# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Pavel Lhotak' _publ_contact_author_address ; Department of Organic Chemistry Prague Institute of Chemical Technology Technicka 5 Prague 6 166 28 CZECH REPUBLIC ; _publ_contact_author_email LHOTAKP@VSCHT.CZ _publ_section_title ; Simple synthesis of calix[4]arenes in a 1,2-alternate conformation ; loop_ _publ_author_name 'Pavel Lhotak' 'Alexandra Bila' 'Jan Budka' 'Michaela Pojarova' 'Ivan Stibor' data_final _database_code_depnum_ccdc_archive 'CCDC 666975' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H80 O4' _chemical_formula_weight 817.20 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' O O 0.0492 0.0322 '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 9.771(4) _cell_length_b 13.056(5) _cell_length_c 20.194(10) _cell_angle_alpha 79.31(4) _cell_angle_beta 80.22(5) _cell_angle_gamma 84.12(5) _cell_volume 2488.0(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 12782 _cell_measurement_theta_min 4.4125 _cell_measurement_theta_max 76.5794 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.767 _exptl_absorpt_correction_T_max 0.902 _exptl_absorpt_process_details 'Analytical Abs.(De Meulenaer & Tompa, 1965)' _exptl_special_details ; Analytical Abs. (De Meulenaer & Tompa, 1965) ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _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 38941 _diffrn_reflns_av_R_equivalents 0.1974 _diffrn_reflns_av_sigmaI/netI 0.1010 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 4.44 _diffrn_reflns_theta_max 77.92 _reflns_number_total 9889 _reflns_number_gt 7270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Xcalibur, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _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. The number of restraints is 63. They were used for modelling of disordered parts of calixarene as propoxy chains. The alkyl groups can rotate around single bonds and can be placed in different possible positions. The distances between the atoms and angles between atoms were fixed with these restratins as well as the thermal parameters of each part. ; _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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0119(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9889 _refine_ls_number_parameters 615 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.1294 _refine_ls_R_factor_gt 0.1125 _refine_ls_wR_factor_ref 0.3463 _refine_ls_wR_factor_gt 0.3084 _refine_ls_goodness_of_fit_ref 1.364 _refine_ls_restrained_S_all 1.364 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.0491(5) 0.6435(3) 0.1434(2) 0.0437(5) Uani 0.45 1 d PD A 1 C29 C -0.0338(6) 0.6190(4) 0.0955(3) 0.0503(12) Uani 0.45 1 d PD A 1 H29A H 0.0079 0.6441 0.0478 0.060 Uiso 0.45 1 calc PR A 1 H29B H -0.1304 0.6507 0.1037 0.060 Uiso 0.45 1 calc PR A 1 C30 C -0.0304(8) 0.5028(5) 0.1105(4) 0.0763(14) Uani 0.45 1 d PD A 1 H30A H -0.0566 0.4793 0.0708 0.092 Uiso 0.45 1 calc PR A 1 H30B H 0.0673 0.4759 0.1133 0.092 Uiso 0.45 1 calc PR A 1 C31 C -0.1176(10) 0.4522(6) 0.1719(5) 0.0958(19) Uani 0.45 1 d PD A 1 H31A H -0.0920 0.4724 0.2123 0.115 Uiso 0.45 1 calc PR A 1 H31B H -0.1032 0.3761 0.1752 0.115 Uiso 0.45 1 calc PR A 1 H31C H -0.2157 0.4742 0.1693 0.115 Uiso 0.45 1 calc PR A 1 O1A O 0.0641(10) 0.6426(6) 0.1425(5) 0.0437(5) Uani 0.25 1 d PD B 2 C29A C 0.0058(12) 0.5994(7) 0.0948(5) 0.0503(12) Uani 0.25 1 d PD B 2 H29C H 0.0803 0.5948 0.0553 0.060 Uiso 0.25 1 calc PR B 2 H29D H -0.0669 0.6518 0.0783 0.060 Uiso 0.25 1 calc PR B 2 C30A C -0.0562(16) 0.4984(11) 0.1117(8) 0.0763(14) Uani 0.25 1 d PD B 2 H30C H -0.1098 0.4924 0.0754 0.092 Uiso 0.25 1 calc PR B 2 H30D H 0.0196 0.4419 0.1122 0.092 Uiso 0.25 1 calc PR B 2 C31A C -0.1482(19) 0.4824(12) 0.1773(9) 0.0958(19) Uani 0.25 1 d PD B 2 H31D H -0.1064 0.5080 0.2114 0.115 Uiso 0.25 1 calc PR B 2 H31E H -0.1612 0.4077 0.1920 0.115 Uiso 0.25 1 calc PR B 2 H31F H -0.2385 0.5208 0.1726 0.115 Uiso 0.25 1 calc PR B 2 O1B O 0.0334(8) 0.6464(6) 0.1417(5) 0.0437(5) Uani 0.30 1 d PD C 3 C29B C -0.0781(9) 0.6278(6) 0.1080(4) 0.0503(12) Uani 0.30 1 d PD C 3 H29E H -0.0456 0.6360 0.0583 0.060 Uiso 0.30 1 calc PR C 3 H29F H -0.1571 0.6802 0.1160 0.060 Uiso 0.30 1 calc PR C 3 C30B C -0.1246(11) 0.5236(7) 0.1330(7) 0.0763(14) Uani 0.30 1 d PD C 3 H30E H -0.2040 0.5157 0.1102 0.092 Uiso 0.30 1 calc PR C 3 H30F H -0.1596 0.5177 0.1824 0.092 Uiso 0.30 1 calc PR C 3 C31B C -0.0149(13) 0.4325(8) 0.1224(7) 0.0958(19) Uani 0.30 1 d PD C 3 H31G H -0.0095 0.4176 0.0762 0.115 Uiso 0.30 1 calc PR C 3 H31H H -0.0414 0.3704 0.1558 0.115 Uiso 0.30 1 calc PR C 3 H31I H 0.0760 0.4516 0.1285 0.115 Uiso 0.30 1 calc PR C 3 O2 O 0.0263(4) 0.6348(2) 0.30861(15) 0.0301(4) Uani 0.45 1 d PD A 1 C32 C -0.0415(4) 0.5427(3) 0.3384(2) 0.0291(7) Uani 0.45 1 d PD A 1 H32A H -0.1358 0.5477 0.3258 0.035 Uiso 0.45 1 calc PR A 1 H32B H -0.0502 0.5321 0.3887 0.035 Uiso 0.45 1 calc PR A 1 C33 C 0.0468(5) 0.4537(4) 0.3113(3) 0.0412(8) Uani 0.45 1 d PD A 1 H33A H 0.1380 0.4475 0.3273 0.049 Uiso 0.45 1 calc PR A 1 H33B H 0.0639 0.4707 0.2609 0.049 Uiso 0.45 1 calc PR A 1 C34 C -0.0159(8) 0.3492(5) 0.3321(4) 0.0647(12) Uani 0.45 1 d PD A 1 H34A H -0.0343 0.3317 0.3819 0.078 Uiso 0.45 1 calc PR A 1 H34B H 0.0494 0.2953 0.3140 0.078 Uiso 0.45 1 calc PR A 1 H34C H -0.1033 0.3529 0.3138 0.078 Uiso 0.45 1 calc PR A 1 O2A O 0.0473(3) 0.6248(2) 0.32100(13) 0.0301(4) Uani 0.55 1 d PD D 2 C32A C -0.0066(4) 0.5259(3) 0.34840(19) 0.0291(7) Uani 0.55 1 d PD D 2 H32C H -0.1019 0.5258 0.3379 0.035 Uiso 0.55 1 calc PR D 2 H32D H -0.0111 0.5119 0.3986 0.035 Uiso 0.55 1 calc PR D 2 C33A C 0.0864(5) 0.4430(3) 0.3178(3) 0.0412(8) Uani 0.55 1 d PD D 2 H33C H 0.1793 0.4387 0.3319 0.049 Uiso 0.55 1 calc PR D 2 H33D H 0.0982 0.4607 0.2674 0.049 Uiso 0.55 1 calc PR D 2 C34A C 0.0220(7) 0.3378(4) 0.3417(4) 0.0647(12) Uani 0.55 1 d PD D 2 H34D H -0.0074 0.3276 0.3912 0.078 Uiso 0.55 1 calc PR D 2 H34E H 0.0910 0.2814 0.3302 0.078 Uiso 0.55 1 calc PR D 2 H34F H -0.0590 0.3372 0.3191 0.078 Uiso 0.55 1 calc PR D 2 O3 O 0.2594(3) 0.7513(2) 0.31472(16) 0.0322(4) Uani 0.50 1 d PD A 1 C35 C 0.2798(4) 0.8422(3) 0.3401(2) 0.0297(7) Uani 0.50 1 d PD A 1 H35A H 0.3806 0.8497 0.3371 0.036 Uiso 0.50 1 calc PR A 1 H35B H 0.2363 0.8368 0.3885 0.036 Uiso 0.50 1 calc PR A 1 C36 C 0.2141(4) 0.9356(3) 0.2977(2) 0.0318(8) Uani 0.50 1 d PD A 1 H36A H 0.1128 0.9290 0.3021 0.038 Uiso 0.50 1 calc PR A 1 H36B H 0.2549 0.9389 0.2490 0.038 Uiso 0.50 1 calc PR A 1 C37 C 0.2395(7) 1.0352(4) 0.3220(3) 