# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Dalgarno, Scott' _publ_contact_author_email S.J.Dalgarno@hw.ac.uk _publ_section_title ; Calixarene nanotubes: Structural tolerance towards pyridine templates ; loop_ _publ_author_name S.Kennedy C.Beavers S.Teat S.Dalgarno # Attachment '- 42EtPy.cif' data_42EtPy _database_code_depnum_ccdc_archive 'CCDC 787577' #TrackingRef '- 42EtPy.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '4.2ETPY ' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C123 H135 N7 O20' _chemical_formula_weight 2031.38 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 11.5487(7) _cell_length_b 16.1638(9) _cell_length_c 16.4446(11) _cell_angle_alpha 113.729(2) _cell_angle_beta 92.529(2) _cell_angle_gamma 95.793(2) _cell_volume 2783.7(3) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.212 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1082 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9718 _exptl_absorpt_correction_T_max 0.9838 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Nonius X8 Apex II CCD Diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21118 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0343 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 20.82 _reflns_number_total 5696 _reflns_number_gt 4493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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^)+(0.0726P)^2^+1.8348P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5696 _refine_ls_number_parameters 718 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0647 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1235 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.031 _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 O1 O 0.60295(16) 0.27868(14) 0.04569(13) 0.0339(5) Uani 1 1 d . . . C1 C 0.5091(3) 0.1555(2) 0.0758(2) 0.0293(8) Uani 1 1 d . . . O2 O 0.45836(17) 0.41407(13) 0.06645(13) 0.0347(5) Uani 1 1 d . . . H2O H 0.5027 0.3745 0.0430 0.042 Uiso 1 1 calc R . . C2 C 0.4179(3) 0.0847(2) 0.0523(2) 0.0329(8) Uani 1 1 d . . . H2 H 0.4119 0.0493 0.0864 0.039 Uiso 1 1 calc R . . O3 O 0.46869(17) 0.52846(13) 0.25759(13) 0.0350(5) Uani 1 1 d . . . C3 C 0.3357(2) 0.0642(2) -0.0192(2) 0.0284(8) Uani 1 1 d . . . O4 O 0.55549(17) 0.36383(14) 0.22892(13) 0.0363(6) Uani 1 1 d . . . H4O H 0.5394 0.4174 0.2536 0.044 Uiso 1 1 calc R . . C4 C 0.3427(3) 0.1173(2) -0.06788(19) 0.0282(8) Uani 1 1 d . . . H4 H 0.2855 0.1041 -0.1162 0.034 Uiso 1 1 calc R . . O5 O 0.22482(18) -0.05327(15) 0.00728(16) 0.0443(6) Uani 1 1 d . . . C5 C 0.4315(2) 0.18913(19) -0.04735(19) 0.0256(7) Uani 1 1 d . . . O6 O 0.16730(19) -0.02575(14) -0.11019(15) 0.0435(6) Uani 1 1 d . . . H6O H 0.1141 -0.0684 -0.1179 0.052 Uiso 1 1 calc R . . C6 C 0.5145(3) 0.2056(2) 0.0229(2) 0.0282(8) Uani 1 1 d . . . O7 O 0.01259(19) 0.25870(16) -0.21282(16) 0.0507(6) Uani 1 1 d . . . H7O H -0.0514 0.2552 -0.2410 0.061 Uiso 1 1 calc R . . C7 C 0.4298(3) 0.2505(2) -0.0970(2) 0.0319(8) Uani 1 1 d . . . H7A H 0.5077 0.2867 -0.0868 0.038 Uiso 1 1 calc R . . H7B H 0.4139 0.2125 -0.1618 0.038 Uiso 1 1 calc R . . O8 O -0.0295(2) 0.39766(17) -0.13250(15) 0.0528(7) Uani 1 1 d . . . C8 C 0.3381(3) 0.31449(19) -0.06694(19) 0.0274(8) Uani 1 1 d . . . O9 O 0.3527(2) 0.19721(15) 0.48652(15) 0.0500(6) Uani 1 1 d . . . H9O H 0.3360 0.1630 0.5127 0.060 Uiso 1 1 calc R . . C9 C 0.2317(3) 0.2971(2) -0.1175(2) 0.0279(8) Uani 1 1 d . . . H9 H 0.2168 0.2440 -0.1717 0.033 Uiso 1 1 calc R . . O10 O 0.44312(19) 0.08114(17) 0.40171(15) 0.0436(6) Uani 1 1 d . . . C10 C 0.1465(3) 0.3551(2) -0.09118(19) 0.0279(8) Uani 1 1 d . . . C11 C 0.1685(3) 0.4321(2) -0.0108(2) 0.0316(8) Uani 1 1 d . . . H11 H 0.1108 0.4722 0.0076 0.038 Uiso 1 1 calc R . . C12 C 0.2716(3) 0.4516(2) 0.0428(2) 0.0297(8) Uani 1 1 d . . . C13 C 0.3567(3) 0.3926(2) 0.0134(2) 0.0301(8) Uani 1 1 d . . . C14 C 0.2902(3) 0.5314(2) 0.1327(2) 0.0386(8) Uani 1 1 d . . . H14A H 0.3719 0.5612 0.1427 0.046 Uiso 1 1 calc R . . H14B H 0.2379 0.5767 0.1338 0.046 Uiso 1 1 calc R . . C15 C 0.2656(3) 0.5008(2) 0.20626(19) 0.0313(8) Uani 1 1 d . . . C16 C 0.1528(3) 0.4687(2) 0.2146(2) 0.0417(9) Uani 1 1 d . . . H16 H 0.0902 0.4698 0.1758 0.050 Uiso 1 1 calc R . . C17 C 0.1294(3) 0.4354(2) 0.2774(2) 0.0473(9) Uani 1 1 d . . . H17 H 0.0510 0.4152 0.2827 0.057 Uiso 1 1 calc R . . C18 C 0.2192(3) 0.4312(2) 0.3332(2) 0.0454(9) Uani 1 1 d . . . H18 H 0.2024 0.4068 0.3758 0.055 Uiso 1 1 calc R . . C19 C 0.3340(3) 0.4622(2) 0.3277(2) 0.0357(8) Uani 1 1 d . . . C20 C 0.3539(3) 0.4984(2) 0.2651(2) 0.0301(8) Uani 1 1 d . . . C21 C 0.4334(3) 0.4531(2) 0.3857(2) 0.0451(9) Uani 1 1 d . . . H21A H 0.5040 0.4932 0.3854 0.054 Uiso 1 1 calc R . . H21B H 0.4122 0.4739 0.4478 0.054 Uiso 1 1 calc R . . C22 C 0.4613(3) 0.3562(2) 0.3541(2) 0.0324(8) Uani 1 1 d . . . C23 C 0.4278(3) 0.3025(2) 0.3989(2) 0.0349(8) Uani 1 1 d . . . H23 H 0.3897 0.3285 