 C203 C202 119.6(7) . . ? O201 C203 C204 118.5(7) . . ? C202 C203 C204 121.8(8) . . ? O202 C204 C205 121.4(7) . . ? O202 C204 C203 119.0(8) . . ? C205 C204 C203 119.6(7) . . ? O203 C205 C204 114.8(7) . . ? O203 C205 C206 124.6(7) . . ? C204 C205 C206 120.6(7) . . ? C205 C206 C207 117.8(7) . . ? C205 C206 C208 118.6(7) . . ? C207 C206 C208 123.5(6) . . ? C202 C207 C206 122.7(7) . . ? C206 C208 C209 113.1(5) . . ? C206 C208 C28A 113.2(6) . . ? C209 C208 C28A 111.7(6) . . ? C210 C209 C214 118.0(6) . . ? C210 C209 C208 120.3(6) . . ? C214 C209 C208 121.6(6) . . ? O204 C210 C209 119.4(6) . . ? O204 C210 C211 119.7(6) . . ? C209 C210 C211 120.8(7) . . ? O205 C211 C212 122.6(6) . . ? O205 C211 C210 117.5(6) . . ? C212 C211 C210 119.9(6) . . ? O206 C212 C211 115.2(6) . . ? O206 C212 C213 123.9(7) . . ? C211 C212 C213 120.8(6) . . ? C212 C213 C214 117.9(6) . . ? C212 C213 C215 120.1(6) . . ? C214 C213 C215 121.9(6) . . ? C209 C214 C213 122.5(6) . . ? C213 C215 C26A 113.4(6) . . ? C213 C215 C216 110.2(6) . . ? C26A C215 C216 112.5(6) . . ? C217 C216 C221 117.2(6) . . ? C217 C216 C215 120.9(6) . . ? C221 C216 C215 121.8(6) . . ? C216 C217 C218 121.5(6) . . ? C216 C217 O207 118.4(7) . . ? C218 C217 O207 120.1(6) . . ? C219 C218 O208 122.6(7) . . ? C219 C218 C217 120.0(7) . . ? O208 C218 C217 117.4(7) . . ? O209 C219 C218 113.8(6) . . ? O209 C219 C220 125.1(6) . . ? C218 C219 C220 121.1(7) . . ? C219 C220 C221 116.5(6) . . ? C219 C220 C222 121.8(6) . . ? C221 C220 C222 121.7(6) . . ? C216 C221 C220 123.5(6) . . ? C223 C222 C22A 112.2(6) . . ? C223 C222 C220 110.6(5) . . ? C22A C222 C220 113.3(6) . . ? C224 C223 C228 118.5(7) . . ? C224 C223 C222 118.4(7) . . ? C228 C223 C222 123.1(7) . . ? C223 C224 C225 120.3(7) . . ? C223 C224 O210 122.9(7) . . ? C225 C224 O210 116.8(7) . . ? O211 C225 C224 118.4(8) . . ? O211 C225 C226 121.5(8) . . ? C224 C225 C226 120.1(7) . . ? O212 C226 C227 125.3(7) . . ? O212 C226 C225 114.3(7) . . ? C227 C226 C225 120.4(7) . . ? C226 C227 C228 116.7(7) . . ? C226 C227 C201 120.3(7) . . ? C228 C227 C201 123.0(6) . . ? C223 C228 C227 124.1(7) . . ? OXX1 C302 OXL1 166(2) . . ? C404 C401 C402 84(2) . . ? C404 C401 C407 96(3) . . ? C402 C401 C407 108(3) . . ? C404 C401 C408 115(2) . . ? C402 C401 C408 43.4(14) . . ? C407 C401 C408 75(3) . . ? C408 C402 C401 75(2) . . ? C408 C402 C409 44.3(19) . . ? C401 C402 C409 111(2) . . ? C408 C402 C403 134(3) . . ? C401 C402 C403 112.1(19) . . ? C409 C402 C403 96.4(19) . . ? C408 C402 C410 85(2) . . ? C401 C402 C410 131.1(19) . . ? C409 C402 C410 41.3(13) . . ? C403 C402 C410 56.0(15) . . ? C408 C402 C404 109(3) . . ? C401 C402 C404 47.3(14) . . ? C409 C402 C404 119.5(18) . . ? C403 C402 C404 64.9(16) . . ? C410 C402 C404 103.8(18) . . ? C406 C403 C410 68.6(18) . . ? C406 C403 C402 121(2) . . ? C410 C403 C402 67.4(17) . . ? C406 C403 C405 52.3(14) . . ? C410 C403 C405 95.7(19) . . ? C402 C403 C405 95.7(17) . . ? C406 C403 C404 99(2) . . ? C410 C403 C404 110(2) . . ? C402 C403 C404 62.5(16) . . ? C405 C403 C404 47.7(13) . . ? C401 C404 C405 126(3) . . ? C401 C404 C415 90(2) . . ? C405 C404 C415 52.5(16) . . ? C401 C404 C402 48.7(15) . . ? C405 C404 C402 98(2) . . ? C415 C404 C402 102(2) . . ? C401 C404 C403 101(2) . . ? C405 C404 C403 61.3(16) . . ? C415 C404 C403 103(2) . . ? C402 C404 C403 52.6(13) . . ? C401 C404 C407 44.5(19) . . ? C405 C404 C407 90(2) . . ? C415 C404 C407 45.2(17) . . ? C402 C404 C407 72(2) . . ? C403 C404 C407 108(2) . . ? C414 C405 C406 73.9(16) . . ? C414 C405 C415 62.1(17) . . ? C406 C405 C415 132(2) . . ? C414 C405 C404 122(2) . . ? C406 C405 C404 118(2) . . ? C415 C405 C404 74(2) . . ? C414 C405 C403 105.2(18) . . ? C406 C405 C403 47.5(12) . . ? C415 C405 C403 126(2) . . ? C404 C405 C403 71.0(18) . . ? C414 C405 C413 30.8(12) . . ? C406 C405 C413 99.4(16) . . ? C415 C405 C413 32.9(14) . . ? C404 C405 C413 94.7(18) . . ? C403 C405 C413 112.4(15) . . ? C403 C406 C405 80.2(18) . . ? C403 C406 C414 113.4(19) . . ? C405 C406 C414 53.0(12) . . ? C403 C406 C410 65.1(16) . . ? C405 C406 C410 108.6(18) . . ? C414 C406 C410 86.1(16) . . ? C401 C407 C415 95(4) . . ? C401 C407 C413 123(4) . . ? C415 C407 C413 43(2) . . ? C401 C407 C411 118(4) . . ? C415 C407 C411 90(3) . . ? C413 C407 C411 49(2) . . ? C401 C407 C408 53(2) . . ? C415 C407 C408 112(3) . . ? C413 C407 C408 100(3) . . ? C411 C407 C408 67(3) . . ? C401 C407 C404 40.0(18) . . ? C415 C407 C404 55(2) . . ? C413 C407 C404 89(3) . . ? C411 C407 C404 114(3) . . ? C408 C407 C404 76(2) . . ? C402 C408 C409 94(3) . . ? C402 C408 C401 62(2) . . ? C409 C408 C401 139(3) . . ? C402 C408 C407 103(3) . . ? C409 C408 C407 111(3) . . ? C401 C408 C407 52(2) . . ? C402 C408 C411 125(3) . . ? C409 C408 C411 62(2) . . ? C401 C408 C411 103(2) . . ? C407 C408 C411 54(2) . . ? C402 C408 C410 63(2) . . ? C409 C408 C410 31.9(19) . . ? C401 C408 C410 110(2) . . ? C407 C408 C410 107(2) . . ? C411 C408 C410 76.6(18) . . ? C408 C409 C410 119(3) . . ? C408 C409 C402 42.0(19) . . ? C410 C409 