0.0561(10) Uani 0.50 1 d PD A 1 H37A H 0.2007 1.0308 0.3704 0.067 Uiso 0.50 1 calc PR A 1 H37B H 0.1943 1.0958 0.2955 0.067 Uiso 0.50 1 calc PR A 1 H37C H 0.3399 1.0428 0.3158 0.067 Uiso 0.50 1 calc PR A 1 O3A O 0.2874(4) 0.7564(3) 0.31580(18) 0.0322(4) Uani 0.50 1 d PD E 2 C35A C 0.3215(4) 0.8445(3) 0.3405(2) 0.0297(7) Uani 0.50 1 d PD E 2 H35C H 0.4236 0.8493 0.3322 0.036 Uiso 0.50 1 calc PR E 2 H35D H 0.2886 0.8378 0.3901 0.036 Uiso 0.50 1 calc PR E 2 C36A C 0.2514(4) 0.9404(3) 0.3030(2) 0.0318(8) Uani 0.50 1 d PD E 2 H36C H 0.2855 0.9448 0.2536 0.038 Uiso 0.50 1 calc PR E 2 H36D H 0.1501 0.9320 0.3103 0.038 Uiso 0.50 1 calc PR E 2 C37A C 0.2735(8) 1.0412(5) 0.3234(4) 0.0561(10) Uani 0.50 1 d PD E 2 H37D H 0.2415 1.0377 0.3724 0.067 Uiso 0.50 1 calc PR E 2 H37E H 0.2208 1.0986 0.2979 0.067 Uiso 0.50 1 calc PR E 2 H37F H 0.3728 1.0532 0.3132 0.067 Uiso 0.50 1 calc PR E 2 O4 O 0.4164(3) 0.79443(19) 0.14762(14) 0.0419(4) Uani 0.70 1 d PD A 1 C38 C 0.5326(4) 0.8394(3) 0.10258(19) 0.0544(8) Uani 0.70 1 d PD A 1 H38A H 0.5305 0.8287 0.0555 0.065 Uiso 0.70 1 calc PR A 1 H38B H 0.6206 0.8051 0.1168 0.065 Uiso 0.70 1 calc PR A 1 C39 C 0.5249(4) 0.9542(2) 0.1048(2) 0.0593(9) Uani 0.70 1 d PD A 1 H39A H 0.5923 0.9881 0.0669 0.071 Uiso 0.70 1 calc PR A 1 H39B H 0.4306 0.9852 0.0978 0.071 Uiso 0.70 1 calc PR A 1 C40 C 0.5554(4) 0.9769(3) 0.1708(2) 0.0624(9) Uani 0.70 1 d PD A 1 H40A H 0.4974 0.9362 0.2090 0.075 Uiso 0.70 1 calc PR A 1 H40B H 0.5347 1.0516 0.1722 0.075 Uiso 0.70 1 calc PR A 1 H40C H 0.6539 0.9578 0.1742 0.075 Uiso 0.70 1 calc PR A 1 O4A O 0.4313(8) 0.7897(5) 0.1522(4) 0.0419(4) Uani 0.30 1 d PD F 2 C38A C 0.5638(10) 0.8199(7) 0.1155(5) 0.0544(8) Uani 0.30 1 d PD F 2 H38C H 0.5650 0.8248 0.0659 0.065 Uiso 0.30 1 calc PR F 2 H38D H 0.6384 0.7672 0.1296 0.065 Uiso 0.30 1 calc PR F 2 C39A C 0.5877(10) 0.9245(5) 0.1311(5) 0.0593(9) Uani 0.30 1 d PD F 2 H39C H 0.5748 0.9205 0.1812 0.071 Uiso 0.30 1 calc PR F 2 H39D H 0.6852 0.9405 0.1128 0.071 Uiso 0.30 1 calc PR F 2 C40A C 0.4916(9) 1.0122(6) 0.1016(5) 0.0624(9) Uani 0.30 1 d PD F 2 H40D H 0.5216 1.0302 0.0523 0.075 Uiso 0.30 1 calc PR F 2 H40E H 0.4941 1.0734 0.1229 0.075 Uiso 0.30 1 calc PR F 2 H40F H 0.3964 0.9900 0.1103 0.075 Uiso 0.30 1 calc PR F 2 C1 C 0.3546(2) 0.65657(15) 0.09829(9) 0.0409(5) Uani 1 1 d . A 1 C2 C 0.2759(2) 0.73499(16) 0.05036(10) 0.0450(5) Uani 1 1 d . A 1 H2A H 0.3423 0.7824 0.0204 0.054 Uiso 1 1 calc R A 1 H2B H 0.2355 0.6971 0.0210 0.054 Uiso 1 1 calc R A 1 C3 C 0.1602(2) 0.79969(16) 0.08725(9) 0.0396(4) Uani 1 1 d . A 1 C4 C 0.1583(2) 0.90737(15) 0.07609(9) 0.0402(5) Uani 1 1 d . A 1 H4 H 0.2278 0.9405 0.0426 0.048 Uiso 1 1 calc R A 1 C5 C 0.0585(2) 0.96980(15) 0.11187(9) 0.0394(4) Uani 1 1 d . A 1 C6 C -0.0370(2) 0.91719(15) 0.16273(9) 0.0391(4) Uani 1 1 d . A 1 H6 H -0.1027 0.9569 0.1900 0.047 Uiso 1 1 calc R A 1 C7 C -0.0401(2) 0.80934(15) 0.17512(9) 0.0387(4) Uani 1 1 d . A 1 C8 C -0.1434(2) 0.75638(15) 0.23277(10) 0.0410(5) Uani 1 1 d . A 1 H8A H -0.1321 0.6799 0.2337 0.049 Uiso 1 1 calc R A 1 H8B H -0.2393 0.7811 0.2245 0.049 Uiso 1 1 calc R A 1 C9 C -0.1226(2) 0.77942(15) 0.30110(9) 0.0391(4) Uani 1 1 d . A 1 C10 C -0.1882(2) 0.86864(15) 0.32393(10) 0.0417(5) Uani 1 1 d . A 1 H10 H -0.2539 0.9102 0.2987 0.050 Uiso 1 1 calc R A 1 C11 C -0.1605(2) 0.89940(15) 0.38300(10) 0.0431(5) Uani 1 1 d . A 1 C12 C -0.0656(2) 0.83445(15) 0.41943(10) 0.0425(5) Uani 1 1 d . A 1 H12 H -0.0452 0.8537 0.4596 0.051 Uiso 1 1 calc R A 1 C13 C 0.0002(2) 0.74271(14) 0.39933(9) 0.0402(5) Uani 1 1 d . A 1 C14 C 0.0971(2) 0.67498(16) 0.44398(10) 0.0434(5) Uani 1 1 d . A 1 H14A H 0.1272 0.7202 0.4723 0.052 Uiso 1 1 calc R A 1 H14B H 0.0407 0.6222 0.4756 0.052 Uiso 1 1 calc R A 1 C15 C 0.2269(2) 0.61701(14) 0.41241(9) 0.0389(4) Uani 1 1 d . A 1 C16 C 0.2661(2) 0.51787(15) 0.44518(10) 0.0420(5) Uani 1 1 d . A 1 H16 H 0.2076 0.4885 0.4853 0.050 Uiso 1 1 calc R A 1 C17 C 0.3865(2) 0.45883(14) 0.42264(10) 0.0409(5) Uani 1 1 d . A 1 C18 C 0.4669(2) 0.50409(14) 0.36227(10) 0.0403(5) Uani 1 1 d . A 1 H18 H 0.5495 0.4663 0.3449 0.048 Uiso 1 1 calc R A 1 C19 C 0.4313(2) 0.60145(14) 0.32682(9) 0.0383(4) Uani 1 1 d . A 1 C20 C 0.5178(2) 0.64442(15) 0.25976(10) 0.0408(5) Uani 1 1 d . A 1 H20A H 0.6162 0.6180 0.2606 0.049 Uiso 1 1 calc R A 1 H20B H 0.5130 0.7216 0.2542 0.049 Uiso 1 1 calc R A 1 C21 C 0.4677(2) 0.61338(15) 0.19909(9) 0.0389(4) Uani 1 1 d . A 1 C22 C 0.4712(2) 0.50872(15) 0.19413(10) 0.0411(5) Uani 1 1 d . A 1 H22 H 0.5083 0.4582 0.2280 0.049 Uiso 1 1 calc R A 1 C23 C 0.4228(2) 0.47445(15) 0.14180(10) 0.0413(5) Uani 1 1 d . A 1 C24 C 0.3606(2) 0.55030(15) 0.09502(10) 0.0424(5) Uani 1 1 d . A 1 H24 H 0.3216 0.5288 0.0603 0.051 Uiso 1 1 calc R A 1 C25 C 0.0548(2) 0.75119(14) 0.13463(9) 0.0394(4) Uani 1 1 d D A 1 C26 C -0.0300(2) 0.71530(14) 0.33972(9) 0.0374(4) Uani 1 1 d D A 1 C27 C 0.3119(2) 0.65864(14) 0.35258(9) 0.0375(4) Uani 1 1 d D A 1 C28 C 0.4156(2) 0.68686(14) 0.14876(9) 0.0384(4) Uani 1 1 d D A 1 C41 C 0.0528(2) 1.08851(16) 0.09959(10) 0.0422(5) Uani 1 1 d . . . C42 C 0.1416(3) 1.13264(17) 0.03246(11) 0.0519(6) Uani 1 1 d . A . H42A H 0.2392 1.1072 0.0337 0.062 Uiso 1 1 calc R . . H42B H 0.1334 1.2092 0.0261 0.062 Uiso 1 1 calc R . . H42C H 0.1092 1.1099 -0.0054 0.062 Uiso 1 1 calc R . . C43 C -0.0963(3) 1.13568(18) 0.09661(12) 0.0524(6) Uani 1 1 d . A . H43A H -0.1330 1.1113 0.0605 0.063 Uiso 1 1 calc R . . H43B H -0.0969 1.2121 0.0869 0.063 Uiso 1 1 calc R . . H43C H -0.1547 1.1139 0.1405 0.063 Uiso 1 1 calc R . . C44 C 0.1069(3) 1.12359(17) 0.15852(12) 0.0534(6) Uani 1 1 d . A . H44A H 0.0558 1.0911 0.2021 0.064 Uiso 1 1 calc R . . H44B H 0.0930 1.1998 0.1542 0.064 Uiso 1 1 calc R . . H44C H 0.2064 1.1022 0.1568 0.064 Uiso 1 1 calc R . . C45 C -0.2304(3) 1.00232(16) 0.40261(11) 0.0489(6) Uani 1 1 d . . . C46 C -0.1856(3) 1.09191(19) 0.34492(15) 0.0725(8) Uani 1 1 d . A . H46A H -0.2286 1.1584 0.3571 0.087 Uiso 1 1 calc R . . H46B H -0.2155 1.0814 0.3029 0.087 Uiso 1 1 calc R . . H46C H -0.0840 1.0933 0.3378 0.087 Uiso 1 1 calc R . . C47 C -0.1952(4) 1.0204(2) 0.46957(15) 0.0802(9) Uani 1 1 d . A . H47A H -0.0952 1.0288 0.4646 0.096 Uiso 1 1 calc R . . H47B H -0.2196 0.9604 0.5052 0.096 Uiso 1 1 calc R . . H47C H -0.2478 1.0837 0.4822 0.096 Uiso 1 1 calc R . . C48 C -0.3886(3) 1.0010(2) 0.40978(14) 0.0630(7) Uani 1 1 d . A . H48A H -0.4199 0.9412 0.4441 0.076 Uiso 1 1 calc R . . H48B H -0.4141 0.9950 0.3658 0.076 Uiso 1 1 calc R . . H48C H -0.4329 1.0659 0.4240 0.076 Uiso 1 1 calc R . . C49 C 0.4223(2) 0.34798(15) 