# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2005 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name 'John Ripmeester' _publ_contact_author_address ; National Res Council Canada Steacie Inst Mol Sci, 100 Sussex Dr Ottawa ON K1A 0R6 CANADA ; _publ_contact_author_email JOHN.RIPMEESTER@NRC.CA _publ_section_title ; Guest-induced Chain Folding in Amphiphilic Calixarene Structures ; loop_ _publ_author_name 'John Ripmeester' A.W.Coleman 'Alix Dubes' 'Adina Lazar' 'Patrick Shahgaldian' ; K.A.Udachin ; data_ad7 _database_code_depnum_ccdc_archive 'CCDC 266645' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common p-hexanoyl-calix(4)arene.Nitrobenzene _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H69 N O10' _chemical_formula_weight 940.14 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 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 15.2643(9) _cell_length_b 19.8739(12) _cell_length_c 22.2367(10) _cell_angle_alpha 90.00 _cell_angle_beta 130.901(3) _cell_angle_gamma 90.00 _cell_volume 5098.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.083 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.9637 _exptl_absorpt_correction_T_max 0.9836 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _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 59868 _diffrn_reflns_av_R_equivalents 0.0517 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 28.73 _reflns_number_total 13161 _reflns_number_gt 8590 _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^)+(0.1156P)^2^+1.4910P] 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 13161 _refine_ls_number_parameters 764 _refine_ls_number_restraints 126 _refine_ls_R_factor_all 0.1040 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.2097 _refine_ls_wR_factor_gt 0.1802 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.025 _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 O7C O -0.0004(3) 0.2696(3) -0.1580(3) 0.0573(6) Uani 0.35 1 d PD A 1 C7C C 0.0776(4) 0.2462(3) -0.1534(3) 0.0345(6) Uani 0.35 1 d PD A 1 C8C C 0.0877(4) 0.2690(3) -0.2141(3) 0.0448(6) Uani 0.35 1 d PD A 1 H8C1 H 0.0110 0.2650 -0.2682 0.054 Uiso 0.35 1 calc PR A 1 H8C2 H 0.1424 0.2391 -0.2110 0.054 Uiso 0.35 1 calc PR A 1 C9C C 0.1298(5) 0.3417(4) -0.2003(4) 0.0605(8) Uani 0.35 1 d PD A 1 H9C1 H 0.1259 0.3562 -0.2446 0.073 Uiso 0.35 1 calc PR A 1 H9C2 H 0.0785 0.3714 -0.1995 0.073 Uiso 0.35 1 calc PR A 1 C10C C 0.2541(6) 0.3484(4) -0.1217(4) 0.0649(10) Uani 0.35 1 d PD A 1 H10A H 0.3027 0.3136 -0.1196 0.078 Uiso 0.35 1 calc PR A 1 H10B H 0.2554 0.3397 -0.0773 0.078 Uiso 0.35 1 calc PR A 1 C11C C 0.3069(8) 0.4180(4) -0.1103(5) 0.0928(15) Uani 0.35 1 d PD A 1 H11A H 0.2458 0.4525 -0.1326 0.111 Uiso 0.35 1 calc PR A 1 H11B H 0.3330 0.4197 -0.1409 0.111 Uiso 0.35 1 calc PR A 1 C12C C 0.4122(8) 0.4360(7) -0.0209(6) 0.128(3) Uani 0.35 1 d PD A 1 H12A H 0.4259 0.3989 0.0134 0.192 Uiso 0.35 1 calc PR A 1 H12B H 0.3945 0.4771 -0.0063 0.192 Uiso 0.35 1 calc PR A 1 H12C H 0.4816 0.4432 -0.0142 0.192 Uiso 0.35 1 calc PR A 1 O7G O 0.0244(5) 0.2812(4) -0.1383(3) 0.0573(6) Uani 0.25 1 d PD A 2 C7G C 0.0907(6) 0.2540(5) -0.1425(4) 0.0345(6) Uani 0.25 1 d PD A 2 C8G C 0.1018(7) 0.2782(6) -0.2018(5) 0.0448(6) Uani 0.25 1 d PD A 2 H8G1 H 0.0305 0.3025 -0.2458 0.054 Uiso 0.25 1 calc PR A 2 H8G2 H 0.1115 0.2392 -0.2246 0.054 Uiso 0.25 1 calc PR A 2 C9G C 0.2058(6) 0.3248(4) -0.1607(5) 0.0605(8) Uani 0.25 1 d PD A 2 H9G1 H 0.2775 0.2991 -0.1202 0.073 Uiso 0.25 1 calc PR A 2 H9G2 H 0.2104 0.3419 -0.2004 0.073 Uiso 0.25 1 calc PR A 2 C10G C 0.1981(7) 0.3833(4) -0.1213(5) 0.0649(10) Uani 0.25 1 d PD A 2 H10C H 0.1215 0.4051 -0.1607 0.078 Uiso 0.25 1 calc PR A 2 H10D H 0.2025 0.3660 -0.0777 0.078 Uiso 0.25 1 calc PR A 2 C11G C 0.2889(8) 0.4344(6) -0.0887(8) 0.0928(15) Uani 0.25 1 d PD A 2 H11C H 0.2700 0.4648 -0.0634 0.111 Uiso 0.25 1 calc PR A 2 H11D H 0.2580 0.4579 -0.1384 0.111 Uiso 0.25 1 calc PR A 2 C12G C 0.4135(10) 0.4494(10) -0.0397(10) 0.128(3) Uani 0.25 1 d PD A 2 H12D H 0.4588 0.4086 -0.0119 0.192 Uiso 0.25 1 calc PR A 2 H12E H 0.4361 0.4843 -0.0006 0.192 Uiso 0.25 1 calc PR A 2 H12F H 0.4284 0.4655 -0.0739 0.192 Uiso 0.25 1 calc PR A 2 O7H O 0.0052(5) 0.2731(5) -0.1627(4) 0.0573(6) Uani 0.31 1 d PD A 3 C7H C 0.0805(6) 0.2454(4) -0.1588(4) 0.0345(6) Uani 0.31 1 d PD A 3 C8H C 0.1065(7) 0.2758(5) -0.2074(5) 0.0448(6) Uani 0.31 1 d PD A 3 H8H1 H 0.0348 0.2732 -0.2640 0.054 Uiso 0.31 1 calc PR A 3 H8H2 H 0.1646 0.2467 -0.2012 0.054 Uiso 0.31 1 calc PR A 3 C9H C 0.1506(7) 0.3478(5) -0.1912(5) 0.0605(8) Uani 0.31 1 d PD A 3 H9H1 H 0.1554 0.3612 -0.2319 0.073 Uiso 0.31 1 calc PR A 3 H9H2 H 0.0939 0.3778 -0.1968 0.073 Uiso 0.31 1 calc PR A 3 C10H C 0.2678(8) 0.3578(5) -0.1098(5) 0.0649(10) Uani 0.31 1 d PD A 3 H10E H 0.3222 0.3237 -0.1012 0.078 Uiso 0.31 1 calc PR A 3 H10F H 0.2607 0.3506 -0.0690 0.078 Uiso 0.31 1 calc PR A 3 C11H C 0.3186(10) 0.4290(5) -0.0984(7) 0.0928(15) Uani 0.31 1 d PD A 3 H11E H 0.2822 0.4480 -0.1514 0.111 Uiso 0.31 1 calc PR A 3 H11F H 0.4028 0.4248 -0.0684 0.111 Uiso 0.31 1 calc PR A 3 C12H C 0.2998(9) 0.4788(7) -0.0536(7) 0.128(3) Uani 0.31 1 d PD A 