# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 data_para-acyl-calix[4]-arene _audit_creation_method SHELXL #_chemical_absolute_configuration unk??? _chemical_name_systematic 'para-octanoyl-calix[4]-arene' ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C60 H78 O8' _chemical_formula_weight 927.22 _chemical_melting_point ? _chemical_compound_source ? 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' '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' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic ??? _symmetry_space_group_name_H-M 'P 21/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 11.588(5) _cell_length_b 15.685(7) _cell_length_c 29.496(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.44(3) _cell_angle_gamma 90.00 _cell_volume 5327.2 _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 prism _exptl_crystal_colour pale pink _cell_angle_beta 96.44(3) _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method ? _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 0.075 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Nonius kappaCCD diffractometer' _diffrn_measurement_method 'area-detector scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16357 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.0875 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 24.23 _reflns_number_total 8428 _reflns_number_gt 4140 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; 'DENZO (Otwinovski & Minor,1997) COLLECT (Hooft,1998)' _computing_cell_refinement ; 'DENZO (Otwinovski & Minor,1997) COLLECT (Hooft,1998)' _computing_data_reduction 'HKL package (Otwinovski & Minor,1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'R3M (RICHE,1983)' _computing_publication_material 'SHELXL-93 (Sheldrick,1993)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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. Disorder is observed on one of the four octanoyl chain. Two sites are located for CD14 , CD14' and CD15 , CD15' ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1303P)^2^+3.1712P] 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 8423 _refine_ls_number_parameters 644 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1886 _refine_ls_R_factor_gt 0.0897 _refine_ls_wR_factor_all 0.2817 _refine_ls_wR_factor_ref 0.2203 _refine_ls_goodness_of_fit_all 1.004 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.034 _refine_ls_restrained_S_obs 1.189 _refine_ls_shift/su_max -0.273 _refine_ls_shift/esd_mean 0.009 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group OA O 0.2307(3) 0.5512(2) 0.29912(10) 0.0714(9) Uani 1 d . . HOA H 0.2296 0.5974 0.3004 0.086 Uiso 1 d G . OB O 0.4508(3) 0.5495(2) 0.27568(9) 0.0698(9) Uani 1 d . . HOB H 0.3909 0.5413 0.2860 0.084 Uiso 1 d G . OC O 0.2332(2) 0.7236(2) 0.30088(10) 0.0753(10) Uani 1 d . . HOC H 0.2897 0.7301 0.2952 0.090 Uiso 1 d G . OD O 0.4525(3) 0.7198(2) 0.27632(11) 0.0755(10) Uani 1 d . . HOD H 0.4565 0.6766 0.2791 0.091 Uiso 1 d G . CA1 C 0.1508(3) 0.5205(2) 0.26514(12) 0.0549(10) Uani 1 d . . CA2 C 0.1800(3) 0.4491(2) 0.24126(12) 0.0504(10) Uani 1 d . . CA3 C 0.0982(3) 0.4185(2) 0.20723(13) 0.0543(10) Uani 1 d . . HA3 H 0.1164 0.3711 0.19051 0.065 Uiso 1 calc R . CA4 C -0.0103(3) 0.4565(3) 0.19725(13) 0.0567(10) Uani 1 d . . CA5 C -0.0366(3) 0.5273(3) 0.22243(13) 0.0583(11) Uani 1 d . . HA5 H -0.1094 0.5524 0.21650 0.070 Uiso 1 calc R . CA6 C 0.0431(3) 0.5615(3) 0.25622(13) 0.0555(10) Uani 1 d . . CA7 C -0.0997(4) 0.4234(3) 0.16138(14) 0.0643(11) Uani 1 d . . OA8 O -0.1986(3) 0.4491(2) 0.15906(11) 0.0879(10) Uani 1 d . . CA9 C -0.0638(4) 0.3624(3) 0.1261(2) 0.0788(13) Uani 1 d . . HA9 H -0.1327 0.3405 0.1082 0.095 Uiso 1 calc R . HA9 H -0.0232 0.3145 0.1414 0.095 Uiso 1 calc R . CA10 C 0.0147(5) 0.4044(4) 0.0943(2) 0.095(2) Uani 1 d . . HA10 H -0.0145 0.4612 0.0870 0.114 Uiso 1 calc R . HA10 H 0.0918 0.4103 0.1106 0.114 Uiso 1 calc R . CA11 C 0.0250(5) 0.3583(3) 0.0510(2) 0.091(2) Uani 1 d . . HA11 H -0.0514 0.3559 0.0338 0.109 Uiso 1 calc R . HA11 H 0.0485 0.3001 0.0583 0.109 Uiso 1 calc R . CA12 C 0.1075(5) 0.3947(4) 0.0208(2) 0.095(2) Uani 1 d D . HA12 H 0.0899 0.4548 0.0166 0.114 Uiso 1 calc R . HA12 H 0.1852 0.3906 0.0368 0.114 Uiso 1 calc R . CA13 C 0.1092(5) 0.3559(3) -0.0249(2) 0.094(2) Uani 1 d D . HA13 H 0.1243 0.2954 -0.0206 0.113 Uiso 1 calc R . HA13 H 0.0319 0.3614 -0.0410 0.113 Uiso 1 calc R . CA14 C 0.1926(5) 0.3894(4) -0.0548(2) 0.105(2) Uani 1 d D . HA14 H 0.2703 0.3795 -0.0398 0.126 Uiso 1 calc R . HA14 H 0.1819 0.4507 -0.0570 0.126 Uiso 1 calc R . CA15 C 0.1873(6) 0.3550(4) -0.1018(2) 0.115(2) Uani 1 d D . HA15 H 0.2476 0.3803 -0.1171 0.138 Uiso 1 calc R . HA15 H 0.1131 0.3680 -0.1181 0.138 Uiso 1 calc R . HA15 H 0.1978 0.2943 -0.1005 0.138 Uiso 1 calc R . CB1 C 0.4519(3) 0.5157(3) 0.23239(12) 0.0538(10) Uani 1 d . . CB2 C 0.5271(3) 0.5526(2) 0.20443(13) 0.0547(10) Uani 1 d . . CB3 C 0.5337(3) 0.5159(2) 0.16177(13) 0.0573(11) Uani 1 d . . HB3 H 0.5843 0.5387 0.14264 0.069 Uiso 1 calc R . CB4 C 0.4662(3) 0.4459(3) 0.14731(14) 0.0590(11) Uani 1 d . . CB5 C 0.3919(3) 0.4121(3) 0.17656(14) 0.0615(11) Uani 1 d . . HB5 H 0.3466 0.3651 0.16702 0.074 Uiso 1 calc R . CB6 C 0.3830(3) 0.4455(2) 0.21899(13) 0.0527(10) Uani 1 d . . CB7 C 0.4721(4) 0.4046(3) 0.1022(2) 0.0751(13) Uani 1 d . . OB8 O 0.3984(4) 0.3524(3) 0.08853(14) 0.135(2) Uani 1 d . . CB9 C 0.5616(4) 0.4289(3) 0.07293(14) 0.0703(12) Uani 1 d . . HB9 H 0.6373 0.4208 0.09007 0.084 Uiso 1 calc R . HB9 H 0.5533 0.4892 0.06601 0.084 Uiso 1 calc R . CB10 C 0.5588(4) 0.3802(3) 0.02826(14) 0.0752(13) Uani 1 d . . HB10 H 0.5672 0.3198 0.03507 0.090 Uiso 1 calc R . HB10 H 0.4833 0.3884 0.01099 0.090 Uiso 1 calc R . CB11 C 0.6504(4) 0.4057(3) -0.00094(14) 0.0748(13) Uani 1 d . . HB11 H 0.7259 0.3967 0.01621 0.090 Uiso 1 calc R . HB11 H 0.6428 0.4662 -0.00729 0.090 Uiso 1 calc R . CB12 C 0.6471(4) 0.3587(3) -0.04560(14) 0.0730(12) Uani 1 d D . HB12 H 0.6567 0.2983 -0.03916 0.088 Uiso 1 calc R . HB12 H 0.5709 0.3664 -0.06233 0.088 Uiso 1 calc R . CB13 C 0.7369(4) 0.3852(3) -0.07579(14) 0.0740(13) Uani 1 d D . HB13 H 0.7269 0.4455 -0.08232 0.089 Uiso 1 calc R . HB13 H 0.8130 0.3779 -0.05888 0.089 Uiso 1 calc R . CB14 C 0.7354(4) 0.3391(3) -0.11970(15) 0.0804(14) Uani 1 d D . HB14 H 0.7494 0.2792 -0.11306 0.096 Uiso 1 calc R . HB14 H 0.6580 0.3439 -0.13583 0.096 Uiso 1 calc R . CB15 C 0.8194(5) 0.3676(3) -0.1507(2) 0.100(2) Uani 1 d D . HB15 H 0.8100 0.3340 -0.1781 0.119 Uiso 1 calc R . HB15 H 0.8970 0.3607 -0.1359 0.119 Uiso 1 calc R . HB15 H 0.8060 0.4265 -0.1582 0.119 Uiso 1 calc R . CC1 C 0.1596(3) 0.7586(3) 0.26577(13) 0.0603(11) Uani 1 d . . CC2 C 0.1946(3) 0.8280(3) 0.24144(13) 0.0569(10) Uani 1 d . . CC3 C 0.1164(4) 0.8600(2) 0.20722(14) 0.0612(11) Uani 1 d . . HC3 H 0.1387 0.9061 0.19039 0.073 Uiso 1 calc R . CC4 C 0.0052(4) 0.8267(3) 0.19654(14) 0.0630(11) Uani 1 d . . CC5 C -0.0257(4) 0.7574(3) 0.22193(13) 0.0611(11) Uani 1 d . . HC5 H -0.0999 0.7347 0.21559 0.073 Uiso 1 calc R . CC6 C 0.0495(3) 0.7210(3) 0.25625(13) 0.0575(10) Uani 1 d . . CC7 C -0.0799(4) 0.8625(3) 0.16006(15) 0.0704(12) Uani 1 d . . OC8 O -0.1822(3) 0.8426(2) 0.15849(11) 0.0906(10) Uani 1 d . . CC9 C -0.0381(4) 0.9171(3) 0.1237(2) 0.090(2) Uani 1 d . . HC9 H 0.0105 0.9623 0.1377 0.108 Uiso 1 calc R . HC9 H -0.1042 0.9431 0.1058 0.108 Uiso 1 calc R . CC10 