0.45854(10) 0.0454(5) Uani 1 1 d . . . C50 C 0.3792(3) 0.33657(17) 0.53612(11) 0.0544(6) Uani 1 1 d . A . H50A H 0.4253 0.3871 0.5534 0.065 Uiso 1 1 calc R . . H50B H 0.4069 0.2656 0.5577 0.065 Uiso 1 1 calc R . . H50C H 0.2780 0.3497 0.5468 0.065 Uiso 1 1 calc R . . C51 C 0.3431(3) 0.27313(17) 0.43163(13) 0.0639(7) Uani 1 1 d . A . H51A H 0.2431 0.2931 0.4399 0.077 Uiso 1 1 calc R . . H51B H 0.3614 0.2016 0.4552 0.077 Uiso 1 1 calc R . . H51C H 0.3743 0.2767 0.3825 0.077 Uiso 1 1 calc R . . C52 C 0.5774(3) 0.3172(2) 0.44618(15) 0.0676(8) Uani 1 1 d . A . H52A H 0.5971 0.2495 0.4745 0.081 Uiso 1 1 calc R . . H52B H 0.6285 0.3703 0.4581 0.081 Uiso 1 1 calc R . . H52C H 0.6068 0.3120 0.3980 0.081 Uiso 1 1 calc R . . C53 C 0.4346(2) 0.35766(15) 0.13810(11) 0.0477(5) Uani 1 1 d . . . C54 C 0.3503(3) 0.29932(17) 0.20233(12) 0.0603(7) Uani 1 1 d . A . H54A H 0.3853 0.3115 0.2427 0.072 Uiso 1 1 calc R . . H54B H 0.3597 0.2243 0.2008 0.072 Uiso 1 1 calc R . . H54C H 0.2521 0.3248 0.2046 0.072 Uiso 1 1 calc R . . C55 C 0.3814(3) 0.33526(18) 0.07528(12) 0.0596(7) Uani 1 1 d . A . H55A H 0.2808 0.3531 0.0793 0.072 Uiso 1 1 calc R . . H55B H 0.4009 0.2610 0.0724 0.072 Uiso 1 1 calc R . . H55C H 0.4287 0.3774 0.0341 0.072 Uiso 1 1 calc R . . C56 C 0.5875(3) 0.31689(19) 0.13357(16) 0.0661(7) Uani 1 1 d . A . H56A H 0.6419 0.3568 0.0936 0.079 Uiso 1 1 calc R . . H56B H 0.5962 0.2428 0.1294 0.079 Uiso 1 1 calc R . . H56C H 0.6225 0.3249 0.1749 0.079 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0455(11) 0.0370(7) 0.0466(7) -0.0117(6) 0.0061(8) -0.0064(7) C29 0.067(3) 0.0447(16) 0.0416(15) -0.0241(13) 0.0043(19) -0.004(2) C30 0.067(3) 0.064(2) 0.101(3) -0.022(2) -0.006(2) -0.017(2) C31 0.096(4) 0.073(4) 0.119(4) -0.035(3) 0.004(3) -0.008(3) O1A 0.0455(11) 0.0370(7) 0.0466(7) -0.0117(6) 0.0061(8) -0.0064(7) C29A 0.067(3) 0.0447(16) 0.0416(15) -0.0241(13) 0.0043(19) -0.004(2) C30A 0.067(3) 0.064(2) 0.101(3) -0.022(2) -0.006(2) -0.017(2) C31A 0.096(4) 0.073(4) 0.119(4) -0.035(3) 0.004(3) -0.008(3) O1B 0.0455(11) 0.0370(7) 0.0466(7) -0.0117(6) 0.0061(8) -0.0064(7) C29B 0.067(3) 0.0447(16) 0.0416(15) -0.0241(13) 0.0043(19) -0.004(2) C30B 0.067(3) 0.064(2) 0.101(3) -0.022(2) -0.006(2) -0.017(2) C31B 0.096(4) 0.073(4) 0.119(4) -0.035(3) 0.004(3) -0.008(3) O2 0.0386(9) 0.0293(6) 0.0213(8) -0.0037(6) -0.0038(7) 0.0007(6) C32 0.0272(16) 0.0235(11) 0.0333(12) 0.0017(9) -0.0079(11) 0.0075(11) C33 0.033(2) 0.0335(11) 0.0555(13) -0.0148(10) -0.0012(14) 0.0068(12) C34 0.072(3) 0.0392(13) 0.081(2) -0.0202(13) 0.005(2) -0.0064(16) O2A 0.0386(9) 0.0293(6) 0.0213(8) -0.0037(6) -0.0038(7) 0.0007(6) C32A 0.0272(16) 0.0235(11) 0.0333(12) 0.0017(9) -0.0079(11) 0.0075(11) C33A 0.033(2) 0.0335(11) 0.0555(13) -0.0148(10) -0.0012(14) 0.0068(12) C34A 0.072(3) 0.0392(13) 0.081(2) -0.0202(13) 0.005(2) -0.0064(16) O3 0.0344(11) 0.0302(6) 0.0345(6) -0.0080(5) -0.0042(7) -0.0113(7) C35 0.014(2) 0.0354(9) 0.0443(10) -0.0091(8) -0.0087(12) -0.0137(11) C36 0.0223(19) 0.0360(10) 0.0437(11) -0.0084(9) -0.0162(12) -0.0111(11) C37 0.076(3) 0.0383(11) 0.0621(14) -0.0099(10) -0.0257(16) -0.0133(15) O3A 0.0344(11) 0.0302(6) 0.0345(6) -0.0080(5) -0.0042(7) -0.0113(7) C35A 0.014(2) 0.0354(9) 0.0443(10) -0.0091(8) -0.0087(12) -0.0137(11) C36A 0.0223(19) 0.0360(10) 0.0437(11) -0.0084(9) -0.0162(12) -0.0111(11) C37A 0.076(3) 0.0383(11) 0.0621(14) -0.0099(10) -0.0257(16) -0.0133(15) O4 0.0491(9) 0.0341(6) 0.0408(7) -0.0085(6) 0.0042(7) -0.0092(6) C38 0.0657(19) 0.0442(13) 0.0490(15) -0.0090(11) 0.0143(13) -0.0204(13) C39 0.066(2) 0.0334(14) 0.075(2) -0.0003(14) -0.0067(17) -0.0094(15) C40 0.063(2) 0.0504(16) 0.076(2) -0.0166(15) -0.0054(16) -0.0129(15) O4A 0.0491(9) 0.0341(6) 0.0408(7) -0.0085(6) 0.0042(7) -0.0092(6) C38A 0.0657(19) 0.0442(13) 0.0490(15) -0.0090(11) 0.0143(13) -0.0204(13) C39A 0.066(2) 0.0334(14) 0.075(2) -0.0003(14) -0.0067(17) -0.0094(15) C40A 0.063(2) 0.0504(16) 0.076(2) -0.0166(15) -0.0054(16) -0.0129(15) C1 0.0466(11) 0.0418(9) 0.0312(8) -0.0113(7) 0.0094(8) -0.0047(8) C2 0.0530(12) 0.0472(10) 0.0319(9) -0.0089(8) 0.0034(8) -0.0020(9) C3 0.0429(10) 0.0454(10) 0.0300(8) -0.0091(7) 0.0017(8) -0.0078(8) C4 0.0442(11) 0.0460(10) 0.0297(8) -0.0066(7) 0.0005(8) -0.0110(9) C5 0.0465(11) 0.0394(9) 0.0331(8) -0.0088(7) -0.0011(8) -0.0101(8) C6 0.0435(10) 0.0395(9) 0.0346(8) -0.0120(7) 0.0025(8) -0.0080(8) C7 0.0436(10) 0.0400(9) 0.0328(8) -0.0100(7) 0.0022(8) -0.0107(8) C8 0.0418(10) 0.0443(10) 0.0366(9) -0.0113(8) 0.0051(8) -0.0131(8) C9 0.0407(10) 0.0402(9) 0.0342(9) -0.0083(7) 0.0072(8) -0.0107(8) C10 0.0474(11) 0.0387(9) 0.0359(9) -0.0082(7) 0.0063(8) -0.0064(8) C11 0.0496(12) 0.0371(9) 0.0396(9) -0.0096(8) 0.0051(9) -0.0037(9) C12 0.0514(12) 0.0402(9) 0.0349(9) -0.0128(8) 0.0024(8) -0.0017(9) C13 0.0485(11) 0.0360(9) 0.0327(9) -0.0092(7) 0.0084(8) -0.0058(8) C14 0.0541(12) 0.0417(9) 0.0318(8) -0.0103(7) 0.0023(8) 0.0010(9) C15 0.0502(11) 0.0353(8) 0.0307(8) -0.0111(7) 0.0011(8) -0.0028(8) C16 0.0530(12) 0.0363(9) 0.0335(9) -0.0086(7) 0.0061(8) -0.0046(9) C17 0.0526(12) 0.0339(8) 0.0365(9) -0.0129(7) 0.0013(8) -0.0062(8) C18 0.0466(11) 0.0345(8) 0.0401(9) -0.0144(7) 0.0034(8) -0.0075(8) C19 0.0477(11) 0.0351(8) 0.0337(8) -0.0110(7) 0.0004(8) -0.0117(8) C20 0.0425(11) 0.0401(9) 0.0389(9) -0.0100(8) 0.0045(8) -0.0104(8) C21 0.0416(10) 0.0389(9) 0.0337(9) -0.0105(7) 0.0103(8) -0.0107(8) C22 0.0437(11) 0.0372(9) 0.0385(9) -0.0090(7) 0.0082(8) -0.0039(8) C23 0.0461(11) 0.0369(9) 0.0380(9) -0.0137(7) 0.0118(8) -0.0061(8) C24 0.0482(11) 0.0441(10) 0.0340(9) -0.0154(8) 0.0089(8) -0.0083(9) C25 0.0470(11) 0.0375(9) 0.0339(8) -0.0110(7) 0.0007(8) -0.0073(8) C26 0.0409(10) 0.0340(8) 0.0346(9) -0.0094(7) 0.0074(8) -0.0058(8) C27 0.0489(11) 0.0303(8) 0.0335(8) -0.0095(7) -0.0012(8) -0.0058(8) C28 0.0431(10) 0.0333(8) 0.0357(9) -0.0096(7) 0.0074(8) -0.0047(8) C41 0.0491(11) 0.0395(9) 0.0386(9) -0.0089(8) -0.0019(8) -0.0101(9) C42 0.0638(14) 0.0435(11) 0.0442(11) -0.0020(9) 0.0021(10) -0.0112(10) C43 0.0602(14) 0.0439(10) 0.0527(12) -0.0110(9) -0.0022(10) -0.0081(10) C44 0.0713(15) 0.0423(10) 0.0510(11) -0.0132(9) -0.0097(11) -0.0150(10) C45 0.0552(13) 0.0400(10) 0.0486(11) -0.0142(9) 0.0026(10) 0.0045(10) C46 0.088(2) 0.0422(12) 0.0780(17) -0.0137(12) 0.0172(15) -0.0063(13) C47 0.106(2) 0.0633(14) 0.0801(17) -0.0418(13) -0.0249(16) 0.0268(15) C48 0.0589(15) 0.0567(13) 0.0692(15) -0.0227(11) 0.0072(12) 0.0089(12) C49 0.0589(13) 0.0323(9) 0.0422(10) -0.0090(8) 0.0011(9) -0.0003(9) C50 0.0733(16) 0.0424(11) 0.0447(11) -0.0080(9) -0.0023(11) -0.0022(11) C51 