0.4518 0.042 Uiso 1 1 calc R . . C24 C 0.4476(3) 0.2121(2) 0.3695(2) 0.0298(8) Uani 1 1 d . . . C25 C 0.5022(2) 0.1739(2) 0.2919(2) 0.0309(8) Uani 1 1 d . . . H25 H 0.5156 0.1120 0.2710 0.037 Uiso 1 1 calc R . . C26 C 0.5377(2) 0.2243(2) 0.2437(2) 0.0306(8) Uani 1 1 d . . . C27 C 0.5175(3) 0.3157(2) 0.2766(2) 0.0334(8) Uani 1 1 d . . . C28 C 0.5932(3) 0.1798(2) 0.1573(2) 0.0388(9) Uani 1 1 d . . . H28A H 0.6608 0.2218 0.1559 0.047 Uiso 1 1 calc R . . H28B H 0.6227 0.1238 0.1556 0.047 Uiso 1 1 calc R . . C29 C 0.7073(3) 0.2549(2) -0.0001(2) 0.0404(9) Uani 1 1 d . . . H29A H 0.6872 0.2259 -0.0654 0.048 Uiso 1 1 calc R . . H29B H 0.7446 0.2117 0.0181 0.048 Uiso 1 1 calc R . . C30 C 0.7890(3) 0.3418(3) 0.0254(3) 0.0568(11) Uani 1 1 d . . . H30A H 0.8568 0.3284 -0.0104 0.068 Uiso 1 1 calc R . . H30B H 0.7481 0.3851 0.0098 0.068 Uiso 1 1 calc R . . C31 C 0.8321(3) 0.3860(3) 0.1206(3) 0.0762(14) Uani 1 1 d . . . H31A H 0.7657 0.4007 0.1568 0.114 Uiso 1 1 calc R . . H31B H 0.8839 0.4422 0.1320 0.114 Uiso 1 1 calc R . . H31C H 0.8754 0.3447 0.1364 0.114 Uiso 1 1 calc R . . C32 C 0.2374(3) -0.0108(2) -0.0389(2) 0.0345(8) Uani 1 1 d . . . C33 C 0.0359(3) 0.3403(2) -0.1459(2) 0.0324(8) Uani 1 1 d . . . C34 C 0.5020(3) 0.6261(2) 0.3062(2) 0.0394(9) Uani 1 1 d . . . H34A H 0.5121 0.6423 0.3711 0.047 Uiso 1 1 calc R . . H34B H 0.4406 0.6596 0.2946 0.047 Uiso 1 1 calc R . . C35 C 0.6132(3) 0.6504(3) 0.2750(2) 0.0566(11) Uani 1 1 d . . . H35A H 0.6339 0.7174 0.3032 0.068 Uiso 1 1 calc R . . H35B H 0.6020 0.6315 0.2096 0.068 Uiso 1 1 calc R . . C36 C 0.7123(4) 0.6071(3) 0.2958(3) 0.0847(15) Uani 1 1 d . . . H36A H 0.7231 0.6246 0.3603 0.127 Uiso 1 1 calc R . . H36B H 0.7840 0.6276 0.2758 0.127 Uiso 1 1 calc R . . H36C H 0.6947 0.5406 0.2649 0.127 Uiso 1 1 calc R . . C37 C 0.4142(3) 0.1561(3) 0.4196(2) 0.0329(8) Uani 1 1 d . . . N38 N 0.0202(2) 0.13693(18) 0.12500(18) 0.0376(7) Uani 1 1 d . . . C39 C 0.0310(3) 0.1743(2) 0.0658(2) 0.0349(8) Uani 1 1 d . . . H39 H -0.0322 0.1623 0.0220 0.042 Uiso 1 1 calc R . . C40 C 0.1302(3) 0.2293(2) 0.0661(2) 0.0354(8) Uani 1 1 d . . . H40 H 0.1346 0.2561 0.0243 0.043 Uiso 1 1 calc R . . C41 C 0.2223(3) 0.2447(2) 0.1280(2) 0.0351(8) Uani 1 1 d . . . H41 H 0.2920 0.2820 0.1294 0.042 Uiso 1 1 calc R . . C42 C 0.2126(3) 0.2056(2) 0.1877(2) 0.0390(9) Uani 1 1 d . . . H42 H 0.2761 0.2152 0.2306 0.047 Uiso 1 1 calc R . . C43 C 0.1104(3) 0.1521(2) 0.1855(2) 0.0405(9) Uani 1 1 d . . . C44 C 0.0958(4) 0.1069(3) 0.2496(3) 0.0634(12) Uani 1 1 d . . . H44A H 0.0169 0.1129 0.2710 0.076 Uiso 1 1 calc R . . H44B H 0.1541 0.1383 0.3020 0.076 Uiso 1 1 calc R . . C45 C 0.1111(5) 0.0066(4) 0.2060(4) 0.1024(18) Uani 1 1 d . . . H45A H 0.1892 0.0004 0.1851 0.154 Uiso 1 1 calc R . . H45B H 0.0519 -0.0251 0.1553 0.154 Uiso 1 1 calc R . . H45C H 0.1020 -0.0203 0.2496 0.154 Uiso 1 1 calc R . . N46 N 0.2820(3) 0.10165(18) 0.57658(17) 0.0390(7) Uani 1 1 d . . . C47 C 0.3493(3) 0.0519(3) 0.6006(2) 0.0512(10) Uani 1 1 d . . . H47 H 0.4234 0.0436 0.5777 0.061 Uiso 1 1 calc R . . C48 C 0.3161(4) 0.0112(2) 0.6577(2) 0.0525(10) Uani 1 1 d . . . H48 H 0.3651 -0.0254 0.6727 0.063 Uiso 1 1 calc R . . C49 C 0.2102(4) 0.0261(2) 0.6915(2) 0.0477(10) Uani 1 1 d . . . H49 H 0.1849 0.0003 0.7313 0.057 Uiso 1 1 calc R . . C50 C 0.1413(3) 0.0779(2) 0.6679(2) 0.0433(9) Uani 1 1 d . . . H50 H 0.0679 0.0885 0.6915 0.052 Uiso 1 1 calc R . . C51 C 0.1785(3) 0.1149(2) 0.6097(2) 0.0379(9) Uani 1 1 d . . . C52 C 0.1048(3) 0.1713(3) 0.5797(2) 0.0550(10) Uani 1 1 d . . . H52A H 0.0554 0.2023 0.6277 0.066 Uiso 1 1 calc R . . H52B H 0.1574 0.2190 0.5713 0.066 Uiso 1 1 calc R . . C53 C 0.0280(5) 0.1188(3) 0.4958(3) 0.0946(17) Uani 1 1 d . . . H53A H 0.0751 0.0841 0.4486 0.142 Uiso 1 1 calc R . . H53B H -0.0105 0.1610 0.4779 0.142 Uiso 1 1 calc R . . H53C H -0.0313 0.0768 0.5055 0.142 Uiso 1 1 calc R . . N54 N -0.1549(3) 0.2543(2) -0.33403(19) 0.0501(8) Uani 1 1 d . . . C55 C -0.1277(4) 0.3218(3) -0.3607(3) 0.0698(12) Uani 1 1 d . . . H55 H -0.0637 0.3670 -0.3290 0.084 Uiso 1 1 calc R . . C56 C -0.1871(4) 0.3292(3) -0.4307(3) 0.0781(14) Uani 1 1 d . . . H56 H -0.1651 0.3783 -0.4470 0.094 Uiso 1 1 calc R . . C57 C -0.2790(4) 0.2640(3) -0.4769(3) 0.0730(13) Uani 1 1 d . . . H57 H -0.3219 0.2668 -0.5261 0.088 Uiso 1 1 calc R . . C58 C -0.3082(3) 0.1941(3) -0.4508(3) 0.0606(11) Uani 1 1 d . . . H58 H -0.3720 0.1484 -0.4818 0.073 Uiso 1 1 calc R . . C59 C -0.2443(3) 0.1909(3) -0.3793(2) 0.0502(10) Uani 1 1 d . . . C60 C -0.2717(3) 0.1183(3) -0.3464(3) 0.0613(11) Uani 1 1 d . . . H60A H -0.1981 0.0968 -0.3346 0.074 Uiso 1 1 calc R . . H60B H -0.3214 0.0659 -0.3934 0.074 Uiso 1 1 calc R . . C61 C -0.3334(5) 0.1505(4) -0.2630(3) 0.1067(18) Uani 1 1 d . . . H61A H -0.4108 0.1645 -0.2762 0.160 Uiso 1 1 calc R . . H61B H -0.2877 0.2055 -0.2177 0.160 Uiso 1 1 calc R . . H61C H -0.3420 0.1027 -0.2406 0.160 Uiso 1 1 calc R . . C77 C -0.1907(10) 0.4698(10) 0.4165(10) 0.079(4) Uani 0.50 1 d PU A -1 H77A H -0.1393 0.4221 0.4009 0.118 Uiso 0.50 1 calc PR A -1 H77B H -0.2416 0.4609 0.3636 0.118 Uiso 0.50 1 calc PR A -1 H77C H -0.2387 0.4667 0.4631 0.118 Uiso 0.50 1 calc PR A -1 C76 C -0.1148(7) 0.5655(6) 0.4516(5) 0.062(2) Uani 0.50 1 d PU A -1 H76A H -0.0815 0.5726 0.3999 0.075 Uiso 0.50 1 calc PR A -1 H76B H -0.1675 0.6127 0.4755 0.075 Uiso 0.50 1 calc PR A -1 C75 C -0.0176(7) 0.5847(6) 0.5211(5) 0.0597(19) Uani 0.50 1 d PU A -1 C71 C 0.1309(11) 0.5289(12) 0.5765(10) 0.077(3) Uani 0.50 1 d PU A -1 H71 H 0.1707 0.4793 0.5738 0.092 Uiso 0.50 1 calc PR A -1 C74 C 0.0154(7) 0.6715(6) 0.5860(5) 0.070(2) Uani 0.50 1 d PU A -1 H74 H -0.0270 0.7199 0.5887 0.084 Uiso 0.50 1 calc PR A -1 C73 C 0.1127(8) 0.6882(8) 0.6486(6) 0.082(2) Uani 0.50 1 d PU A -1 H73 H 0.1366 0.7474 0.6941 0.098 Uiso 0.50 1 calc PR A -1 C72 C 0.1712(8) 0.6163(8) 0.6413(6) 0.079(2) Uani 0.50 1 d PU A -1 H72 H 0.2391 0.6257 0.6803 0.095 Uiso 0.50 1 calc PR A -1 N70 N 0.0369(5) 0.5129(6) 0.5174(5) 0.067(2) Uani 0.50 1 d PU A -1 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 0.0261(12) 0.0382(13) 0.0394(13) 0.0194(10) 0.0033(10) -0.0022(10) C1 0.0296(18) 0.0344(19) 0.0316(19) 0.0208(16) 0.0069(15) 0.0049(16) O2 0.0351(13) 0.0321(13) 0.0367(13) 0.0150(10) -0.0058(11) 0.0032(10) C2 0.037(2) 0.038(2) 0.037(2) 0.0279(16) 0.0101(17) 0.0079(17) O3 0.0355(14) 0.0259(13) 0.0398(13) 0.0118(10) -0.0036(10) -0.0027(10) C3 0.0282(18) 0.0278(18) 0.0318(19) 0.0151(16) 0.0047(16) 0.0022(14) O4 0.0441(13) 0.0300(12) 0.0407(13) 0.0229(11) -0.0006(10) -0.0043(10) C4 0.0312(18) 0.0296(19) 0.0238(18) 0.0112(15) 0.0028(14) 0.0031(15) O5 0.0452(14) 0.0406(14) 0.0587(16) 0.0342(13) 0.0056(12) -0.0035(11) C5 0.0268(18) 0.0280(18) 0.0262(18) 0.0153(15) 0.0045(15) 0.0032(15) O6 0.0404(14) 0.0432(14) 0.0473(15) 0.0247(12) -0.0029(12) -0.0164(11) C6 0.0279(18) 0.0281(18) 0.0290(19) 0.0128(15) 0.0062(16) -0.0005(15) O7 0.0458(15) 0.0416(16) 0.0525(16) 0.0098(14) -0.0220(12) 0.0041(11) C7 0.0317(18) 0.038(2) 0.0333(19) 0.0239(16) 0.0018(15) -0.0021(15) O8 0.0502(16) 0.0539(17) 0.0425(15) 0.0072(12) -0.0159(12) 0.0173(14) C8 0.034(2) 0.0258(19) 0.0280(19) 0.0185(16) 0.0006(16) -0.0035(15) O9 0.0752(17) 0.0451(15) 0.0441(15) 0.0313(12) 0.0223(14) 0.0077(13) C9 0.037(2) 0.0238(18) 0.0256(18) 0.0154(14) -0.0021(16) -0.0056(16) O10 0.0516(15) 0.0414(16) 0.0502(15) 0.0314(12) 0.0119(12) 0.0041(12) C10 0.035(2) 0.0247(19) 0.0270(19) 0.0153(16) -0.0050(16) -0.0008(15) C11 0.040(2) 0.030(2) 0.030(2) 0.0182(17) -0.0025(16) 0.0054(15) C12 0.037(2) 0.0258(19) 0.0296(19) 0.0168(16) -0.0056(16) -0.0011(16) C13 0.030(2) 0.034(2) 0.033(2) 0.0249(18) -0.0100(16) -0.0064(16) C14 0.050(2) 0.031(2) 0.035(2) 0.0161(17) -0.0092(16) 0.0001(16) C15 0.036(2) 0.0266(18) 0.0268(18) 0.0078(15) -0.0071(16) 0.0009(15) C16 0.033(2) 0.043(2) 0.045(2) 0.0147(18) -0.0051(17) 0.0039(16) C17 0.037(2) 0.050(2) 0.048(2) 0.015(2) 0.007(2) -0.0001(17) C18 0.058(3) 0.043(2) 0.033(2) 0.0150(17) 0.0068(19) -0.0029(18) C19 0.048(2) 0.0302(19) 0.0251(19) 0.0097(16) -0.0050(16) -0.0012(16) C20 0.030(2) 0.0252(18) 0.0297(19) 0.0075(15) -0.0021(16) -0.0018(14) C21 0.064(2) 0.037(2) 0.034(2) 0.0181(17) -0.0130(18) -0.0048(17) C22 0.0392(19) 0.033(2) 0.0256(19) 0.0163(16) -0.0088(16) -0.0052(15) C23 0.039(2) 0.044(2) 0.0230(18) 0.0170(17) -0.0048(15) -0.0001(16) C24 0.0317(18) 0.033(2) 0.0284(19) 0.0187(16) -0.0036(15) -0.0047(15) C25 0.0283(18) 0.0335(19) 0.035(2) 0.0203(16) -0.0069(16) -0.0030(14) C26 0.0215(17) 0.045(2) 0.0316(19) 0.0256(17) -0.0061(14) -0.0055(15) C27 0.0313(19) 0.038(2) 0.039(2) 0.0295(18) -0.0125(16) -0.0136(16) C28 0.0284(18) 0.061(2) 0.041(2) 0.0351(18) 0.0022(16) 0.0035(16) C29 0.034(2) 0.051(2) 0.045(2) 0.0287(18) 0.0100(17) 0.0054(17) C30 0.043(2) 0.056(3) 0.088(3) 0.048(2) 0.010(2) -0.0025(19) C31 0.042(2) 0.058(3) 0.116(4) 0.027(3) -0.003(3) -0.012(2) C32 0.034(2) 0.030(2) 0.041(2) 0.0159(18) 0.0068(18) 0.0039(16) C33 0.040(2) 0.031(2) 0.026(2) 0.0127(18) -0.0036(17) -0.0004(18) C34 0.049(2) 0.027(2) 0.036(2) 0.0100(16) -0.0063(17) -0.0056(16) C35 0.067(3) 0.046(2) 0.047(2) 0.0137(19) 0.012(2) -0.014(2) C36 0.052(3) 0.055(3) 0.123(4) 0.015(3) 0.029(3) -0.017(2) C37 0.035(2) 0.039(2) 0.029(2) 0.0189(18) 0.0001(16) -0.0006(17) N38 0.0368(17) 0.0410(17) 0.0376(17) 0.0215(14) -0.0002(15) -0.0055(13) C39 0.036(2) 0.037(2) 0.036(2) 0.0199(17) 0.0008(16) 0.0031(16) C40 0.040(2) 0.035(2) 0.038(2) 0.0209(16) 0.0091(18) 0.0035(16) C41 0.031(2) 0.034(2) 0.038(2) 0.0149(17) 0.0041(17) -0.0054(15) C42 0.034(2) 0.046(2) 0.036(2) 0.0198(18) -0.0039(16) -0.0071(17) C43 0.042(2) 0.046(2) 0.036(2) 0.0230(17) -0.0001(18) -0.0086(17) C44 0.067(3) 0.077(3) 0.058(3) 0.046(2) -0.005(2) -0.016(2) C45 0.129(5) 0.118(5) 0.116(4) 0.094(4) 0.054(4) 0.048(4) N46 0.050(2) 0.0360(17) 0.0329(16) 0.0157(14) 0.0091(15) 0.0038(14) C47 