C 0.0315(6) 0.8646(3) 0.0920(2) 0.104(2) Uani 1 d . . HC10 H 0.1017 0.8447 0.1099 0.124 Uiso 1 calc R . HC10 H -0.0140 0.8146 0.0823 0.124 Uiso 1 calc R . CC11 C 0.0652(5) 0.9068(4) 0.0511(2) 0.115(2) Uani 1 d . . HC11 H -0.0052 0.9252 0.0328 0.138 Uiso 1 calc R . HC11 H 0.1087 0.9577 0.0608 0.138 Uiso 1 calc R . CC12 C 0.1338(6) 0.8579(4) 0.0219(2) 0.125(2) Uani 1 d D . HC12 H 0.0901 0.8066 0.0132 0.150 Uiso 1 calc R . HC12 H 0.2036 0.8400 0.0407 0.150 Uiso 1 calc R . CC13 C 0.1706(7) 0.8936(5) -0.0198(2) 0.141(3) Uani 1 d D . HC13 H 0.1008 0.9116 -0.0387 0.169 Uiso 1 calc R . HC13 H 0.2145 0.9449 -0.0112 0.169 Uiso 1 calc R . CC14 C 0.2383(7) 0.8447(5) -0.0486(2) 0.158(3) Uani 1 d D . HC14 H 0.3071 0.8260 -0.0293 0.190 Uiso 1 calc R . HC14 H 0.1937 0.7937 -0.0572 0.190 Uiso 1 calc R . CC15 C 0.2769(9) 0.8768(6) -0.0889(3) 0.203(4) Uani 1 d D . HC15 H 0.3309 0.8375 -0.0999 0.244 Uiso 1 calc R . HC15 H 0.3144 0.9308 -0.0827 0.244 Uiso 1 calc R . HC15 H 0.2116 0.8841 -0.1117 0.244 Uiso 1 calc R . CD1 C 0.4635(3) 0.7533(3) 0.23383(13) 0.0574(11) Uani 1 d . . CD2 C 0.3996(3) 0.8268(3) 0.22114(14) 0.0612(11) Uani 1 d . . CD3 C 0.4144(4) 0.8625(3) 0.1794(2) 0.0681(12) Uani 1 d . . HD3 H 0.3730 0.9115 0.1703 0.082 Uiso 1 calc R . CD4 C 0.4876(4) 0.8282(3) 0.1508(2) 0.0689(12) Uani 1 d . . CD5 C 0.5491(3) 0.7541(3) 0.16496(14) 0.0596(11) Uani 1 d . . HD5 H 0.5996 0.7307 0.14597 0.072 Uiso 1 calc R . CD6 C 0.5375(3) 0.7145(3) 0.20603(13) 0.0565(10) Uani 1 d . . CD7 C 0.4999(5) 0.8672(3) 0.1057(2) 0.098(2) Uani 1 d . . OD8 O 0.4310(6) 0.9239(4) 0.0926(2) 0.200(3) Uani 1 d . . CD9 C 0.5830(4) 0.8359(3) 0.0754(2) 0.0830(14) Uani 1 d . . CD10 C 0.5790(6) 0.8778(4) 0.0296(2) 0.113(2) Uani 1 d . . HD10 H 0.5017 0.8703 0.0137 0.136 Uiso 1 calc R . HD10 H 0.5914 0.9385 0.0342 0.136 Uiso 1 calc R . CD11 C 0.6630(6) 0.8465(4) 0.0003(2) 0.113(2) Uani 1 d . . HD11 H 0.7399 0.8574 0.0159 0.135 Uiso 1 calc R . HD11 H 0.6541 0.7851 -0.0018 0.135 Uiso 1 calc R . CD12 C 0.6605(8) 0.8792(5) -0.0457(2) 0.161(3) Uani 1 d D . HD12 H 0.5837 0.8684 -0.0613 0.193 Uiso 1 calc R . HD12 H 0.6697 0.9406 -0.0436 0.193 Uiso 1 calc R . CD13 C 0.7424(9) 0.8482(6) -0.0738(2) 0.187(4) Uani 1 d D . HD13 H 0.7145 0.7920 -0.0834 0.224 Uiso 1 calc R 1 HD13 H 0.8128 0.8389 -0.0534 0.224 Uiso 1 calc R 1 CD14 C 0.7809(23) 0.8869(16) -0.1146(7) 0.243(11) Uiso 0.50 d PD 1 H14 H 0.7330 0.9360 -0.1238 0.292 Uiso 0.50 calc PR 1 H14 H 0.8608 0.9057 -0.1083 0.292 Uiso 0.50 calc PR 1 CD15 C 0.7717(16) 0.8274(11) -0.1486(5) 0.166(6) Uiso 0.50 d PD 1 H15 H 0.8235 0.7808 -0.1402 0.200 Uiso 0.50 calc PR 1 H15 H 0.7919 0.8529 -0.1762 0.200 Uiso 0.50 calc PR 1 H15 H 0.6933 0.8067 -0.1534 0.200 Uiso 0.50 calc PR 1 CD14'C 0.6872(16) 0.8672(12) -0.1270(5) 0.163(6) Uiso 0.50 d PD 2 H14' H 0.6648 0.8136 -0.1418 0.196 Uiso 0.50 calc PR 2 H14' H 0.6178 0.9017 -0.1268 0.196 Uiso 0.50 calc PR 2 CD15'C 0.7572(19) 0.9049(15) -0.1495(7) 0.229(10) Uiso 0.50 d PD 2 H15' H 0.7313 0.9000 -0.1815 0.275 Uiso 0.50 calc PR 2 H15' H 0.8327 0.8796 -0.1432 0.275 Uiso 0.50 calc PR 2 H15' H 0.7611 0.9640 -0.1410 0.275 Uiso 0.50 calc PR 2 CAB C 0.2987(3) 0.4079(3) 0.24938(14) 0.0620(11) Uani 1 d . . HAB H 0.2912 0.3472 0.24361 0.074 Uiso 1 calc R . HAB H 0.3295 0.4156 0.28108 0.074 Uiso 1 calc R . CAC C 0.0147(4) 0.6421(3) 0.28091(14) 0.0666(12) Uani 1 d . . HAC H -0.0680 0.6440 0.28336 0.080 Uiso 1 calc R . HAC H 0.0551 0.6414 0.31155 0.080 Uiso 1 calc R . CBD C 0.5996(3) 0.6317(2) 0.21851(14) 0.0599(11) Uani 1 d . . HBD H 0.6209 0.6303 0.25126 0.072 Uiso 1 calc R . HBD H 0.6706 0.6298 0.20402 0.072 Uiso 1 calc R . CCD C 0.3148(4) 0.8657(3) 0.2511(2) 0.0672(12) Uani 1 d . . HCD H 0.3433 0.8562 0.2829 0.081 Uiso 1 calc R . HCD H 0.3107 0.9267 0.2459 0.081 Uiso 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 OA 0.074(2) 0.077(2) 0.061(2) -0.003(2) 0.001(2) -0.001(2) OB 0.063(2) 0.090(2) 0.057(2) 0.005(2) 0.011(2) 0.003(2) OC 0.063(2) 0.095(2) 0.068(2) -0.010(2) 0.003(2) 0.000(2) OD 0.076(2) 0.080(2) 0.069(2) -0.002(2) 0.003(2) -0.003(2) CA1 0.052(3) 0.060(3) 0.054(2) 0.004(2) 0.011(2) -0.007(2) CA2 0.047(2) 0.052(2) 0.053(2) 0.012(2) 0.011(2) 0.000(2) CA3 0.058(3) 0.052(2) 0.057(2) 0.007(2) 0.023(2) -0.003(2) CA4 0.055(3) 0.061(3) 0.055(2) 0.012(2) 0.014(2) -0.004(2) CA5 0.046(3) 0.064(3) 0.068(3) 0.006(2) 0.017(2) 0.001(2) CA6 0.050(3) 0.063(3) 0.057(2) 0.002(2) 0.020(2) 0.002(2) CA7 0.054(3) 0.070(3) 0.069(3) 0.004(2) 0.010(2) -0.005(2) OA8 0.056(2) 0.109(3) 0.097(2) -0.006(2) 0.001(2) 0.003(2) CA9 0.066(3) 0.083(3) 0.085(3) -0.011(3) 0.002(3) -0.010(3) CA10 0.108(4) 0.105(4) 0.075(3) -0.008(3) 0.023(3) -0.016(3) CA11 0.087(4) 0.104(4) 0.084(3) -0.014(3) 0.013(3) -0.002(3) CA12 0.100(4) 0.106(4) 0.078(3) -0.008(3) 0.014(3) -0.006(3) CA13 0.093(4) 0.100(4) 0.092(4) -0.011(3) 0.021(3) -0.005(3) CA14 0.111(5) 0.110(4) 0.096(4) -0.007(3) 0.021(4) -0.014(4) CA15 0.130(5) 0.108(5) 