# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 loop_ _publ_author_name 'Andrea Pochini' 'Annalinda Contino' 'Elisa Longo' 'Chiara Massera' 'Giuseppe Spoto' 'Franco Ugozzoli' _publ_contact_author_name 'Prof Andrea Pochini' _publ_contact_author_address ; Chimica Organica e Industriale Universitą di Parma Parco Area delle Scienze 17/a Parma N/A I-43100 ITALY ; _publ_contact_author_email ANDREA.POCHINI@UNIPR.IT _publ_section_title ; An Integrated Approach to the Study of the Recognition of Guests Containing CH3 and CH2 Acidic Groups by Differently Rigidified Cone p-tert-Butylcalix[4]arene Derivatives ; data_dc3tbs1 _database_code_CSD 215593 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H71 N O6' _chemical_formula_weight 830.12 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' 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 ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.064(5) _cell_length_b 19.817(5) _cell_length_c 11.242(5) _cell_angle_alpha 90.268(5) _cell_angle_beta 114.159(5) _cell_angle_gamma 88.532(5) _cell_volume 2451.4(16) _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 1.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 0.072 _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 0.71069 _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 9264 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.2416 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.71 _reflns_number_total 9264 _reflns_number_gt 1957 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0695P)^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 SHELXL _refine_ls_extinction_coef 0.0016(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9264 _refine_ls_number_parameters 549 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2354 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.1980 _refine_ls_wR_factor_gt 0.1853 _refine_ls_goodness_of_fit_ref 0.832 _refine_ls_restrained_S_all 0.832 _refine_ls_shift/su_max 14.004 _refine_ls_shift/su_mean 0.261 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 O1D O 0.9154(2) 0.32969(17) 0.5197(2) 0.0779(9) Uani 1 1 d . . . O1A O 0.9050(2) 0.17982(17) 0.5176(2) 0.0766(9) Uani 1 1 d . . . O1C O 0.8170(2) 0.32695(16) 0.2171(3) 0.0755(8) Uani 1 1 d . . . O1B O 0.7989(2) 0.18341(18) 0.2040(2) 0.0792(9) Uani 1 1 d . . . O1 O 0.7840(4) 0.2607(3) 0.6482(4) 0.1132(13) Uani 1 1 d . . . O2 O 0.5766(3) 0.2672(3) 0.0825(4) 0.1161(14) Uani 1 1 d . . . C1A C 1.0224(3) 0.1552(2) 0.5563(3) 0.0616(10) Uani 1 1 d . . . C2A C 1.1168(3) 0.1849(2) 0.6586(3) 0.0666(11) Uani 1 1 d . . . C3A C 1.2360(4) 0.1578(3) 0.6989(4) 0.0823(14) Uani 1 1 d . . . H3A H 1.2993 0.1773 0.7682 0.319(6) Uiso 1 1 calc R . . C4A C 1.2602(4) 0.1018(3) 0.6356(4) 0.0799(13) Uani 1 1 d . . . C5A C 1.1667(4) 0.0759(3) 0.5289(4) 0.0818(13) Uani 1 1 d . . . H5A H 1.1836 0.0403 0.4843 0.319(6) Uiso 1 1 calc R . . C6A C 1.0459(4) 0.1015(2) 0.4846(3) 0.0641(10) Uani 1 1 d . . . C7A C 1.3911(5) 0.0715(3) 0.6888(5) 0.1030(18) Uani 1 1 d . . . C8A C 1.4111(12) 0.0264(7) 0.8075(13) 0.111(4) Uiso 0.50 1 d P . . C8A' C 1.4344(11) 0.0590(6) 0.8361(11) 0.090(3) Uiso 0.50 1 d P . . C9A C 1.4684(14) 0.1133(8) 0.6624(16) 0.131(5) Uiso 0.50 1 d P . . C9A' C 1.4837(12) 0.1390(7) 0.7330(14) 0.113(4) Uiso 0.50 1 d P . . CXA' C 1.3931(12) -0.0047(7) 0.6149(12) 0.108(4) Uiso 0.50 1 d P . . C10A C 1.4268(15) 0.0378(9) 0.5921(17) 0.147(6) Uiso 0.50 1 d P . . C11A C 0.9501(4) 0.0741(2) 0.3607(4) 0.0696(11) Uani 1 1 d . . . H11A H 0.8698 0.0853 0.3568 0.319(6) Uiso 1 1 calc R . . H11B H 0.9588 0.0254 0.3594 0.319(6) Uiso 1 1 calc R . . C12A C 0.8432(5) 0.1503(3) 0.5902(6) 0.1105(19) Uani 1 1 d . . . H12A H 0.8993 0.1429 0.6803 0.319(6) Uiso 1 1 calc R . . H12B H 0.8098 0.1073 0.5528 0.319(6) Uiso 1 1 calc R . . C13A C 0.7419(5) 0.1996(4) 0.5824(7) 0.124(2) Uani 1 1 d . . . H13A H 0.6914 0.2096 0.4915 0.319(6) Uiso 1 1 calc R . . H13B H 0.6914 0.1783 0.6192 0.319(6) Uiso 1 1 calc R . . C1B C 0.8925(4) 0.1595(2) 0.1740(4) 0.0667(10) Uani 1 1 d . . . C2B C 0.9644(4) 0.1051(2) 0.2432(4) 0.0664(10) Uani 1 1 d . . . C3B C 1.0526(4) 0.0798(2) 0.2070(4) 0.0746(12) Uani 1 1 d . . . H3B H 1.0970 0.0418 0.2512 0.319(6) Uiso 1 1 calc R . . C4B C 1.0812(4) 0.1071(2) 0.1081(4) 0.0715(11) Uani 1 1 d . . . C5B C 1.0108(4) 0.1645(2) 0.0469(3) 0.0728(11) Uani 1 1 d . . . H5B H 1.0275 0.1859 -0.0172 0.319(6) Uiso 1 1 calc R . . C6B C 0.9157(3) 0.1920(2) 0.0772(3) 0.0578(9) Uani 1 1 d . . . C7B C 1.1803(4) 0.0787(3) 0.0703(4) 0.0831(14) Uani 1 1 d . . . C8B C 1.2151(6) 0.0048(4) 0.1157(6) 0.128(2) Uani 1 1 d . . . H8B1 H 1.2049 -0.0230 0.0420 0.319(6) Uiso 1 1 calc R . . H8B2 H 1.1636 -0.0106 0.1558 0.319(6) Uiso 1 1 calc R . . H8B3 H 1.2983 0.0020 0.1777 0.319(6) Uiso 1 1 calc R . . C9B C 1.2633(15) 0.1418(8) 0.0776(16) 0.128(5) Uiso 0.50 1 d P . . C9B' C 1.2919(11) 0.1169(6) 0.1298(12) 0.092(3) Uiso 0.50 1 d P . . C10B C 1.1265(6) 0.0746(4) -0.0818(5) 0.133(3) Uani 1 1 d . . . H10A H 1.0933 0.1180 -0.1186 0.319(6) Uiso 1 1 calc R . . H10B H 1.0636 0.0420 -0.1113 0.319(6) Uiso 1 1 calc R . . H10C H 1.1897 0.0613 -0.1088 0.319(6) Uiso 1 1 calc R . . C11B C 0.8516(4) 0.2570(2) 0.0121(3) 0.0706(11) Uani 1 1 d . . . H11C H 0.8401 0.2570 -0.0785 0.319(6) Uiso 1 1 calc R . . H11D H 0.7722 0.2601 0.0144 0.319(6) Uiso 1 1 calc R . . C12B C 0.6824(5) 0.1576(4) 0.1171(7) 0.123(2) Uani 1 1 d . . . H12C H 0.6765 0.1110 0.1397 0.319(6) Uiso 1 1 calc R . . H12D H 0.6756 0.1588 0.0281 0.319(6) Uiso 1 1 calc R . . C13B C 0.5833(5) 0.1983(4) 0.1269(7) 0.125(2) Uani 1 1 d . . . H13C H 0.5068 0.1770 0.0759 0.319(6) Uiso 1 1 calc R . . H13D H 0.5936 0.1986 0.2171 0.319(6) Uiso 1 1 calc R . . C1C C 0.9060(3) 0.3502(2) 0.1837(4) 0.0639(10) Uani 1 1 d . . . C2C C 0.9242(3) 0.3168(2) 0.0796(3) 0.0615(10) Uani 1 1 d . . . C3C C 1.0131(4) 0.3406(3) 0.0448(3) 0.0766(13) Uani 1 1 d . . . H3C H 1.0219 0.3214 -0.0266 0.319(6) Uiso 1 1 calc R . . C4C C 1.0908(4) 0.3924(3) 0.1119(4) 0.0846(14) Uani 1 1 d . . . C5C C 1.0713(4) 0.4226(3) 0.2143(4) 0.0784(12) Uani 1 1 d . . . H5C H 1.1193 0.4583 0.2587 0.319(6) Uiso 1 1 calc R . . C6C C 0.9807(4) 0.4005(2) 0.2517(4) 0.0672(10) Uani 1 1 d . . . C7C C 1.1905(5) 0.4151(4) 0.0713(5) 0.114(2) Uani 1 1 d . . . C8C C 1.1311(7) 0.4309(4) -0.0809(6) 0.154(3) Uani 1 1 d . . . H8C1 H 1.1940 0.4346 -0.1118 0.319(6) Uiso 1 1 calc R . . H8C2 H 1.0849 0.4726 -0.0967 0.319(6) Uiso 1 1 calc R . . H8C3 H 1.0784 0.3950 -0.1259 0.319(6) Uiso 1 1 calc R . . C9C C 1.1988(10) 0.5051(6) 0.0996(10) 0.094(3) Uiso 0.50 1 d P . . C9C' C 1.2683(19) 0.4617(11) 0.148(2) 0.173(7) Uiso 0.50 1 d P . . C10C C 1.2995(16) 0.3907(9) 0.1401(17) 0.147(5) Uiso 0.50 1 d P . . CXC' C 1.2742(10) 0.3434(6) 0.0661(11) 0.093(3) Uiso 0.50 1 d P . . C11C C 0.9717(4) 0.4326(2) 0.3719(4) 0.0749(12) Uani 1 1 d . . . H11E H 0.9878 0.4804 0.3743 0.319(6) Uiso 1 1 calc R . . H11F H 0.8904 0.4275 0.3678 0.319(6) Uiso 1 1 calc R . . C12C C 0.7030(5) 0.3629(4) 0.1511(8) 0.138(3) Uani 1 1 d . . . H12E H 0.6844 0.3680 0.0590 0.319(6) Uiso 1 1 calc R . . H12F H 0.7053 0.4073 0.1885 0.319(6) Uiso 1 1 calc R . . C13C C 0.6090(7) 0.3199(5) 0.1706(12) 0.196(5) Uani 1 1 d . . . H13E H 0.6423 0.3020 0.2588 0.319(6) Uiso 1 1 calc R . . H13F H 0.5376 0.3475 0.1584 0.319(6) Uiso 1 1 calc R . . C1D C 1.0344(4) 0.3476(2) 0.5585(3) 0.0678(10) Uani 1 1 d . . . C2D C 1.0651(4) 0.3975(2) 0.4954(4) 0.0713(11) Uani 1 1 d . . . C3D C 1.1873(4) 0.4153(3) 0.5423(4) 0.0766(12) Uani 1 1 d . . . H3D H 1.2079 0.4507 0.5017 0.319(6) Uiso 1 1 calc R . . C4D C 1.2792(4) 0.3826(3) 0.6465(4) 0.0810(14) Uani 1 1 d . . . C5D C 1.2465(4) 0.3290(2) 0.7058(4) 0.0754(12) Uani 1 1 d . . . H5D H 1.3060 0.3060 0.7756 