3 H12G H 0.2180 0.4920 -0.0886 0.192 Uiso 0.31 1 calc PR A 3 H12H H 0.3480 0.5188 -0.0379 0.192 Uiso 0.31 1 calc PR A 3 H12I H 0.3216 0.4568 -0.0060 0.192 Uiso 0.31 1 calc PR A 3 O7I O -0.0061(11) 0.2620(15) -0.1582(13) 0.0573(6) Uani 0.09 1 d PD A 4 C7I C 0.0890(11) 0.2567(8) -0.1381(10) 0.0345(6) Uani 0.09 1 d PD A 4 C8I C 0.1253(13) 0.2970(7) -0.1755(9) 0.0448(6) Uani 0.09 1 d PD A 4 H8I1 H 0.0615 0.2946 -0.2339 0.054 Uiso 0.09 1 calc PR A 4 H8I2 H 0.1929 0.2740 -0.1633 0.054 Uiso 0.09 1 calc PR A 4 C9I C 0.1572(12) 0.3703(8) -0.1538(11) 0.0605(8) Uani 0.09 1 d PD A 4 H9I1 H 0.0857 0.3974 -0.1906 0.073 Uiso 0.09 1 calc PR A 4 H9I2 H 0.1853 0.3770 -0.0995 0.073 Uiso 0.09 1 calc PR A 4 C10I C 0.2471(14) 0.3979(10) -0.1558(10) 0.0649(10) Uani 0.09 1 d PD A 4 H10G H 0.2908 0.3599 -0.1538 0.078 Uiso 0.09 1 calc PR A 4 H10H H 0.2073 0.4217 -0.2069 0.078 Uiso 0.09 1 calc PR A 4 C11I C 0.3314(16) 0.4455(13) -0.0887(16) 0.0928(15) Uani 0.09 1 d PD A 4 H11G H 0.3612 0.4782 -0.1052 0.111 Uiso 0.09 1 calc PR A 4 H11H H 0.3978 0.4204 -0.0418 0.111 Uiso 0.09 1 calc PR A 4 C12I C 0.264(2) 0.483(2) -0.068(2) 0.128(3) Uani 0.09 1 d PD A 4 H12J H 0.2998 0.5266 -0.0444 0.192 Uiso 0.09 1 calc PR A 4 H12K H 0.2655 0.4557 -0.0307 0.192 Uiso 0.09 1 calc PR A 4 H12L H 0.1830 0.4895 -0.1171 0.192 Uiso 0.09 1 calc PR A 4 O7B O 0.3221(2) 0.31190(19) 0.30054(15) 0.0384(4) Uani 0.44 1 d PD B 5 C7B C 0.2633(3) 0.2837(2) 0.2362(2) 0.0310(4) Uani 0.44 1 d PD B 5 C8B C 0.1435(3) 0.3112(2) 0.1663(2) 0.0340(6) Uani 0.44 1 d PD B 5 H8B1 H 0.1364 0.3118 0.1187 0.041 Uiso 0.44 1 calc PR B 5 H8B2 H 0.0845 0.2795 0.1553 0.041 Uiso 0.44 1 calc PR B 5 C9B C 0.1147(4) 0.3810(2) 0.1767(2) 0.0464(7) Uani 0.44 1 d PD B 5 H9B1 H 0.1710 0.4138 0.1856 0.056 Uiso 0.44 1 calc PR B 5 H9B2 H 0.1214 0.3815 0.2241 0.056 Uiso 0.44 1 calc PR B 5 C10B C -0.0071(4) 0.4018(2) 0.1040(2) 0.0485(8) Uani 0.44 1 d PD B 5 H10E' H -0.0624 0.3684 0.0956 0.058 Uiso 0.44 1 calc PR B 5 H10F' H -0.0131 0.4001 0.0569 0.058 Uiso 0.44 1 calc PR B 5 C11B C -0.0439(4) 0.4715(2) 0.1084(3) 0.0557(9) Uani 0.44 1 d PD B 5 H11E' H -0.0420 0.4727 0.1538 0.067 Uiso 0.44 1 calc PR B 5 H11F' H 0.0130 0.5049 0.1191 0.067 Uiso 0.44 1 calc PR B 5 C12B C -0.1639(4) 0.4919(3) 0.0334(3) 0.0690(12) Uani 0.44 1 d PD B 5 H12G' H -0.1661 0.4920 -0.0116 0.083 Uiso 0.44 1 calc PR B 5 H12H' H -0.1820 0.5370 0.0403 0.083 Uiso 0.44 1 calc PR B 5 H12I' H -0.2211 0.4598 0.0231 0.083 Uiso 0.44 1 calc PR B 5 O7F O 0.3400(3) 0.3071(2) 0.31626(17) 0.0384(4) Uani 0.44 1 d PD B 6 C7F C 0.2764(3) 0.2834(3) 