C402 79(2) . . ? C408 C409 C412 116(3) . . ? C410 C409 C412 80(2) . . ? C402 C409 C412 122(2) . . ? C408 C409 C411 83(3) . . ? C410 C409 C411 111(3) . . ? C402 C409 C411 108(2) . . ? C412 C409 C411 37.7(14) . . ? C409 C410 C403 115(3) . . ? C409 C410 C406 132(3) . . ? C403 C410 C406 46.3(13) . . ? C409 C410 C402 60(2) . . ? C403 C410 C402 56.6(14) . . ? C406 C410 C402 94.5(18) . . ? C409 C410 C412 61(2) . . ? C403 C410 C412 121(2) . . ? C406 C410 C412 90.2(17) . . ? C402 C410 C412 101.7(19) . . ? C409 C410 C408 29.1(17) . . ? C403 C410 C408 86.2(18) . . ? C406 C410 C408 112.5(19) . . ? C402 C410 C408 32.0(10) . . ? C412 C410 C408 75.5(18) . . ? C412 C411 C413 81(3) . . ? C412 C411 C407 128(4) . . ? C413 C411 C407 62(3) . . ? C412 C411 C409 68(3) . . ? C413 C411 C409 111(3) . . ? C407 C411 C409 91(3) . . ? C412 C411 C408 99(3) . . ? C413 C411 C408 103(2) . . ? C407 C411 C408 59(2) . . ? C409 C411 C408 34.7(13) . . ? C412 C411 C414 54(2) . . ? C413 C411 C414 30.9(15) . . ? C407 C411 C414 78(2) . . ? C409 C411 C414 85.7(19) . . ? C408 C411 C414 92.3(18) . . ? C411 C412 C413 57(2) . . ? C411 C412 C414 94(3) . . ? C413 C412 C414 39.7(12) . . ? C411 C412 C409 75(3) . . ? C413 C412 C409 103(2) . . ? C414 C412 C409 102.2(18) . . ? C411 C412 C410 108(3) . . ? C413 C412 C410 105.0(19) . . ? C414 C412 C410 79.9(17) . . ? C409 C412 C410 39.6(12) . . ? C414 C413 C415 80(3) . . ? C414 C413 C411 109(3) . . ? C415 C413 C411 128(3) . . ? C414 C413 C407 121(3) . . ? C415 C413 C407 64(3) . . ? C411 C413 C407 69(3) . . ? C414 C413 C412 71(2) . . ? C415 C413 C412 135(3) . . ? C411 C413 C412 41.8(18) . . ? C407 C413 C412 102(3) . . ? C414 C413 C405 39.4(16) . . ? C415 C413 C405 43.0(19) . . ? C411 C413 C405 118(2) . . ? C407 C413 C405 87(2) . . ? C412 C413 C405 96.8(18) . . ? C413 C414 C405 110(3) . . ? C413 C414 C415 50.9(19) . . ? C405 C414 C415 60.9(17) . . ? C413 C414 C412 69(2) . . ? C405 C414 C412 131.1(19) . . ? C415 C414 C412 111(2) . . ? C413 C414 C406 145(2) . . ? C405 C414 C406 53.2(13) . . ? C415 C414 C406 111(2) . . ? C412 C414 C406 98.4(17) . . ? C413 C414 C411 39.6(19) . . ? C405 C414 C411 117.9(19) . . ? C415 C414 C411 79(2) . . ? C412 C414 C411 32.4(13) . . ? C406 C414 C411 115.4(17) . . ? C413 C415 C405 104(3) . . ? C413 C415 C414 49.0(19) . . ? C405 C415 C414 57.0(16) . . ? C413 C415 C407 73(3) . . ? C405 C415 C407 119(3) . . ? C414 C415 C407 107(3) . . ? C413 C415 C404 127(3) . . ? C405 C415 C404 53.2(16) . . ? C414 C415 C404 101(2) . . ? C407 C415 C404 79(3) . . ? C302 OXX1 C303 166.1(18) . . ? _diffrn_measured_fraction_theta_max 0.771 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.771 _refine_diff_density_max 0.698 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.076 ########END data_as950 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common resorcinarene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H51 N O9' _chemical_formula_weight 713.84 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' _cell_length_a 14.5152(9) _cell_length_b 14.5152(9) _cell_length_c 9.3463(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1969.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17235 _diffrn_reflns_av_R_equivalents 0.0287 _diffrn_reflns_av_sigmaI/netI 0.0191 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 28.02 _reflns_number_total 2386 _reflns_number_gt 1970 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1206P)^2^+0.4608P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2386 _refine_ls_number_parameters 142 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1842 _refine_ls_wR_factor_gt 0.1737 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.020 _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 0.47484(9) 0.14519(9) 0.88871(15) 0.0272(3) Uani 1 1 d . . . H1X H 0.5348(13) 0.1182(12) 0.8665(19) 0.035(4) Uiso 1 1 d . . . C1A C 0.46848(11) 0.14814(10) 1.05305(16) 0.0347(4) Uani 1 1 d . . . H1A1 H 0.4106 0.1767 1.0801 0.042 Uiso 1 1 calc R . . H1A2 H 0.4681 0.0856 1.0894 0.042 Uiso 1 1 calc R . . C1B C 0.54750(15) 0.20092(15) 1.1231(2) 0.0530(5) Uani 1 1 d . . . H1B1 H 0.6026 0.1632 1.1209 0.064 Uiso 1 1 calc R . . H1B2 H 0.5597 0.2564 1.0684 0.064 Uiso 1 1 calc R . . C1C C 0.5269(2) 0.2269(2) 1.2751(3) 0.0829(8) Uani 1 1 d . . . H1C1 H 0.4792 0.2727 1.2768 0.124 Uiso 1 1 calc R . . H1C2 H 0.5815 0.2513 1.3190 0.124 Uiso 1 1 calc R . . H1C3 H 0.5069 0.1734 1.3268 0.124 Uiso 1 1 calc R . . C2 C 0.40003(9) 0.08517(9) 0.82154(14) 0.0263(3) Uani 1 1 d . . . C3 C 0.31095(9) 0.08249(9) 0.87653(14) 0.0270(3) Uani 1 1 d . . . H3 H 0.2971 0.1203 0.9539 0.032 Uiso 1 1 calc . . . C4 C 0.24142(9) 0.02650(9) 0.82244(14) 0.0261(3) Uani 1 1 d . . . C5 C 0.26349(10) -0.02882(10) 0.70520(15) 0.0301(3) Uani 1 1 d . . . C6 C 0.34999(11) -0.02521(11) 0.64354(16) 0.0344(4) Uani 1 1 d . . . H6 H 0.3630 -0.0609 0.5634 0.041 Uiso 1 1 calc . . . C7 C 0.41722(10) 0.03143(10) 0.70083(15) 0.0313(3) Uani 1 1 d . . . C100 C 0.2500 0.2500 1.3709(13) 0.125(3) Uani 1 4 d S . . C200 C 0.2500 0.2500 1.5293(13) 0.204(6) Uani 1 4 d S . . HN2A H 0.1898 0.2661 1.5635 0.306 Uiso 0.25 1 calc PR . . HN2B H 0.2941 0.2941 1.5635 0.306 Uiso 0.25 1 calc PR . . HN2C H 0.2662 0.1898 1.5635 0.306 Uiso 0.25 1 calc PR . . O1 O 0.19910(8) -0.08874(8) 0.64943(14) 0.0429(4) Uani 1 1 d D . . H1 H 0.220(2) -0.1329(19) 0.608(4) 0.039(10) Uiso 0.50 1 d PD . . H1W H 0.1449(17) -0.073(3) 0.653(5) 0.068(15) Uiso 0.50 1 d PD . . O2 O 0.50294(8) 0.03245(9) 0.63715(14) 0.0464(4) Uani 1 1 d D . . H2 H 0.533(2) 0.0806(18) 0.643(4) 0.037(9) Uiso 0.50 1 d PD . . H2W H 0.504(4) 0.003(3) 0.565(3) 0.061(14) Uiso 0.50 1 d PD . . O3 O 0.2500 -0.2500 0.5000 0.0397(5) Uani 1 4 d S . . N1 N 0.2500 0.2500 1.2440(12) 0.135(2) Uani 1 4 d S . . 