0.319(6) Uiso 1 1 calc R . . C6D C 1.1259(3) 0.3098(2) 0.6616(3) 0.0609(10) Uani 1 1 d . . . C7D C 1.4111(4) 0.4041(3) 0.7003(5) 0.1010(18) Uani 1 1 d . . . C8D C 1.4255(11) 0.4620(7) 0.8139(12) 0.103(4) Uiso 0.50 1 d P . . C8D' C 1.4465(8) 0.4291(5) 0.8446(9) 0.070(2) Uiso 0.50 1 d P . . C9D C 1.4326(13) 0.4692(7) 0.6176(14) 0.116(4) Uiso 0.50 1 d P . . C9D' C 1.4441(10) 0.4323(6) 0.5968(10) 0.087(3) Uiso 0.50 1 d P . . C10D C 1.5030(5) 0.3411(4) 0.7416(7) 0.143(3) Uani 1 1 d . . . H10D H 1.4780 0.3086 0.6726 0.319(6) Uiso 1 1 calc R . . H10E H 1.5034 0.3209 0.8192 0.319(6) Uiso 1 1 calc R . . H10F H 1.5832 0.3557 0.7580 0.319(6) Uiso 1 1 calc R . . C11D C 1.0938(4) 0.2486(2) 0.7226(3) 0.0691(11) Uani 1 1 d . . . H11G H 1.1435 0.2471 0.8157 0.319(6) Uiso 1 1 calc R . . H11H H 1.0091 0.2518 0.7092 0.319(6) Uiso 1 1 calc R . . C12D C 0.8523(5) 0.3635(3) 0.5939(6) 0.1063(18) Uani 1 1 d . . . H12G H 0.9071 0.3670 0.6852 0.319(6) Uiso 1 1 calc R . . H12H H 0.8249 0.4087 0.5598 0.319(6) Uiso 1 1 calc R . . C13D C 0.7475(5) 0.3223(4) 0.5795(8) 0.130(3) Uani 1 1 d . . . H13G H 0.6954 0.3476 0.6114 0.319(6) Uiso 1 1 calc R . . H13H H 0.7007 0.3132 0.4878 0.319(6) Uiso 1 1 calc R . . N1G N 1.4233(6) 0.2511(5) 0.3974(7) 0.189(3) Uani 1 1 d . . . C1G C 1.2039(5) 0.2464(3) 0.3766(5) 0.1057(18) Uani 1 1 d . . . H1G1 H 1.1493 0.2483 0.2861 0.319(6) Uiso 1 1 calc R . . H1G2 H 1.1867 0.2839 0.4213 0.319(6) Uiso 1 1 calc R . . H1G3 H 1.1936 0.2049 0.4143 0.319(6) Uiso 1 1 calc R . . C2G C 1.3199(6) 0.2494(4) 0.3881(5) 0.113(2) 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 O1D 0.0581(15) 0.137(3) 0.0413(13) -0.0019(14) 0.0230(11) -0.0138(17) O1A 0.0474(14) 0.134(3) 0.0498(14) 0.0081(15) 0.0210(12) -0.0009(15) O1C 0.0605(16) 0.112(3) 0.0589(16) 0.0124(15) 0.0295(13) 0.0000(16) O1B 0.0591(15) 0.134(3) 0.0529(15) 0.0048(15) 0.0312(13) -0.0014(16) O1 0.092(3) 0.189(5) 0.082(2) 0.008(3) 0.059(2) 0.001(3) O2 0.065(2) 0.177(5) 0.088(3) 0.013(3) 0.0124(19) -0.002(2) C1A 0.0534(19) 0.099(3) 0.0362(17) 0.0174(17) 0.0219(14) -0.0030(19) C2A 0.0520(19) 0.114(3) 0.0350(16) 0.0111(18) 0.0194(14) -0.001(2) C3A 0.066(3) 0.134(4) 0.054(2) 0.020(2) 0.032(2) 0.006(3) C4A 0.069(2) 0.129(4) 0.046(2) 0.018(2) 0.0290(19) 0.015(3) C5A 0.086(3) 0.112(4) 0.057(2) 0.025(2) 0.039(2) 0.007(3) C6A 0.065(2) 0.089(3) 0.0429(18) 0.0106(17) 0.0257(16) -0.006(2) C7A 0.085(3) 0.151(5) 0.082(3) 0.020(3) 0.045(3) 0.022(3) C11A 0.063(2) 0.100(3) 0.0453(19) 0.0027(18) 0.0215(17) -0.016(2) C12A 0.095(4) 0.156(6) 0.115(4) 0.018(4) 0.078(3) -0.003(3) C13A 0.082(4) 0.172(7) 0.146(6) -0.028(5) 0.073(4) -0.029(4) C1B 0.064(2) 0.094(3) 0.0457(18) 0.0031(18) 0.0260(16) -0.003(2) C2B 0.073(2) 0.088(3) 0.050(2) 0.0035(19) 0.0368(19) -0.008(2) C3B 0.076(3) 0.104(3) 0.053(2) -0.007(2) 0.035(2) -0.011(2) C4B 0.074(2) 0.099(3) 0.051(2) 0.003(2) 0.0354(19) 0.001(2) C5B 0.067(2) 0.108(3) 0.0416(18) 0.0047(19) 0.0202(17) -0.001(2) C6B 0.0492(18) 0.091(3) 0.0381(16) 0.0008(16) 0.0216(14) -0.0121(18) C7B 0.079(3) 0.119(4) 0.058(2) 0.000(2) 0.036(2) 0.008(3) C8B 0.123(5) 0.180(7) 0.108(5) 0.029(4) 0.077(4) 0.048(5) C10B 0.145(6) 0.202(8) 0.072(4) 0.004(4) 0.066(4) 0.022(5) C11B 0.073(2) 0.095(3) 0.0406(19) -0.0015(19) 0.0194(17) -0.005(2) C12B 0.072(4) 0.160(6) 0.142(6) -0.012(4) 0.048(4) -0.010(4) C13B 0.075(3) 0.160(7) 0.157(6) 0.028(5) 0.062(4) -0.011(4) C1C 0.0546(19) 0.087(3) 0.052(2) 0.0097(18) 0.0240(17) -0.0037(19) C2C 0.0468(18) 0.097(3) 0.0410(17) 0.0124(18) 0.0187(14) 0.0111(18) C3C 0.067(2) 0.130(4) 0.0321(17) 0.004(2) 0.0183(16) -0.013(2) C4C 0.073(3) 0.138(4) 0.049(2) -0.004(2) 0.0299(19) -0.016(3) C5C 0.067(3) 0.117(4) 0.050(2) 0.005(2) 0.0225(19) -0.017(2) C6C 0.070(2) 0.085(3) 0.046(2) 0.0055(18) 0.0237(19) -0.001(2) C7C 0.084(3) 0.205(7) 0.057(3) 0.002(3) 0.028(2) -0.047(4) C8C 0.157(7) 0.235(9) 0.113(5) 0.011(5) 0.096(5) -0.023(6) C11C 0.080(3) 0.101(3) 0.047(2) 0.002(2) 0.0296(19) 0.006(2) C12C 0.087(4) 0.180(7) 0.167(7) 0.029(5) 0.073(4) 0.027(4) C13C 0.116(6) 0.212(10) 0.319(14) -0.094(9) 0.148(8) -0.055(6) C1D 0.065(2) 0.100(3) 0.0469(19) -0.0126(19) 0.0311(18) -0.011(2) C2D 0.074(2) 0.094(3) 0.055(2) -0.010(2) 0.0338(19) -0.011(2) C3D 0.074(3) 0.112(4) 0.053(2) -0.013(2) 0.035(2) -0.008(2) C4D 0.060(2) 0.135(4) 0.051(2) -0.012(2) 0.0249(18) -0.022(3) C5D 0.066(2) 0.117(4) 0.054(2) -0.008(2) 0.0348(19) -0.020(2) C6D 0.0516(19) 0.102(3) 0.0353(16) -0.0031(17) 0.0234(14) -0.0055(19) C7D 0.069(3) 0.161(6) 0.075(3) -0.014(3) 0.030(2) -0.031(3) C10D 0.074(4) 0.230(9) 0.125(5) -0.001(5) 0.042(4) -0.006(5) C11D 0.060(2) 0.112(3) 0.0371(17) -0.0001(19) 0.0220(16) -0.008(2) C12D 0.082(3) 0.154(5) 0.107(4) -0.007(4) 0.063(3) 0.002(3) C13D 0.085(4) 0.167(7) 0.163(6) 0.049(5) 0.078(4) 0.022(4) N1G 0.110(5) 0.282(10) 0.151(6) -0.008(6) 0.029(4) -0.004(6) C1G 0.085(4) 0.155(6) 0.071(3) 0.010(3) 0.026(3) 0.004(3) C2G 0.105(5) 0.151(6) 0.075(3) 0.001(3) 0.029(3) 0.002(4) _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 O1D C1D 1.375(5) . ? O1D C12D 1.488(6) . ? O1A C1A 1.377(4) . ? O1A C12A 1.445(5) . ? O1C C1C 1.365(4) . ? O1C C12C 1.439(6) . ? O1B C1B 1.378(5) . ? O1B C12B 1.449(6) . ? O1 C13D 1.410(7) . ? O1 C13A 1.409(7) . ? O2 C13C 1.385(9) . ? O2 C13B 1.446(7) . ? C1A C2A 1.386(5) . ? C1A C6A 1.424(6) . ? C2A C3A 1.411(6) . ? C2A C11D 1.525(6) . ? C3A C4A 1.402(7) . ? C4A C5A 1.375(7) . ? C4A C7A 1.547(7) . ? C5A C6A 1.414(6) . ? C6A C11A 1.509(5) . ? C7A C9A 1.383(16) . ? C7A C10A 1.475(18) . ? C7A C8A' 1.539(12) . ? C7A C8A 1.541(14) . ? C7A CXA' 1.725(14) . ? C7A C9A' 1.703(15) . ? C8A C8A' 0.729(16) . ? C9A C9A' 0.897(18) . ? C9A C10A 1.68(2) . ? CXA' C10A 1.023(18) . ? C11A C2B 1.534(5) . ? C12A C13A 1.519(8) . ? C1B C2B 1.387(6) . ? C1B C6B 1.393(5) . ? C2B C3B 1.369(5) . ? C3B C4B 1.406(5) . ? C4B C5B 1.404(6) . ? C4B C7B 1.518(6) . ? C5B C6B 1.419(6) . ? C6B C11B 1.513(5) . ? C7B C9B' 1.463(13) . ? C7B C8B 1.544(8) . ? C7B C10B 1.563(7) . ? C7B C9B 1.603(16) . ? C9B C9B' 0.732(17) . ? C11B C2C 1.499(6) . ? C12B C13B 1.466(8) . ? C1C C6C 1.364(6) . ? C1C C2C 1.433(5) . ? C2C C3C 1.377(5) . ? C3C C4C 1.402(6) . ? C4C C5C 1.396(6) . ? C4C C7C 1.529(6) . ? C5C C6C 1.402(5) . ? C6C C11C 1.534(6) . ? C7C C10C 1.304(17) . ? C7C C9C' 1.36(2) . ? C7C C8C 1.590(8) . ? C7C CXC' 1.735(13) . ? C7C C9C 1.809(14) . ? C9C C9C' 1.15(2) . ? C9C' C10C 1.46(2) . ? C10C CXC' 1.209(19) . ? C11C C2D 1.539(6) . ? C12C C13C 1.521(9) . ? C1D C2D 1.362(6) . ? C1D C6D 1.429(5) . ? C2D C3D 1.402(6) . ? C3D C4D 1.389(6) . ? C4D C5D 1.404(6) . ? C4D C7D 1.525(6) . ? C5D C6D 1.393(5) . ? C6D C11D 1.531(5) . ? C7D C9D' 1.489(11) . ? C7D C8D' 1.579(10) . ? C7D C10D 1.586(9) . ? C7D C8D 1.671(14) . ? C7D C9D 1.679(15) . ? C8D C8D' 0.729(13) . ? C9D C9D' 0.794(15) . ? C12D C13D 1.475(7) . ? N1G C2G 1.210(9) . ? C1G C2G 1.354(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 C1D O1D C12D 113.9(3) . . ? C1A O1A C12A 112.6(3) . . ? C1C O1C C12C 112.4(4) . . ? C1B O1B C12B 112.3(4) . . ? C13D O1 C13A 119.6(6) . . ? C13C O2 C13B 120.7(7) . . ? O1A C1A C2A 120.4(4) . . ? O1A C1A C6A 118.8(3) . . ? C2A C1A C6A 120.7(4) . . ? C1A C2A C3A 119.5(4) . . ? C1A C2A C11D 120.5(3) . . ? C3A C2A C11D 119.9(4) . . ? C2A C3A C4A 120.8(5) . . ? C5A C4A C3A 118.8(4) . . ? C5A C4A C7A 122.5(5) . . ? C3A C4A C7A 118.7(5) . . ? C4A C5A C6A 122.4(5) . . ? C1A C6A C5A 117.5(4) . . ? C1A C6A C11A 123.0(4) . . ? C5A C6A C11A 119.3(4) . . ? C9A C7A C10A 71.9(10) . . ? C9A C7A C8A' 111.5(9) . . ? C10A C7A C8A' 130.6(9) . . ? C9A C7A C4A 111.3(8) . . ? C10A C7A C4A 115.8(8) . . ? C8A' C7A C4A 108.4(5) . . ? C9A C7A C8A 131.6(9) . . ? C10A C7A C8A 113.1(10) . . ? C8A' C7A C8A 27.4(6) . . ? C4A C7A C8A 108.6(6) . . ? C9A