0.2494(2) 0.0310(4) Uani 0.44 1 d PD B 6 C8F C 0.1700(3) 0.3210(2) 0.1783(2) 0.0340(6) Uani 0.44 1 d PD B 6 H8F1 H 0.1806 0.3310 0.1398 0.041 Uiso 0.44 1 calc PR B 6 H8F2 H 0.1010 0.2918 0.1514 0.041 Uiso 0.44 1 calc PR B 6 C9F C 0.1491(4) 0.3865(3) 0.2028(2) 0.0464(7) Uani 0.44 1 d PD B 6 H9F1 H 0.2156 0.4170 0.2258 0.056 Uiso 0.44 1 calc PR B 6 H9F2 H 0.1455 0.3768 0.2448 0.056 Uiso 0.44 1 calc PR B 6 C10F C 0.0375(4) 0.4225(2) 0.1338(2) 0.0485(8) Uani 0.44 1 d PD B 6 H10G' H -0.0282 0.3910 0.1097 0.058 Uiso 0.44 1 calc PR B 6 H10H' H 0.0248 0.4609 0.1557 0.058 Uiso 0.44 1 calc PR B 6 C11F C 0.0351(4) 0.4483(2) 0.0693(2) 0.0557(9) Uani 0.44 1 d PD B 6 H11I H 0.0344 0.4095 0.0411 0.067 Uiso 0.44 1 calc PR B 6 H11J H 0.1067 0.4743 0.0939 0.067 Uiso 0.44 1 calc PR B 6 C12F C -0.0698(4) 0.4928(3) 0.0091(3) 0.0690(12) Uani 0.44 1 d PD B 6 H12J' H -0.1410 0.4686 -0.0124 0.083 Uiso 0.44 1 calc PR B 6 H12K' H -0.0712 0.5043 -0.0344 0.083 Uiso 0.44 1 calc PR B 6 H12L' H -0.0646 0.5341 0.0353 0.083 Uiso 0.44 1 calc PR B 6 O7L O 0.3090(10) 0.3169(7) 0.2869(6) 0.0384(4) Uani 0.12 1 d PD B 7 C7L C 0.2490(11) 0.2835(7) 0.2267(7) 0.0310(4) Uani 0.12 1 d PD B 7 C8L C 0.1474(11) 0.3179(7) 0.1525(8) 0.0340(6) Uani 0.12 1 d PD B 7 H8L1 H 0.0780 0.2894 0.1274 0.041 Uiso 0.12 1 calc PR B 7 H8L2 H 0.1615 0.3206 0.1149 0.041 Uiso 0.12 1 calc PR B 7 C9L C 0.1204(12) 0.3889(8) 0.1636(8) 0.0464(7) Uani 0.12 1 d PD B 7 H9L1 H 0.1260 0.3896 0.2105 0.056 Uiso 0.12 1 calc PR B 7 H9L2 H 0.1780 0.4211 0.1732 0.056 Uiso 0.12 1 calc PR B 7 C10L C -0.0008(13) 0.4102(7) 0.0899(9) 0.0485(8) Uani 0.12 1 d PD B 7 H10I H -0.0589 0.3852 0.0877 0.058 Uiso 0.12 1 calc PR B 7 H10J H -0.0127 0.3987 0.0417 0.058 Uiso 0.12 1 calc PR B 7 C11L C -0.0187(12) 0.4868(7) 0.0909(9) 0.0557(9) Uani 0.12 1 d PD B 7 H11G' H -0.0081 0.4985 0.1386 0.067 Uiso 0.12 1 calc PR B 7 H11H' H 0.0391 0.5121 0.0930 0.067 Uiso 0.12 1 calc PR B 7 C12L C -0.1417(15) 0.5056(10) 0.0154(10) 0.0690(12) Uani 0.12 1 d PD B 7 H12M H -0.1851 0.4647 -0.0137 0.083 Uiso 0.12 1 calc PR B 7 H12N H -0.1373 0.5343 -0.0184 0.083 Uiso 0.12 1 calc PR B 7 H12O H -0.1811 0.5300 0.0301 0.083 Uiso 0.12 1 calc PR B 7 O1N O 0.60275(17) 0.33808(12) 0.37689(9) 0.1046(8) Uani 1 1 d . C 8 N1N N 0.52814(13) 0.36925(8) 0.31648(9) 0.0512(4) Uani 1 1 d . C 8 C2N C 0.47969(13) 0.33842(8) 0.24008(9) 0.0387(4) Uani 1 1 d . C 8 C3N C 0.38460(15) 0.36776(10) 0.17107(10) 0.0508(5) Uani 1 1 d . C 8 H3N H 0.3518 0.4079 0.1721 0.061 Uiso 1 1 calc R C 8 C4N C 0.33826(19) 0.33671(13) 0.10002(12) 0.0670(7) Uani 1 1 d . C 8 