0.100(2) 0.0368(10) 0.0592(13) -0.0094(10) -0.0195(13) -0.0096(12) C52 0.0621(16) 0.0501(13) 0.0760(17) 0.0034(12) 0.0055(13) 0.0115(12) C53 0.0570(13) 0.0370(9) 0.0479(10) -0.0183(8) 0.0099(9) -0.0072(9) C54 0.0851(17) 0.0434(11) 0.0510(12) -0.0139(9) 0.0100(12) -0.0210(11) C55 0.0777(17) 0.0468(11) 0.0540(12) -0.0223(9) 0.0119(11) -0.0153(11) C56 0.0645(16) 0.0476(11) 0.0892(17) -0.0349(12) 0.0011(13) 0.0023(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 O1 C25 1.390(5) . ? O1 C29 1.458(7) . ? C29 C30 1.489(8) . ? C30 C31 1.467(10) . ? O1A C29A 1.422(12) . ? C29A C30A 1.466(13) . ? C30A C31A 1.462(15) . ? O1B C29B 1.441(11) . ? C29B C30B 1.451(11) . ? C30B C31B 1.537(12) . ? O2 C26 1.346(4) . ? O2 C32 1.415(5) . ? C32 C33 1.505(6) . ? C33 C34 1.511(8) . ? O2A C32A 1.423(4) . ? C32A C33A 1.495(5) . ? C33A C34A 1.531(7) . ? O3 C27 1.405(3) . ? O3 C35 1.421(5) . ? C35 C36 1.507(5) . ? C36 C37 1.530(7) . ? O3A C35A 1.424(6) . ? C35A C36A 1.502(6) . ? C36A C37A 1.496(7) . ? O4 C28 1.401(3) . ? O4 C38 1.431(4) . ? C38 C39 1.502(5) . ? C39 C40 1.500(5) . ? O4A C38A 1.433(10) . ? C38A C39A 1.507(11) . ? C39A C40A 1.505(11) . ? C1 C24 1.396(3) . ? C1 C28 1.398(3) . ? C1 C2 1.517(3) . ? C2 C3 1.516(3) . ? C3 C4 1.381(3) . ? C3 C25 1.397(3) . ? C4 C5 1.397(3) . ? C5 C6 1.393(3) . ? C5 C41 1.520(3) . ? C6 C7 1.386(3) . ? C7 C25 1.390(3) . ? C7 C8 1.516(3) . ? C8 C9 1.516(3) . ? C9 C10 1.388(3) . ? C9 C26 1.403(3) . ? C10 C11 1.402(3) . ? C11 C12 1.400(3) . ? C11 C45 1.532(3) . ? C12 C13 1.395(3) . ? C13 C26 1.402(3) . ? C13 C14 1.521(3) . ? C14 C15 1.515(3) . ? C15 C16 1.388(3) . ? C15 C27 1.397(3) . ? C16 C17 1.396(3) . ? C17 C18 1.398(3) . ? C17 C49 1.528(3) . ? C18 C19 1.381(3) . ? C19 C27 1.396(3) . ? C19 C20 1.513(3) . ? C20 C21 1.527(3) . ? C21 C22 1.385(3) . ? C21 C28 1.388(3) . ? C22 C23 1.389(3) . ? C23 C24 1.403(3) . ? C23 C53 1.532(3) . ? C41 C42 1.528(3) . ? C41 C43 1.529(3) . ? C41 C44 1.540(3) . ? C45 C47 1.515(4) . ? C45 C48 1.529(4) . ? C45 C46 1.531(3) . ? C49 C52 1.519(4) . ? C49 C51 1.531(3) . ? C49 C50 1.535(3) . ? C53 C56 1.527(4) . ? C53 C54 1.530(3) . ? C53 C55 1.535(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 C25 O1 C29 109.2(4) . . ? O1 C29 C30 103.2(5) . . ? C31 C30 C29 118.9(6) . . ? O1A C29A C30A 123.1(10) . . ? C31A C30A C29A 114.2(13) . . ? O1B C29B C30B 111.1(8) . . ? C29B C30B C31B 116.1(9) . . ? C26 O2 C32 110.8(3) . . ? O2 C32 C33 106.7(4) . . ? C32 C33 C34 114.6(5) . . ? O2A C32A C33A 109.0(3) . . ? C32A C33A C34A 109.3(4) . . ? C27 O3 C35 113.0(3) . . ? O3 C35 C36 108.2(3) . . ? C35 C36 C37 109.4(4) . . ? O3A C35A C36A 107.7(4) . . ? C37A C36A C35A 115.3(4) . . ? C28 O4 C38 112.7(2) . . ? O4 C38 C39 108.9(3) . . ? C40 C39 C38 113.1(3) . . ? O4A C38A C39A 108.2(7) . . ? C40A C39A C38A 113.2(8) . . ? C24 C1 C28 118.36(19) . . ? C24 C1 C2 119.75(19) . . ? C28 C1 C2 121.79(18) . . ? C3 C2 C1 113.22(16) . . ? C4 C3 C25 118.52(18) . . ? C4 C3 C2 120.96(18) . . ? C25 C3 C2 120.51(18) . . ? C3 C4 C5 122.94(18) . . ? C6 C5 C4 116.24(18) . . ? C6 C5 C41 119.86(18) . . ? C4 C5 C41 123.87(17) . . ? C7 C6 C5 122.72(18) . . ? C6 C7 C25 118.74(17) . . ? C6 C7 C8 120.24(17) . . ? C25 C7 C8 121.01(17) . . ? C7 C8 C9 111.42(17) . . ? C10 C9 C26 119.18(19) . . ? C10 C9 C8 119.95(19) . . ? C26 C9 C8 120.73(17) . . ? C9 C10 C11 122.1(2) . . ? C12 C11 C10 116.99(18) . . ? C12 C11 C45 123.9(2) . . ? C10 C11 C45 119.1(2) . . ? C13 C12 C11 122.9(2) . . ? C12 C13 C26 118.15(19) . . ? C12 C13 C14 118.95(18) . . ? C26 C13 C14 122.86(17) . . ? C15 C14 C13 120.70(17) . . ? C16 C15 C27 117.72(18) . . ? C16 C15 C14 118.60(17) . . ? C27 C15 C14 123.66(17) . . ? C15 C16 C17 123.82(18) . . ? C16 C17 C18 115.92(18) . . ? C16 C17 C49 122.02(18) . . ? C18 C17 C49 121.89(18) . . ? C19 C18 C17 122.68(19) . . ? C18 C19 C27 119.16(17) . . ? C18 C19 C20 120.56(18) . . ? C27 C19 C20 120.25(17) . . ? C19 C20 C21 112.03(16) . . ? C22 C21 C28 118.22(19) . . ? C22 C21 C20 119.65(18) . . ? C28 C21 C20 122.13(17) . . ? C21 C22 C23 122.86(19) . . ? C22 C23 C24 117.25(18) . . ? C22 C23 C53 120.04(19) . . ? C24 C23 C53 122.69(19) . . ? C1 C24 C23 121.6(2) . . ? C7 C25 O1 120.0(2) . . ? C7 C25 C3 120.36(18) . . ? O1 C25 C3 119.6(2) . . ? O2 C26 C13 128.6(2) . . ? O2 C26 C9 110.6(2) . . ? C13 C26 C9 120.64(17) . . ? C19 C27 C15 120.67(17) . . ? C19 C27 O3 121.9(2) . . ? C15 C27 O3 116.6(2) . . ? C21 C28 C1 121.24(18) . . ? C21 C28 O4 121.8(2) . . ? C1 C28 O4 116.9(2) . . ? C5 C41 C42 112.12(17) . . ? C5 C41 C43 110.99(18) . . ? C42 C41 C43 107.28(19) . . ? C5 C41 C44 108.78(17) . . ? C42 C41 C44 108.65(19) . . ? C43 C41 C44 108.95(19) . . ? C47 C45 C48 108.2(2) . . ? C47 C45 C46 110.7(2) . . ? C48 C45 C46 107.4(2) . . ? C47 C45 C11 112.0(2) . . ? C48 C45 C11 109.8(2) . . ? C46 C45 C11 108.65(18) . . ? C52 C49 C17 112.17(19) . . ? C52 C49 C51 109.8(2) . . ? C17 C49 C51 107.85(19) . . ? C52 C49 C50 106.5(2) . . ? C17 C49 C50 111.56(17) . . ? C51 C49 C50 108.9(2) . . ? C56 C53 C54 109.7(2) . . ? C56 C53 C23 109.06(19) . . ? C54 C53 C23 109.14(17) . . ? C56 C53 C55 107.5(2) . . ? C54 C53 C55 108.81(19) . . ? C23 C53 C55 112.57(19) . . ? _diffrn_measured_fraction_theta_max 0.928 _diffrn_reflns_theta_full 77.92 _diffrn_measured_fraction_theta_full 0.928 _refine_diff_density_max 0.937 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.108 # Attachment 'JB2_01_08.cif' data_final_used _database_code_depnum_ccdc_archive 'CCDC 666976' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H77 O4' _chemical_formula_weight 910.26 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' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.940(7) _cell_length_b 20.167(9) _cell_length_c 19.074(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.46(4) _cell_angle_gamma 90.00 _cell_volume 5511(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7904 _cell_measurement_theta_min 3.7810 _cell_measurement_theta_max 76.6581 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1972 _exptl_absorpt_coefficient_mu 0.509 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.748 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_process_details ; Analytical Absorption (De Meulenaer & Tompa, 1965) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54180 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCALIBUR' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 84230 _diffrn_reflns_av_R_equivalents 0.1178 _diffrn_reflns_av_sigmaI/netI 0.0686 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 