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 0.0270(7) 0.0263(6) 0.0283(7) 0.0014(5) 0.0004(5) 0.0002(5) C1A 0.0417(8) 0.0339(7) 0.0283(7) 0.0044(5) -0.0054(6) -0.0007(6) C1B 0.0544(11) 0.0611(12) 0.0434(9) 0.0053(8) -0.0190(8) -0.0099(9) C1C 0.102(2) 0.0846(18) 0.0622(14) -0.0207(13) -0.0335(14) 0.0045(15) C2 0.0289(7) 0.0245(6) 0.0256(6) 0.0013(5) 0.0011(5) 0.0002(5) C3 0.0297(7) 0.0266(6) 0.0248(6) -0.0014(5) 0.0025(5) 0.0010(5) C4 0.0270(6) 0.0253(6) 0.0259(6) 0.0008(5) 0.0016(5) 0.0014(5) C5 0.0298(7) 0.0290(7) 0.0313(7) -0.0048(5) -0.0006(5) -0.0009(5) C6 0.0359(8) 0.0364(8) 0.0311(7) -0.0099(6) 0.0062(6) -0.0007(6) C7 0.0306(7) 0.0324(7) 0.0309(7) -0.0021(5) 0.0067(5) -0.0005(5) C100 0.115(4) 0.115(4) 0.147(8) 0.000 0.000 0.000 C200 0.241(10) 0.241(10) 0.128(9) 0.000 0.000 0.000 O1 0.0345(6) 0.0404(7) 0.0539(8) -0.0205(5) -0.0013(5) -0.0033(5) O2 0.0369(6) 0.0523(8) 0.0501(7) -0.0166(6) 0.0185(5) -0.0091(5) O3 0.0361(7) 0.0361(7) 0.0469(12) 0.000 0.000 0.000 N1 0.129(4) 0.129(4) 0.145(6) 0.000 0.000 0.000 _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 1.5272(18) . ? C1 C4 1.5281(18) 3 ? C1 C1A 1.539(2) . ? C1A C1B 1.527(2) . ? C1B C1C 1.500(3) . ? C2 C3 1.3920(18) . ? C2 C7 1.3941(19) . ? C3 C4 1.3908(19) . ? C4 C5 1.3958(19) . ? C4 C1 1.5281(18) 4 ? C5 O1 1.3790(18) . ? C5 C6 1.382(2) . ? C6 C7 1.384(2) . ? C7 O2 1.3794(17) . ? C100 N1 1.186(13) . ? C100 C200 1.480(15) . ? 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 C4 110.23(11) . 3 ? C2 C1 C1A 112.54(11) . . ? C4 C1 C1A 112.22(11) 3 . ? C1B C1A C1 113.38(13) . . ? C1C C1B C1A 112.52(19) . . ? C3 C2 C7 116.70(12) . . ? C3 C2 C1 121.65(12) . . ? C7 C2 C1 121.64(12) . . ? C4 C3 C2 123.79(12) . . ? C3 C4 C5 117.06(12) . . ? C3 C4 C1 121.56(12) . 4 ? C5 C4 C1 121.37(12) . 4 ? O1 C5 C6 118.81(13) . . ? O1 C5 C4 120.27(13) . . ? C6 C5 C4 120.92(13) . . ? C5 C6 C7 120.11(13) . . ? O2 C7 C6 118.39(13) . . ? O2 C7 C2 120.30(13) . . ? C6 C7 C2 121.29(13) . . ? N1 C100 C200 180.000(9) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.741 _refine_diff_density_min -0.401 _refine_diff_density_rms 0.072 ########END data_als066 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common pyrrogallolarene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H136 O11' _chemical_formula_weight 1273.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.157(3) _cell_length_b 16.173(4) _cell_length_c 23.393(7) _cell_angle_alpha 108.866(16) _cell_angle_beta 91.142(12) _cell_angle_gamma 96.117(14) _cell_volume 3964.9(19) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.067 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12139 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0547 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 0.92 _diffrn_reflns_theta_max 28.06 _reflns_number_total 12139 _reflns_number_gt 7857 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0800P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12139 _refine_ls_number_parameters 892 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0864 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1583 _refine_ls_wR_factor_gt 0.1396 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.07939(16) 0.03320(13) 0.45599(8) 0.0252(5) Uani 1 1 d . . . H1 H 0.1509 0.0575 0.4640 0.038 Uiso 1 1 calc R . . O2 O -0.13945(16) 0.08283(13) 0.48875(8) 0.0297(5) Uani 1 1 d . . . H2 H -0.0928 0.0566 0.5035 0.045 Uiso 1 1 calc R . . O3 O -0.27039(16) 0.15544(13) 0.42757(8) 0.0286(5) Uani 1 1 d . . . H3 H -0.2846 0.2022 0.4218 0.043 Uiso 1 1 calc R . . O4 O -0.31013(15) 0.30404(12) 0.40107(8) 0.0227(5) Uani 1 1 d . . . H4 H -0.3439 0.3453 0.4241 0.034 Uiso 1 1 calc R . . O5 O -0.28015(15) 0.48111(13) 0.41873(7) 0.0224(5) Uani 1 1 d . . . H5 H -0.2380 0.5138 0.4495 0.034 Uiso 1 1 calc R . . O6 O -0.10309(16) 0.54914(13) 0.35598(8) 0.0255(5) Uani 1 1 d . . . H6 H -0.1627 0.5735 0.3717 0.038 Uiso 1 1 calc R . . O7 O 0.13128(16) 0.61992(12) 0.36629(8) 0.0257(5) Uani 1 1 d . . . H7 H 0.0573 0.6013 0.3624 0.039 Uiso 1 1 calc R . . O8 O 0.34409(16) 0.65329(13) 0.43181(8) 0.0255(5) Uani 1 1 d . . . H8 H 0.2985 0.6886 0.4265 0.038 Uiso 1 1 calc R . . O9 O 0.49599(15) 0.53849(12) 0.41768(7) 0.0226(5) Uani 1 1 d . . . H9 H 0.5414 0.4985 0.4093 