0.056(2) 0.056(2) 0.048(2) 0.024(2) 0.0163(19) 0.018(2) C48 0.081(3) 0.043(2) 0.043(2) 0.0240(19) 0.009(2) 0.019(2) C49 0.074(3) 0.037(2) 0.024(2) 0.0089(17) 0.007(2) -0.015(2) C50 0.048(2) 0.046(2) 0.032(2) 0.0153(18) 0.0015(17) -0.0105(19) C51 0.045(2) 0.034(2) 0.0281(19) 0.0086(16) -0.0017(17) -0.0065(16) C52 0.050(2) 0.070(3) 0.043(2) 0.023(2) -0.0007(19) 0.004(2) C53 0.132(4) 0.063(3) 0.087(4) 0.042(3) -0.054(3) -0.015(3) N54 0.053(2) 0.0394(19) 0.0457(19) 0.0065(16) -0.0155(16) 0.0080(16) C55 0.086(3) 0.043(3) 0.070(3) 0.016(2) -0.030(3) 0.005(2) C56 0.114(4) 0.049(3) 0.066(3) 0.021(2) -0.033(3) 0.017(3) C57 0.091(3) 0.063(3) 0.053(3) 0.011(3) -0.026(3) 0.029(3) C58 0.052(2) 0.066(3) 0.045(3) 0.002(2) -0.016(2) 0.020(2) C59 0.044(2) 0.053(3) 0.040(2) 0.006(2) -0.004(2) 0.012(2) C60 0.057(3) 0.064(3) 0.057(3) 0.021(2) 0.007(2) -0.001(2) C61 0.132(5) 0.105(4) 0.063(3) 0.019(3) 0.021(3) -0.008(3) C77 0.072(8) 0.097(8) 0.074(7) 0.054(6) -0.018(7) -0.024(8) C76 0.059(5) 0.082(5) 0.056(5) 0.044(4) -0.002(4) -0.008(4) C75 0.051(4) 0.080(4) 0.055(4) 0.039(4) 0.005(3) -0.010(4) C71 0.057(6) 0.119(7) 0.056(6) 0.040(5) 0.009(5) -0.003(7) C74 0.065(5) 0.091(5) 0.061(5) 0.044(4) 0.002(4) -0.018(4) C73 0.068(5) 0.108(6) 0.075(5) 0.048(5) 0.012(4) -0.014(5) C72 0.055(5) 0.119(7) 0.066(5) 0.043(5) 0.010(4) 0.000(5) N70 0.053(5) 0.098(5) 0.052(5) 0.034(4) 0.008(4) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C6 1.395(3) . ? O1 C29 1.452(4) . ? C1 C2 1.390(4) . ? C1 C6 1.405(4) . ? C1 C28 1.509(4) . ? O2 C13 1.358(3) . ? C2 C3 1.385(4) . ? O3 C20 1.393(3) . ? O3 C34 1.454(4) . ? C3 C4 1.389(4) . ? C3 C32 1.495(4) . ? O4 C27 1.365(3) . ? C4 C5 1.389(4) . ? O5 C32 1.217(4) . ? C5 C6 1.389(4) . ? C5 C7 1.518(4) . ? O6 C32 1.318(4) . ? O7 C33 1.326(4) . ? C7 C8 1.514(4) . ? O8 C33 1.212(4) . ? C8 C9 1.389(4) . ? C8 C13 1.401(4) . ? O9 C37 1.317(4) . ? C9 C10 1.389(4) . ? O10 C37 1.211(4) . ? C10 C11 1.394(4) . ? C10 C33 1.470(4) . ? C11 C12 1.379(4) . ? C12 C13 1.402(4) . ? C12 C14 1.510(4) . ? C14 C15 1.507(4) . ? C15 C16 1.386(4) . ? C15 C20 1.389(4) . ? C16 C17 1.367(5) . ? C17 C18 1.379(5) . ? C18 C19 1.389(5) . ? C19 C20 1.390(4) . ? C19 C21 1.516(5) . ? C21 C22 1.514(5) . ? C22 C23 1.385(4) . ? C22 C27 1.400(4) . ? C23 C24 1.389(4) . ? C24 C25 1.387(4) . ? C24 C37 1.485(4) . ? C25 C26 1.392(4) . ? C26 C27 1.403(4) . ? C26 C28 1.516(4) . ? C29 C30 1.504(5) . ? C30 C31 1.473(6) . ? C34 C35 1.478(5) . ? C35 C36 1.495(6) . ? N38 C43 1.339(4) . ? N38 C39 1.339(4) . ? C39 C40 1.376(4) . ? C40 C41 1.370(4) . ? C41 C42 1.368(4) . ? C42 C43 1.381(4) . ? C43 C44 1.512(5) . ? C44 C45 1.519(6) . ? N46 C47 1.327(4) . ? N46 C51 1.337(4) . ? C47 C48 1.392(5) . ? C48 C49 1.369(5) . ? C49 C50 1.360(5) . ? C50 C51 1.381(5) . ? C51 C52 1.509(5) . ? C52 C53 1.486(5) . ? N54 C59 1.332(5) . ? N54 C55 1.345(5) . ? C55 C56 1.367(6) . ? C56 C57 1.368(6) . ? C57 C58 1.378(6) . ? C58 C59 1.382(5) . ? C59 C60 1.492(5) . ? C60 C61 1.497(6) . ? C77 C76 1.567(15) . ? C76 C75 1.481(11) . ? C75 N70 1.358(11) . ? C75 C74 1.380(12) . ? C71 N70 1.355(15) . ? C71 C72 1.400(19) . ? C74 C73 1.417(12) . ? C73 C72 1.370(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 O1 C29 113.9(2) . . ? C2 C1 C6 116.6(3) . . ? C2 C1 C28 120.9(3) . . ? C6 C1 C28 122.4(3) . . ? C3 C2 C1 122.2(3) . . ? C20 O3 C34 114.0(2) . . ? C2 C3 C4 119.1(3) . . ? C2 C3 C32 119.5(3) . . ? C4 C3 C32 121.3(3) . . ? C3 C4 C5 121.3(3) . . ? C4 C5 C6 117.8(3) . . ? C4 C5 C7 119.6(3) . . ? C6 C5 C7 122.5(3) . . ? C5 C6 O1 118.6(2) . . ? C5 C6 C1 122.9(3) . . ? O1 C6 C1 118.4(3) . . ? C8 C7 C5 111.9(2) . . ? C9 C8 C13 117.6(3) . . ? C9 C8 C7 121.2(3) . . ? C13 C8 C7 121.2(3) . . ? C10 C9 C8 122.1(3) . . ? C9 C10 C11 118.5(3) . . ? C9 C10 C33 122.8(3) . . ? C11 C10 C33 118.6(3) . . ? C12 C11 C10 121.8(3) . . ? C11 C12 C13 118.2(3) . . ? C11 C12 C14 121.0(3) . . ? C13 C12 C14 120.7(3) . . ? O2 C13 C8 121.0(3) . . ? O2 C13 C12 117.2(3) . . ? C8 C13 C12 121.8(3) . . ? C15 C14 C12 110.9(2) . . ? C16 C15 C20 117.0(3) . . ? C16 C15 C14 120.7(3) . . ? C20 C15 C14 122.2(3) . . ? C17 C16 C15 121.7(3) . . ? C16 C17 C18 120.2(3) . . ? C17 C18 C19 120.7(3) . . ? C18 C19 C20 117.5(3) . . ? C18 C19 C21 120.7(3) . . ? C20 C19 C21 121.8(3) . . ? C15 C20 C19 122.9(3) . . ? C15 C20 O3 118.7(3) . . ? C19 C20 O3 118.3(3) . . ? C22 C21 C19 112.4(3) . . ? C23 C22 C27 117.2(3) . . ? C23 C22 C21 121.1(3) . . ? C27 C22 C21 121.6(3) . . ? C22 C23 C24 122.6(3) . . ? C25 C24 C23 118.7(3) . . ? C25 C24 C37 119.3(3) . . ? C23 C24 C37 122.0(3) . . ? C24 C25 C26 121.5(3) . . ? C25 C26 C27 117.9(3) . . ? C25 C26 C28 120.3(3) . . ? C27 C26 C28 121.8(3) . . ? O4 C27 C22 121.3(3) . . ? O4 C27 C26 116.5(3) . . ? C22 C27 C26 122.2(3) . . ? C1 C28 C26 112.8(2) . . ? O1 C29 C30 107.2(3) . . ? C31 C30 C29 114.3(3) . . ? O5 C32 O6 124.0(3) . . ? O5 C32 C3 122.3(3) . . ? O6 C32 C3 113.7(3) . . ? O8 