77.70 _reflns_number_total 11474 _reflns_number_gt 5307 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Xcalibur, (Oxford Diffraction, 2002)' _computing_cell_refinement 'CrysAlis RED, (Oxford Diffraction, 2002)' _computing_data_reduction 'CrysAlis RED, (Oxford Diffraction, 2002)' _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. The t-butyl group can rotate around the single bond and be found in lot of different positions. Some of these positions were modelled. Therefore, the distances between the atoms of each position, the angles between the atoms and thermal parameters were fixed using 66 restraints. The disorder was modelled for one of the propoxy group where again the positins change with the rotation around single bonds. ; _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^)+(0.1408P)^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 11474 _refine_ls_number_parameters 603 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1345 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2439 _refine_ls_wR_factor_gt 0.2212 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.961 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.17115(16) 0.53158(10) 0.63665(12) 0.0478(6) Uani 1 1 d . A 1 C2 C 0.11110(18) 0.53794(11) 0.55808(12) 0.0559(7) Uani 1 1 d . A 1 H2A H 0.1403 0.5120 0.5263 0.067 Uiso 1 1 calc R A 1 H2B H 0.0492 0.5182 0.5540 0.067 Uiso 1 1 calc R A 1 C3 C 0.09735(17) 0.60868(11) 0.53019(11) 0.0502(6) Uani 1 1 d . A 1 C4 C 0.00893(17) 0.63668(12) 0.50865(12) 0.0548(7) Uani 1 1 d . A 1 H4 H -0.0433 0.6096 0.5081 0.066 Uiso 1 1 calc R A 1 C5 C -0.00648(17) 0.70273(12) 0.48784(12) 0.0547(7) Uani 1 1 d . A 1 C6 C 0.07327(18) 0.74097(12) 0.49442(12) 0.0569(7) Uani 1 1 d . A 1 H6 H 0.0656 0.7870 0.4839 0.068 Uiso 1 1 calc R A 1 C7 C 0.16324(17) 0.71538(11) 0.51553(11) 0.0497(6) Uani 1 1 d . A 1 C8 C 0.24671(19) 0.75990(12) 0.52481(13) 0.0611(7) Uani 1 1 d . A 1 H8A H 0.2434 0.7811 0.4773 0.073 Uiso 1 1 calc R A 1 H8B H 0.3041 0.7326 0.5391 0.073 Uiso 1 1 calc R A 1 C9 C 0.25293(17) 0.81352(12) 0.58199(12) 0.0541(6) Uani 1 1 d . A 1 C10 C 0.22824(18) 0.87859(12) 0.56073(13) 0.0641(8) Uani 1 1 d . A 1 H10 H 0.2097 0.8890 0.5101 0.077 Uiso 1 1 calc R A 1 C11 C 0.22965(18) 0.92880(12) 0.61061(14) 0.0651(8) Uani 1 1 d . A 1 C12 C 0.25665(18) 0.91103(12) 0.68422(14) 0.0629(7) Uani 1 1 d . A 1 H12 H 0.2568 0.9443 0.7195 0.075 Uiso 1 1 calc R A 1 C13 C 0.28336(16) 0.84715(12) 0.70876(12) 0.0513(6) Uani 1 1 d . A 1 C14 C 0.31196(18) 0.83693(12) 0.79088(12) 0.0593(7) Uani 1 1 d . A 1 H14A H 0.3715 0.8610 0.8106 0.071 Uiso 1 1 calc R A 1 H14B H 0.2649 0.8602 0.8095 0.071 Uiso 1 1 calc R A 1 C15 C 0.32504(17) 0.76985(12) 0.82574(12) 0.0521(6) Uani 1 1 d . A 1 C16 C 0.41024(17) 0.75223(12) 0.87412(12) 0.0558(7) Uani 1 1 d . A 1 H16 H 0.4604 0.7830 0.8831 0.067 Uiso 1 1 calc R A 1 C17 C 0.42511(17) 0.69112(13) 0.91014(12) 0.0552(7) Uani 1 1 d . A 1 C18 C 0.35258(16) 0.64711(13) 0.89363(11) 0.0530(6) Uani 1 1 d . A 1 H18 H 0.3613 0.6049 0.9166 0.064 Uiso 1 1 calc R A 1 C19 C 0.26584(16) 0.66169(12) 0.84421(11) 0.0496(6) Uani 1 1 d . A 1 C20 C 0.19072(16) 0.60854(12) 0.82324(12) 0.0526(6) Uani 1 1 d . A 1 H20A H 0.1286 0.6298 0.8055 0.063 Uiso 1 1 calc R A 1 H20B H 0.1914 0.5815 0.8668 0.063 Uiso 1 1 calc R A 1 C21 C 0.20728(16) 0.56377(11) 0.76349(12) 0.0484(6) Uani 1 1 d . A 1 C22 C 0.28355(16) 0.52137(11) 0.77867(12) 0.0528(6) Uani 1 1 d . A 1 H22 H 0.3223 0.5184 0.8276 0.063 Uiso 1 1 calc R A 1 C23 C 0.30552(16) 0.48316(12) 0.72542(12) 0.0534(6) Uani 1 1 d . A 1 C24 C 0.24929(16) 0.49089(11) 0.65424(12) 0.0500(6) Uani 1 1 d . A 1 H24 H 0.2649 0.4674 0.6161 0.060 Uiso 1 1 calc R A 1 C25 C 0.17352(15) 0.64802(11) 0.52998(11) 0.0482(6) Uani 1 1 d D A 1 C26 C 0.28209(16) 0.79906(11) 0.65623(12) 0.0506(6) Uani 1 1 d . A 1 C27 C 0.25224(15) 0.72390(11) 0.81310(10) 0.0450(6) Uani 1 1 d . A 1 C28 C 0.14990(15) 0.56636(10) 0.69247(12) 0.0467(6) Uani 1 1 d . A 1 O1 O 0.2602(3) 0.6178(3) 0.5448(2) 0.0666(4) Uani 0.46 1 d PD A 1 C29 C 0.2689(4) 0.5905(3) 0.4754(3) 0.0666(4) Uani 0.46 1 d PD A 1 H29A H 0.2152 0.5609 0.4540 0.080 Uiso 0.46 1 calc PR A 1 H29B H 0.2668 0.6272 0.4405 0.080 Uiso 0.46 1 calc PR A 1 C30 C 0.3557(3) 0.5533(3) 0.4855(3) 0.0666(4) Uani 0.46 1 d PD A 1 H30A H 0.3596 0.5378 0.4372 0.080 Uiso 0.46 1 calc PR A 1 H30B H 0.3541 0.5137 0.5157 0.080 Uiso 0.46 1 calc PR A 1 C31 C 0.4427(4) 0.5934(3) 0.5218(3) 0.0666(4) Uani 0.46 1 d PD A 1 O1A O 0.2604(4) 0.6186(5) 0.5453(4) 0.0666(4) Uani 0.33 1 d PD B 2 C29A C 0.2923(5) 0.6082(5) 0.4803(4) 0.0666(4) Uani 0.33 1 d PD B 2 H29C H 0.2788 0.6476 0.4481 0.080 Uiso 0.33 1 calc PR B 2 H29D H 0.2611 0.5692 0.4524 0.080 Uiso 0.33 1 calc PR B 2 C30A C 0.3934(5) 0.5973(4) 0.5080(4) 0.0666(4) Uani 0.33 1 d PD B 2 H30C H 0.4215 0.6357 0.5387 0.080 Uiso 0.33 1 calc PR B 2 H30D H 0.4197 0.5962 0.4658 0.080 Uiso 0.33 1 calc PR B 2 C31A C 0.4234(6) 0.5339(4) 0.5529(4) 0.0666(4) Uani 0.33 1 d PD B 2 O1B O 0.2601(6) 0.6187(9) 0.5460(6) 0.0666(4) Uani 0.21 1 d PD C 3 C29B C 0.3025(7) 0.6094(7) 0.4870(6) 0.0666(4) Uani 0.21 1 d PD C 3 H29E H 0.3277 0.6518 0.4747 0.080 Uiso 0.21 1 calc PR C 3 H29F H 0.2560 0.5923 0.4428 0.080 Uiso 0.21 1 calc PR C 3 C30B C 0.3780(7) 0.5611(6) 0.5140(5) 0.0666(4) Uani 0.21 1 d PD C 3 H30E H 0.3533 0.5188 0.5271 0.080 Uiso 0.21 1 calc PR C 3 H30F H 0.4254 0.5785 0.5575 0.080 Uiso 0.21 1 calc PR C 3 C31B C 0.4195(8) 0.5515(6) 0.4504(5) 0.0666(4) Uani 0.21 1 d PD C 3 O2 O 0.30784(10) 0.73397(7) 0.67679(8) 0.0491(4) Uani 1 1 d . A 1 C32 C 0.40513(17) 0.72241(13) 0.69018(13) 0.0597(7) Uani 1 1 d . A 1 H32A H 0.4407 0.7530 0.7286 0.072 Uiso 1 1 calc R A 1 H32B H 0.4236 0.7309 0.6451 0.072 Uiso 1 1 calc R A 1 C33 C 0.42709(17) 0.65232(13) 0.71411(14) 0.0615(7) Uani 1 1 d . A 1 H33A H 0.3873 0.6220 0.6775 0.074 Uiso 1 1 calc R A 1 H33B H 0.4132 0.6450 0.7613 0.074 Uiso 1 1 calc R A 1 C34 C 0.5294(2) 0.63689(18) 0.72275(19) 0.0988(11) Uani 1 1 d . A 1 H34A H 0.5416 0.6396 0.6750 0.119 Uiso 1 1 calc R A 1 H34B H 0.5437 0.5921 0.7426 0.119 Uiso 1 1 calc R A 1 H34C H 0.5687 0.6690 0.7562 0.119 Uiso 1 1 calc R A 1 O3 O 0.16611(11) 0.74404(8) 0.76835(8) 0.0530(4) Uani 1 1 d . A 1 C35 C 0.11168(17) 0.77524(13) 0.80999(13) 0.0599(7) Uani 1 1 d . A 1 H35A H 0.1539 0.7966 0.8537 0.072 Uiso 1 1 calc R A 1 H35B H 0.0748 0.7412 0.8269 0.072 Uiso 1 1 calc R A 1 C36 C 0.04755(17) 0.82592(11) 0.76606(12) 0.0524(6) Uani 1 1 d . A 1 C37 C 0.04091(18) 0.83953(13) 0.69421(13) 0.0613(7) Uani 1 1 d . A 1 H37 H 0.0794 0.8167 0.6702 0.074 