0.034 Uiso 1 1 calc R . . O10 O 0.50285(19) 0.38508(16) 0.46194(8) 0.0209(6) Uani 1 1 d . . . H10 H 0.4962 0.4019 0.4995 0.031 Uiso 1 1 calc R . . O11 O 0.43207(16) 0.26775(14) 0.52778(7) 0.0251(5) Uani 1 1 d . . . H11 H 0.5022 0.2947 0.5355 0.038 Uiso 1 1 calc R . . O12 O 0.30413(16) 0.11066(13) 0.46953(8) 0.0259(5) Uani 1 1 d . . . H12 H 0.3601 0.1163 0.4955 0.039 Uiso 1 1 calc R . . OZ1 O -0.45254(18) -0.11181(15) 0.44100(10) 0.0391(6) Uani 1 1 d . . . HZ1 H -0.5241 -0.1351 0.4391 0.059 Uiso 1 1 calc R . . OZ2 O -0.70350(18) -0.18633(14) 0.43190(8) 0.0335(6) Uani 1 1 d . . . HZ2 H -0.7334 -0.1620 0.4650 0.050 Uiso 1 1 calc R . . OX2 O -0.2294(3) 0.67299(19) 0.40818(15) 0.0859(12) Uani 1 1 d . . . OZ3 O -0.1822(2) 0.56523(19) 0.52805(9) 0.0478(7) Uani 1 1 d . . . HZ3 H -0.2291 0.5621 0.5552 0.072 Uiso 1 1 calc R . . C1 C 0.1955(3) 0.0657(2) 0.35243(11) 0.0208(9) Uani 1 1 d . . . H1A H 0.2162 0.0235 0.3733 0.025 Uiso 1 1 calc R . . C1A C 0.2054(3) 0.0190(2) 0.28477(11) 0.0261(8) Uani 1 1 d . . . H1A1 H 0.1903 0.0596 0.2623 0.031 Uiso 1 1 calc R . . H1A2 H 0.1427 -0.0326 0.2706 0.031 Uiso 1 1 calc R . . C1B C 0.3300(2) -0.0117(2) 0.27117(11) 0.0290(8) Uani 1 1 d . . . H1B1 H 0.3907 0.0408 0.2801 0.035 Uiso 1 1 calc R . . H1B2 H 0.3497 -0.0442 0.2988 0.035 Uiso 1 1 calc R . . C1C C 0.3406(3) -0.0699(2) 0.20664(12) 0.0355(8) Uani 1 1 d . . . H1C1 H 0.3316 -0.0355 0.1790 0.043 Uiso 1 1 calc R . . H1C2 H 0.2747 -0.1193 0.1958 0.043 Uiso 1 1 calc R . . C1D C 0.4615(3) -0.1063(2) 0.19842(13) 0.0406(9) Uani 1 1 d . . . H1D1 H 0.4690 -0.1409 0.2261 0.049 Uiso 1 1 calc R . . H1D2 H 0.5265 -0.0563 0.2108 0.049 Uiso 1 1 calc R . . C1E C 0.4820(3) -0.1644(2) 0.13451(13) 0.0409(9) Uani 1 1 d . . . H1E1 H 0.4159 -0.2137 0.1215 0.049 Uiso 1 1 calc R . . H1E2 H 0.5585 -0.1900 0.1353 0.049 Uiso 1 1 calc R . . C1F C 0.4879(3) -0.1170(2) 0.08769(13) 0.0396(9) Uani 1 1 d . . . H1F1 H 0.4051 -0.1180 0.0712 0.048 Uiso 1 1 calc R . . H1F2 H 0.5212 -0.0547 0.1077 0.048 Uiso 1 1 calc R . . C1G C 0.5653(3) -0.1588(2) 0.03608(13) 0.0379(9) Uani 1 1 d . . . H1G1 H 0.6476 -0.1579 0.0531 0.045 Uiso 1 1 calc R . . H1G2 H 0.5318 -0.2211 0.0167 0.045 Uiso 1 1 calc R . . C1H C 0.5749(3) -0.1150(2) -0.01212(13) 0.0395(9) Uani 1 1 d . . . H1H1 H 0.5983 -0.0510 0.0075 0.047 Uiso 1 1 calc R . . H1H2 H 0.4948 -0.1232 -0.0334 0.047 Uiso 1 1 calc R . . C1I C 0.6666(3) -0.1515(2) -0.05825(13) 0.0404(9) Uani 1 1 d . . . H1I1 H 0.7465 -0.1430 -0.0366 0.048 Uiso 1 1 calc R . . H1I2 H 0.6434 -0.2156 -0.0772 0.048 Uiso 1 1 calc R . . C1J C 0.6788(3) -0.1104(2) -0.10790(14) 0.0456(10) Uani 1 1 d . . . H1J1 H 0.6981 -0.0458 -0.0893 0.055 Uiso 1 1 calc R . . H1J2 H 0.6005 -0.1220 -0.1314 0.055 Uiso 1 1 calc R . . C1K C 0.7763(3) -0.1455(2) -0.15067(14) 0.0520(10) Uani 1 1 d . . . H1K1 H 0.8544 -0.1332 -0.1278 0.078 Uiso 1 1 calc R . . H1K2 H 0.7806 -0.1168 -0.1817 0.078 Uiso 1 1 calc R . . H1K3 H 0.7568 -0.2092 -0.1700 0.078 Uiso 1 1 calc R . . C2 C 0.0684(2) 0.08581(18) 0.36898(11) 0.0190(7) Uani 1 1 d . . . C3 C 0.0195(2) 0.07090(18) 0.41981(11) 0.0202(7) Uani 1 1 d . . . C4 C -0.0924(2) 0.09465(18) 0.43759(11) 0.0229(7) Uani 1 1 d . . . C5 C -0.1614(2) 0.13298(18) 0.40494(11) 0.0197(7) Uani 1 1 d . . . C6 C -0.1178(2) 0.14482(18) 0.35211(11) 0.0197(7) Uani 1 1 d . . . C7 C -0.0034(2) 0.12257(18) 0.33645(10) 0.0197(7) Uani 1 1 d . . . H7A H 0.0277 0.1329 0.3016 0.024 Uiso 1 1 calc R . . C8 C -0.1953(2) 0.17923(18) 0.31197(11) 0.0219(7) Uani 1 1 d . . . H8A H -0.2807 0.1690 0.3227 0.026 Uiso 1 1 calc R . . C8A C -0.1911(2) 0.1268(2) 0.24470(11) 0.0278(8) Uani 1 1 d . . . H8A1 H -0.1097 0.1395 0.2313 0.033 Uiso 1 1 calc R . . H8A2 H -0.2042 0.0632 0.2394 0.033 Uiso 1 1 calc R . . C8B C -0.2847(3) 0.1474(2) 0.20466(12) 0.0330(8) Uani 1 1 d . . . H8B1 H -0.2772 0.2119 0.2133 0.040 Uiso 1 1 calc R . . H8B2 H -0.3663 0.1288 0.2153 0.040 Uiso 1 1 calc R . . C8C C -0.2727(3) 0.1024(2) 0.13649(12) 0.0362(8) Uani 1 1 d . . . H8C1 H -0.2691 0.0388 0.1290 0.043 Uiso 1 1 calc R . . H8C2 H -0.3464 0.1080 0.1144 0.043 Uiso 1 1 calc R . . C8D C -0.1645(3) 0.1381(2) 0.11062(13) 0.0442(9) Uani 1 1 d . . . H8D1 H -0.0904 0.1250 0.1283 0.053 Uiso 1 1 calc R . . H8D2 H -0.1617 0.2028 0.1225 0.053 Uiso 1 1 calc R . . C8E C -0.1653(3) 0.0999(2) 0.04170(12) 0.0420(9) Uani 1 1 d . . . H8E1 H -0.1680 0.0351 0.0300 0.050 Uiso 1 1 calc R . . H8E2 H -0.2398 0.1127 0.0242 0.050 Uiso 1 1 calc R . . C8F C -0.0578(3) 0.1349(3) 0.01447(13) 0.0523(10) Uani 1 1 d . . . H8F1 H 0.0165 0.1187 0.0299 0.063 Uiso 1 1 calc R . . H8F2 H -0.0519 0.1999 0.0283 0.063 Uiso 1 1 calc R . . C8G C -0.0631(3) 0.1006(2) -0.05476(13) 0.0433(9) Uani 1 1 d . . . H8G1 H -0.0716 0.0355 -0.0686 0.052 Uiso 1 1 calc R . . H8G2 H -0.1359 0.1185 -0.0702 0.052 Uiso 1 1 calc R . . C8H C 0.0465(3) 0.1334(3) -0.08204(14) 0.0517(10) Uani 1 1 d . . . H8H1 H 0.1185 0.1116 -0.0691 0.062 Uiso 1 1 calc R . . H8H2 H 0.0588 0.1985 -0.0656 0.062 Uiso 1 1 calc R . . C8I C 0.0383(3) 0.1056(2) -0.15057(13) 