C33 O7 121.7(3) . . ? O8 C33 C10 123.6(3) . . ? O7 C33 C10 114.8(3) . . ? O3 C34 C35 107.5(3) . . ? C34 C35 C36 113.3(3) . . ? O10 C37 O9 123.8(3) . . ? O10 C37 C24 123.2(3) . . ? O9 C37 C24 113.0(3) . . ? C43 N38 C39 118.7(3) . . ? N38 C39 C40 122.5(3) . . ? C41 C40 C39 118.6(3) . . ? C42 C41 C40 119.2(3) . . ? C41 C42 C43 119.9(3) . . ? N38 C43 C42 121.1(3) . . ? N38 C43 C44 117.1(3) . . ? C42 C43 C44 121.8(3) . . ? C43 C44 C45 111.7(3) . . ? C47 N46 C51 118.9(3) . . ? N46 C47 C48 122.9(3) . . ? C49 C48 C47 117.4(4) . . ? C50 C49 C48 120.0(3) . . ? C49 C50 C51 119.7(3) . . ? N46 C51 C50 121.1(3) . . ? N46 C51 C52 116.8(3) . . ? C50 C51 C52 122.1(3) . . ? C53 C52 C51 114.7(3) . . ? C59 N54 C55 117.7(3) . . ? N54 C55 C56 123.7(4) . . ? C55 C56 C57 118.3(4) . . ? C56 C57 C58 118.9(4) . . ? C57 C58 C59 119.6(4) . . ? N54 C59 C58 121.7(4) . . ? N54 C59 C60 115.5(3) . . ? C58 C59 C60 122.7(4) . . ? C59 C60 C61 112.6(4) . . ? C75 C76 C77 117.3(8) . . ? N70 C75 C74 122.1(8) . . ? N70 C75 C76 116.6(8) . . ? C74 C75 C76 121.3(9) . . ? N70 C71 C72 121.9(15) . . ? C75 C74 C73 119.7(9) . . ? C72 C73 C74 117.8(10) . . ? C73 C72 C71 120.1(11) . . ? C71 N70 C75 118.3(10) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.374 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.046 # Attachment '42Pic.CIF' data_42Pic _database_code_depnum_ccdc_archive 'CCDC 787578' #TrackingRef '42Pic.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 4.2Pic _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H42 N O10' _chemical_formula_weight 732.78 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' N N 0.0061 0.0033 '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 trigonal _symmetry_space_group_name_H-M R-3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 46.4651(11) _cell_length_b 46.4651(11) _cell_length_c 12.0334(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 22499.5(9) _cell_formula_units_Z 18 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used . _cell_measurement_theta_min . _cell_measurement_theta_max . _exptl_crystal_description Rod _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.973 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6966 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9931 _exptl_absorpt_correction_T_max 0.9986 _exptl_absorpt_process_details Bruker-SADABS _exptl_special_details ; Data were corrected for decay and absorption using the program SADABS based on the method of R.H. Blessing (Acta Cryst. A51, 33-38, 1995). ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.77490 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Advanced Light Source station 11.3.1' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker Apex II CCD Diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45185 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0308 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -47 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 23.33 _reflns_number_total 5584 _reflns_number_gt 4599 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II' _computing_cell_refinement 'SAINT (Bruker, 1998)' _computing_data_reduction 'SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 2001)' _computing_publication_material 'local program' _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. Due to the nature of the tubular structure, there was diffuse electron density in the resulting channel and interstitial voids present between neighbouring tubules. Given this, the routine SQUEEZE was applied in order to remove this density, improving the agreement indices significantly. For the cavity occcupying 2-picoline, this molecule was disordered over two positions and was subsequently modeled at partial occupancies. In addition to this, one of the calixarene upper rim carboxylic acid groups is disordered across the skeleton of the molecule and has been modeled at partial occupancies consistent with refined occupancies. Numerous restraints were applied to the structure due to disorder of carboxylate groups over two positions across the macrocycle at the upper rim, and distortion of aromatic rings and carboxylate groups. ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5584 _refine_ls_number_parameters 554 _refine_ls_number_restraints 275 _refine_ls_R_factor_all 0.1219 _refine_ls_R_factor_gt 0.1118 _refine_ls_wR_factor_ref 0.3288 _refine_ls_wR_factor_gt 0.3220 _refine_ls_goodness_of_fit_ref 2.584 _refine_ls_restrained_S_all 2.624 _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 O1 O 0.05837(8) 0.14663(8) 0.8501(3) 0.0889(10) Uani 1 1 d . . . C1 C 0.09227(12) 0.19647(15) 0.9571(4) 0.0867(15) Uani 1 1 d . . . O2 O 0.08271(9) 0.14630(9) 0.6402(3) 0.0892(10) Uani 1 1 d . . . H2O H 0.0692 0.1449 0.6892 0.107 Uiso 1 1 calc R . . C2 C 0.10583(12) 0.23188(16) 0.9633(5) 0.100(2) Uani 1 1 d . . . H2A H 0.1193 0.2436 1.0252 0.120 Uiso 1 1 calc R . . O3 O 0.12882(8) 0.12544(8) 0.6722(3) 0.0906(10) Uani 1 1 d DU . . C3 C 0.10005(15) 0.24921(14) 0.8839(6) 0.0954(16) Uani 1 1 d D . . O4 O 0.11658(8) 0.14494(9) 0.8755(3) 0.0925(11) Uani 1 1 d . . . H4O H 0.1229 0.1340 0.8373 0.111 Uiso 1 1 calc R . . C4 C 0.08212(14) 0.23300(14) 0.7972(5) 0.0940(16) Uani 1 1 d . . . H4A H 0.0789 0.2454 0.7407 0.113 Uiso 1 1 calc R . . O5 O 0.13306(16) 0.30094(15) 0.9685(8) 0.154(3) Uani 0.75 1 d PU . . H5O H 0.1406 0.3216 0.9670 0.185 Uiso 0.38 1 calc PR . . C5 C 0.06751(12) 0.19886(12) 0.7827(4) 0.0765(13) Uani 1 1 d . . . O6 O 0.1088(2) 0.30132(14) 0.8134(7) 0.136(2) Uani 0.75 1 d PU . . H6O H 0.1182 0.3219 0.8237 0.163 Uiso 0.38 1 calc PR . . C6 C 0.07244(11) 0.18111(11) 0.8638(4) 0.0749(13) Uani 1 1 d . . . O7 O 0.09288(14) 0.26360(14) 0.3536(5) 0.1451(17) Uani 1 1 d . . . H7O H 0.0969 0.2771 0.3013 0.174 Uiso 1 1 calc R . . C7 C 0.04876(14) 0.18272(15) 0.6777(4) 0.0928(15) Uani 1 1 d . . . H7A H 0.0339 0.1915 0.6593 0.111 Uiso 1 1 calc R . . H7B H 0.0348 0.1585 0.6896 0.111 Uiso 1 1 calc R . . O8 O 0.11936(18) 0.24675(14) 0.2423(4) 0.153(2) Uani 1 1 d . . . C8 C 0.07228(13) 0.18914(14) 0.5814(4) 0.0885(15) Uani 1 1 d . . . O9 O 0.2487(7) 0.2631(6) 0.494(2) 0.254(13) Uani 0.25 1 d PDU . . H9O H 0.2672 0.2807 0.4950 0.305 Uiso 0.25 1 calc PR . . C9 C 0.07753(15) 0.21288(16) 0.5017(5) 0.0973(17) Uani 1 1 d . . . H9 H 0.0661 0.2250 0.5078 0.117 Uiso 1 1 calc R . . O10 O 0.2686(5) 0.2583(5) 0.6570(19) 0.203(10) Uani 0.25 1 d PDU . . C10 C 0.09866(15) 0.21918(14) 0.4152(4) 0.0941(16) Uani 1 1 d . . . O11 O 0.24664(15) 0.23147(15) 1.1462(5) 0.160(2) Uani 1 1 d U . . H11O H 0.2599 0.2425 1.1973 0.193 Uiso 1 1 calc R . . C11 C 0.11519(15) 0.20120(16) 0.4055(4) 0.0996(17) Uani 1 1 d . . . H11 H 0.1301 0.2056 0.3453 0.120 Uiso 1 1 calc R . . O12 O 0.20956(15) 0.2318(2) 1.2649(5) 0.191(3) Uani 1 1 d U . . C12 C 0.11022(15) 0.17696(15) 0.4824(5) 0.0928(16) Uani 1 1 d . . . C13 C 0.08854(13) 0.17103(13) 0.5699(4) 0.0811(14) Uani 1 1 d . . . C14 C 0.12901(16) 0.15792(16) 0.4704(4) 0.1006(17) Uani 1 1 d . . . H14A H 0.1137 0.1341 0.4862 0.121 Uiso 1 1 calc R . . H14B H 0.1369 0.1598 0.3929 0.121 Uiso 1 1 calc R . . C15 C 0.15861(12) 0.17109(12) 0.5490(4) 0.0815(13) Uani 1 1 d DU . . C16 C 0.18708(14) 0.20091(13) 0.5264(4) 0.0897(14) Uani 1 1 d DU . . H16 H 0.1884 0.2122 0.4592 0.108 Uiso 1 1 calc R . . C17 C 0.21353(14) 0.21465(13) 0.5988(5) 0.0982(15) Uani 1 1 d DU . . C18 C 0.21118(14) 0.19849(13) 0.6976(5) 0.0967(15) Uani 1 1 d DU . . H18 H 0.2291 0.2080 0.7487 0.116 Uiso 1 1 calc R . . C19 C 0.18307(13) 0.16871(12) 0.7230(4) 0.0859(13) Uani 1 1 d DU . . C20 C 0.15750(12) 0.15541(12) 0.6475(4) 0.0810(12) Uani 1 1 d DU . . C21 C 0.18047(15) 0.15225(15) 0.8358(5) 0.1024(17) Uani 1 1 d . . . H21A H 0.2016 0.1528 0.8517 0.123 Uiso 1 1 calc R . . H21B H 0.1626 0.1287 0.8325 0.123 Uiso 1 1 calc R . . C22 C 0.17302(14) 0.16979(14) 0.9301(4) 0.0907(15) Uani 1 1 d . . . C23 C 0.19730(14) 0.18916(15) 1.0046(5) 0.0972(17) Uani 1 1 d . . . H23 H 0.2189 0.1921 0.9963 0.117 Uiso 1 1 calc R . . C24 C 0.19101(15) 0.20462(16) 1.0918(5) 0.1041(19) Uani 1 1 d . . . C25 C 0.15879(15) 0.20045(17) 1.1030(4) 0.1042(18) Uani 1 1 d . . . H25 H 0.1543 0.2109 1.1628 0.125 Uiso 1 1 calc R . . C26 C 0.13430(13) 0.18173(15) 1.0297(4) 0.0944(16) Uani 1 1 d . . . C27 C 0.14153(12) 0.16568(14) 0.9447(4) 0.0889(16) Uani 1 1 d . . . C28 C 0.09952(14) 0.17695(19) 1.0407(5) 0.113(2) Uani 1 1 d . . . H28A H 0.0830 0.1531 1.0319 0.136 Uiso 1 1 calc R . . H28B H 0.0969 0.1837 1.1164 0.136 Uiso 1 1 calc R . . C29 C 0.02455(12) 0.12716(13) 0.8904(5) 0.0966(16) Uani 1 1 d . . . H29A H 0.0107 0.1360 0.8606 0.116 Uiso 1 1 calc R . . H29B H 0.0241 0.1278 0.9725 0.116 Uiso 1 1 calc R . . C30 C 0.01165(15) 0.09206(15) 0.8507(6) 0.116(2) Uani 1 1 d . . . H30A H 0.0144 0.0923 0.7691 0.139 Uiso 1 1 calc R . . H30B H -0.0124 0.0788 0.8672 0.139 Uiso 1 1 calc R . . C31 C 0.02907(16) 0.07544(16) 0.9038(8) 0.132(2) Uani 1 1 d . . . H31A H 0.0529 0.0882 0.8870 0.198 Uiso 1 1 calc R . . H31B H 0.0198 0.0529 0.8743 0.198 Uiso 1 1 calc R . . H31C H 0.0258 0.0745 0.9844 0.198 Uiso 1 1 calc R . . C32 C 0.1159(2) 0.28846(19) 0.8895(9) 0.095(2) Uani 0.75 1 d PDU . . C33 C 0.10403(18) 0.24449(18) 0.3295(6) 0.1100(19) Uani 1 1 d . . . C34 C 0.12953(15) 0.09600(13) 0.6364(6) 0.1068(19) Uani 1 1 d . . . H34A H 0.1486 0.0954 0.6705 0.128 Uiso 1 1 calc R . . H34B H 0.1318 0.0961 0.5546 0.128 Uiso 1 1 calc R . . C35 C 0.0975(2) 0.06628(14) 0.6726(7) 0.131(3) Uani 1 1 d . . . H35A H 0.0950 0.0678 0.7537 0.157 Uiso 1 1 calc R . . H35B H 0.0989 0.0461 0.6588 0.157 Uiso 1 1 calc R . . C36 C 0.06666(19) 0.06218(18) 0.6162(9) 0.148(3) Uani 1 1 d . . . H36A H 0.0631 0.0805 0.6375 0.222 Uiso 1 1 calc R . . H36B H 0.0474 0.0410 0.6390 0.222 Uiso 1 1 calc R . . H36C H 0.0694 0.0623 0.5354 0.222 Uiso 1 1 calc R . . C37 C 0.2450(5) 0.2462(4) 0.588(2) 0.147(6) Uani 0.25 1 d PDU . . C38 C 0.2159(2) 0.2237(2) 1.1755(7) 0.143(3) Uani 1 1 d U . . N40 N 0.1445(2) 0.36569(14) 0.8710(7) 0.088(3) Uani 0.50 1 d PGDU A 2 C41 C 0.1593(2) 0.37753(19) 0.9740(6) 0.091(3) Uani 0.50 1 d PGDU A 2 H41 H 0.1609 0.3629 1.0256 0.109 Uiso 0.50 1 calc PR A 2 C42 C 0.1717(2) 0.4107(2) 1.0015(6) 0.088(3) Uani 0.50 1 d PGDU A 2 H42 H 0.1818 0.4188 1.0719 0.106 Uiso 0.50 1 calc PR A 2 C43 C 0.1693(3) 0.43209(13) 0.9261(8) 0.086(3) Uani 0.50 1 d PGDU A 2 H43 H 0.1778 0.4548 0.9449 0.104 Uiso 0.50 1 calc PR A 2 C44 C 0.1545(3) 0.42025(18) 0.8231(7) 0.095(3) Uani 0.50 1 d PGDU A 2 H44 H 0.1529 0.4349 0.7715 0.114 Uiso 0.50 1 calc PR A 2 C45 C 0.14210(17) 0.38706(19) 0.7956(5) 0.092(3) Uani 0.50 1 d PGDU A 2 N47 N 0.15239(15) 0.36308(10) 0.9217(5) 0.074(2) Uani 0.50 1 d PGDU B 1 C48 C 0.14099(16) 0.37514(14) 0.8369(5) 0.066(2) Uani 0.50 1 d PGDU B 1 H48 H 0.1265 0.3604 0.7817 0.079 Uiso 0.50 1 calc PR B 1 C49 C 0.1508(2) 0.40871(15) 0.8330(6) 0.075(2) Uani 0.50 1 d PGDU B 1 H49 H 0.1430 0.4170 0.7751 0.091 Uiso 0.50 1 calc PR B 1 C50 C 0.1720(3) 0.43022(11) 0.9139(7) 0.081(2) Uani 0.50 1 d PGDU B 1 H50 H 0.1787 0.4532 0.9112 0.097 Uiso 0.50 1 calc PR B 1 C51 C 0.1834(2) 0.41816(12) 0.9987(6) 0.086(3) Uani 0.50 1 d PGDU B 1 H51 H 0.1979 0.4329 1.0540 0.103 Uiso 0.50 1 calc PR B 1 C52 C 0.17360(15) 0.38459(12) 1.0026(4) 0.084(2) Uani 0.50 1 d PGDU B 1 C53 C 0.1848(2) 0.3702(2) 1.0891(6) 0.100(3) Uani 0.50 1 d PGDU B 1 H53A H 0.1991 0.3627 1.0560 0.149 Uiso 0.50 1 calc PR B 1 H53B H 0.1654 0.3513 1.1235 0.149 Uiso 0.50 1 calc PR B 1 H53C H 0.1972 0.3871 1.1458 0.149 Uiso 0.50 1 calc PR B 1 C46 C 0.1259(3) 0.3732(4) 0.6841(11) 0.140(5) Uani 0.50 1 d PDU A 2 H46A H 0.1184 0.3878 0.6516 0.210 Uiso 0.50 1 calc PR A 2 H46B H 0.1067 0.3509 0.6944 0.210 Uiso 0.50 1 calc PR A 2 H46C H 0.1419 0.3721 0.6342 0.210 Uiso 0.50 1 calc PR A 2 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 0.075(2) 0.073(2) 0.110(2) -0.0054(17) 0.0140(17) 0.0305(17) C1 0.073(3) 0.119(4) 0.056(3) 0.000(3) 0.010(2) 0.039(3) O2 0.104(2) 0.102(2) 0.077(2) -0.021(2) -0.0078(18) 0.064(2) C2 0.063(3) 0.105(4) 0.094(4) -0.056(4) 0.003(3) 0.015(3) O3 0.088(2) 0.073(2) 0.108(2) -0.0054(17) 0.0221(18) 0.0386(17) C3 0.105(4) 0.087(4) 0.091(4) -0.013(3) 0.011(3) 0.045(3) O4 0.080(2) 0.105(2) 0.092(2) 0.012(2) 0.0118(19) 0.0455(19) C4 0.105(4) 0.092(4) 0.095(4) -0.009(3) 0.012(3) 0.057(3) O5 0.116(4) 0.089(4) 0.246(8) -0.065(5) 0.004(5) 0.043(3) C5 0.087(3) 0.080(3) 0.068(3) -0.018(2) -0.003(2) 0.046(3) O6 0.190(6) 0.076(3) 0.143(5) 0.000(3) 0.032(5) 0.068(4) C6 0.067(3) 0.070(3) 0.078(3) -0.012(2) 0.004(2) 0.028(2) O7 0.153(4) 0.130(4) 0.165(4) 0.014(3) -0.003(3) 0.080(3) C7 0.096(3) 0.112(4) 0.085(3) -0.023(3) -0.012(3) 0.063(3) O8 0.239(6) 0.161(4) 0.075(3) -0.011(3) -0.012(3) 0.113(4) C8 0.102(4) 0.101(4) 0.072(3) -0.023(3) -0.026(3) 0.057(3) O9 0.206(17) 0.185(17) 0.226(18) 0.074(15) -0.033(16) -0.011(16) C9 0.114(4) 0.118(4) 0.081(4) -0.029(3) -0.021(3) 0.074(4) O10 0.145(14) 0.162(15) 0.203(16) 0.045(14) -0.056(13) 0.002(13) C10 0.118(4) 0.108(4) 0.070(3) -0.018(3) -0.024(3) 0.066(4) O11 0.116(4) 0.178(5) 0.153(4) 0.002(4) -0.048(3) 0.048(3) C11 0.118(4) 0.124(4) 0.064(3) -0.034(3) -0.017(3) 0.065(4) O12 0.140(4) 0.273(7) 0.083(3) 0.005(4) -0.025(3) 0.046(4) C12 0.117(4) 0.110(4) 0.071(3) -0.030(3) -0.019(3) 0.071(3) C13 0.095(3) 0.094(3) 0.067(3) -0.029(3) -0.021(3) 0.056(3) C14 0.130(5) 0.121(4) 0.069(3) -0.027(3) -0.012(3) 0.076(4) C15 0.100(3) 0.077(3) 0.077(3) -0.006(2) 0.014(3) 0.051(3) C16 0.110(4) 0.088(3) 0.081(3) 0.013(2) 0.019(3) 0.057(3) C17 0.095(3) 0.093(3) 0.106(4) 0.019(3) 0.015(3) 0.046(3) C18 0.088(3) 0.090(3) 0.107(4) 0.011(3) 0.005(3) 0.041(3) C19 0.086(3) 0.081(3) 0.095(3) 0.010(3) 0.008(3) 0.044(3) C20 0.083(3) 0.078(3) 0.087(3) 0.000(2) 0.011(2) 0.043(2) C21 0.100(4) 0.106(4) 0.110(4) 0.026(3) 0.003(3) 0.058(3) C22 0.094(4) 0.105(4) 0.074(3) 0.029(3) 0.002(3) 0.050(3) C23 0.089(4) 0.120(4) 0.080(4) 0.036(3) 0.006(3) 0.050(3) C24 0.090(4) 0.127(5) 0.067(3) 0.029(3) -0.009(3) 0.034(3) C25 0.096(4) 0.139(5) 0.057(3) 0.023(3) 0.002(3) 0.044(4) C26 0.085(4) 0.127(4) 0.057(3) 0.019(3) 0.010(3) 0.043(3) C27 0.064(3) 0.103(4) 0.082(3) 0.028(3) -0.005(3) 0.029(3) C28 0.083(4) 0.162(6) 0.078(3) 0.027(4) 0.017(3) 0.050(4) C29 0.061(3) 0.084(3) 0.122(4) -0.009(3) 0.012(3) 0.020(3) C30 0.079(3) 0.093(4) 0.145(5) -0.024(4) 0.004(3) 0.019(3) C31 0.096(4) 0.083(4) 0.201(8) -0.007(4) 0.017(5) 0.032(3) C32 0.091(5) 0.073(5) 0.118(6) -0.044(5) 0.017(4) 0.038(4) C33 0.134(5) 0.123(5) 0.078(4) -0.033(4) -0.022(4) 0.068(4) C34 0.112(4) 0.076(3) 0.137(5) 0.008(3) 0.038(4) 0.050(3) C35 0.151(6) 0.074(4) 0.164(6) 0.005(4) 0.054(5) 0.054(4) C36 0.104(5) 0.098(5) 0.228(9) -0.027(5) 0.007(5) 0.040(4) C37 0.121(9) 0.131(9) 0.142(9) 0.045(8) -0.010(9) 0.029(8) C38 