0.112(5) -0.010(4) 0.043(4) -0.004(4) CB1 0.047(3) 0.066(3) 0.048(2) 0.007(2) 0.006(2) 0.014(2) CB2 0.041(2) 0.060(3) 0.063(3) 0.008(2) 0.002(2) 0.009(2) CB3 0.047(3) 0.062(3) 0.064(3) 0.006(2) 0.011(2) 0.009(2) CB4 0.051(3) 0.061(3) 0.065(3) 0.002(2) 0.006(2) 0.004(2) CB5 0.054(3) 0.056(3) 0.076(3) 0.004(2) 0.010(2) 0.001(2) CB6 0.045(2) 0.051(2) 0.062(3) 0.009(2) 0.008(2) 0.009(2) CB7 0.068(3) 0.079(3) 0.079(3) -0.016(3) 0.014(3) -0.015(3) OB8 0.137(4) 0.162(4) 0.116(3) -0.065(3) 0.061(3) -0.075(3) CB9 0.059(3) 0.086(3) 0.067(3) -0.006(2) 0.012(2) -0.005(2) CB10 0.068(3) 0.087(3) 0.073(3) -0.019(3) 0.019(2) -0.002(3) CB11 0.068(3) 0.090(3) 0.066(3) -0.011(3) 0.010(2) -0.002(3) CB12 0.070(3) 0.081(3) 0.069(3) -0.006(3) 0.012(2) 0.005(3) CB13 0.068(3) 0.087(3) 0.067(3) -0.010(3) 0.008(2) -0.005(3) CB14 0.078(3) 0.091(4) 0.076(3) -0.009(3) 0.021(3) -0.001(3) CB15 0.122(5) 0.102(4) 0.079(3) -0.007(3) 0.034(3) -0.004(3) CC1 0.056(3) 0.071(3) 0.054(2) -0.020(2) 0.006(2) 0.013(2) CC2 0.050(3) 0.056(3) 0.065(3) -0.014(2) 0.012(2) 0.003(2) CC3 0.062(3) 0.052(2) 0.070(3) -0.012(2) 0.014(2) 0.002(2) CC4 0.056(3) 0.063(3) 0.070(3) -0.016(2) 0.008(2) 0.003(2) CC5 0.049(3) 0.057(3) 0.079(3) -0.019(2) 0.014(2) -0.001(2) CC6 0.049(3) 0.061(3) 0.064(3) -0.014(2) 0.014(2) 0.005(2) CC7 0.063(3) 0.074(3) 0.073(3) -0.017(3) 0.003(3) 0.008(3) OC8 0.064(2) 0.112(3) 0.092(2) -0.006(2) -0.003(2) 0.002(2) CC9 0.075(3) 0.095(4) 0.098(4) 0.014(3) 0.003(3) 0.006(3) CC10 0.132(5) 0.094(4) 0.088(4) 0.005(3) 0.026(3) 0.001(3) CC11 0.126(5) 0.122(5) 0.098(4) 0.006(4) 0.017(4) 0.013(4) CC12 0.151(6) 0.127(5) 0.100(4) 0.000(4) 0.031(4) -0.001(5) CC13 0.168(7) 0.152(6) 0.106(5) 0.024(5) 0.033(5) 0.030(5) CC14 0.186(8) 0.191(8) 0.106(5) -0.006(5) 0.048(5) -0.004(6) CC15 0.246(11) 0.256(11) 0.113(6) 0.011(7) 0.046(7) 0.031(8) CD1 0.047(2) 0.059(3) 0.064(3) -0.010(2) -0.003(2) -0.013(2) CD2 0.049(3) 0.056(3) 0.077(3) -0.015(2) 0.002(2) -0.009(2) CD3 0.056(3) 0.058(3) 0.090(3) -0.005(3) 0.004(3) 0.002(2) CD4 0.065(3) 0.054(3) 0.087(3) 0.003(3) 0.008(3) -0.004(2) CD5 0.047(2) 0.061(3) 0.071(3) -0.004(2) 0.009(2) -0.006(2) CD6 0.042(2) 0.060(3) 0.067(3) -0.009(2) 0.001(2) -0.006(2) CD7 0.103(4) 0.074(3) 0.118(5) 0.039(3) 0.017(4) 0.026(3) OD8 0.261(7) 0.184(5) 0.176(5) 0.101(4) 0.117(5) 0.123(5) CD9 0.076(3) 0.102(4) 0.072(3) 0.018(3) 0.016(3) 0.003(3) CD10 0.123(5) 0.116(5) 0.101(4) 0.028(4) 0.014(4) 0.021(4) CD11 0.136(6) 0.110(5) 