0.0427(9) Uani 1 1 d . . . H8I1 H 0.0260 0.0405 -0.1671 0.051 Uiso 1 1 calc R . . H8I2 H -0.0333 0.1276 -0.1637 0.051 Uiso 1 1 calc R . . C8J C 0.1487(3) 0.1388(3) -0.17705(15) 0.0527(10) Uani 1 1 d . . . H8J1 H 0.1651 0.2034 -0.1576 0.063 Uiso 1 1 calc R . . H8J2 H 0.2190 0.1126 -0.1668 0.063 Uiso 1 1 calc R . . C8K C 0.1383(3) 0.1185(2) -0.24456(15) 0.0548(11) Uani 1 1 d . . . H8K1 H 0.1259 0.0546 -0.2645 0.082 Uiso 1 1 calc R . . H8K2 H 0.2126 0.1431 -0.2578 0.082 Uiso 1 1 calc R . . H8K3 H 0.0696 0.1447 -0.2553 0.082 Uiso 1 1 calc R . . C9 C -0.1668(2) 0.27811(18) 0.32549(10) 0.0171(7) Uani 1 1 d . . . C10 C -0.2275(2) 0.33737(19) 0.36842(10) 0.0184(7) Uani 1 1 d . . . C11 C -0.2074(2) 0.42726(18) 0.37919(10) 0.0167(7) Uani 1 1 d . . . C12 C -0.1233(2) 0.46074(19) 0.34746(11) 0.0190(7) Uani 1 1 d . . . C13 C -0.0534(2) 0.40443(19) 0.30665(10) 0.0173(7) Uani 1 1 d . . . C14 C -0.0781(2) 0.31513(19) 0.29629(10) 0.0187(7) Uani 1 1 d . . . H14 H -0.0324 0.2766 0.2678 0.022 Uiso 1 1 calc R . . C15 C 0.0487(2) 0.44364(18) 0.27760(10) 0.0191(7) Uani 1 1 d . . . H15 H 0.0252 0.5007 0.2756 0.023 Uiso 1 1 calc R . . C15A C 0.0657(2) 0.38672(19) 0.21231(11) 0.0259(8) Uani 1 1 d . . . H15A H 0.0862 0.3287 0.2123 0.031 Uiso 1 1 calc R . . H15B H -0.0115 0.3769 0.1882 0.031 Uiso 1 1 calc R . . C15B C 0.1640(3) 0.4276(2) 0.18211(11) 0.0304(8) Uani 1 1 d . . . H15C H 0.1535 0.4902 0.1898 0.036 Uiso 1 1 calc R . . H15D H 0.2437 0.4254 0.2005 0.036 Uiso 1 1 calc R . . C15C C 0.1616(3) 0.3809(2) 0.11423(11) 0.0306(8) Uani 1 1 d . . . H15E H 0.0837 0.3864 0.0956 0.037 Uiso 1 1 calc R . . H15F H 0.1667 0.3175 0.1066 0.037 Uiso 1 1 calc R . . C15D C 0.2646(3) 0.4178(2) 0.08401(11) 0.0310(8) Uani 1 1 d . . . H15G H 0.2644 0.4822 0.0948 0.037 Uiso 1 1 calc R . . H15H H 0.3425 0.4071 0.0997 0.037 Uiso 1 1 calc R . . C15E C 0.2543(3) 0.3762(2) 0.01520(11) 0.0311(8) Uani 1 1 d . . . H15I H 0.2536 0.3117 0.0046 0.037 Uiso 1 1 calc R . . H15J H 0.1766 0.3873 -0.0003 0.037 Uiso 1 1 calc R . . C15F C 0.3569(3) 0.4114(2) -0.01608(11) 0.0311(8) Uani 1 1 d . . . H15K H 0.3620 0.4763 -0.0032 0.037 Uiso 1 1 calc R . . H15L H 0.4343 0.3959 -0.0034 0.037 Uiso 1 1 calc R . . C15G C 0.3382(3) 0.3738(2) -0.08470(12) 0.0333(8) Uani 1 1 d . . . H15M H 0.3291 0.3088 -0.0969 0.040 Uiso 1 1 calc R . . H15N H 0.2618 0.3911 -0.0970 0.040 Uiso 1 1 calc R . . C15H C 0.4389(3) 0.4031(2) -0.11891(12) 0.0343(8) Uani 1 1 d . . . H15O H 0.5145 0.3823 -0.1091 0.041 Uiso 1 1 calc R . . H15P H 0.4516 0.4682 -0.1054 0.041 Uiso 1 1 calc R . . C15I C 0.4121(3) 0.3682(2) -0.18712(12) 0.0395(9) Uani 1 1 d . . . H15Q H 0.3365 0.3892 -0.1967 0.047 Uiso 1 1 calc R . . H15R H 0.3984 0.3031 -0.2004 0.047 Uiso 1 1 calc R . . C15J C 0.5123(3) 0.3959(3) -0.22293(14) 0.0532(11) Uani 1 1 d . . . H15S H 0.5319 0.4607 -0.2072 0.064 Uiso 1 1 calc R . . H15T H 0.5857 0.3695 -0.2170 0.064 Uiso 1 1 calc R . . C15K C 0.4769(4) 0.3676(3) -0.28995(15) 0.0777(14) Uani 1 1 d . . . H15U H 0.4584 0.3034 -0.3059 0.117 Uiso 1 1 calc R . . H15V H 0.5439 0.3863 -0.3112 0.117 Uiso 1 1 calc R . . H15W H 0.4056 0.3949 -0.2961 0.117 Uiso 1 1 calc R . . C16 C 0.1647(2) 0.46610(19) 0.31813(10) 0.0186(7) Uani 1 1 d . . . C17 C 0.1979(2) 0.55046(19) 0.35826(11) 0.0207(8) Uani 1 1 d . . . C18 C 0.3080(2) 0.5706(2) 0.39207(11) 0.0197(8) Uani 1 1 d . . . C19 C 0.3863(2) 0.5070(2) 0.38530(11) 0.0196(8) Uani 1 1 d . . . C20 C 0.3534(2) 0.42108(19) 0.34830(10) 0.0163(7) Uani 1 1 d . . . C21 C 0.2426(2) 0.40283(18) 0.31587(10) 0.0199(7) Uani 1 1 d . . . H21 H 0.2183 0.3440 0.2907 0.024 Uiso 1 1 calc R . . C22 C 0.4365(2) 0.34897(17) 0.34119(10) 0.0187(7) Uani 1 1 d . . . H22 H 0.5163 0.3795 0.3616 0.022 Uiso 1 1 calc R . . C22A C 0.4599(2) 0.30322(19) 0.27483(11) 0.0258(8) Uani 1 1 d . . . H22A H 0.4977 0.2492 0.2712 0.031 Uiso 1 1 calc R . . H22B H 0.3820 0.2856 0.2506 0.031 Uiso 1 1 calc R . . C22B C 0.5422(2) 0.36295(19) 0.24969(11) 0.0262(7) Uani 1 1 d . . . H22C H 0.5124 0.4213 0.2607 0.031 Uiso 1 1 calc R . . H22D H 0.6244 0.3713 0.2690 0.031 Uiso 1 1 calc R . . C22C C 0.5495(2) 0.3274(2) 0.18136(11) 0.0289(8) Uani 1 1 d . . . H22E H 0.5585 0.2639 0.1694 0.035 Uiso 1 1 calc R . . H22F H 0.4724 0.3332 0.1621 0.035 Uiso 1 1 calc R . . C22D C 0.6518(3) 0.3728(2) 0.15719(11) 0.0309(8) Uani 1 1 d . . . H22G H 0.7292 0.3656 0.1754 0.037 Uiso 1 1 calc R . . H22H H 0.6442 0.4365 0.1698 0.037 Uiso 1 1 calc R . . C22E C 0.6545(3) 0.3372(2) 0.08863(12) 0.0370(9) Uani 1 1 d . . . H22I H 0.6568 0.2728 0.0761 0.044 Uiso 1 1 calc R . . H22J H 0.5787 0.3475 0.0707 0.044 Uiso 1 1 calc R . . C22F C 0.7600(3) 0.3775(2) 0.06296(12) 0.0367(9) Uani 1 1 d . . . H22K H 0.8360 0.3669 0.0805 0.044 Uiso 1 1 calc R . . H22L H 0.7580 0.4419 0.0755 0.044 Uiso 1 1 calc R . . C22G C 0.7606(3) 0.3414(2) -0.00572(12) 0.0405(9) Uani 1 1 d . . . H22M H 0.7621 0.2769 -0.0182 0.049 Uiso 1 1 calc R . . H22N H 0.6847 0.3521 -0.0233 0.049 Uiso 1 1 calc R . . C22H C 0.8661(3) 0.3811(2) -0.03163(13) 0.0454(10) Uani 1 1 d . . . H22O H 0.9419 0.3712 -0.0134 0.054 Uiso 1 1 calc R . . H22P H 0.8638 0.4455 -0.0196 0.054 Uiso 1 1 calc R . . C22I C 0.8692(3) 0.3448(2) -0.09995(13) 0.0470(10) Uani 1 1 d . . . H22Q H 0.8727 0.2806 -0.1120 0.056 Uiso 1 1 calc R . . H22R H 0.7931 0.3541 -0.1182 0.056 Uiso 1 1 calc R . . C22J C 0.9733(3) 0.3853(3) -0.12534(15) 0.0662(13) Uani 1 1 d . . . H22S H 1.0493 0.3775 -0.1062 0.079 Uiso 1 1 calc R . . H22T H 0.9685 0.4493 -0.1141 0.079 Uiso 1 1 calc R . . C22K C 0.9791(4) 0.3476(3) -0.19368(16) 0.0795(14) Uani 1 1 d . . . H22U H 0.9903 0.2852 -0.2052 0.119 Uiso 1 1 calc R . . H22V H 1.0470 0.3796 -0.2067 0.119 Uiso 1 1 calc R . . H22W H 0.9037 0.3539 -0.2133 0.119 Uiso 1 1 calc R . . C23 C 0.3916(3) 0.2854(2) 0.37466(12) 0.0181(8) Uani 1 1 d . . . C24 C 0.4303(3) 0.3073(2) 0.43571(12) 0.0160(9) Uani 1 1 d . . . C25 C 0.4002(3) 0.2484(2) 0.46698(11) 0.0180(8) Uani 1 1 d . . . C26 C 0.3313(3) 0.1701(2) 0.43890(12) 0.0187(8) Uani 1 1 d . . . C27 C 0.2838(3) 0.1478(2) 0.37900(11) 0.0165(9) Uani 1 1 d . . . C28 C 0.3176(3) 0.2075(2) 0.34840(11) 0.0176(8) Uani 1 1 d . . . H28 H 0.2882 0.1937 0.3076 0.021 Uiso 1 1 calc R . . CV1 C -0.1589(8) 0.7554(4) 0.4121(4) 0.219(6) Uani 1 1 d . . . HV1A H -0.1963 0.8009 0.4434 0.263 Uiso 1 1 calc R . . HV1B H -0.0790 0.7527 0.4301 0.263 Uiso 1 1 calc R . . CX1 C -0.0954(4) 0.6409(3) 0.55124(15) 0.0496(11) Uani 1 1 d . . . HX1A H -0.0640 0.6447 0.5920 0.059 Uiso 1 1 calc R . . HX1B H -0.1344 0.6945 0.5551 0.059 Uiso 1 1 calc R . . CX2 C 0.0055(3) 0.6365(3) 0.51098(15) 0.0573(11) Uani 1 1 d . . . HX2A H 0.0480 0.5860 0.5097 0.086 Uiso 1 1 calc R . . HX2B H 0.0616 0.6908 0.5264 0.086 Uiso 1 1 calc R . . HX2C H -0.0260 0.6299 0.4701 0.086 Uiso 1 1 calc R . . CV2 C -0.1387(7) 0.7847(6) 0.3754(4) 0.206(5) Uani 1 1 d . . . HV2A H -0.0594 0.7710 0.3603 0.309 Uiso 1 1 calc R . . HV2B H -0.1385 0.8487 0.3917 0.309 Uiso 1 1 calc R . . HV2C H -0.2006 0.7600 0.3422 0.309 Uiso 1 1 calc R . . CZQ C -0.4501(3) -0.0365(2) 0.42110(14) 0.0409(9) Uani 1 1 d . . . HZQ1 H -0.4080 0.0158 0.4528 0.049 Uiso 1 1 calc R . . HZQ2 H -0.5338 -0.0248 0.4147 0.049 Uiso 1 1 calc R . . CZ3 C -0.7709(3) -0.1719(2) 0.38347(15) 0.0514(10) Uani 1 1 d . . . HZ3A H -0.7666 -0.1081 0.3898 0.062 Uiso 1 1 calc R . . HZ3B H -0.8568 -0.1955 0.3826 0.062 Uiso 1 1 calc R . . CZ4 C -0.7182(3) -0.2174(2) 0.32505(14) 0.0560(11) Uani 1 1 d . . . HZ4A H -0.6332 -0.1938 0.3263 0.084 Uiso 1 1 calc R . . HZ4B H -0.7628 -0.2078 0.2917 0.084 Uiso 1 1 calc R . . HZ4C H -0.7239 -0.2807 0.3188 0.084 Uiso 1 1 calc R . . CZ7 C -0.3871(3) -0.0514(2) 0.36361(14) 0.0501(10) Uani 1 1 d . . . HZ7A H -0.3037 -0.0617 0.3701 0.075 Uiso 1 1 calc R . . HZ7B H -0.3869 0.0006 0.3507 0.075 Uiso 1 1 calc R . . HZ7C H -0.4292 -0.1028 0.3322 0.075 Uiso 1 1 calc R . . H4U H -0.301(3) 0.680(2) 0.4210(14) 0.043(9) Uiso 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 O1 0.0245(10) 0.0271(15) 0.0298(10) 0.0189(10) -0.0013(9) -0.0018(11) O2 0.0303(11) 0.0397(15) 0.0321(10) 0.0269(10) 0.0098(9) 0.0105(11) O3 0.0318(11) 0.0307(15) 0.0332(10) 0.0207(10) 0.0112(9) 0.0123(11) O4 0.0240(10) 0.0204(14) 0.0253(9) 0.0100(9) 0.0077(8) 0.0001(10) O5 0.0213(10) 0.0177(15) 0.0214(9) -0.0014(9) 0.0022(8) -0.0033(11) O6 0.0241(11) 0.0216(15) 0.0317(10) 0.0094(10) 0.0088(9) 0.0028(11) O7 0.0209(10) 0.0219(15) 0.0329(10) 0.0073(10) -0.0014(9) 0.0023(11) O8 0.0260(11) 0.0187(15) 0.0288(10) 0.0034(10) -0.0045(9) 0.0044(11) O9 0.0230(10) 0.0207(14) 0.0215(9) 0.0033(9) -0.0027(8) 0.0038(10) O10 0.0247(11) 0.0180(16) 0.0168(8) 0.0039(10) 0.0001(9) -0.0057(12) O11 0.0269(10) 0.0298(16) 0.0186(9) 0.0113(10) -0.0041(8) -0.0067(12) O12 0.0274(11) 0.0269(15) 0.0261(10) 0.0160(10) -0.0052(8) -0.0069(11) OZ1 0.0385(12) 0.0421(17) 0.0441(12) 0.0290(12) -0.0111(11) -0.0077(13) OZ2 0.0375(12) 0.0308(15) 0.0333(11) 0.0101(11) 0.0066(9) 0.0087(12) OX2 0.085(2) 0.044(2) 0.144(3) 0.0409(19) 0.086(2) 0.0281(19) OZ3 0.0468(15) 0.063(2) 0.0248(11) 0.0083(13) 0.0048(11) -0.0134(17) C1 0.0229(16) 0.019(2) 0.0203(12) 0.0068(15) 0.0007(12) 0.0011(19) C1A 0.0338(17) 0.023(2) 0.0200(12) 0.0061(14) -0.0001(12) -0.0015(17) C1B 0.0271(16) 0.030(2) 0.0252(13) 0.0036(14) 0.0021(12) 0.0005(17) C1C 0.0404(18) 0.038(2) 0.0272(14) 0.0073(15) 0.0043(13) 0.0086(18) C1D 0.0368(18) 0.051(3) 0.0305(15) 0.0064(16) 0.0040(14) 0.0118(19) C1E 0.0446(19) 0.043(3) 0.0331(16) 0.0063(16) 0.0100(15) 0.0127(19) C1F 0.0437(19) 0.040(3) 0.0342(16) 0.0093(16) 0.0064(15) 0.0079(19) C1G 0.0362(18) 0.044(2) 0.0298(15) 0.0057(16) 0.0035(14) 0.0065(19) C1H 0.0350(18) 0.046(3) 0.0371(16) 0.0129(17) 0.0021(14) 0.0048(19) C1I 0.0411(19) 0.049(3) 0.0301(15) 0.0120(16) 0.0028(14) 0.0064(19) C1J 0.052(2) 0.049(3) 0.0379(17) 0.0186(18) 0.0022(16) 0.002(2) C1K 0.056(2) 0.068(3) 0.0313(16) 0.0164(19) 0.0048(16) 0.002(2) C2 0.0222(14) 0.012(2) 0.0202(12) 0.0030(12) -0.0006(11) -0.0043(15) C3 0.0246(15) 0.014(2) 0.0232(12) 0.0092(13) -0.0034(11) -0.0035(15) C4 0.0291(15) 0.021(2) 0.0210(12) 0.0119(13) 