Uiso 1 1 calc R A 1 C38 C -0.0225(2) 0.88698(14) 0.65656(15) 0.0741(9) Uani 1 1 d . A 1 H38 H -0.0251 0.8972 0.6074 0.089 Uiso 1 1 calc R A 1 C39 C -0.0805(2) 0.91884(14) 0.68856(16) 0.0756(9) Uani 1 1 d . A 1 H39 H -0.1247 0.9500 0.6616 0.091 Uiso 1 1 calc R A 1 C40 C -0.0745(2) 0.90551(13) 0.76098(16) 0.0749(8) Uani 1 1 d . A 1 H40 H -0.1153 0.9272 0.7838 0.090 Uiso 1 1 calc R A 1 C41 C -0.00959(18) 0.86097(12) 0.80001(14) 0.0613(7) Uani 1 1 d . A 1 H41 H -0.0035 0.8539 0.8504 0.074 Uiso 1 1 calc R A 1 O4 O 0.06867(10) 0.60371(8) 0.67684(8) 0.0544(4) Uani 1 1 d . A 1 C42 C -0.00817(17) 0.56638(13) 0.68539(17) 0.0710(8) Uani 1 1 d . A 1 H42A H 0.0092 0.5447 0.7339 0.085 Uiso 1 1 calc R A 1 H42B H -0.0246 0.5314 0.6475 0.085 Uiso 1 1 calc R A 1 C43 C -0.09085(18) 0.61092(14) 0.67860(15) 0.0675(8) Uani 1 1 d D A 1 C44 C -0.1771(2) 0.58279(19) 0.6634(2) 0.1143(14) Uani 1 1 d D A 1 H44 H -0.1838 0.5362 0.6569 0.137 Uiso 1 1 calc R A 1 C45 C -0.2556(3) 0.6221(2) 0.6574(3) 0.1325(15) Uani 1 1 d DU A 1 H45 H -0.3160 0.6028 0.6443 0.159 Uiso 1 1 calc R A 1 C46 C -0.2449(2) 0.68912(19) 0.6705(2) 0.1064(12) Uani 1 1 d D A 1 H46 H -0.2976 0.7155 0.6706 0.128 Uiso 1 1 calc R A 1 C47 C -0.1581(2) 0.71816(17) 0.68359(18) 0.0898(10) Uani 1 1 d D A 1 H47 H -0.1512 0.7648 0.6899 0.108 Uiso 1 1 calc R A 1 C48 C -0.0810(2) 0.67849(15) 0.68743(16) 0.0779(9) Uani 1 1 d D A 1 H48 H -0.0210 0.6981 0.6962 0.093 Uiso 1 1 calc R A 1 C49 C -0.1057(4) 0.7320(2) 0.4633(3) 0.0758(6) Uani 0.66 1 d PD A 1 C50 C -0.1815(3) 0.6827(2) 0.4676(2) 0.0758(6) Uani 0.66 1 d PD A 1 H50A H -0.1683 0.6656 0.5176 0.091 Uiso 0.66 1 calc PR A 1 H50B H -0.1826 0.6458 0.4338 0.091 Uiso 0.66 1 calc PR A 1 H50C H -0.2423 0.7050 0.4541 0.091 Uiso 0.66 1 calc PR A 1 C51 C -0.1287(3) 0.7544(2) 0.3816(2) 0.0758(6) Uani 0.66 1 d PD A 1 H51A H -0.1287 0.7156 0.3506 0.091 Uiso 0.66 1 calc PR A 1 H51B H -0.0816 0.7862 0.3761 0.091 Uiso 0.66 1 calc PR A 1 H51C H -0.1904 0.7754 0.3669 0.091 Uiso 0.66 1 calc PR A 1 C52 C -0.1047(3) 0.7906(2) 0.5144(2) 0.0758(6) Uani 0.66 1 d PD A 1 H52A H -0.1649 0.8137 0.4990 0.091 Uiso 0.66 1 calc PR A 1 H52B H -0.0546 0.8213 0.5125 0.091 Uiso 0.66 1 calc PR A 1 H52C H -0.0941 0.7744 0.5645 0.091 Uiso 0.66 1 calc PR A 1 C49A C -0.0996(7) 0.7355(5) 0.4581(5) 0.0758(6) Uani 0.34 1 d PD D 2 C50A C -0.1772(6) 0.6868(4) 0.4295(5) 0.0758(6) Uani 0.34 1 d PD D 2 H50D H -0.1786 0.6551 0.4682 0.091 Uiso 0.34 1 calc PR D 2 H50E H -0.1668 0.6629 0.3878 0.091 Uiso 0.34 1 calc PR D 2 H50F H -0.2368 0.7105 0.4140 0.091 Uiso 0.34 1 calc PR D 2 C51A C -0.0968(6) 0.7807(4) 0.3881(4) 0.0758(6) Uani 0.34 1 d PD D 2 H51D H -0.0869 0.7521 0.3494 0.091 Uiso 0.34 1 calc PR D 2 H51E H -0.0457 0.8128 0.4028 0.091 Uiso 0.34 1 calc PR D 2 H51F H -0.1562 0.8043 0.3698 0.091 Uiso 0.34 1 calc PR D 2 C52A C -0.1277(6) 0.7904(5) 0.5007(5) 0.0758(6) Uani 0.34 1 d PD D 2 H52D H -0.1926 0.8030 0.4770 0.091 Uiso 0.34 1 calc PR D 2 H52E H -0.0871 0.8288 0.5022 0.091 Uiso 0.34 1 calc PR D 2 H52F H -0.1219 0.7752 0.5506 0.091 Uiso 0.34 1 calc PR D 2 C53 C 0.1997(3) 1.0026(2) 0.5902(3) 0.0821(7) Uani 0.67 1 d PD A 1 C54 C 0.1885(3) 1.0141(2) 0.5085(2) 0.0821(7) Uani 0.67 1 d PD A 1 H54A H 0.1417 0.9834 0.4794 0.099 Uiso 0.67 1 calc PR A 1 H54B H 0.2484 1.0064 0.4984 0.099 Uiso 0.67 1 calc PR A 1 H54C H 0.1684 1.0599 0.4956 0.099 Uiso 0.67 1 calc PR A 1 C55 C 0.1095(3) 1.0202(2) 0.6068(2) 0.0821(7) Uani 0.67 1 d PD A 1 H55A H 0.0969 1.0676 0.5981 0.099 Uiso 0.67 1 calc PR A 1 H55B H 0.1148 1.0098 0.6580 0.099 Uiso 0.67 1 calc PR A 1 H55C H 0.0583 0.9944 0.5749 0.099 Uiso 0.67 1 calc PR A 1 C56 C 0.2791(3) 1.0476(2) 0.6324(3) 0.0821(7) Uani 0.67 1 d PD A 1 H56A H 0.2655 1.0935 0.6160 0.099 Uiso 0.67 1 calc PR A 1 H56B H 0.3376 1.0334 0.6234 0.099 Uiso 0.67 1 calc PR A 1 H56C H 0.2850 1.0447 0.6848 0.099 Uiso 0.67 1 calc PR A 1 C53A C 0.2125(7) 0.9964(5) 0.5811(5) 0.0821(7) Uani 0.33 1 d PD E 2 C54A C 0.2781(6) 1.0131(4) 0.5302(5) 0.0821(7) Uani 0.33 1 d PD E 2 H54D H 0.2552 0.9896 0.4835 0.099 Uiso 0.33 1 calc PR E 2 H54E H 0.3421 0.9989 0.5546 0.099 Uiso 0.33 1 calc PR E 2 H54F H 0.2773 1.0609 0.5212 0.099 Uiso 0.33 1 calc PR E 2 C55A C 0.1155(6) 0.9987(4) 0.5327(5) 0.0821(7) Uani 0.33 1 d PD E 2 H55D H 0.0717 0.9933 0.5620 0.099 Uiso 0.33 1 calc PR E 2 H55E H 0.1062 0.9627 0.4967 0.099 Uiso 0.33 1 calc PR E 2 H55F H 0.1044 1.0414 0.5072 0.099 Uiso 0.33 1 calc PR E 2 C56A C 0.2375(7) 1.0464(4) 0.6411(5) 0.0821(7) Uani 0.33 1 d PD E 2 H56D H 0.2499 1.0891 0.6213 0.099 Uiso 0.33 1 calc PR E 2 H56E H 0.2935 1.0317 0.6786 0.099 Uiso 0.33 1 calc PR E 2 H56F H 0.1857 1.0512 0.6627 0.099 Uiso 0.33 1 calc PR E 2 C57 C 0.5176(4) 0.6740(3) 0.9688(3) 0.0760(4) Uani 0.56 1 d PD A 1 C58 C 0.5102(4) 0.6984(3) 1.0437(3) 0.0760(4) Uani 0.56 1 d PD A 1 H58A H 0.5689 0.6892 1.0813 0.091 Uiso 0.56 1 calc PR A 1 H58B H 0.4589 0.6752 1.0559 0.091 Uiso 0.56 1 calc PR A 1 H58C H 0.4981 0.7462 1.0414 0.091 Uiso 0.56 1 calc PR A 1 C59 C 0.6010(3) 0.7071(3) 0.9535(3) 0.0760(4) Uani 0.56 1 d PD A 1 H59A H 0.5990 0.7549 0.9622 0.091 Uiso 0.56 1 calc PR A 1 H59B H 0.5996 0.6992 0.9025 0.091 Uiso 0.56 1 calc PR A 1 H59C H 0.6586 0.6885 0.9860 0.091 Uiso 0.56 1 calc PR A 1 C60 C 0.5397(4) 0.5984(2) 0.9771(3) 0.0760(4) Uani 0.56 1 d PD A 1 H60A H 0.5973 0.5915 1.0166 0.091 Uiso 0.56 1 calc PR A 1 H60B H 0.5477 0.5811 0.9312 0.091 Uiso 0.56 1 calc PR A 1 H60C H 0.4881 0.5752 0.9887 0.091 Uiso 0.56 1 calc PR A 1 C57A C 0.5187(6) 0.6771(4) 0.9647(4) 0.0760(4) Uani 0.44 1 d PD F 2 C58A C 0.5432(5) 0.7293(3) 1.0240(3) 0.0760(4) Uani 0.44 1 d PD F 2 H58D H 0.5959 0.7139 1.0641 0.091 Uiso 0.44 1 calc PR F 2 H58E H 0.4893 0.7374 1.0424 0.091 Uiso 0.44 1 calc PR F 2 H58F H 0.5604 0.7706 1.0039 0.091 Uiso 0.44 1 calc PR F 2 C59A C 0.5931(4) 0.6785(3) 0.9219(3) 0.0760(4) Uani 0.44 1 d PD F 2 H59D H 0.6058 0.7246 0.9114 0.091 Uiso 0.44 1 calc PR F 2 H59E H 0.5696 0.6542 0.8759 0.091 Uiso 0.44 1 calc PR F 2 H59F H 0.6507 0.6577 0.9514 0.091 Uiso 0.44 1 calc PR F 2 C60A C 0.5169(5) 0.6082(3) 0.9979(4) 0.0760(4) Uani 0.44 1 d PD F 2 H60D H 0.5792 0.5972 1.0295 0.091 Uiso 0.44 1 calc PR F 2 H60E H 0.4981 0.5753 0.9586 0.091 Uiso 0.44 1 calc PR F 2 H60F H 0.4721 0.6079 1.0268 0.091 Uiso 0.44 1 calc PR F 2 C61 C 0.3816(4) 0.4306(3) 0.7452(3) 0.0760(4) Uani 0.53 1 d PD A 1 C62 C 0.4688(4) 0.4540(3) 0.8021(3) 0.0760(4) Uani 0.53 1 d PD A 1 H62A H 0.4917 0.4947 0.7851 0.091 Uiso 0.53 1 calc PR A 1 H62B H 0.5170 0.4196 0.8099 0.091 Uiso 0.53 1 calc PR A 1 H62C H 0.4541 0.4628 0.8482 0.091 Uiso 0.53 1 