C7A CXA' 107.0(9) . . ? C10A C7A CXA' 36.3(7) . . ? C8A' C7A CXA' 108.4(7) . . ? C4A C7A CXA' 110.2(6) . . ? C8A C7A CXA' 83.3(8) . . ? C9A C7A C9A' 31.7(7) . . ? C10A C7A C9A' 102.4(9) . . ? C8A' C7A C9A' 85.4(8) . . ? C4A C7A C9A' 105.3(6) . . ? C8A C7A C9A' 111.1(8) . . ? CXA' C7A C9A' 134.7(7) . . ? C8A' C8A C7A 76.2(17) . . ? C8A C8A' C7A 76.5(16) . . ? C9A' C9A C7A 94.2(18) . . ? C9A' C9A C10A 147(2) . . ? C7A C9A C10A 56.6(9) . . ? C9A C9A' C7A 54.1(14) . . ? C10A CXA' C7A 58.5(13) . . ? CXA' C10A C7A 85.3(15) . . ? CXA' C10A C9A 134.7(19) . . ? C7A C10A C9A 51.5(8) . . ? C6A C11A C2B 109.2(3) . . ? O1A C12A C13A 107.1(5) . . ? O1 C13A C12A 113.6(5) . . ? O1B C1B C2B 119.7(3) . . ? O1B C1B C6B 119.1(4) . . ? C2B C1B C6B 121.2(4) . . ? C3B C2B C1B 118.7(4) . . ? C3B C2B C11A 119.4(4) . . ? C1B C2B C11A 121.9(4) . . ? C2B C3B C4B 124.8(4) . . ? C5B C4B C3B 114.0(4) . . ? C5B C4B C7B 121.9(4) . . ? C3B C4B C7B 124.1(4) . . ? C4B C5B C6B 123.9(4) . . ? C1B C6B C5B 117.2(4) . . ? C1B C6B C11B 123.2(4) . . ? C5B C6B C11B 119.4(3) . . ? C9B' C7B C4B 111.5(6) . . ? C9B' C7B C8B 106.4(6) . . ? C4B C7B C8B 112.0(4) . . ? C9B' C7B C10B 115.0(6) . . ? C4B C7B C10B 107.7(4) . . ? C8B C7B C10B 104.0(5) . . ? C9B' C7B C9B 27.1(6) . . ? C4B C7B C9B 104.8(7) . . ? C8B C7B C9B 130.9(7) . . ? C10B C7B C9B 94.2(7) . . ? C9B' C9B C7B 65.7(17) . . ? C9B C9B' C7B 87.1(19) . . ? C2C C11B C6B 110.7(3) . . ? O1B C12B C13B 110.2(6) . . ? O2 C13B C12B 113.9(5) . . ? C6C C1C O1C 121.8(4) . . ? C6C C1C C2C 120.6(4) . . ? O1C C1C C2C 117.5(4) . . ? C3C C2C C1C 117.7(4) . . ? C3C C2C C11B 120.6(4) . . ? C1C C2C C11B 121.7(3) . . ? C2C C3C C4C 123.0(4) . . ? C5C C4C C3C 117.2(4) . . ? C5C C4C C7C 122.2(5) . . ? C3C C4C C7C 120.6(4) . . ? C4C C5C C6C 121.4(4) . . ? C1C C6C C5C 119.8(4) . . ? C1C C6C C11C 122.0(4) . . ? C5C C6C C11C 118.2(4) . . ? C10C C7C C9C' 66.4(10) . . ? C10C C7C C4C 116.0(9) . . ? C9C' C7C C4C 116.7(10) . . ? C10C C7C C8C 127.3(10) . . ? C9C' C7C C8C 116.2(11) . . ? C4C C7C C8C 108.6(4) . . ? C10C C7C CXC' 44.1(9) . . ? C9C' C7C CXC' 108.6(11) . . ? C4C C7C CXC' 107.2(6) . . ? C8C C7C CXC' 97.4(6) . . ? C10C C7C C9C 105.6(10) . . ? C9C' C7C C9C 39.6(10) . . ? C4C C7C C9C 104.6(6) . . ? C8C C7C C9C 88.2(6) . . ? CXC' C7C C9C 143.8(6) . . ? C9C' C9C C7C 48.9(12) . . ? C9C C9C' C7C 91.5(16) . . ? C9C C9C' C10C 145(2) . . ? C7C C9C' C10C 54.9(11) . . ? CXC' C10C C7C 87.3(14) . . ? CXC' C10C C9C' 142.1(19) . . ? C7C C10C C9C' 58.8(11) . . ? C10C CXC' C7C 48.6(10) . . ? C2D C11C C6C 109.0(4) . . ? O1C C12C C13C 105.2(6) . . ? O2 C13C C12C 110.2(7) . . ? C2D C1D O1D 121.0(4) . . ? C2D C1D C6D 120.7(4) . . ? O1D C1D C6D 118.2(4) . . ? C1D C2D C3D 118.5(4) . . ? C1D C2D C11C 122.4(4) . . ? C3D C2D C11C 119.1(4) . . ? C4D C3D C2D 123.0(4) . . ? C3D C4D C5D 117.6(4) . . ? C3D C4D C7D 122.6(5) . . ? C5D C4D C7D 119.7(5) . . ? C6D C5D C4D 120.9(4) . . ? C5D C6D C1D 119.0(4) . . ? C5D C6D C11D 119.8(4) . . ? C1D C6D C11D 121.2(3) . . ? C9D' C7D C4D 112.1(6) . . ? C9D' C7D C8D' 129.4(7) . . ? C4D C7D C8D' 107.6(5) . . ? C9D' C7D C10D 98.5(6) . . ? C4D C7D C10D 111.8(5) . . ? C8D' C7D C10D 94.5(5) . . ? C9D' C7D C8D 110.9(7) . . ? C4D C7D C8D 106.1(6) . . ? C8D' C7D C8D 25.7(5) . . ? C10D C7D C8D 117.6(6) . . ? C9D' C7D C9D 28.2(6) . . ? C4D C7D C9D 112.9(6) . . ? C8D' C7D C9D 106.7(7) . . ? C10D C7D C9D 120.8(7) . . ? C8D C7D C9D 84.3(8) . . ? C8D' C8D C7D 70.1(14) . . ? C8D C8D' C7D 84.2(14) . . ? C9D' C9D C7D 62.5(14) . . ? C9D C9D' C7D 89.3(15) . . ? C2A C11D C6D 108.6(3) . . ? C13D C12D O1D 107.4(5) . . ? O1 C13D C12D 112.0(5) . . ? N1G C2G C1G 179.0(9) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.71 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.460 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.062 data_dc3tbcl _database_code_CSD 215594 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H70 Cl N O6' _chemical_formula_weight 864.56 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.237(5) _cell_length_b 19.743(5) _cell_length_c 12.286(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 113.688(5) _cell_angle_gamma 90.000(5) _cell_volume 2496.0(16) _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 1.150 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 932 _exptl_absorpt_coefficient_mu 0.125 _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 0.71069 _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 26845 _diffrn_reflns_av_R_equivalents 0.0246 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 27.01 _reflns_number_total 10604 _reflns_number_gt 5717 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.2000P)^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 SHELXL _refine_ls_extinction_coef 0.0000(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(3) _refine_ls_number_reflns 10604 _refine_ls_number_parameters 578 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.1478 _refine_ls_R_factor_gt 0.0977 _refine_ls_wR_factor_ref 0.3275 _refine_ls_wR_factor_gt 0.2830 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.125 _refine_ls_shift/su_max 2.209 _refine_ls_shift/su_mean 0.514 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 O1A O -0.9729(4) -0.2362(2) -1.0760(3) 0.0616(10) Uani 1 1 d . . . C1A C -0.9368(5) -0.2575(3) -0.9611(5) 0.0528(13) Uani 1 1 d . . . C2A C -0.8359(5) -0.2229(3) -0.8694(5) 0.0626(15) Uani 1 1 d . . . C3A C -0.7951(5) -0.2475(3) -0.7547(5) 0.0636(15) Uani 1 1 d . . . H3A H -0.7234 -0.2256 -0.6928 0.073(4) Uiso 1 1 calc R . . C4A C -0.8525(7) -0.3015(4) -0.7257(7) 0.083(2) Uani 1 1 d . A . C5A C -0.9599(6) -0.3327(3) -0.8171(6) 0.0666(16) Uani 1 1 d . . . H5A H -1.0011 -0.3706 -0.7977 0.073(4) Uiso 1 1 calc R . . C6A C -1.0075(6) -0.3098(3) -0.9348(5) 0.0624(15) Uani 1 1 d . . . C7A C -0.8043(6) -0.3359(4) -0.6000(6) 0.091(2) Uani 1 1 d D . . C8A C -0.9061(18) -0.366(2) -0.5663(15) 0.177(12) Uani 0.50 1 d P A . C9A C -0.761(3) -0.2765(9) -0.5150(19) 0.147(8) Uiso 0.50 1 d PD A . C10A C -0.6742(14) -0.3742(8) -0.5700(13) 0.083(4) Uiso 0.50 1 d P A . C81 C -0.857(2) -0.4066(7) -0.591(2) 0.131(7) Uiso 0.50 1 d PD A 1 C91 C -0.855(3) -0.3037(15) -0.528(3) 0.171(9) Uiso 0.50 1 d P A 1 C101 C -0.651(2) -0.3463(12) -0.5527(18) 0.102(6) Uiso 0.50 1 d P A 1 C11A C -1.1265(6) -0.3397(3) -1.0253(6) 0.0668(16) Uani 1 1 d . . . H11A H -1.1250 -0.3879 -1.0147 0.096(3) Uiso 1 1 calc R . . H11B H -1.1291 -0.3307 -1.1030 0.096(3) Uiso 1 1 calc R . . C12A C -0.9035(8) -0.2641(4) -1.1345(6) 0.084(2) Uani 1 1 d . . . H12A H -0.9343 -0.3092 -1.1594 0.096(3) Uiso 1 1 calc R . . H12B H -0.8135 -0.2669 -1.0811 0.096(3) Uiso 1 1 calc R . . C13A C -0.9159(9) -0.2227(4) -1.2411(6) 0.097(2) Uani 1 1 d . . . H13A H -0.8822 -0.2475 -1.2897 0.096(3) Uiso 1 1 calc R . . H13B H -1.0057 -0.2126 -1.2879 0.096(3) Uiso 1 1 calc R . . O1B O -1.2871(4) -0.2346(2) -1.1790(3) 0.0630(10) Uani 1 1 d . . . C1B C -1.3174(5) -0.2571(3) -1.0879(5) 0.0538(12) Uani 1 1 d . . . C2B C -1.2485(5) -0.3103(3) -1.0162(5) 0.0577(14) Uani 1 1 d . . . C3B C -1.2863(6) -0.3337(3) -0.9298(6) 0.0660(16) Uani 1 1 d . . . H3B H -1.2383 -0.3704 -0.8802 0.073(4) Uiso 1 1 calc R . . C4B C -1.3898(6) -0.3072(3) -0.9107(6) 0.0680(16) Uani 1 1 d . . . C5B C -1.4525(5) -0.2508(3) -0.9792(5) 0.0598(15) Uani 1 1 d . . . H5B H -1.5219 -0.2298 -0.9648 0.073(4) Uiso 1 1 calc R . . C6B C -1.4178(5) -0.2239(3) -1.0680(4) 0.0523(13) Uani 1 1 d . . . C7B C -1.4309(7) -0.3330(5) -0.8162(6) 0.094(2) Uani 1 1 d . . . C8B C -1.3937(8) -0.4140(4) -0.7908(9) 0.106(3) Uani 1 1 d . . . H8B1 H -1.4311 -0.4387 -0.8641 0.135(5) Uiso 1 1 calc R . . H8B2 H -1.4275 -0.4312 -0.7358 0.135(5) Uiso 1 1 calc R . . H8B3 H -1.3010 -0.4192 -0.7578 0.135(5) Uiso 1 1 calc R . . C9B C -1.4006(14) -0.2897(9) -0.7178(10) 0.203(8) Uani 1 1 d . . . H9B1 H -1.3082 -0.2834 -0.6803 0.135(5) Uiso 1 1 calc R . . H9B2 H -1.4307 -0.3095 -0.6621 0.135(5) Uiso 1 1 calc R . . H9B3 H -1.4422 -0.2467 -0.7439 0.135(5) Uiso 1 1 calc R . . C10B C -1.5786(8) -0.3437(5) -0.8687(8) 0.110(3) Uani 1 1 d . . . H10A H -1.6213 -0.3006 -0.8791 0.135(5) Uiso 1 1 calc R . . H10B H -1.6016 -0.3711 -0.8156 0.135(5) Uiso 1 1 calc R . . H10C H -1.6052 -0.3660 -0.9442 0.135(5) Uiso 1 1 calc R . . C11B C -1.4837(3) -0.1617(4) -1.1348(3) 0.0587(9) Uani 1 1 d . . . H11C H -1.5735 -0.1622 -1.1466 0.096(3) Uiso 1 1 calc R . . H11D H -1.4800 -0.1616 -1.2115 0.096(3) Uiso 1 1 calc R . . C12B C -1.3580(11) -0.2635(5) -1.2894(7) 0.107(3) Uani 1 1 d . . . H12C H -1.4470 -0.2682 -1.3001 0.096(3) Uiso 1 1 calc R . . H12D H -1.3244 -0.3078 -1.2924 0.096(3) Uiso 1 1 calc R . . C13B C -1.3514(10) -0.2206(5) -1.3887(6) 0.109(3) Uani 1 1 d . . . H13C H -1.2618 -0.2114 -1.3719 0.096(3) Uiso 1 1 calc R . . H13D H -1.3863 -0.2463 -1.4612 0.096(3) Uiso 1 1 calc R . . O1C O -1.2859(4) -0.0891(2) -1.1786(4) 0.0676(11) Uani 1 1 d . . . C1C C -1.3189(6) -0.0661(3) -1.0876(5) 0.0551(13) Uani 1 1 d . . . C2C C -1.4178(5) -0.0965(3) -1.0660(5) 0.0510(12) Uani 1 1 d . . . C3C C -1.4525(5) -0.0701(3) -0.9776(5) 0.0632(15) Uani 1 1 d . . . H3C H -1.5217 -0.0912 -0.9632 0.073(4) Uiso 1 1 calc R . . C4C C -1.3905(6) -0.0143(3) -0.9099(5) 0.0614(15) Uani 1 1 d . . . C5C C -1.2875(6) 0.0143(3) -0.9283(6) 0.0672(16) Uani 1 1 d . . . H5C H -1.2421 0.0523 -0.8812 0.073(4) Uiso 1 1 calc R . . C6C C -1.2480(6) -0.0126(3) -1.0178(5) 0.0556(13) Uani 1 1 d . . . C7C C -1.4367(9) 0.0176(4) -0.8175(7) 0.092(2) Uani 1 1 d . . . C8C C -1.5848(10) 0.0213(5) -0.8661(10) 0.112(3) Uani 1 1 d . . . H8C1 H -1.6207 -0.0228 -0.8918 0.135(5) Uiso 1 1 calc R . . H8C2 H -1.6161 0.0521 -0.9322 0.135(5) Uiso 1 1 calc R . . H8C3 H -1.6106 0.0371 -0.8049 0.135(5) Uiso 1 1 calc R . . C9C C -1.3816(16) -0.0249(8) -0.7075(10) 0.206(8) Uani 1 1 d . . . H9C1 H -1.2885 -0.0218 -0.6742 0.135(5) Uiso 1 1 calc R . . H9C2 H -1.4072 -0.0712 -0.7272 0.135(5) Uiso 1 1 calc R . . H9C3 H -1.4137 -0.0090 -0.6505 0.135(5) Uiso 1 1 calc R . . C10C C -1.3817(11) 0.0856(6) -0.7796(10) 0.171(5) Uani 1 1 d . . . H10D H -1.4266 0.1074 -0.7372 0.135(5) Uiso 1 1 calc R . . H10E H -1.3915 0.1121 -0.8482 0.135(5) Uiso 1 1 calc R . . H10F H -1.2911 0.0817 -0.7287 0.135(5) Uiso 1 1 calc R . . C11C C -1.1320(6) 0.0172(3) -1.0332(6) 0.0650(15) Uani 1 1 d . . . H11E H -1.1337 0.0657 -1.0277 0.096(3) Uiso 1 1 calc R . . H11F H -1.1352 0.0056 -1.1102 0.096(3) Uiso 1 1 calc R . . C12C C -1.3660(9) -0.0598(4) -1.2943(6) 0.094(2) Uani 1 1 d . . . H12E H -1.3417 -0.0135 -1.2978 0.096(3) Uiso 1 1 calc R . . H12F H -1.4561 -0.0610 -1.3071 0.096(3) Uiso 1 1 calc R . . C13C C -1.3450(15) -0.0992(5) -1.3828(10) 0.136(4) Uani 1 1 d . . . H13E H -1.3701 -0.0733 -1.4548 0.096(3) Uiso 1 1 calc R . . H13F H -1.2542 -0.1096 -1.3560 0.096(3) Uiso 1 1 calc R . . O1D O -0.9779(3) -0.0859(2) -1.0768(3) 0.0649(11) Uani 1 1 d . . . C1D C -0.9405(5) -0.0646(3) -0.9596(5) 0.0582(14) Uani 1 1 d . . . C2D C -1.0026(6) -0.0114(3) -0.9332(6) 0.0564(14) Uani 1 1 d . . . C3D C -0.9624(7) 0.0131(4) -0.8214(7) 0.081(2) Uani 1 1 d . . . H3D H -1.0082 0.0505 -0.8062 0.073(4) Uiso 1 1 calc R . . C4D C -0.8548(7) -0.0149(4) -0.7264(6) 0.0739(18) Uani 1 1 d . . . C5D C -0.7962(7) -0.0705(4) -0.7567(7) 0.084(2) Uani 1 1 d . . . H5D H -0.7237 -0.0916 -0.6945 0.073(4) Uiso 1 1 calc R . . C6D C -0.8360(5) -0.0967(3) -0.8698(4) 0.0563(14) Uani 1 1 d . . . C7D C -0.7970(10) 0.0066(4) -0.5956(8) 0.133(4) Uani 1 1 d D . . C8D C -0.8901(12) 0.0635(12) -0.5881(12) 0.325(18) Uani 1 1 d . . . H8D1 H -0.9787 0.0490 -0.6288 0.135(5) Uiso 1 1 calc R . . H8D2 H -0.8763 0.1040 -0.6246 0.135(5) Uiso 1 1 calc R . . H8D3 H -0.8727 0.0724 -0.5062 0.135(5) Uiso 1 1 calc R . . C9D C -0.6700(11) 0.0394(8) -0.5729(9) 0.181(6) Uani 1 1 d . . . H9D1 H -0.6265 0.0499 -0.4899 0.135(5) Uiso 1 1 calc R . . H9D2 H -0.6845 0.0804 -0.6185 0.135(5) Uiso 1 1 calc R . . H9D3 H -0.6172 0.0092 -0.5957 0.135(5) Uiso 1 1 calc R . . C10D C -0.7850(13) -0.0508(6) -0.5077(7) 0.176(6) Uani 1 1 d D . . H10G H -0.8688 -0.0708 -0.5267 0.135(5) Uiso 1 1 calc R . . H10H H -0.7527 -0.0328 -0.4284 0.135(5) Uiso 1 1 calc R . . H10I H -0.7260 -0.0845 -0.5129 0.135(5) Uiso 1 1 calc R . . C11D C -0.7745(3) -0.1631(4) -0.8948(3) 0.0640(10) Uani 1 1 d . . . H11G H -0.7858 -0.1639 -0.9765 0.096(3) Uiso 1 1 calc R . . H11H H -0.6830 -0.1637 -0.8461 0.096(3) Uiso 1 1 calc R . . C12D C -0.8998(9) -0.0535(4) -1.1361(6) 0.091(2) Uani 1 1 d . . . H12G H -0.8107 -0.0489 -1.0815 0.096(3) Uiso 1 1 calc R . . H12H H -0.9337 -0.0095 -1.1658 0.096(3) Uiso 1 1 calc R . . C13D C -0.9107(10) -0.0994(6) -1.2352(8) 0.123(3) Uani 1 1 d . . . H13G H -1.0010 -0.1085 -1.2812 0.096(3) Uiso 1 1 calc R . . H13H H -0.8775 -0.0763 -1.2859 0.096(3) Uiso 1 1 calc R . . O1 O -0.8447(3) -0.1619(4) -1.2006(3) 0.0893(9) Uani 1 1 d . . . O2 O -1.4172(3) -0.1600(5) -1.4063(3) 0.1004(12) Uani 1 1 d . . . C1G C -1.1264(12) -0.1513(11) -0.6168(7) 0.181(5) Uani 1 1 d D . . N1G N -1.1211(9) -0.1539(9) -0.5267(6) 0.191(4) Uani 1 1 d . . . Cl1G Cl -1.0740(8) -0.1948(4) -0.7680(8) 0.135(2) Uiso 0.33 1 d PD . . Cl1' Cl -1.0868(7) -0.1420(4) -0.8066(6) 0.119(2) Uiso 0.33 1 d PD . . Cl1" Cl -1.1623(7) -0.1851(3) -0.8283(6) 0.1185(18) Uiso 0.33 1 d PD . . C2G' C -1.181(3) -0.2078(14) -0.7041(17) 0.42(4) Uiso 0.50 1 d PD . . C2G C -1.1877(11) -0.1336(7) -0.7474(8) 0.101(4) Uiso 0.50 1 d PD . . 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 O1A 0.059(2) 0.072(2) 0.058(2) 0.0070(19) 0.0276(19) 0.0034(19) C1A 0.040(3) 0.064(3) 0.057(3) 0.000(3) 0.022(2) 0.005(2) C2A 0.050(3) 0.079(4) 0.073(4) 0.006(3) 0.040(3) 0.014(3) C3A 0.041(3) 0.111(5) 0.043(3) 0.010(3) 0.021(2) 0.006(3) C4A 0.050(4) 0.114(6) 0.081(4) 0.031(4) 0.023(3) 0.024(4) C5A 0.057(3) 0.070(4) 0.077(4) 0.025(3) 0.031(3) 0.014(3) C6A 0.056(3) 0.074(4) 0.066(3) 0.007(3) 0.034(3) 0.023(3) C7A 0.056(4) 0.150(6) 0.055(3) 0.028(4) 0.010(3) 0.005(4) C8A 0.092(10) 0.38(4) 0.059(8) 0.089(14) 0.032(8) -0.024(16) C11A 0.056(4) 0.063(4) 0.091(4) 0.003(3) 0.038(3) 0.016(3) C12A 0.103(5) 0.078(4) 0.078(4) -0.011(3) 0.043(4) -0.008(4) C13A 0.141(7) 0.094(5) 0.064(4) -0.009(4) 0.051(4) -0.016(5) O1B 0.072(3) 0.062(2) 0.068(2) 0.0034(19) 0.041(2) -0.003(2) C1B 0.041(3) 0.067(3) 0.055(3) -0.008(3) 0.021(2) 0.001(2) C2B 0.048(3) 0.054(3) 0.069(4) 0.000(3) 0.021(3) 0.002(3) C3B 0.061(4) 0.069(4) 0.074(4) 0.019(3) 0.034(3) 0.002(3) C4B 0.048(3) 0.086(5) 0.073(4) 0.017(3) 0.027(3) 0.012(3) C5B 0.039(3) 0.089(4) 0.053(3) 0.006(3) 0.020(2) 0.006(3) C6B 0.041(3) 0.061(3) 0.048(3) -0.006(2) 0.010(2) -0.001(2) C7B 0.071(4) 0.147(7) 0.061(4) 0.038(4) 0.025(3) 0.016(4) C8B 0.097(5) 0.098(6) 0.136(7) 0.030(5) 0.060(5) 0.020(4) C9B 0.204(14) 0.34(2) 0.100(7) -0.100(10) 0.097(9) -0.131(14) C10B 0.081(5) 0.148(7) 0.118(6) 0.062(5) 0.057(4) 0.001(4) C11B 0.0399(15) 0.074(2) 0.0572(19) -0.011(3) 0.0146(14) -0.006(3) C12B 0.158(9) 0.098(6) 0.085(5) -0.020(5) 0.069(6) -0.023(6) C13B 0.135(7) 0.149(7) 0.059(4) -0.023(4) 0.054(4) 0.001(6) O1C 0.061(2) 0.073(3) 0.074(3) 0.006(2) 0.032(2) 0.005(2) C1C 0.063(4) 0.050(3) 0.055(3) 0.004(2) 0.027(3) 0.018(3) C2C 0.037(3) 0.062(3) 0.052(3) 0.002(2) 0.016(2) 0.004(2) C3C 0.051(3) 0.078(4) 0.063(3) 0.001(3) 0.026(3) -0.008(3) C4C 0.057(4) 0.082(4) 0.045(3) 0.001(3) 0.020(2) 0.002(3) C5C 0.049(3) 0.080(4) 0.068(4) -0.003(3) 0.019(3) -0.013(3) C6C 0.051(3) 0.060(3) 0.062(3) 0.011(3) 0.029(3) 0.004(3) C7C 0.096(5) 0.113(6) 0.092(5) -0.022(5) 