0.0035(12) -0.0011(16) C5 0.0205(14) 0.014(2) 0.0236(12) 0.0059(13) 0.0012(11) -0.0020(15) C6 0.0260(15) 0.013(2) 0.0181(12) 0.0048(12) -0.0021(11) -0.0022(15) C7 0.0242(14) 0.018(2) 0.0153(11) 0.0053(12) -0.0003(11) -0.0055(15) C8 0.0245(15) 0.022(2) 0.0196(12) 0.0077(13) -0.0005(11) 0.0015(16) C8A 0.0296(16) 0.028(2) 0.0256(13) 0.0080(14) -0.0018(12) 0.0038(17) C8B 0.0344(17) 0.036(2) 0.0251(14) 0.0055(15) -0.0068(13) 0.0038(18) C8C 0.0352(18) 0.042(2) 0.0253(14) 0.0020(15) -0.0069(13) 0.0062(18) C8D 0.050(2) 0.054(3) 0.0270(15) 0.0135(17) -0.0016(15) 0.001(2) C8E 0.044(2) 0.048(3) 0.0268(15) 0.0038(16) -0.0013(14) 0.002(2) C8F 0.050(2) 0.075(3) 0.0303(16) 0.0189(19) -0.0016(16) 0.000(2) C8G 0.0417(19) 0.050(3) 0.0286(15) 0.0033(17) -0.0027(14) -0.004(2) C8H 0.044(2) 0.073(3) 0.0363(17) 0.0199(19) -0.0009(16) -0.004(2) C8I 0.0420(19) 0.050(3) 0.0309(16) 0.0075(17) 0.0005(15) 0.000(2) C8J 0.057(2) 0.052(3) 0.0426(19) 0.0124(19) 0.0035(18) -0.011(2) C8K 0.067(3) 0.051(3) 0.0456(19) 0.0156(19) 0.0165(19) 0.001(2) C9 0.0154(13) 0.019(2) 0.0161(11) 0.0067(13) -0.0046(10) -0.0021(15) C10 0.0153(14) 0.023(2) 0.0179(12) 0.0106(13) -0.0013(11) -0.0035(16) C11 0.0155(14) 0.015(2) 0.0173(12) 0.0041(13) -0.0025(11) -0.0036(15) C12 0.0209(15) 0.016(2) 0.0195(12) 0.0069(13) -0.0037(11) -0.0026(16) C13 0.0168(14) 0.019(2) 0.0164(11) 0.0073(13) -0.0016(11) -0.0025(16) C14 0.0189(14) 0.023(2) 0.0136(11) 0.0051(13) -0.0008(11) 0.0027(16) C15 0.0238(14) 0.0152(19) 0.0186(12) 0.0064(12) 0.0021(11) 0.0002(15) C15A 0.0276(15) 0.032(2) 0.0193(12) 0.0100(14) 0.0033(12) 0.0017(16) C15B 0.0344(17) 0.036(2) 0.0220(13) 0.0117(14) 0.0067(12) -0.0004(17) C15C 0.0341(17) 0.036(2) 0.0217(13) 0.0102(14) 0.0055(12) -0.0011(17) C15D 0.0319(16) 0.040(2) 0.0220(13) 0.0129(15) 0.0055(12) -0.0010(17) C15E 0.0322(16) 0.039(2) 0.0222(13) 0.0114(14) 0.0060(12) -0.0006(17) C15F 0.0353(17) 0.035(2) 0.0238(13) 0.0113(15) 0.0068(13) 0.0000(17) C15G 0.0409(18) 0.035(2) 0.0246(14) 0.0108(15) 0.0073(13) 0.0021(18) C15H 0.0403(18) 0.037(2) 0.0252(14) 0.0114(15) 0.0079(13) 0.0007(18) C15I 0.054(2) 0.040(3) 0.0241(14) 0.0119(16) 0.0100(14) -0.002(2) C15J 0.067(2) 0.061(3) 0.0389(18) 0.0239(19) 0.0240(18) 0.010(2) C15K 0.123(4) 0.084(3) 0.0390(19) 0.033(2) 0.037(2) 0.018(3) C16 0.0184(14) 0.022(2) 0.0161(12) 0.0083(14) 0.0031(11) -0.0021(16) C17 0.0208(15) 0.024(2) 0.0198(12) 0.0102(14) 0.0044(11) 0.0045(16) C18 0.0247(15) 0.013(2) 0.0189(12) 0.0039(14) 0.0030(12) -0.0025(17) C19 0.0190(15) 0.024(2) 0.0170(12) 0.0097(14) 0.0013(11) -0.0005(17) C20 0.0222(15) 0.012(2) 0.0151(11) 0.0058(13) 0.0029(11) -0.0009(16) C21 0.0275(15) 0.015(2) 0.0144(11) 0.0033(12) 0.0028(11) -0.0033(15) C22 0.0227(14) 0.0142(19) 0.0184(12) 0.0046(12) 0.0022(11) 0.0007(15) C22A 0.0286(15) 0.030(2) 0.0215(12) 0.0100(13) 0.0061(12) 0.0073(16) C22B 0.0322(16) 0.026(2) 0.0199(12) 0.0079(13) 0.0042(12) -0.0008(16) C22C 0.0330(16) 0.036(2) 0.0212(13) 0.0127(14) 0.0030(12) 0.0086(17) C22D 0.0366(17) 0.033(2) 0.0243(13) 0.0119(14) 0.0056(13) 0.0024(18) C22E 0.0464(19) 0.043(2) 0.0261(14) 0.0157(15) 0.0092(14) 0.0090(19) C22F 0.0419(18) 0.044(2) 0.0268(14) 0.0155(16) 0.0085(14) 0.0029(19) C22G 0.0457(19) 0.051(3) 0.0281(15) 0.0163(16) 0.0122(14) 0.008(2) C22H 0.046(2) 0.064(3) 0.0328(16) 0.0241(18) 0.0139(15) 0.007(2) C22I 0.056(2) 0.058(3) 0.0355(16) 0.0221(17) 0.0195(16) 0.020(2) C22J 0.058(2) 0.111(4) 0.047(2) 0.047(2) 0.0225(18) 0.021(3) C22K 0.106(3) 0.106(4) 0.050(2) 0.045(2) 0.046(2) 0.044(3) C23 0.0177(15) 0.018(2) 0.0197(12) 0.0076(14) 0.0031(12) 0.0025(18) C24 0.0148(15) 0.008(3) 0.0207(12) 0.0005(15) -0.0012(12) -0.0061(19) C25 0.0178(15) 0.017(2) 0.0169(12) 0.0040(14) -0.0013(12) -0.0022(18) C26 0.0156(15) 0.020(2) 0.0221(13) 0.0106(15) 0.0012(12) -0.0012(18) C27 0.0148(15) 0.010(3) 0.0208(12) 0.0020(15) -0.0015(12) -0.0046(19) C28 0.0186(15) 0.016(2) 0.0153(11) 0.0013(14) -0.0017(12) -0.0006(18) CV1 0.287(10) 0.053(5) 0.325(12) 0.052(6) 0.256(10) 0.047(6) CX1 0.054(2) 0.053(3) 0.0318(17) 0.005(2) -0.0004(17) -0.008(3) CX2 0.049(2) 0.074(3) 0.0425(19) 0.018(2) -0.0018(17) -0.015(2) CV2 0.155(7) 0.260(11) 0.317(12) 0.256(10) 0.028(7) 0.006(7) CZQ 0.051(2) 0.038(2) 0.0388(17) 0.0208(17) 0.0001(15) 0.001(2) CZ3 0.058(2) 0.054(3) 0.053(2) 0.030(2) 0.0022(18) 0.020(2) CZ4 0.067(3) 0.060(3) 0.0414(19) 0.022(2) 0.0009(18) -0.006(2) CZ7 0.061(2) 0.050(3) 0.0372(18) 0.0190(18) -0.0020(17) -0.016(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 O1 C3 1.390(3) . ? O2 C4 1.377(3) . ? O3 C5 1.373(3) . ? O4 C10 1.383(3) . ? O5 C11 1.390(3) . ? O6 C12 1.371(3) . ? O7 C17 1.377(3) . ? O8 C18 1.371(3) . ? O9 C19 1.382(3) . ? O10 C24 1.370(4) . ? O11 C25 1.384(3) . ? O12 C26 1.386(3) . ? OZ1 CZQ 1.436(3) . ? OZ2 CZ3 1.442(3) . ? OX2 CV1 1.448(7) . ? OZ3 CX1 1.424(4) . ? C1 C27 1.511(4) . ? C1 C2 1.519(3) . ? C1 C1A 1.530(3) . ? C1A C1B 1.530(3) . ? C1B C1C 1.514(4) . ? C1C C1D 1.520(4) . ? C1D C1E 1.523(4) . ? C1E C1F 1.526(4) . ? C1F C1G 1.516(4) . ? C1G C1H 1.512(4) . ? C1H