calc PR A 1 C63 C 0.3438(4) 0.3700(3) 0.7814(3) 0.0760(4) Uani 0.53 1 d PD A 1 H63A H 0.3263 0.3854 0.8244 0.091 Uiso 0.53 1 calc PR A 1 H63B H 0.3927 0.3362 0.7961 0.091 Uiso 0.53 1 calc PR A 1 H63C H 0.2891 0.3509 0.7459 0.091 Uiso 0.53 1 calc PR A 1 C64 C 0.4082(4) 0.4029(3) 0.6803(3) 0.0760(4) Uani 0.53 1 d PDU A 1 H64A H 0.3557 0.3777 0.6494 0.091 Uiso 0.53 1 calc PR A 1 H64B H 0.4624 0.3736 0.6975 0.091 Uiso 0.53 1 calc PR A 1 H64C H 0.4239 0.4394 0.6520 0.091 Uiso 0.53 1 calc PR A 1 C61A C 0.3911(5) 0.4352(4) 0.7448(4) 0.0760(4) Uani 0.47 1 d PD G 2 C62A C 0.4607(5) 0.4563(4) 0.8183(3) 0.0760(4) Uani 0.47 1 d PD G 2 H62D H 0.5130 0.4251 0.8312 0.091 Uiso 0.47 1 calc PR G 2 H62E H 0.4289 0.4563 0.8568 0.091 Uiso 0.47 1 calc PR G 2 H62F H 0.4842 0.5010 0.8134 0.091 Uiso 0.47 1 calc PR G 2 C63A C 0.3529(4) 0.3655(3) 0.7485(3) 0.0760(4) Uani 0.47 1 d PD G 2 H63D H 0.3103 0.3537 0.7008 0.091 Uiso 0.47 1 calc PR G 2 H63E H 0.3191 0.3642 0.7857 0.091 Uiso 0.47 1 calc PR G 2 H63F H 0.4047 0.3338 0.7613 0.091 Uiso 0.47 1 calc PR G 2 C64A C 0.4407(4) 0.4384(3) 0.6851(3) 0.0760(4) Uani 0.47 1 d PDU G 2 H64D H 0.4679 0.4825 0.6848 0.091 Uiso 0.47 1 calc PR G 2 H64E H 0.3958 0.4297 0.6375 0.091 Uiso 0.47 1 calc PR G 2 H64F H 0.4903 0.4049 0.6947 0.091 Uiso 0.47 1 calc PR G 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 C1 0.0568(13) 0.0358(12) 0.0457(12) 0.0001(9) 0.0061(10) -0.0035(10) C2 0.0650(15) 0.0422(13) 0.0492(13) -0.0029(10) -0.0019(11) 0.0034(11) C3 0.0634(14) 0.0451(13) 0.0344(11) -0.0055(9) 0.0012(10) 0.0078(11) C4 0.0604(14) 0.0501(14) 0.0427(12) -0.0073(10) -0.0034(11) 0.0038(11) C5 0.0663(15) 0.0471(13) 0.0399(12) -0.0096(10) -0.0027(11) 0.0108(12) C6 0.0826(17) 0.0444(13) 0.0360(11) -0.0011(10) 0.0039(11) 0.0130(13) C7 0.0687(15) 0.0493(13) 0.0278(10) 0.0009(9) 0.0080(10) 0.0049(11) C8 0.0801(17) 0.0611(16) 0.0441(12) 0.0130(11) 0.0212(12) -0.0015(13) C9 0.0634(14) 0.0526(14) 0.0443(12) 0.0082(10) 0.0118(11) -0.0072(12) C10 0.0751(17) 0.0555(15) 0.0526(14) 0.0151(12) 0.0032(12) -0.0096(13) C11 0.0675(16) 0.0518(15) 0.0619(15) 0.0089(12) -0.0045(13) -0.0138(13) C12 0.0719(17) 0.0458(14) 0.0616(15) -0.0016(12) 0.0038(13) -0.0127(12) C13 0.0525(13) 0.0480(13) 0.0484(13) 0.0013(10) 0.0062(11) -0.0087(11) C14 0.0656(15) 0.0565(15) 0.0503(13) -0.0040(11) 0.0073(12) -0.0069(12) C15 0.0625(14) 0.0528(14) 0.0399(11) -0.0036(10) 0.0126(10) -0.0043(12) C16 0.0545(14) 0.0645(15) 0.0443(12) -0.0056(11) 0.0072(11) -0.0040(12) C17 0.0608(14) 0.0685(16) 0.0355(11) -0.0057(11) 0.0121(10) 0.0047(13) C18 0.0590(14) 0.0606(15) 0.0388(11) 0.0032(10) 0.0126(10) 0.0066(12) C19 0.0588(13) 0.0572(14) 0.0331(10) -0.0021(10) 0.0134(10) 0.0045(11) C20 0.0596(14) 0.0550(14) 0.0447(12) 0.0064(10) 0.0170(11) -0.0043(11) C21 0.0531(13) 0.0446(13) 0.0472(12) 0.0038(10) 0.0136(10) -0.0057(10) C22 0.0571(14) 0.0497(14) 0.0455(12) 0.0088(10) 0.0047(11) 0.0005(11) C23 0.0555(14) 0.0498(14) 0.0514(13) 0.0040(11) 0.0096(11) -0.0002(11) C24 0.0589(14) 0.0407(12) 0.0470(12) 0.0013(10) 0.0093(11) 0.0026(11) C25 0.0582(13) 0.0515(13) 0.0303(10) -0.0013(9) 0.0052(10) 0.0111(11) C26 0.0534(13) 0.0463(13) 0.0506(13) 0.0094(10) 0.0123(11) -0.0039(11) C27 0.0503(12) 0.0551(14) 0.0276(10) -0.0026(9) 0.0077(9) 0.0030(11) C28 0.0490(12) 0.0360(11) 0.0521(13) 0.0060(10) 0.0094(10) -0.0009(10) O1 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) C29 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) C30 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) C31 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) O1A 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) C29A 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) C30A 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) C31A 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) O1B 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) C29B 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) C30B 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) C31B 0.0709(9) 0.0765(10) 0.0534(7) 0.0086(7) 0.0193(7) 0.0176(8) O2 0.0537(9) 0.0498(9) 0.0453(8) 0.0088(7) 0.0164(7) 0.0023(7) C32 0.0583(14) 0.0716(17) 0.0537(13) 0.0126(12) 0.0233(11) 0.0040(13) C33 0.0632(15) 0.0684(16) 0.0565(14) 0.0144(12) 0.0229(12) 0.0170(13) C34 0.076(2) 0.110(3) 0.116(3) 0.029(2) 0.0377(18) 0.0226(19) O3 0.0554(9) 0.0615(10) 0.0384(8) -0.0009(7) 0.0075(7) 0.0073(8) C35 0.0580(14) 0.0726(17) 0.0500(13) -0.0036(12) 0.0170(11) 0.0126(13) C36 0.0629(14) 0.0468(13) 0.0461(12) -0.0053(10) 0.0132(11) -0.0054(11) C37 0.0689(16) 0.0624(16) 0.0496(14) 0.0010(12) 0.0118(12) 0.0084(13) C38 0.089(2) 0.0645(18) 0.0626(16) 0.0055(14) 0.0109(15) 0.0067(15) C39 0.090(2) 0.0589(17) 0.0744(18) 0.0040(14) 0.0183(16) 0.0176(15) C40 0.090(2) 0.0483(15) 0.090(2) -0.0024(14) 0.0316(16) 0.0089(14) C41 0.0755(16) 0.0479(14) 0.0618(15) 0.0018(12) 0.0216(13) 0.0039(13) O4 0.0508(9) 0.0483(9) 0.0603(9) 0.0021(7) 0.0098(8) 0.0038(7) C42 0.0525(15) 0.0613(17) 0.094(2) 0.0021(14) 0.0129(14) 0.0024(13) C43 0.0518(14) 0.0717(18) 0.0810(18) -0.0030(14) 0.0222(13) 0.0038(13) C44 0.0660(19) 0.085(2) 0.197(4) -0.003(2) 0.045(2) 0.0002(18) C45 0.075(2) 0.114(3) 0.223(4) -0.016(3) 0.065(2) 0.000(2) C46 0.075(2) 0.102(3) 0.156(3) -0.004(2) 0.055(2) 0.0164(19) C47 0.081(2) 0.089(2) 0.103(2) -0.0131(18) 0.0301(18) 0.0128(18) C48 0.0603(17) 0.076(2) 0.091(2) -0.0179(16) 0.0114(15) 0.0061(15) C49 0.0688(11) 0.0727(11) 0.0696(11) -0.0116(9) -0.0070(9) 0.0197(8) C50 0.0688(11) 0.0727(11) 0.0696(11) -0.0116(9) -0.0070(9) 0.0197(8) C51 0.0688(11) 0.0727(11) 0.0696(11) -0.0116(9) -0.0070(9) 0.0197(8) C52 0.0688(11) 0.0727(11) 0.0696(11) -0.0116(9) -0.0070(9) 0.0197(8) C49A 0.0688(11) 0.0727(11) 0.0696(11) -0.0116(9) -0.0070(9) 0.0197(8) C50A 0.0688(11) 0.0727(11) 0.0696(11) -0.0116(9) -0.0070(9) 0.0197(8) C51A 0.0688(11) 0.0727(11) 0.0696(11) -0.0116(9) -0.0070(9) 0.0197(8) C52A 0.0688(11) 0.0727(11) 0.0696(11) -0.0116(9) -0.0070(9) 0.0197(8) C53 0.0835(14) 0.0508(10) 0.0994(14) 0.0169(9) 0.0054(12) 0.0005(10) C54 0.0835(14) 0.0508(10) 0.0994(14) 0.0169(9) 0.0054(12) 0.0005(10) C55 0.0835(14) 0.0508(10) 0.0994(14) 0.0169(9) 0.0054(12) 0.0005(10) C56 0.0835(14) 0.0508(10) 0.0994(14) 0.0169(9) 0.0054(12) 0.0005(10) C53A 0.0835(14) 0.0508(10) 0.0994(14) 0.0169(9) 0.0054(12) 0.0005(10) C54A 0.0835(14) 0.0508(10) 0.0994(14) 0.0169(9) 0.0054(12) 0.0005(10) C55A 0.0835(14) 0.0508(10) 0.0994(14) 0.0169(9) 0.0054(12) 0.0005(10) C56A 0.0835(14) 0.0508(10) 0.0994(14) 0.0169(9) 0.0054(12) 0.0005(10) C57 