0.093(4) 0.022(4) 0.020(4) 0.000(4) CD12 0.235(10) 0.160(7) 0.093(5) 0.047(5) 0.041(6) 0.028(6) CD13 0.278(12) 0.200(9) 0.089(5) 0.024(5) 0.050(6) -0.028(8) CAB 0.059(3) 0.060(3) 0.068(3) 0.010(2) 0.010(2) 0.006(2) CAC 0.052(3) 0.080(3) 0.072(3) -0.006(2) 0.023(2) 0.002(2) CBD 0.040(2) 0.074(3) 0.065(2) 0.002(2) 0.003(2) 0.003(2) CCD 0.061(3) 0.059(3) 0.082(3) -0.023(2) 0.010(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag OA CA1 1.373(5) . ? OB CB1 1.384(5) . ? OC CC1 1.379(5) . ? OD CD1 1.378(5) . ? CA1 CA2 1.386(5) . ? CA1 CA6 1.402(5) . ? CA2 CA3 1.387(5) . ? CA2 CAB 1.514(5) . ? CA3 CA4 1.392(5) . ? CA4 CA5 1.389(5) . ? CA4 CA7 1.489(6) . ? CA5 CA6 1.388(5) . ? CA6 CAC 1.514(5) . ? CA7 OA8 1.211(5) . ? CA7 CA9 1.505(6) . ? CA9 CA10 1.528(6) . ? CA10 CA11 1.486(6) . ? CA11 CA12 1.490(7) . ? CA12 CA13 1.480(6) . ? CA13 CA14 1.477(7) . ? CA14 CA15 1.482(7) . ? CB1 CB6 1.391(5) . ? CB1 CB2 1.391(5) . ? CB2 CB3 1.394(5) . ? CB2 CBD 1.528(5) . ? CB3 CB4 1.387(5) . ? CB4 CB5 1.390(5) . ? CB4 CB7 1.489(6) . ? CB5 CB6 1.371(5) . ? CB6 CAB 1.517(5) . ? CB7 OB8 1.220(5) . ? CB7 CB9 1.471(6) . ? CB9 CB10 1.520(5) . ? CB10 CB11 1.495(6) . ? CB11 CB12 1.507(6) . ? CB12 CB13 1.502(6) . ? CB13 CB14 1.482(6) . ? CB14 CB15 1.477(6) . ? CC1 CC2 1.390(6) . ? CC1 CC6 1.404(6) . ? CC2 CC3 1.373(5) . ? CC2 CCD 1.511(5) . ? CC3 CC4 1.393(6) . ? CC4 CC5 1.389(6) . ? CC4 CC7 1.486(6) . ? CC5 CC6 1.383(5) . ? CC6 CAC 1.513(5) . ? CC7 OC8 1.221(5) . ? CC7 CC9 1.495(6) . ? CC9 CC10 1.539(7) . ? CC10 CC11 1.468(7) . ? CC11 CC12 1.455(8) . ? CC12 CC13 1.458(8) . ? CC13 CC14 1.441(9) . ? CC14 CC15 1.411(9) . ? CD1 CD6 1.392(6) . ? CD1 CD2 1.398(6) . ? CD2 CD3 1.381(6) . ? CD2 CCD 1.520(6) . ? CD3 CD4 1.371(6) . ? CD4 CD5 1.403(6) . ? CD4 CD7 1.485(7) . ? CD5 CD6 1.381(5) . ? CD6 CBD 1.510(5) . ? CD7 OD8 1.229(6) . ? CD7 CD9 1.468(7) . ? CD9 CD10 1.499(7) . ? CD10 CD11 1.457(8) . ? CD11 CD12 1.450(8) . ? CD12 CD13 1.414(11) . ? CD13 CD14 1.46(2) . ? CD13 CD14'1.65(2) . ? CD14 CD15 1.37(2) . ? CD14'CD15'1.25(2) . ? 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 OA CA1 CA2 118.1(4) . . ? OA CA1 CA6 119.3(4) . . ? CA2 CA1 CA6 122.6(4) . . ? CA1 CA2 CA3 117.5(4) . . ? CA1 CA2 CAB 122.3(4) . . ? CA3 CA2 CAB 120.1(4) . . ? CA2 CA3 CA4 122.2(4) . . ? CA5 CA4 CA3 118.4(4) . . ? CA5 CA4 CA7 118.8(4) . . ? CA3 CA4 CA7 122.8(4) . . ? CA6 CA5 CA4 121.7(4) . . ? CA5 CA6 CA1 117.7(4) . . ? CA5 CA6 CAC 120.4(4) . . ? CA1 CA6 CAC 