0.063(4) -0.023(5) C8C 0.103(7) 0.123(7) 0.133(8) -0.001(6) 0.073(6) -0.001(5) C9C 0.33(2) 0.216(12) 0.107(8) 0.028(8) 0.123(11) 0.151(13) C10C 0.182(11) 0.227(12) 0.155(9) -0.126(9) 0.120(8) -0.065(8) C11C 0.068(4) 0.058(4) 0.077(4) 0.010(3) 0.037(3) 0.008(3) C12C 0.135(7) 0.087(5) 0.068(4) 0.027(4) 0.050(4) 0.019(5) C13C 0.222(13) 0.112(7) 0.109(7) -0.006(6) 0.104(9) -0.016(8) O1D 0.050(2) 0.091(3) 0.051(2) -0.005(2) 0.0177(18) -0.002(2) C1D 0.049(3) 0.072(4) 0.059(3) -0.012(3) 0.028(3) -0.018(3) C2D 0.048(3) 0.053(3) 0.074(4) -0.008(3) 0.030(3) -0.007(2) C3D 0.062(4) 0.094(5) 0.104(5) -0.030(4) 0.048(4) -0.016(4) C4D 0.064(4) 0.109(5) 0.059(3) -0.030(4) 0.036(3) -0.020(4) C5D 0.058(4) 0.112(6) 0.073(4) -0.020(4) 0.018(3) -0.018(4) C6D 0.035(3) 0.088(4) 0.041(3) -0.006(3) 0.010(2) -0.005(3) C7D 0.138(7) 0.180(8) 0.121(7) -0.085(6) 0.092(6) -0.063(6) C8D 0.121(9) 0.61(4) 0.206(14) -0.29(2) 0.029(9) 0.061(16) C9D 0.133(7) 0.269(14) 0.122(7) -0.134(9) 0.030(6) -0.082(9) C10D 0.237(13) 0.254(12) 0.061(4) -0.059(6) 0.086(6) -0.116(11) C11D 0.0402(16) 0.093(3) 0.058(2) -0.010(4) 0.0191(14) -0.016(4) C12D 0.113(6) 0.117(6) 0.063(4) 0.004(4) 0.054(4) -0.018(5) C13D 0.126(8) 0.174(9) 0.093(6) 0.041(6) 0.069(6) 0.039(7) O1 0.0761(18) 0.119(3) 0.085(2) 0.008(4) 0.0449(16) 0.001(4) O2 0.087(2) 0.140(3) 0.0598(18) -0.001(4) 0.0142(16) -0.017(5) C1G 0.228(11) 0.239(14) 0.089(5) 0.008(10) 0.078(6) -0.004(13) N1G 0.218(8) 0.272(12) 0.076(4) 0.034(8) 0.049(4) -0.003(11) _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 O1A C1A 1.368(6) . ? O1A C12A 1.371(8) . ? C1A C2A 1.412(8) . ? C1A C6A 1.418(8) . ? C2A C3A 1.383(8) . ? C2A C11D 1.464(9) . ? C3A C4A 1.365(10) . ? C4A C5A 1.417(10) . ? C4A C7A 1.571(10) . ? C5A C6A 1.400(8) . ? C6A C11A 1.476(9) . ? C7A C91 1.39(3) . ? C7A C8A 1.489(19) . ? C7A C9A 1.513(5) . ? C7A C101 1.59(2) . ? C7A C81 1.538(10) . ? C7A C10A 1.554(16) . ? C8A C81 1.08(3) . ? C8A C91 1.36(4) . ? C9A C91 1.14(4) . ? C9A C101 2.02(3) . ? C10A C101 0.61(2) . ? C11A C2B 1.534(8) . ? C12A C13A 1.502(10) . ? C13A O1 1.418(10) . ? O1B C1B 1.368(6) . ? O1B C12B 1.389(9) . ? C1B C6B 1.408(7) . ? C1B C2B 1.391(7) . ? C2B C3B 1.372(8) . ? C3B C4B 1.378(9) . ? C4B C5B 1.404(8) . ? C4B C7B 1.500(9) . ? C5B C6B 1.402(7) . ? C6B C11B 1.497(9) . ? C7B C9B 1.407(14) . ? C7B C10B 1.535(11) . ? C7B C8B 1.650(12) . ? C11B C2C 1.555(9) . ? C12B C13B 1.511(12) . ? C13B O2 1.377(11) . ? O1C C1C 1.387(6) . ? O1C C12C 1.462(8) . ? C1C C6C 1.391(8) . ? C1C C2C 1.379(8) . ? C2C C3C 1.393(8) . ? C3C C4C 1.387(8) . ? C4C C5C 1.386(9) . ? C4C C7C 1.559(10) . ? C5C C6C 1.442(9) . ? C6C C11C 1.510(8) . ? C7C C9C 1.498(15) . ? C7C C10C 1.473(13) . ? C7C C8C 1.527(13) . ? C11C C2D 1.584(9) . ? C12C C13C 1.433(12) . ? C13C O2 1.412(13) . ? O1D C1D 1.392(7) . ? O1D C12D 1.491(7) . ? C1D C2D 1.370(8) . ? C1D C6D 1.399(8) . ? C2D C3D 1.351(9) . ? C3D C4D 1.414(11) . ? C4D C5D 1.405(10) . ? C4D C7D 1.531(10) . ? C5D C6D 1.378(8) . ? C6D C11D 1.569(9) . ? C7D C10D 1.532(9) . ? C7D C9D 1.488(14) . ? C7D C8D 1.564(17) . ? C12D C13D 1.483(13) . ? C13D O1 1.412(11) . ? C1G N1G 1.085(9) . ? C1G C2G' 1.498(5) . ? C1G C2G 1.511(5) . ? Cl1G Cl1" 0.990(9) . ? Cl1G Cl1' 1.131(9) . ? Cl1G C2G' 1.696(10) . ? Cl1G C2G 1.848(14) . ? Cl1' Cl1" 1.155(8) . ? Cl1' C2G 1.584(9) . ? Cl1" C2G 1.526(13) . ? Cl1" C2G' 1.681(10) . ? C2G' C2G 1.55(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 C1A O1A C12A 114.9(5) . . ? O1A C1A C2A 119.0(5) . . ? O1A C1A C6A 119.9(5) . . ? C2A C1A C6A 120.9(5) . . ? C3A C2A C1A 118.3(6) . . ? C3A C2A C11D 120.6(5) . . ? C1A C2A C11D 121.0(5) . . ? C4A C3A C2A 122.8(6) . . ? C3A C4A C5A 118.3(6) . . ? C3A C4A C7A 125.6(6) . . ? C5A C4A C7A 116.0(6) . . ? C4A C5A C6A 121.9(6) . . ? C5A C6A C1A 117.0(6) . . ? C5A C6A C11A 120.3(6) . . ? C1A C6A C11A 122.7(5) . . ? C91 C7A C8A 56.3(16) . . ? C91 C7A C9A 46.1(15) . . ? C8A C7A C9A 100.9(17) . . ? C91 C7A C101 119.4(15) . . ? C8A C7A C101 133.3(13) . . ? C9A C7A C101 81.2(14) . . ? C91 C7A C81 95.8(15) . . ? C8A C7A C81 41.9(14) . . ? C9A C7A C81 132.7(14) . . ? C101 C7A C81 104.2(13) . . ? C91 C7A C10A 131.7(14) . . ? C8A C7A C10A 119.6(15) . . ? C9A C7A C10A 101.7(13) . . ? C101 C7A C10A 22.3(8) . . ? C81 C7A C10A 83.7(11) . . ? C91 C7A C4A 111.1(13) . . ? C8A C7A C4A 116.5(8) . . ? C9A C7A C4A 103.4(12) . . ? C101 C7A C4A 108.0(9) . . ? C81 C7A C4A 118.3(10) . . ? C10A C7A C4A 111.3(7) . . ? C81 C8A C91 125(2) . . ? C81 C8A C7A 71.5(12) . . ? C91 C8A C7A 58.0(16) . . ? C91 C9A C7A 61.0(15) . . ? C91 C9A C101 105.5(18) . . ? C7A C9A C101 51.1(9) . . ? C101 C10A C7A 83(3) . . ? C8A C81 C7A 66.6(14) . . ? C9A C91 C7A 72.9(17) . . ? C9A C91 C8A 135(3) . . ? C7A C91 C8A 65.7(15) . . ? C10A C101 C7A 75(3) . . ? C10A C101 C9A 119(3) . . ? C7A C101 C9A 47.6(8) . . ? C6A C11A C2B 111.1(5) . . ? O1A C12A C13A 111.4(6) . . ? O1 C13A C12A 108.2(6) . . ? C1B O1B C12B 115.6(5) . . ? O1B C1B C6B 118.2(5) . . ? O1B C1B C2B 120.3(5) . . ? C6B C1B C2B 121.5(5) . . ? C1B C2B C3B 118.6(5) . . ? C1B C2B C11A 121.7(5) . . ? C3B C2B C11A 119.5(5) . . ? C4B C3B C2B 123.3(6) . . ? C3B C4B C5B 117.0(5) . . ? C3B C4B C7B 123.1(6) . . ? C5B C4B C7B 119.8(6) . . ? C6B C5B C4B 122.5(5) . . ? C5B C6B C1B 116.9(5) . . ? C5B C6B C11B 120.4(4) . . ? C1B C6B C11B 122.7(5) . . ? C4B C7B C9B 114.6(9) . . ? C4B C7B C10B 109.8(5) . . ? C9B C7B C10B 107.0(8) . . ? C4B C7B C8B 110.0(6) . . ? C9B C7B C8B 118.1(9) . . ? C10B C7B C8B 95.5(7) . . ? C6B C11B C2C 111.0(2) . . ? O1B C12B C13B 111.4(7) . . ? O2 C13B C12B 114.6(7) . . ? C1C O1C C12C 113.2(5) . . ? C6C C1C C2C 121.1(5) . . ? C6C C1C O1C 118.2(5) . . ? C2C C1C O1C 120.6(5) . . ? C1C C2C C3C 119.1(5) . . ? C1C C2C C11B 120.0(4) . . ? C3C C2C C11B 120.8(5) . . ? C4C C3C C2C 122.3(5) . . ? C3C C4C C5C 118.4(5) . . ? C3C C4C C7C 121.7(5) . . ? C5C C4C C7C 119.9(6) . . ? C6C C5C C4C 120.5(6) . . ? C1C C6C C5C 118.3(5) . . ? C1C C6C C11C 121.9(5) . . ? C5C C6C C11C 119.8(5) . . ? C9C C7C C10C 104.9(10) . . ? C9C C7C C8C 111.8(9) . . ? C10C C7C C8C 109.4(8) . . ? C9C C7C C4C 107.0(7) . . ? C10C C7C C4C 112.3(6) . . ? C8C C7C C4C 111.3(7) . . ? C6C C11C C2D 109.5(5) . . ? O1C C12C C13C 107.4(7) . . ? O2 C13C C12C 111.1(9) . . ? C1D O1D C12D 112.6(5) . . ? C2D C1D C6D 120.4(5) . . ? C2D C1D O1D 120.4(5) . . ? C6D C1D O1D 119.1(5) . . ? C3D C2D C1D 121.5(6) . . ? C3D C2D C11C 119.2(5) . . ? C1D C2D C11C 119.0(5) . . ? C2D C3D C4D 121.7(6) . . ? C3D C4D C5D 115.0(6) . . ? C3D C4D C7D 128.3(7) . . ? C5D C4D C7D 116.6(7) . . ? C6D C5D C4D 124.3(7) . . ? C5D C6D C1D 117.0(6) . . ? C5D C6D C11D 121.4(5) . . ? C1D C6D C11D 121.4(4) . . ? C10D C7D C4D 114.5(6) . . ? C10D C7D C9D 112.6(10) . . ? C4D C7D C9D 106.7(6) . . ? C10D C7D C8D 111.2(10) . . ? C4D C7D C8D 104.4(9) . . ? C9D C7D C8D 106.9(11) . . ? C2A C11D C6D 110.4(3) . . ? O1D C12D C13D 105.6(7) . . ? O1 C13D C12D 115.2(7) . . ? C13D O1 C13A 118.7(5) . . ? C13B O2 C13C 118.6(6) . . ? N1G C1G C2G' 122.4(17) . . ? N1G C1G C2G 155.4(14) . . ? C2G' C1G C2G 62.0(13) . . ? Cl1" Cl1G Cl1' 65.6(7) . . ? Cl1" Cl1G C2G' 72.1(8) . . ? Cl1' Cl1G C2G' 109.9(11) . . ? Cl1" Cl1G C2G 55.6(6) . . ? Cl1' Cl1G C2G 58.5(6) . . ? C2G' Cl1G C2G 51.7(10) . . ? Cl1G Cl1' Cl1" 51.3(6) . . ? Cl1G Cl1' C2G 84.1(8) . . ? Cl1" Cl1' C2G 65.6(7) . . ? Cl1G Cl1" Cl1' 63.1(6) . . ? Cl1G Cl1" C2G 92.0(8) . . ? Cl1' Cl1" C2G 70.9(6) . . ? Cl1G Cl1" C2G' 73.8(8) . . ? Cl1' Cl1" C2G' 109.6(8) . . ? C2G Cl1" C2G' 57.6(11) . . ? C1G C2G' C2G 59.4(7) . . ? C1G C2G' Cl1" 106.7(9) . . ? C2G C2G' Cl1" 56.2(8) . . ? C1G C2G' Cl1G 93.3(9) . . ? C2G C2G' Cl1G 69.2(7) . . ? Cl1" C2G' Cl1G 34.1(4) . . ? C1G C2G C2G' 58.6(6) . . ? C1G C2G Cl1" 114.4(9) . . ? C2G' C2G Cl1" 66.2(8) . . ? C1G C2G Cl1' 111.0(8) . . ? C2G' C2G Cl1' 96.4(10) . . ? Cl1" C2G Cl1' 43.6(4) . . ? C1G C2G Cl1G 87.1(7) . . ? C2G' C2G Cl1G 59.1(8) . . ? Cl1" C2G Cl1G 32.4(4) . . ? Cl1' C2G Cl1G 37.5(4) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.01 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.700 _refine_diff_density_min -0.807 _refine_diff_density_rms 0.076 data_diprtb _database_code_CSD 215595 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H71 N O4' _chemical_formula_weight 774.