C1I 1.523(4) . ? C1I C1J 1.515(4) . ? C1J C1K 1.522(4) . ? C2 C7 1.394(3) . ? C2 C3 1.398(3) . ? C3 C4 1.378(3) . ? C4 C5 1.395(3) . ? C5 C6 1.400(3) . ? C6 C7 1.386(3) . ? C6 C8 1.533(3) . ? C8 C9 1.523(4) . ? C8 C8A 1.532(3) . ? C8A C8B 1.522(4) . ? C8B C8C 1.539(4) . ? C8C C8D 1.505(4) . ? C8D C8E 1.528(4) . ? C8E C8F 1.511(4) . ? C8F C8G 1.530(4) . ? C8G C8H 1.515(4) . ? C8H C8I 1.516(4) . ? C8I C8J 1.515(4) . ? C8J C8K 1.505(4) . ? C9 C10 1.389(3) . ? C9 C14 1.404(3) . ? C10 C11 1.385(4) . ? C11 C12 1.380(3) . ? C12 C13 1.403(3) . ? C13 C14 1.381(4) . ? C13 C15 1.522(3) . ? C15 C16 1.528(4) . ? C15 C15A 1.535(3) . ? C15A C15B 1.521(4) . ? C15B C15C 1.520(3) . ? C15C C15D 1.528(4) . ? C15D C15E 1.527(4) . ? C15E C15F 1.527(4) . ? C15F C15G 1.523(4) . ? C15G C15H 1.514(4) . ? C15H C15I 1.522(4) . ? C15I C15J 1.525(4) . ? C15J C15K 1.515(5) . ? C16 C17 1.389(4) . ? C16 C21 1.401(3) . ? C17 C18 1.396(4) . ? C18 C19 1.393(3) . ? C19 C20 1.384(4) . ? C20 C21 1.389(4) . ? C20 C22 1.536(3) . ? C22 C22A 1.530(3) . ? C22 C23 1.533(4) . ? C22A C22B 1.524(4) . ? C22B C22C 1.521(3) . ? C22C C22D 1.509(4) . ? C22D C22E 1.521(4) . ? C22E C22F 1.512(4) . ? C22F C22G 1.522(4) . ? C22G C22H 1.512(4) . ? C22H C22I 1.517(4) . ? C22I C22J 1.498(4) . ? C22J C22K 1.521(5) . ? C23 C28 1.379(4) . ? C23 C24 1.402(4) . ? C24 C25 1.395(4) . ? C25 C26 1.364(4) . ? C26 C27 1.406(4) . ? C27 C28 1.403(4) . ? CV1 CV2 1.123(9) . ? CX1 CX2 1.475(4) . ? CZQ CZ7 1.492(4) . ? CZ3 CZ4 1.494(4) . ? 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 C27 C1 C2 109.8(2) . . ? C27 C1 C1A 114.4(2) . . ? C2 C1 C1A 113.2(2) . . ? C1 C1A C1B 111.6(2) . . ? C1C C1B C1A 114.5(2) . . ? C1B C1C C1D 111.5(2) . . ? C1C C1D C1E 115.5(3) . . ? C1D C1E C1F 114.5(3) . . ? C1G C1F C1E 112.2(2) . . ? C1H C1G C1F 115.0(2) . . ? C1G C1H C1I 112.9(2) . . ? C1J C1I C1H 115.0(3) . . ? C1I C1J C1K 112.8(3) . . ? C7 C2 C3 116.6(2) . . ? C7 C2 C1 122.7(2) . . ? C3 C2 C1 120.6(2) . . ? C4 C3 O1 115.8(2) . . ? C4 C3 C2 121.0(2) . . ? O1 C3 C2 123.2(2) . . ? O2 C4 C3 121.3(2) . . ? O2 C4 C5 117.5(2) . . ? C3 C4 C5 121.2(2) . . ? O3 C5 C4 116.0(2) . . ? O3 C5 C6 124.7(2) . . ? C4 C5 C6 119.3(2) . . ? C7 C6 C5 118.0(2) . . ? C7 C6 C8 121.0(2) . . ? C5 C6 C8 120.9(2) . . ? C6 C7 C2 123.7(2) . . ? C9 C8 C8A 112.9(2) . . ? C9 C8 C6 112.3(2) . . ? C8A C8 C6 112.1(2) . . ? C8B C8A C8 113.4(2) . . ? C8A C8B C8C 113.8(2) . . ? C8D C8C C8B 115.2(3) . . ? C8C C8D C8E 113.2(3) . . ? C8F C8E C8D 114.3(3) . . ? C8E C8F C8G 114.0(3) . . ? C8H C8G C8F 114.0(3) . . ? C8G C8H C8I 114.6(3) . . ? C8J C8I C8H 113.8(3) . . ? C8K C8J C8I 114.7(3) . . ? C10 C9 C14 115.9(3) . . ? C10 C9 C8 121.3(2) . . ? C14 C9 C8 122.8(2) . . ? O4 C10 C11 119.9(2) . . ? O4 C10 C9 117.8(2) . . ? C11 C10 C9 122.2(2) . . ? C12 C11 C10 120.0(2) . . ? C12 C11 O5 121.4(2) . . ? C10 C11 O5 118.4(2) . . ? O6 C12 C11 121.6(2) . . ? O6 C12 C13 118.3(2) . . ? C11 C12 C13 120.1(3) . . ? C14 C13 C12 117.9(2) . . ? C14 C13 C15 122.7(2) . . ? C12 C13 C15 119.3(3) . . ? C13 C14 C9 123.6(2) . . ? C13 C15 C16 110.39(19) . . ? C13 C15 C15A 113.1(2) . . ? C16 C15 C15A 113.05(19) . . ? C15B C15A C15 113.4(2) . . ? C15C C15B C15A 112.5(3) . . ? C15B C15C C15D 113.0(3) . . ? C15E C15D C15C 112.3(3) . . ? C15F C15E C15D 113.4(3) . . ? C15G C15F C15E 111.8(3) . . ? C15H C15G C15F 114.8(3) . . ? C15G C15H C15I 112.6(3) . . ? C15H C15I C15J 113.9(3) . . ? C15K C15J C15I 112.2(3) . . ? C17 C16 C21 117.3(2) . . ? C17 C16 C15 121.3(2) . . ? C21 C16 C15 121.4(3) . . ? O7 C17 C16 124.6(2) . . ? O7 C17 C18 115.2(3) . . ? C16 C17 C18 120.1(2) . . ? O8 C18 C19 117.7(2) . . ? O8 C18 C17 121.8(2) . . ? C19 C18 C17 120.5(3) . . ? O9 C19 C20 125.2(2) . . ? O9 C19 C18 113.9(3) . . ? C20 C19 C18 120.9(3) . . ? C19 C20 C21 117.1(2) . . ? C19 C20 C22 122.1(2) . . ? C21 C20 C22 120.8(3) . . ? C20 C21 C16 123.8(3) . . ? C22A C22 C23 113.8(2) . . ? C22A C22 C20 111.82(19) . . ? C23 C22 C20 111.64(18) . . ? C22B C22A C22 111.6(2) . . ? C22C C22B C22A 113.6(2) . . ? C22D C22C C22B 114.5(3) . . ? C22C C22D C22E 113.1(3) . . ? C22F C22E C22D 114.6(3) . . ? C22E C22F C22G 113.8(3) . . ? C22H C22G C22F 114.0(3) . . ? C22G C22H C22I 114.7(3) . . ? C22J C22I C22H 114.4(3) . . ? C22I C22J C22K 114.8(4) . . ? C28 C23 C24 118.1(3) . . ? C28 C23 C22 124.3(2) . . ? C24 C23 C22 117.6(3) . . ? O10 C24 C25 121.9(3) . . ? O10 C24 C23 118.1(3) . . ? C25 C24 C23 119.9(3) . . ? C26 C25 O11 116.9(2) . . ? C26 C25 C24 120.5(3) . . ? O11 C25 C24 122.5(3) . . ? C25 C26 O12 120.4(2) . . ? C25 C26 C27 121.6(3) . . ? O12 C26 C27 118.0(3) . . ? C28 C27 C26 116.5(3) . . ? C28 C27 C1 123.8(2) . . ? C26 C27 C1 119.6(3) . . ? C23 C28 C27 123.2(3) . . ? CV2 CV1 OX2 129.2(11) . . ? OZ3 CX1 CX2 110.8(3) . . ? OZ1 CZQ CZ7 110.8(3) . . ? OZ2 CZ3 CZ4 108.6(3) . . ? _diffrn_measured_fraction_theta_max 0.630 _diffrn_reflns_theta_full 28.06 _diffrn_measured_fraction_theta_full 0.630 _refine_diff_density_max 0.580 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.082