121.9(4) . . ? OA8 CA7 CA4 120.2(4) . . ? OA8 CA7 CA9 120.4(4) . . ? CA4 CA7 CA9 119.2(4) . . ? CA7 CA9 CA10 112.3(4) . . ? CA11 CA10 CA9 115.5(4) . . ? CA10 CA11 CA12 116.5(5) . . ? CA13 CA12 CA11 117.4(5) . . ? CA14 CA13 CA12 118.3(5) . . ? CA13 CA14 CA15 117.9(5) . . ? OB CB1 CB6 120.0(4) . . ? OB CB1 CB2 117.3(4) . . ? CB6 CB1 CB2 122.6(4) . . ? CB1 CB2 CB3 117.7(4) . . ? CB1 CB2 CBD 122.5(4) . . ? CB3 CB2 CBD 119.8(4) . . ? CB4 CB3 CB2 121.3(4) . . ? CB3 CB4 CB5 118.6(4) . . ? CB3 CB4 CB7 122.5(4) . . ? CB5 CB4 CB7 118.9(4) . . ? CB6 CB5 CB4 122.4(4) . . ? CB5 CB6 CB1 117.5(4) . . ? CB5 CB6 CAB 120.6(4) . . ? CB1 CB6 CAB 121.8(4) . . ? OB8 CB7 CB9 119.6(4) . . ? OB8 CB7 CB4 119.1(4) . . ? CB9 CB7 CB4 121.2(4) . . ? CB7 CB9 CB10 115.5(4) . . ? CB11 CB10 CB9 114.6(4) . . ? CB10 CB11 CB12 115.0(4) . . ? CB13 CB12 CB11 115.6(4) . . ? CB14 CB13 CB12 116.2(4) . . ? CB15 CB14 CB13 116.7(4) . . ? OC CC1 CC2 120.5(4) . . ? OC CC1 CC6 117.1(4) . . ? CC2 CC1 CC6 122.5(4) . . ? CC3 CC2 CC1 117.4(4) . . ? CC3 CC2 CCD 120.9(4) . . ? CC1 CC2 CCD 121.7(4) . . ? CC2 CC3 CC4 123.1(4) . . ? CC5 CC4 CC3 117.4(4) . . ? CC5 CC4 CC7 119.7(4) . . ? CC3 CC4 CC7 123.0(4) . . ? CC6 CC5 CC4 122.5(4) . . ? CC5 CC6 CC1 117.2(4) . . ? CC5 CC6 CAC 120.6(4) . . ? CC1 CC6 CAC 122.1(4) . . ? OC8 CC7 CC4 119.6(5) . . ? OC8 CC7 CC9 120.7(4) . . ? CC4 CC7 CC9 119.6(4) . . ? CC7 CC9 CC10 111.3(4) . . ? CC11 CC10 CC9 117.6(5) . . ? CC12 CC11 CC10 117.5(6) . . ? CC11 CC12 CC13 121.9(6) . . ? CC14 CC13 CC12 121.4(7) . . ? CC15 CC14 CC13 123.4(8) . . ? OD CD1 CD6 119.6(4) . . ? OD CD1 CD2 117.3(4) . . ? CD6 CD1 CD2 123.1(4) . . ? CD3 CD2 CD1 117.2(4) . . ? CD3 CD2 CCD 120.6(4) . . ? CD1 CD2 CCD 122.1(4) . . ? CD4 CD3 CD2 122.5(4) . . ? CD3 CD4 CD5 118.0(4) . . ? CD3 CD4 CD7 121.2(4) . . ? CD5 CD4 CD7 120.8(5) . . ? CD6 CD5 CD4 122.6(4) . . ? CD5 CD6 CD1 116.5(4) . . ? CD5 CD6 CBD 120.7(4) . . ? CD1 CD6 CBD 122.8(4) . . ? OD8 CD7 CD9 119.9(5) . . ? OD8 CD7 CD4 117.0(6) . . ? CD9 CD7 CD4 122.8(4) . . ? CD7 CD9 CD10 116.4(5) . . ? CD11 CD10 CD9 115.5(5) . . ? CD12 CD11 CD10 119.4(6) . . ? CD13 CD12 CD11 118.9(7) . . ? CD12 CD13 CD14 128.8(14) . . ? CD12 CD13 C14' 106.3(10) . . ? CD15 CD14 CD13 108.4(19) . . ? CD15' CD14' CD13 112.6(16) . . ? CA2 CAB CB6 112.0(3) . . ? CC6 CAC CA6 111.6(3) . . ? CD6 CBD CB2 113.5(3) . . ? CC2 CCD CD2 112.1(3) . . ? _refine_diff_density_max 0.324 _refine_diff_density_min -0.266 _refine_diff_density_rms 0.042