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 19.892(5) _cell_length_b 19.296(5) _cell_length_c 12.102(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.690(5) _cell_angle_gamma 90.000(5) _cell_volume 4645(3) _cell_formula_units_Z 4 _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 1.107 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 0.526 _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 1.54178 _diffrn_radiation_type CuK\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 9056 _diffrn_reflns_av_R_equivalents 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 70.35 _reflns_number_total 8620 _reflns_number_gt 7380 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8620 _refine_ls_number_parameters 551 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0505 _refine_ls_wR_factor_ref 0.1818 _refine_ls_wR_factor_gt 0.1735 _refine_ls_goodness_of_fit_ref 1.472 _refine_ls_restrained_S_all 1.472 _refine_ls_shift/su_max 2.706 _refine_ls_shift/su_mean 0.076 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 O1A O 0.59108(6) 0.01895(6) 0.59999(10) 0.0343(3) Uani 1 1 d . . . C1A C 0.64556(8) 0.05576(8) 0.56423(13) 0.0279(3) Uani 1 1 d . . . C2A C 0.70976(8) 0.03463(8) 0.59905(13) 0.0284(3) Uani 1 1 d . . . C3A C 0.76585(8) 0.07059(8) 0.56164(13) 0.0299(3) Uani 1 1 d . . . H3A H 0.8097 0.0559 0.5860 0.0318(17) Uiso 1 1 calc R . . C4A C 0.76067(8) 0.12700(8) 0.49020(14) 0.0312(3) Uani 1 1 d . . . C5A C 0.69571(8) 0.14565(8) 0.45526(13) 0.0312(3) Uani 1 1 d . . . H5A H 0.6906 0.1836 0.4046 0.0318(17) Uiso 1 1 calc R . . C6A C 0.63855(8) 0.11161(8) 0.49066(13) 0.0290(3) Uani 1 1 d . . . C7A C 0.82223(9) 0.16603(9) 0.44673(15) 0.0377(4) Uani 1 1 d . . . C8A C 0.81098(10) 0.24435(10) 0.44866(19) 0.0471(5) Uani 1 1 d . . . H8A1 H 0.8001 0.2587 0.5223 0.0762(13) Uiso 1 1 calc R . . H8A2 H 0.7746 0.2561 0.3993 0.0762(13) Uiso 1 1 calc R . . H8A3 H 0.8512 0.2675 0.4256 0.0762(13) Uiso 1 1 calc R . . C9A C 0.83334(13) 0.14288(13) 0.3270(2) 0.0608(6) Uani 1 1 d . . . H9A1 H 0.8718 0.1664 0.2979 0.0762(13) Uiso 1 1 calc R . . H9A2 H 0.7943 0.1540 0.2831 0.0762(13) Uiso 1 1 calc R . . H9A3 H 0.8409 0.0938 0.3252 0.0762(13) Uiso 1 1 calc R . . C10A C 0.88506(10) 0.15084(13) 0.5150(2) 0.0612(6) Uani 1 1 d . . . H10A H 0.9219 0.1778 0.4876 0.0762(13) Uiso 1 1 calc R . . H10B H 0.8957 0.1024 0.5098 0.0762(13) Uiso 1 1 calc R . . H10C H 0.8773 0.1627 0.5908 0.0762(13) Uiso 1 1 calc R . . C20A C 0.71874(8) -0.02498(8) 0.68042(14) 0.0301(3) Uani 1 1 d . . . H20A H 0.6797 -0.0542 0.6776 0.0409(14) Uiso 1 1 calc R . . H20B H 0.7568 -0.0524 0.6594 0.0409(14) Uiso 1 1 calc R . . O1B O 0.61330(5) -0.01875(6) 0.84276(10) 0.0333(3) Uani 1 1 d . . . C1B C 0.67704(7) 0.00544(7) 0.87293(14) 0.0277(3) Uani 1 1 d . . . C2B C 0.68590(8) 0.03636(7) 0.97620(13) 0.0276(3) Uani 1 1 d . . . C3B C 0.75006(8) 0.05940(8) 1.00646(14) 0.0283(3) Uani 1 1 d . . . H3B H 0.7568 0.0792 1.0785 0.0318(17) Uiso 1 1 calc R . . C4B C 0.80456(8) 0.05465(7) 0.93571(13) 0.0280(3) Uani 1 1 d . . . C5B C 0.79266(8) 0.02627(7) 0.83135(14) 0.0279(3) Uani 1 1 d . . . H5B H 0.8292 0.0237 0.7803 0.0318(17) Uiso 1 1 calc R . . C6B C 0.72929(8) 0.00137(7) 0.79813(13) 0.0276(3) Uani 1 1 d . . . C7B C 0.87390(8) 0.08059(8) 0.97449(14) 0.0325(4) Uani 1 1 d . . . C8B C 0.86858(9) 0.15656(9) 1.01185(17) 0.0413(4) Uani 1 1 d . . . H8B1 H 0.8516 0.1843 0.9519 0.0762(13) Uiso 1 1 calc R . . H8B2 H 0.9123 0.1731 1.0338 0.0762(13) Uiso 1 1 calc R . . H8B3 H 0.8386 0.1597 1.0732 0.0762(13) Uiso 1 1 calc R . . C9B C 0.89888(9) 0.03585(10) 1.07210(17) 0.0429(4) Uani 1 1 d . . . H9B1 H 0.8668 0.0378 1.1307 0.0762(13) Uiso 1 1 calc R . . H9B2 H 0.9414 0.0531 1.0983 0.0762(13) Uiso 1 1 calc R . . H9B3 H 0.9039 -0.0113 1.0482 0.0762(13) Uiso 1 1 calc R . . C10B C 0.92603(9) 0.07660(10) 0.88241(16) 0.0425(4) Uani 1 1 d . . . H10D H 0.9318 0.0292 0.8604 0.0762(13) Uiso 1 1 calc R . . H10E H 0.9682 0.0947 0.9090 0.0762(13) Uiso 1 1 calc R . . H10F H 0.9108 0.1034 0.8202 0.0762(13) Uiso 1 1 calc R . . C11B C 0.60428(9) -0.09204(8) 0.86027(16) 0.0364(4) Uani 1 1 d . . . H11A H 0.5927 -0.1005 0.9358 0.0409(14) Uiso 1 1 calc R . . H11B H 0.6454 -0.1161 0.8452 0.0409(14) Uiso 1 1 calc R . . C12B C 0.54906(9) -0.11820(9) 0.78474(18) 0.0431(4) Uani 1 1 d . . . H12A H 0.5591 -0.1060 0.7098 0.0409(14) Uiso 1 1 calc R . . H12B H 0.5074 -0.0964 0.8038 0.0409(14) Uiso 1 1 calc R . . C13B C 0.54160(11) -0.19610(10) 0.79361(19) 0.0476(5) Uani 1 1 d . . . H13A H 0.5838 -0.2179 0.7777 0.0762(13) Uiso 1 1 calc R . . H13B H 0.5081 -0.2117 0.7416 0.0762(13) Uiso 1 1 calc R . . H13C H 0.5282 -0.2081 0.8671 0.0762(13) Uiso 1 1 calc R . . C20B C 0.62655(8) 0.05233(8) 1.04994(14) 0.0299(3) Uani 1 1 d . . . H20C H 0.5918 0.0185 1.0386 0.0409(14) Uiso 1 1 calc R . . H20D H 0.6404 0.0508 1.1261 0.0409(14) Uiso 1 1 calc R . . O1C O 0.51606(6) 0.07967(6) 0.89321(11) 0.0346(3) Uani 1 1 d . . . C1C C 0.54900(7) 0.13443(8) 0.94178(13) 0.0276(3) Uani 1 1 d . . . C2C C 0.52901(7) 0.20170(8) 0.91229(13) 0.0270(3) Uani 1 1 d . . . C3C C 0.56103(8) 0.25745(8) 0.96307(14) 0.0297(3) Uani 1 1 d . . . H3C H 0.5474 0.3035 0.9427 0.0318(17) Uiso 1 1 calc R . . C4C C 0.61221(8) 0.24968(8) 1.04259(14) 0.0309(4) Uani 1 1 d . . . C5C C 0.63030(8) 0.18207(8) 1.07027(14) 0.0298(3) Uani 1 1 d . . . H5C H 0.6649 0.1749 1.1251 0.0318(17) Uiso 1 1 calc R . . C6C C 0.60000(7) 0.12434(8) 1.02129(13) 0.0278(3) Uani 1 1 d . . . C7C C 0.64642(9) 0.31372(9) 1.09280(16) 0.0382(4) Uani 1 1 d . . . C8C C 0.59282(11) 0.36191(10) 1.14095(19) 0.0498(5) Uani 1 1 d . . . H8C1 H 0.5642 0.3787 1.0824 0.0762(13) Uiso 1 1 calc R . . H8C2 H 0.6144 0.4004 1.1771 0.0762(13) Uiso 1 1 calc R . . H8C3 H 0.5664 0.3368 1.1934 0.0762(13) Uiso 1 1 calc R . . C9C C 0.68498(11) 0.35200(10) 1.00265(19) 0.0513(5) Uani 1 1 d . . . H9C1 H 0.6541 0.3668 0.9458 0.0762(13) Uiso 1 1 calc R . . H9C2 H 0.7178 0.3215 0.9715 0.0762(13) Uiso 1 1 calc R . . H9C3 H 0.7071 0.3917 1.0342 0.0762(13) Uiso 1 1 calc R . . C10C C 0.69613(13) 0.29498(11) 1.1855(2) 0.0601(6) Uani 1 1 d . . . H10G H 0.7145 0.3366 1.2170 0.0762(13) Uiso 1 1 calc R . . H10H H 0.7318 0.2673 1.1561 0.0762(13) Uiso 1 1 calc R . . H10I H 0.6733 0.2693 1.2416 0.0762(13) Uiso 1 1 calc R . . C20C C 0.47526(7) 0.21396(8) 0.82380(13) 0.0298(3) Uani 1 1 d . . . H20E H 0.4481 0.1731 0.8161 0.0409(14) Uiso 1 1 calc R . . H20F H 0.4466 0.2512 0.8465 0.0409(14) Uiso 1 1 calc R . . O1D O 0.49161(5) 0.11438(5) 0.64730(10) 0.0319(3) Uani 1 1 d . . . C1D C 0.51493(7) 0.18162(8) 0.63124(14) 0.0280(3) Uani 1 1 d . . . C2D C 0.54970(7) 0.19645(8) 0.53478(14) 0.0294(3) Uani 1 1 d . . . C3D C 0.57266(8) 0.26391(8) 0.51844(14) 0.0318(4) Uani 1 1 d . . . H3D H 0.5963 0.2746 0.4519 0.0318(17) Uiso 1 1 calc R . . C4D C 0.56239(8) 0.31627(8) 0.59592(15) 0.0328(4) Uani 1 1 d . . . C5D C 0.52966(8) 0.29844(8) 0.69242(14) 0.0307(3) Uani 1 1 d . . . H5D H 0.5230 0.3336 0.7474 0.0318(17) Uiso 1 1 calc R . . C6D C 0.50594(7) 0.23164(8) 0.71300(13) 0.0277(3) Uani 1 1 d . . . C7D C 0.58992(10) 0.38983(9) 0.57654(17) 0.0427(4) Uani 1 1 d . . . C8D C 0.57394(16) 0.41350(13) 0.4580(2) 0.0732(8) Uani 1 1 d . . . H8D1 H 0.5858 0.4614 