0.109(5) 0.184(7) 0.093(5) 0.032(5) -0.016(4) 0.042(5) N40 0.100(4) 0.079(4) 0.087(5) -0.014(4) -0.016(4) 0.047(4) C41 0.099(5) 0.084(4) 0.089(5) -0.009(4) -0.012(4) 0.046(4) C42 0.089(5) 0.083(4) 0.085(4) -0.019(4) -0.008(4) 0.038(4) C43 0.090(4) 0.079(4) 0.084(4) -0.014(4) 0.005(4) 0.037(4) C44 0.096(4) 0.083(5) 0.086(4) -0.010(4) 0.004(4) 0.030(4) C45 0.103(4) 0.080(5) 0.085(5) -0.005(4) -0.001(4) 0.039(4) N47 0.098(4) 0.071(4) 0.054(4) -0.011(3) -0.024(4) 0.043(3) C48 0.095(4) 0.063(4) 0.053(4) 0.005(4) -0.022(4) 0.050(4) C49 0.091(4) 0.067(4) 0.072(4) 0.002(4) -0.002(3) 0.042(4) C50 0.088(4) 0.074(4) 0.083(4) -0.011(4) 0.004(4) 0.042(3) C51 0.088(5) 0.080(4) 0.083(4) -0.008(4) 0.001(4) 0.037(4) C52 0.089(5) 0.081(4) 0.082(4) -0.009(4) -0.022(4) 0.044(4) C53 0.134(8) 0.080(6) 0.088(6) -0.005(5) -0.035(6) 0.055(6) C46 0.136(10) 0.136(10) 0.111(9) -0.037(8) -0.029(8) 0.042(8) _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 C6 1.405(6) . ? O1 C29 1.450(6) . ? C1 C6 1.400(7) . ? C1 C2 1.440(8) . ? C1 C28 1.502(8) . ? O2 C13 1.341(6) . ? C2 C3 1.360(9) . ? O3 C20 1.396(6) . ? O3 C34 1.450(6) . ? C3 C4 1.313(8) . ? C3 C32 1.590(9) . ? O4 C27 1.360(6) . ? C4 C5 1.390(7) . ? O5 C32 1.189(11) . ? C5 C6 1.369(7) . ? C5 C7 1.504(7) . ? O6 C32 1.226(11) . ? O7 C33 1.265(8) . ? C7 C8 1.517(8) . ? O8 C33 1.242(8) . ? C8 C9 1.388(8) . ? C8 C13 1.391(7) . ? O9 C37 1.33(4) . ? C9 C10 1.359(8) . ? O10 C37 1.27(3) . ? C10 C11 1.394(8) . ? C10 C33 1.489(9) . ? O11 C38 1.335(10) . ? C11 C12 1.386(8) . ? O12 C38 1.222(11) . ? C12 C13 1.386(8) . ? C12 C14 1.529(8) . ? C14 C15 1.523(8) . ? C15 C20 1.379(7) . ? C15 C16 1.382(7) . ? C16 C17 1.376(8) . ? C17 C18 1.380(8) . ? C17 C37 1.470(18) . ? C18 C19 1.381(7) . ? C19 C20 1.373(7) . ? C19 C21 1.533(8) . ? C21 C22 1.534(8) . ? C22 C23 1.368(8) . ? C22 C27 1.389(8) . ? C23 C24 1.383(9) . ? C24 C25 1.417(9) . ? C24 C38 1.453(10) . ? C25 C26 1.356(8) . ? C26 C27 1.402(8) . ? C26 C28 1.523(8) . ? C29 C30 1.506(8) . ? C30 C31 1.511(10) . ? C34 C35 1.503(9) . ? C35 C36 1.507(11) . ? N40 C41 1.3900 . ? N40 C45 1.3900 . ? C41 C42 1.3900 . ? C42 C43 1.3900 . ? C43 C44 1.3900 . ? C44 C45 1.3900 . ? C45 C46 1.516(14) . ? N47 C48 1.3900 . ? N47 C52 1.3900 . ? C48 C49 1.3900 . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.4650 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 O1 C29 114.4(3) . . ? C6 C1 C2 115.1(5) . . ? C6 C1 C28 121.2(5) . . ? C2 C1 C28 123.6(5) . . ? C3 C2 C1 122.5(5) . . ? C20 O3 C34 114.7(3) . . ? C4 C3 C2 118.4(5) . . ? C4 C3 C32 119.2(7) . . ? C2 C3 C32 122.3(7) . . ? C3 C4 C5 124.2(6) . . ? C6 C5 C4 117.7(5) . . ? C6 C5 C7 121.9(4) . . ? C4 C5 C7 120.4(5) . . ? C5 C6 C1 122.0(4) . . ? C5 C6 O1 118.7(4) . . ? C1 C6 O1 119.2(5) . . ? C5 C7 C8 111.3(4) . . ? C9 C8 C13 118.7(5) . . ? C9 C8 C7 120.5(5) . . ? C13 C8 C7 120.8(5) . . ? C10 C9 C8 121.4(5) . . ? C9 C10 C11 119.4(6) . . ? C9 C10 C33 121.2(6) . . ? C11 C10 C33 119.4(6) . . ? C12 C11 C10 120.9(5) . . ? C11 C12 C13 118.6(5) . . ? C11 C12 C14 119.7(5) . . ? C13 C12 C14 121.7(5) . . ? O2 C13 C12 117.7(5) . . ? O2 C13 C8 121.2(5) . . ? C12 C13 C8 121.1(5) . . ? C15 C14 C12 111.8(4) . . ? C20 C15 C16 117.6(5) . . ? C20 C15 C14 122.3(5) . . ? C16 C15 C14 120.0(5) . . ? C17 C16 C15 121.7(5) . . ? C16 C17 C18 118.9(5) . . ? C16 C17 C37 128.1(13) . . ? C18 C17 C37 113.0(14) . . ? C17 C18 C19 120.9(6) . . ? C20 C19 C18 118.4(5) . . ? C20 C19 C21 121.8(5) . . ? C18 C19 C21 119.7(5) . . ? C19 C20 C15 122.4(5) . . ? C19 C20 O3 119.2(5) . . ? C15 C20 O3 118.4(5) . . ? C19 C21 C22 111.9(4) . . ? C23 C22 C27 118.2(6) . . ? C23 C22 C21 120.2(5) . . ? C27 C22 C21 121.5(5) . . ? C22 C23 C24 121.3(5) . . ? C23 C24 C25 119.0(5) . . ? C23 C24 C38 122.2(7) . . ? C25 C24 C38 118.8(7) . . ? C26 C25 C24 121.1(6) . . ? C25 C26 C27 117.9(5) . . ? C25 C26 C28 121.7(6) . . ? C27 C26 C28 120.3(5) . . ? O4 C27 C22 119.1(6) . . ? O4 C27 C26 118.6(5) . . ? C22 C27 C26 122.4(5) . . ? C1 C28 C26 113.3(4) . . ? O1 C29 C30 106.9(4) . . ? C29 C30 C31 113.2(6) . . ? O5 C32 O6 129.7(8) . . ? O5 C32 C3 113.9(9) . . ? O6 C32 C3 116.4(8) . . ? O8 C33 O7 123.6(7) . . ? O8 C33 C10 120.9(7) . . ? O7 C33 C10 115.5(6) . . ? O3 C34 C35 107.5(4) . . ? C34 C35 C36 115.4(7) . . ? O10 C37 O9 118(2) . . ? O10 C37 C17 126(2) . . ? O9 C37 C17 116(2) . . ? O12 C38 O11 122.6(7) . . ? O12 C38 C24 123.9(8) . . ? O11 C38 C24 113.5(8) . . ? C41 N40 C45 120.0 . . ? C42 C41 N40 120.0 . . ? C43 C42 C41 120.0 . . ? C42 C43 C44 120.0 . . ? C43 C44 C45 120.0 . . ? C44 C45 N40 120.0 . . ? C44 C45 C46 121.6(9) . . ? N40 C45 C46 118.4(9) . . ? C48 N47 C52 120.0 . . ? N47 C48 C49 120.0 . . ? C50 C49 C48 120.0 . . ? C51 C50 C49 120.0 . . ? C50 C51 C52 120.0 . . ? C51 C52 N47 120.0 . . ? C51 C52 C53 122.9 . . ? N47 C52 C53 117.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.872 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.066