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C58 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C59 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C60 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C57A 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C58A 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C59A 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C60A 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C61 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C62 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C63 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C64 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C61A 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C62A 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C63A 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) C64A 0.0657(8) 0.0843(9) 0.0696(8) -0.0014(7) 0.0056(6) 0.0167(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C28 1.385(3) . ? C1 C24 1.388(3) . ? C1 C2 1.519(3) . ? C2 C3 1.516(3) . ? C3 C4 1.387(3) . ? C3 C25 1.388(3) . ? C4 C5 1.390(3) . ? C5 C6 1.395(4) . ? C5 C49 1.539(6) . ? C6 C7 1.389(3) . ? C7 C25 1.386(3) . ? C7 C8 1.506(3) . ? C8 C9 1.520(3) . ? C9 C26 1.390(3) . ? C9 C10 1.392(3) . ? C10 C11 1.385(4) . ? C11 C12 1.394(3) . ? C11 C53 1.571(5) . ? C12 C13 1.390(3) . ? C13 C26 1.391(3) . ? C13 C14 1.516(3) . ? C14 C15 1.496(3) . ? C15 C16 1.390(3) . ? C15 C27 1.397(3) . ? C16 C17 1.398(3) . ? C17 C18 1.367(3) . ? C17 C57 1.550(6) . ? C18 C19 1.401(3) . ? C19 C27 1.378(3) . ? C19 C20 1.521(3) . ? C20 C21 1.528(3) . ? C21 C28 1.384(3) . ? C21 C22 1.388(3) . ? C22 C23 1.386(3) . ? C23 C24 1.388(3) . ? C23 C61 1.521(7) . ? C25 O1 1.386(5) . ? C26 O2 1.393(3) . ? C27 O3 1.388(3) . ? C28 O4 1.387(3) . ? O1 C29 1.473(6) . ? C29 C30 1.463(6) . ? C30 C31 1.521(6) . ? O1A C29A 1.463(7) . ? C29A C30A 1.469(7) . ? C30A C31A 1.533(7) . ? O1B C29B 1.451(9) . ? C29B C30B 1.469(9) . ? C30B C31B 1.523(9) . ? O2 C32 1.422(3) . ? C32 C33 1.493(3) . ? C33 C34 1.522(4) . ? O3 C35 1.433(3) . ? C35 C36 1.486(3) . ? C36 C37 1.373(3) . ? C36 C41 1.400(4) . ? C37 C38 1.394(4) . ? C38 C39 1.355(4) . ? C39 C40 1.385(4) . ? C40 C41 1.376(4) . ? O4 C42 1.420(3) . ? C42 C43 1.503(4) . ? C43 C44 1.362(4) . ? C43 C48 1.376(4) . ? C44 C45 1.393(5) . ? C45 C46 1.376(5) . ? C46 C47 1.380(4) . ? C47 C48 1.387(4) . ? C49 C50 1.527(6) . ? C49 C52 1.530(6) . ? C49 C51 1.566(6) . ? C49A C50A 1.500(11) . ? C49A C52A 1.503(11) . ? C49A C51A 1.626(11) . ? C53 C55 1.510(6) . ? C53 C56 1.528(6) . ? C53 C54 1.538(6) . ? C53A C55A 1.483(11) . ? C53A C56A 1.490(11) . ? C53A C54A 1.600(12) . ? C57 C59 1.513(8) . ? C57 C58 1.543(7) . ? C57 C60 1.559(7) . ? C57A C58A 1.512(9) . ? C57A C60A 1.531(9) . ? C57A C59A 1.555(10) . ? C61 C64 1.510(8) . ? C61 C62 1.516(7) . ? C61 C63 1.583(8) . ? C61A C63A 1.526(9) . ? C61A C64A 1.526(9) . ? C61A C62A 1.550(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 C28 C1 C24 118.3(2) . . ? C28 C1 C2 121.1(2) . . ? C24 C1 C2 120.6(2) . . ? C3 C2 C1 114.15(18) . . ? C4 C3 C25 118.6(2) . . ? C4 C3 C2 120.7(2) . . ? C25 C3 C2 120.6(2) . . ? C3 C4 C5 122.8(2) . . ? C4 C5 C6 115.8(2) . . ? C4 C5 C49 121.4(3) . . ? C6 C5 C49 122.7(3) . . ? C7 C6 C5 123.5(2) . . ? C25 C7 C6 117.7(2) . . ? C25 C7 C8 121.3(2) . . ? C6 C7 C8 120.9(2) . . ? C7 C8 C9 112.9(2) . . ? C26 C9 C10 118.4(2) . . ? C26 C9 C8 121.3(2) . . ? C10 C9 C8 120.3(2) . . ? C11 C10 C9 122.5(2) . . ? C10 C11 C12 116.6(2) . . ? C10 C11 C53 125.1(3) . . ? C12 C11 C53 118.3(3) . . ? C13 C12 C11 123.5(2) . . ? C12 C13 C26 117.4(2) . . ? C12 C13 C14 116.4(2) . . ? C26 C13 C14 126.3(2) . . ? C15 C14 C13 123.0(2) . . ? C16 C15 C27 117.8(2) . . ? C16 C15 C14 120.4(2) . . ? C27 C15 C14 121.7(2) . . ? C15 C16 C17 122.7(2) . . ? C18 C17 C16 117.0(2) . . ? C18 C17 C57 120.6(3) . . ? C16 C17 C57 122.4(3) . . ? C17 C18 C19 122.7(2) . . ? C27 C19 C18 118.4(2) . . ? C27 C19 C20 121.4(2) . . ? C18 C19 C20 120.1(2) . . ? C19 C20 C21 110.43(19) . . ? C28 C21 C22 118.2(2) . . ? C28 C21 C20 121.4(2) . . ? C22 C21 C20 120.3(2) . . ? C23 C22 C21 122.7(2) . . ? C22 C23 C24 116.8(2) . . ? C22 C23 C61 121.4(3) . . ? C24 C23 C61 121.5(3) . . ? C23 C24 C1 122.5(2) . . ? C7 C25 O1 121.0(3) . . ? C7 C25 C3 121.1(2) . . ? O1 C25 C3 117.9(3) . . ? C9 C26 C13 121.6(2) . . ? C9 C26 O2 117.8(2) . . ? C13 C26 O2 120.55(19) . . ? C19 C27 O3 121.9(2) . . ? C19 C27 C15 121.1(2) . . ? O3 C27 C15 116.9(2) . . ? C21 C28 C1 121.3(2) . . ? C21 C28 O4 119.5(2) . . ? C1 C28 O4 119.14(19) . . ? C25 O1 C29 107.2(3) . . ? C30 C29 O1 111.9(4) . . ? C29 C30 C31 113.5(5) . . ? O1A C29A C30A 105.4(6) . . ? C29A C30A C31A 115.7(7) . . ? O1B C29B C30B 105.9(9) . . ? C29B C30B C31B 104.5(8) . . ? C26 O2 C32 113.08(17) . . ? O2 C32 C33 109.6(2) . . ? C32 C33 C34 110.7(2) . . ? C27 O3 C35 111.11(16) . . ? O3 C35 C36 111.5(2) . . ? C37 C36 C41 118.6(2) . . ? C37 C36 C35 123.5(2) . . ? C41 C36 C35 117.8(2) . . ? C36 C37 C38 119.8(3) . . ? C39 C38 C37 121.4(3) . . ? C38 C39 C40 119.2(3) . . ? C41 C40 C39 120.2(3) . . ? C40 C41 C36 120.5(3) . . ? C28 O4 C42 111.96(18) . . ? O4 C42 C43 110.2(2) . . ? C44 C43 C48 120.0(3) . . ? C44 C43 C42 118.3(3) . . ? C48 C43 C42 121.7(2) . . ? C43 C44 C45 120.3(3) . . ? C46 C45 C44 119.5(3) . . ? C45 C46 C47 120.3(3) . . ? C46 C47 C48 119.2(3) . . ? C43 C48 C47 120.4(3) . . ? C50 C49 C52 110.0(4) . . ? C50 C49 C5 113.5(4) . . ? C52 C49 C5 105.6(3) . . ? C50 C49 C51 106.5(4) . . ? C52 C49 C51 111.8(4) . . ? C5 C49 C51 109.5(4) . . ? C50A C49A C52A 111.9(9) . . ? C50A C49A C51A 105.4(7) . . ? C52A C49A C51A 96.2(7) . . ? C55 C53 C56 110.9(4) . . ? C55 C53 C54 109.2(4) . . ? C56 C53 C54 106.8(4) . . ? C55 C53 C11 112.3(4) . . ? C56 C53 C11 107.9(3) . . ? C54 C53 C11 109.6(4) . . ? C55A C53A C56A 116.5(8) . . ? C55A C53A C54A 105.9(8) . . ? C56A C53A C54A 105.1(8) . . ? C59 C57 C58 108.5(5) . . ? C59 C57 C17 112.2(4) . . ? C58 C57 C17 108.3(4) . . ? C59 C57 C60 106.7(5) . . ? C58 C57 C60 106.6(4) . . ? C17 C57 C60 114.2(4) . . ? C58A C57A C60A 110.6(6) . . ? C58A C57A C59A 108.8(6) . . ? C60A C57A C59A 109.4(6) . . ? C64 C61 C62 109.3(5) . . ? C64 C61 C23 114.0(4) . . ? C62 C61 C23 113.0(5) . . ? C64 C61 C63 106.3(5) . . ? C62 C61 C63 105.5(5) . . ? C23 C61 C63 108.2(5) . . ? C63A C61A C64A 109.9(6) . . ? C63A C61A C62A 112.1(6) . . ? C64A C61A C62A 108.6(6) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 77.70 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.644 _refine_diff_density_min -0.541 _refine_diff_density_rms 0.063