0.4499 0.0762(13) Uiso 1 1 calc R . . H8D2 H 0.5268 0.4077 0.4429 0.0762(13) Uiso 1 1 calc R . . H8D3 H 0.5993 0.3861 0.4069 0.0762(13) Uiso 1 1 calc R . . C9D C 0.55445(18) 0.44307(12) 0.6476(3) 0.0884(10) Uani 1 1 d . . . H9D1 H 0.5664 0.4358 0.7238 0.0762(13) Uiso 1 1 calc R . . H9D2 H 0.5067 0.4383 0.6382 0.0762(13) Uiso 1 1 calc R . . H9D3 H 0.5678 0.4888 0.6257 0.0762(13) Uiso 1 1 calc R . . C10D C 0.66354(15) 0.38971(16) 0.5948(5) 0.142(2) Uani 1 1 d . . . H10J H 0.6733 0.3828 0.6718 0.0762(13) Uiso 1 1 calc R . . H10K H 0.6818 0.4333 0.5715 0.0762(13) Uiso 1 1 calc R . . H10L H 0.6833 0.3529 0.5527 0.0762(13) Uiso 1 1 calc R . . C11D C 0.42007(8) 0.10664(8) 0.62525(15) 0.0333(4) Uani 1 1 d . . . H11C H 0.4121 0.1010 0.5474 0.0409(14) Uiso 1 1 calc R . . H11D H 0.3965 0.1472 0.6493 0.0409(14) Uiso 1 1 calc R . . C12D C 0.39551(9) 0.04399(9) 0.68665(17) 0.0396(4) Uani 1 1 d . . . H12C H 0.4099 0.0467 0.7625 0.0409(14) Uiso 1 1 calc R . . H12D H 0.4146 0.0029 0.6551 0.0409(14) Uiso 1 1 calc R . . C13D C 0.31895(9) 0.03952(11) 0.68066(18) 0.0471(5) Uani 1 1 d . . . H13D H 0.2999 0.0780 0.7196 0.0762(13) Uiso 1 1 calc R . . H13E H 0.3044 -0.0030 0.7138 0.0762(13) Uiso 1 1 calc R . . H13F H 0.3044 0.0408 0.6048 0.0762(13) Uiso 1 1 calc R . . C20D C 0.56971(8) 0.13929(9) 0.45552(14) 0.0316(3) Uani 1 1 d . . . H20G H 0.5716 0.1571 0.3816 0.0409(14) Uiso 1 1 calc R . . H20H H 0.5371 0.1026 0.4570 0.0409(14) Uiso 1 1 calc R . . C1G C 0.69178(11) 0.19550(12) 0.7657(2) 0.0463(5) Uani 1 1 d . . . C2G C 0.75474(10) 0.23238(12) 0.76362(18) 0.0500(5) Uani 1 1 d . . . N3G N 0.80437(12) 0.26207(17) 0.7622(2) 0.0929(9) Uani 1 1 d . . . H1C H 0.5409(14) 0.0487(14) 0.878(2) 0.068(8) Uiso 1 1 d . . . H1A H 0.5573(13) 0.0503(13) 0.613(2) 0.065(7) Uiso 1 1 d . . . H1G H 0.671(2) 0.207(2) 0.824(4) 0.134(16) Uiso 1 1 d . . . H2G H 0.667(3) 0.209(3) 0.707(5) 0.17(2) Uiso 1 1 d . . . H3G H 0.701(3) 0.146(3) 0.764(4) 0.155(18) 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 O1A 0.0264(6) 0.0296(6) 0.0469(7) 0.0020(5) 0.0001(5) 0.0008(4) C1A 0.0272(7) 0.0255(7) 0.0310(8) -0.0048(6) 0.0004(6) 0.0011(6) C2A 0.0315(8) 0.0253(7) 0.0283(8) -0.0029(6) -0.0013(6) 0.0038(6) C3A 0.0249(7) 0.0318(8) 0.0330(8) -0.0022(6) -0.0021(6) 0.0051(6) C4A 0.0271(8) 0.0323(8) 0.0341(9) -0.0007(6) 0.0022(6) 0.0032(6) C5A 0.0324(8) 0.0310(8) 0.0302(8) 0.0035(6) 0.0001(6) 0.0061(6) C6A 0.0269(7) 0.0304(8) 0.0295(8) -0.0048(6) -0.0021(6) 0.0059(6) C7A 0.0313(8) 0.0409(9) 0.0411(10) 0.0048(7) 0.0063(7) -0.0004(7) C8A 0.0410(10) 0.0406(10) 0.0597(12) 0.0025(9) 0.0040(9) -0.0064(8) C9A 0.0646(14) 0.0607(13) 0.0578(14) -0.0029(11) 0.0281(11) -0.0080(11) C10A 0.0280(9) 0.0700(14) 0.0857(17) 0.0271(13) -0.0011(10) -0.0054(9) C20A 0.0310(8) 0.0237(7) 0.0355(9) -0.0010(6) -0.0022(6) 0.0035(6) O1B 0.0255(5) 0.0249(5) 0.0492(7) 0.0024(5) -0.0066(5) -0.0020(4) C1B 0.0236(7) 0.0202(7) 0.0392(9) 0.0042(6) -0.0047(6) 0.0003(5) C2B 0.0269(7) 0.0203(7) 0.0356(8) 0.0054(6) 0.0005(6) 0.0013(5) C3B 0.0277(7) 0.0247(7) 0.0324(8) 0.0021(6) -0.0018(6) 0.0008(6) C4B 0.0261(7) 0.0227(7) 0.0353(8) 0.0040(6) -0.0025(6) -0.0004(6) C5B 0.0241(7) 0.0237(7) 0.0359(8) 0.0040(6) -0.0008(6) 0.0020(6) C6B 0.0301(8) 0.0199(7) 0.0325(8) 0.0022(6) -0.0041(6) 0.0032(5) C7B 0.0265(7) 0.0316(8) 0.0393(9) 0.0020(7) -0.0035(6) -0.0045(6) C8B 0.0395(9) 0.0339(9) 0.0504(11) -0.0023(8) -0.0017(8) -0.0090(7) C9B 0.0352(9) 0.0444(10) 0.0488(11) 0.0069(8) -0.0120(8) -0.0032(7) C10B 0.0270(8) 0.0489(10) 0.0516(11) -0.0027(8) 0.0011(7) -0.0094(7) C11B 0.0343(8) 0.0260(8) 0.0488(10) 0.0037(7) -0.0029(7) -0.0030(6) C12B 0.0373(9) 0.0376(9) 0.0543(11) 0.0051(8) -0.0061(8) -0.0078(7) C13B 0.0469(11) 0.0364(10) 0.0595(13) -0.0015(8) -0.0012(9) -0.0100(8) C20B 0.0283(7) 0.0259(8) 0.0355(9) 0.0043(6) 0.0027(6) 0.0003(6) O1C 0.0274(6) 0.0262(6) 0.0500(7) -0.0024(5) -0.0056(5) -0.0012(5) C1C 0.0217(7) 0.0251(7) 0.0362(8) -0.0008(6) 0.0037(6) -0.0014(6) C2C 0.0213(7) 0.0289(8) 0.0310(8) -0.0015(6) 0.0031(6) 0.0013(6) C3C 0.0295(8) 0.0240(7) 0.0355(9) 0.0012(6) 0.0026(6) 0.0039(6) C4C 0.0300(8) 0.0268(8) 0.0359(9) -0.0030(6) 0.0006(6) -0.0002(6) C5C 0.0273(7) 0.0288(8) 0.0332(8) 0.0000(6) -0.0016(6) 0.0007(6) C6C 0.0242(7) 0.0258(7) 0.0333(8) 0.0021(6) 0.0050(6) 0.0018(6) C7C 0.0415(9) 0.0273(8) 0.0455(10) -0.0048(7) -0.0067(8) -0.0013(7) C8C 0.0553(12) 0.0371(10) 0.0569(12) -0.0161(9) 0.0030(9) -0.0021(8) C9C 0.0515(12) 0.0383(10) 0.0641(14) -0.0066(9) 0.0051(10) -0.0160(9) C10C 0.0690(14) 0.0394(11) 0.0712(15) -0.0102(10) -0.0323(12) -0.0039(10) C20C 0.0223(7) 0.0306(8) 0.0366(9) -0.0003(6) 0.0007(6) 0.0028(6) O1D 0.0235(5) 0.0249(5) 0.0475(7) 0.0022(5) -0.0020(5) 0.0003(4) C1D 0.0220(7) 0.0236(7) 0.0382(9) 0.0024(6) -0.0042(6) 0.0027(5) C2D 0.0232(7) 0.0303(8) 0.0347(9) 0.0006(6) -0.0039(6) 0.0040(6) C3D 0.0261(7) 0.0315(8) 0.0379(9) 0.0048(7) 0.0016(6) 0.0026(6) C4D 0.0272(8) 0.0284(8) 0.0427(9) 0.0045(7) -0.0030(6) 0.0005(6) C5D 0.0257(7) 0.0275(8) 0.0388(9) -0.0026(6) -0.0027(6) 0.0017(6) C6D 0.0205(7) 0.0282(7) 0.0344(8) 0.0023(6) -0.0028(6) 0.0038(5) C7D 0.0413(10) 0.0294(9) 0.0575(12) 0.0061(8) 0.0003(8) -0.0089(7) C8D 0.102(2) 0.0461(12) 0.0716(16) 0.0183(12) -0.0003(15) -0.0178(13) C9D 0.128(3) 0.0313(11) 0.106(2) -0.0015(13) 0.038(2) -0.0171(13) C10D 0.0567(17) 0.0623(18) 0.305(7) 0.070(3) -0.063(3) -0.0294(14) C11D 0.0253(8) 0.0326(8) 0.0420(9) -0.0006(7) -0.0049(6) -0.0009(6) C12D 0.0329(9) 0.0345(9) 0.0513(11) 0.0046(8) -0.0074(7) -0.0048(7) C13D 0.0327(9) 0.0508(11) 0.0578(12) -0.0008(9) -0.0044(8) -0.0090(8) C20D 0.0291(8) 0.0341(8) 0.0313(8) -0.0016(6) -0.0035(6) 0.0059(6) C1G 0.0391(10) 0.0450(11) 0.0549(13) -0.0057(9) 0.0043(9) -0.0013(8) C2G 0.0398(10) 0.0621(13) 0.0481(12) 0.0083(9) -0.0015(8) -0.0025(9) N3G 0.0562(13) 0.134(2) 0.0880(18) 0.0248(16) -0.0073(12) -0.0355(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1A C1A 1.3702(19) . ? O1A H1A 0.92(3) . ? C1A C2A 1.401(2) . ? C1A C6A 1.404(2) . ? C2A C3A 1.394(2) . ? C2A C20A 1.523(2) . ? C3A C4A 1.393(2) . ? C3A H3A 0.9600 . ? C4A C5A 1.402(2) . ? C4A C7A 1.536(2) . ? C5A C6A 1.385(2) . ? C5A H5A 0.9600 . ? C6A C20D 1.525(2) . ? C7A C10A 1.519(3) . ? C7A C8A 1.528(3) . ? C7A C9A 1.534(3) . ? C8A H8A1 0.9599 . ? C8A H8A2 0.9599 . ? C8A H8A3 0.9599 . ? C9A H9A1 0.9599 . ? C9A H9A2 0.9599 . ? C9A H9A3 0.9599 . ? C10A H10A 0.9599 . ? C10A H10B 0.9599 . ? C10A H10C 0.9599 . ? C20A C6B 1.525(2) . ? C20A H20A 0.9600 . ? C20A H20B 0.9600 . ? O1B C1B 1.3955(18) . ? O1B C11B 1.4414(19) . ? C1B C6B 1.389(2) . ? C1B C2B 1.394(2) . ? C2B C3B 1.396(2) . ? C2B C20B 1.520(2) . ? C3B C4B 1.393(2) . ? C3B H3B 0.9600 . ? C4B C5B 1.394(2) . ? C4B C7B 1.535(2) . ? C5B C6B 1.403(2) . ? C5B H5B 0.9600 . ? C7B C8B 1.538(2) . ? C7B C9B 1.541(2) . ? C7B C10B 1.533(2) . ? C8B H8B1 0.9599 . ? C8B H8B2 0.9599 . ? C8B H8B3 0.9599 . ? C9B H9B1 0.9599 . ? C9B H9B2 0.9599 . ? C9B H9B3 0.9599 . ? C10B H10D 0.9599 . ? C10B H10E 0.9599 . ? C10B H10F 0.9599 . ? C11B C12B 1.507(2) . ? C11B H11A 0.9600 . ? C11B H11B 0.9600 . ? C12B C13B 1.514(2) . ? C12B H12A 0.9600 . ? C12B H12B 0.9600 . ? C13B H13A 0.9599 . ? C13B H13B 0.9599 . ? C13B H13C 0.9599 . ? C20B C6C 1.525(2) . ? C20B H20C 0.9600 . ? C20B H20D 0.9600 . ? O1C C1C 1.3719(19) . ? O1C H1C 0.80(3) . ? C1C C6C 1.403(2) . ? C1C C2C 1.402(2) . ? C2C C3C 1.390(2) . ? C2C C20C 1.523(2) . ? C3C C4C 1.401(2) . ? C3C H3C 0.9600 . ? C4C C5C 1.393(2) . ? C4C C7C 1.533(2) . ? C5C C6C 1.395(2) . ? C5C H5C 0.9600 . ? C7C C8C 1.535(3) . ? C7C C9C 1.531(3) . ? C7C C10C 1.530(3) . ? C8C H8C1 0.9599 . ? C8C H8C2 0.9599 . ? C8C H8C3 0.9599 . ? C9C H9C1 0.9599 . ? C9C H9C2 0.9599 . ? C9C H9C3 0.9599 . ? C10C H10G 0.9599 . ? C10C H10H 0.9599 . ? C10C H10I 0.9599 . ? C20C C6D 1.519(2) . ? C20C H20E 0.9600 . ? C20C H20F 0.9600 . ? O1D C1D 1.3923(18) . ? O1D C11D 1.4524(18) . ? C1D C6D 1.395(2) . ? C1D C2D 1.394(2) . ? C2D C3D 1.394(2) . ? C2D C20D 1.518(2) . ? C3D C4D 1.395(2) . ? C3D H3D 0.9600 . ? C4D C5D 1.387(2) . ? C4D C7D 1.540(2) . ? C5D C6D 1.396(2) . ? C5D H5D 0.9600 . ? C7D C10D 1.478(3) . ? C7D C8D 1.536(3) . ? C7D C9D 1.519(3) . ? C8D H8D1 0.9599 . ? C8D H8D2 0.9599 . ? C8D H8D3 0.9599 . ? C9D H9D1 0.9599 . ? C9D H9D2 0.9599 . ? C9D H9D3 0.9599 . ? C10D H10J 0.9599 . ? C10D H10K 0.9599 . ? C10D H10L 0.9599 . ? C11D C12D 1.504(2) . ? C11D H11C 0.9600 . ? C11D H11D 0.9600 . ? C12D C13D 1.526(2) . ? C12D H12C 0.9600 . ? C12D H12D 0.9600 . ? C13D H13D 0.9599 . ? C13D H13E 0.9599 . ? C13D H13F 0.9599 . ? C20D H20G 0.9600 . ? C20D H20H 0.9600 . ? C1G C2G 1.441(3) . ? C1G H1G 0.85(5) . ? C1G H2G 0.89(6) . ? C1G H3G 0.96(5) . ? C2G N3G 1.142(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 C1A O1A H1A 107.1(16) . . ? O1A C1A C2A 118.41(14) . . ? O1A C1A C6A 121.69(14) . . ? C2A C1A C6A 119.84(14) . . ? C3A C2A C1A 119.20(15) . . ? C3A C2A C20A 119.84(14) . . ? C1A C2A C20A 120.92(14) . . ? C2A C3A C4A 122.47(14) . . ? C2A C3A H3A 118.8 . . ? C4A C3A H3A 118.8 . . ? C3A C4A C5A 116.67(15) . . ? C3A C4A C7A 122.84(14) . . ? C5A C4A C7A 120.44(15) . . ? C6A C5A C4A 122.82(15) . . ? C6A C5A H5A 118.6 . . ? C4A C5A H5A 118.6 . . ? C5A C6A C1A 118.98(14) . . ? C5A C6A C20D 119.01(14) . . ? C1A C6A C20D 121.85(14) . . ? C10A C7A C8A 107.59(17) . . ? C10A C7A C4A 111.92(15) . . ? C8A C7A C4A 111.24(14) . . ? C10A C7A C9A 109.30(18) . . ? C8A C7A C9A 108.97(17) . . ? C4A C7A C9A 107.77(16) . . ? C7A C8A H8A1 109.5 . . ? C7A C8A H8A2 109.5 . . ? H8A1 C8A H8A2 109.5 . . ? C7A C8A H8A3 109.5 . . ? H8A1 C8A H8A3 109.5 . . ? H8A2 C8A H8A3 109.5 . . ? C7A C9A H9A1 109.5 . . ? C7A C9A H9A2 109.5 . . ? H9A1 C9A H9A2 109.5 . . ? C7A C9A H9A3 109.5 . . ? H9A1 C9A H9A3 109.5 . . ? H9A2 C9A H9A3 109.5 . . ? C7A C10A H10A 109.5 . . ? C7A C10A H10B 109.5 . . ? H10A C10A H10B 109.5 . . ? C7A C10A H10C 109.5 . . ? H10A C10A H10C 109.5 . . ? H10B C10A H10C 109.5 . . ? C6B C20A C2A 111.47(12) . . ? C6B C20A H20A 109.3 . . ? C2A C20A H20A 109.3 . . ? C6B C20A H20B 109.3 . . ? C2A C20A H20B 109.3 . . ? H20A C20A H20B 108.0 . . ? C1B O1B C11B 113.83(12) . . ? C6B C1B C2B 121.40(14) . . ? C6B C1B O1B 119.69(15) . . ? C2B C1B O1B 118.84(14) . . ? C1B C2B C3B 118.47(14) . . ? C1B C2B C20B 121.49(14) . . ? C3B C2B C20B 119.70(15) . . ? C2B C3B C4B 122.27(15) . . ? C2B C3B H3B 118.9 . . ? C4B C3B H3B 118.9 . . ? C5B C4B C3B 117.24(14) . . ? C5B C4B C7B 123.17(14) . . ? C3B C4B C7B 119.59(15) . . ? C4B C5B C6B 122.42(15) . . ? C4B C5B H5B 118.8 . . ? C6B C5B H5B 118.8 . . ? C1B C6B C5B 118.08(15) . . ? C1B C6B C20A 122.16(14) . . ? C5B C6B C20A 119.66(14) . . ? C4B C7B C8B 109.62(13) . . ? C4B C7B C9B 109.38(13) . . ? C8B C7B C9B 109.35(15) . . ? C4B C7B C10B 111.98(14) . . ? C8B C7B C10B 108.12(14) . . ? C9B C7B C10B 108.33(15) . . ? C7B C8B H8B1 109.5 . . ? C7B C8B H8B2 109.5 . . ? H8B1 C8B H8B2 109.5 . . ? C7B C8B H8B3 109.5 . . ? H8B1 C8B H8B3 109.5 . . ? H8B2 C8B H8B3 109.5 . . ? C7B C9B H9B1 109.5 . . ? C7B C9B H9B2 109.5 . . ? H9B1 C9B H9B2 109.5 . . ? C7B C9B H9B3 109.5 . . ? H9B1 C9B H9B3 109.5 . . ? H9B2 C9B H9B3 109.5 . . ? C7B C10B H10D 109.5 . . ? C7B C10B H10E 109.5 . . ? H10D C10B H10E 109.5 . . ? C7B C10B H10F 109.5 . . ? H10D C10B H10F 109.5 . . ? H10E C10B H10F 109.5 . . ? O1B C11B C12B 109.30(14) . . ? O1B C11B H11A 109.8 . . ? C12B C11B H11A 109.8 . . ? O1B C11B H11B 109.8 . . ? C12B C11B H11B 109.8 . . ? H11A C11B H11B 108.3 . . ? C11B C12B C13B 111.15(16) . . ? C11B C12B H12A 109.4 . . ? C13B C12B H12A 109.4 . . ? C11B C12B H12B 109.4 . . ? C13B C12B H12B 109.4 . . ? H12A C12B H12B 108.0 . . ? C12B C13B H13A 109.5 . . ? C12B C13B H13B 109.5 . . ? H13A C13B H13B 109.5 . . ? C12B C13B H13C 109.5 . . ? H13A C13B H13C 109.5 . . ? H13B C13B H13C 109.5 . . ? C6C C20B C2B 108.70(12) . . ? C6C C20B H20C 110.0 . . ? C2B C20B H20C 109.9 . . ? C6C C20B H20D 110.0 . . ? C2B C20B H20D 110.0 . . ? H20C C20B H20D 108.3 . . ? C1C O1C H1C 113(2) . . ? O1C C1C C6C 121.63(14) . . ? O1C C1C C2C 118.12(14) . . ? C6C C1C C2C 120.22(14) . . ? C3C C2C C1C 118.48(14) . . ? C3C C2C C20C 120.33(14) . . ? C1C C2C C20C 121.15(14) . . ? C2C C3C C4C 123.13(14) . . ? C2C C3C H3C 118.4 . . ? C4C C3C H3C 118.4 . . ? C3C C4C C5C 116.68(14) . . ? C3C C4C C7C 120.12(14) . . ? C5C C4C C7C 123.19(15) . . ? C4C C5C C6C 122.44(15) . . ? C4C C5C H5C 118.8 . . ? C6C C5C H5C 118.8 . . ? C1C C6C C5C 119.05(14) . . ? C1C C6C C20B 121.86(14) . . ? C5C C6C C20B 118.96(14) . . ? C8C C7C C4C 109.38(15) . . ? C8C C7C C9C 109.54(16) . . ? C4C C7C C9C 109.29(15) . . ? C8C C7C C10C 108.09(17) . . ? C4C C7C C10C 112.35(15) . . ? C9C C7C C10C 108.15(18) . . ? C7C C8C H8C1 109.5 . . ? C7C C8C H8C2 109.5 . . ? H8C1 C8C H8C2 109.5 . . ? C7C C8C H8C3 109.5 . . ? H8C1 C8C H8C3 109.5 . . ? H8C2 C8C H8C3 109.5 . . ? C7C C9C H9C1 109.5 . . ? C7C C9C H9C2 109.5 . . ? H9C1 C9C H9C2 109.5 . . ? C7C C9C H9C3 109.5 . . ? H9C1 C9C H9C3 109.5 . . ? H9C2 C9C H9C3 109.5 . . ? C7C C10C H10G 109.5 . . ? C7C C10C H10H 109.5 . . ? H10G C10C H10H 109.5 . . ? C7C C10C H10I 109.5 . . ? H10G C10C H10I 109.5 . . ? H10H C10C H10I 109.5 . . ? C6D C20C C2C 111.69(12) . . ? C6D C20C H20E 109.3 . . ? C2C C20C H20E 109.3 . . ? C6D C20C H20F 109.3 . . ? C2C C20C H20F 109.3 . . ? H20E C20C H20F 107.9 . . ? C1D O1D C11D 113.43(11) . . ? C6D C1D O1D 119.99(14) . . ? C6D C1D C2D 121.40(14) . . ? O1D C1D C2D 118.55(14) . . ? C3D C2D C1D 118.51(15) . . ? C3D C2D C20D 119.99(15) . . ? C1D C2D C20D 121.10(14) . . ? C2D C3D C4D 122.00(15) . . ? C2D C3D H3D 119.0 . . ? C4D C3D H3D 119.0 . . ? C5D C4D C3D 117.41(15) . . ? C5D C4D C7D 121.87(16) . . ? C3D C4D C7D 120.65(16) . . ? C4D C5D C6D 122.83(15) . . ? C4D C5D H5D 118.6 . . ? C6D C5D H5D 118.6 . . ? C1D C6D C5D 117.76(15) . . ? C1D C6D C20C 121.80(14) . . ? C5D C6D C20C 120.34(14) . . ? C10D C7D C4D 109.23(17) . . ? C10D C7D C8D 109.5(3) . . ? C4D C7D C8D 110.26(17) . . ? C10D C7D C9D 112.5(3) . . ? C4D C7D C9D 111.63(17) . . ? C8D C7D C9D 103.6(2) . . ? C7D C8D H8D1 109.5 . . ? C7D C8D H8D2 109.4 . . ? H8D1 C8D H8D2 109.5 . . ? C7D C8D H8D3 109.5 . . ? H8D1 C8D H8D3 109.5 . . ? H8D2 C8D H8D3 109.5 . . ? C7D C9D H9D1 109.5 . . ? C7D C9D H9D2 109.4 . . ? H9D1 C9D H9D2 109.5 . . ? C7D C9D H9D3 109.5 . . ? H9D1 C9D H9D3 109.5 . . ? H9D2 C9D H9D3 109.5 . . ? C7D C10D H10J 109.5 . . ? C7D C10D H10K 109.5 . . ? H10J C10D H10K 109.5 . . ? C7D C10D H10L 109.5 . . ? H10J C10D H10L 109.5 . . ? H10K C10D H10L 109.5 . . ? O1D C11D C12D 108.38(13) . . ? O1D C11D H11C 110.0 . . ? C12D C11D H11C 110.0 . . ? O1D C11D H11D 110.0 . . ? C12D C11D H11D 110.0 . . ? H11C C11D H11D 108.4 . . ? C11D C12D C13D 110.60(15) . . ? C11D C12D H12C 109.5 . . ? C13D C12D H12C 109.5 . . ? C11D C12D H12D 109.5 . . ? C13D C12D H12D 109.5 . . ? H12C C12D H12D 108.1 . . ? C12D C13D H13D 109.5 . . ? C12D C13D H13E 109.5 . . ? H13D C13D H13E 109.5 . . ? C12D C13D H13F 109.5 . . ? H13D C13D H13F 109.5 . . ? H13E C13D H13F 109.5 . . ? C2D C20D C6A 108.64(13) . . ? C2D C20D H20G 110.0 . . ? C6A C20D H20G 110.0 . . ? C2D C20D H20H 110.0 . . ? C6A C20D H20H 110.0 . . ? H20G C20D H20H 108.3 . . ? C2G C1G H1G 108(3) . . ? C2G C1G H2G 108(3) . . ? H1G C1G H2G 108(4) . . ? C2G C1G H3G 109(3) . . ? H1G C1G H3G 112(4) . . ? H2G C1G H3G 111(4) . . ? N3G C2G C1G 179.5(3) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 70.35 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.570 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.049