H4N H 0.2716 0.3553 0.0513 0.080 Uiso 1 1 calc R C 8 C5N C 0.38803(18) 0.27868(13) 0.09918(12) 0.0625(6) Uani 1 1 d . C 8 H5N H 0.3557 0.2580 0.0500 0.075 Uiso 1 1 calc R C 8 C6N C 0.48375(14) 0.25126(11) 0.16920(11) 0.0525(5) Uani 1 1 d . C 8 H6N H 0.5183 0.2119 0.1684 0.063 Uiso 1 1 calc R C 8 C7N C 0.53003(14) 0.28039(9) 0.24068(10) 0.0461(4) Uani 1 1 d . C 8 H7N H 0.5953 0.2610 0.2895 0.055 Uiso 1 1 calc R C 8 O1N1 O 0.48988(12) 0.42234(7) 0.31670(8) 0.0628(4) Uani 1 1 d . C 8 O7D O 0.61744(11) 0.31194(9) 0.01290(8) 0.0507(4) Uani 0.89 1 d PD A 9 C7D C 0.67954(14) 0.29030(11) 0.08124(11) 0.0395(5) Uani 0.89 1 d PD A 9 C8D C 0.77759(16) 0.33306(12) 0.14847(12) 0.0481(5) Uani 0.89 1 d PD A 9 H8D1 H 0.7987 0.3672 0.1274 0.058 Uiso 0.89 1 calc PR A 9 H8D2 H 0.8464 0.3045 0.1870 0.058 Uiso 0.89 1 calc PR A 9 C9D C 0.74082(18) 0.36832(12) 0.19060(13) 0.0554(5) Uani 0.89 1 d PD A 9 H9D1 H 0.6701 0.3953 0.1514 0.067 Uiso 0.89 1 calc PR A 9 H9D2 H 0.7221 0.3340 0.2129 0.067 Uiso 0.89 1 calc PR A 9 C10D C 0.8367(2) 0.41407(13) 0.25726(15) 0.0691(6) Uani 0.89 1 d PD A 9 H10K H 0.9079 0.3871 0.2952 0.083 Uiso 0.89 1 calc PR A 9 H10L H 0.8537 0.4489 0.2343 0.083 Uiso 0.89 1 calc PR A 9 C11D C 0.8058(2) 0.44835(14) 0.30206(16) 0.0773(7) Uani 0.89 1 d PD A 9 H11I' H 0.8651 0.4829 0.3375 0.093 Uiso 0.89 1 calc PR A 9 H11J' H 0.7306 0.4717 0.2633 0.093 Uiso 0.89 1 calc PR A 9 C12D C 0.7972(2) 0.40213(15) 0.35065(15) 0.0738(7) Uani 0.89 1 d PD A 9 H12P H 0.7377 0.3680 0.3160 0.111 Uiso 0.89 1 calc PR A 9 H12Q H 0.7761 0.4279 0.3771 0.111 Uiso 0.89 1 calc PR A 9 H12R H 0.8720 0.3800 0.3908 0.111 Uiso 0.89 1 calc PR A 9 O7K O 0.5914(12) 0.3176(9) 0.0125(7) 0.0507(4) Uani 0.11 1 d PD A 10 C7K C 0.6604(15) 0.2948(7) 0.0786(8) 0.0395(5) Uani 0.11 1 d PD A 10 C8K C 0.7479(13) 0.3367(7) 0.1484(9) 0.0481(5) Uani 0.11 1 d PD A 10 H8K1 H 0.7598 0.3150 0.1933 0.058 Uiso 0.11 1 calc PR A 10 H8K2 H 0.8204 0.3291 0.1581 0.058 Uiso 0.11 1 calc PR A 10 C9K C 0.7465(12) 0.4085(7) 0.1604(8) 0.0554(5) Uani 0.11 1 d PD A 10 H9K1 H 0.6942 0.4320 0.1085 0.067 Uiso 0.11 1 calc PR A 10 H9K2 H 0.8253 0.4276 0.1915 0.067 Uiso 0.11 1 calc PR A 10 C10K C 0.7029(13) 0.4172(10) 0.2059(8) 0.0691(6) Uani 0.11 1 d PD A 10 H10M H 0.6940 0.4660 0.2096 0.083 Uiso 0.11 1 calc PR A 10 H10N H 0.6248 0.3968 0.1734 0.083 Uiso 0.11 1 calc PR A 10 C11K C 0.7759(16) 0.3879(9) 0.2887(8) 0.0773(7) Uani 0.11 1 d PD A 10 H11K H 0.8185 0.3489 0.2914 0.093 Uiso 0.11 1 calc PR A 10 H11L H 0.7226 0.3705 0.2960 0.093 Uiso 0.11 1 calc PR A 10 C12K C 0.8651(18) 0.4345(11) 0.3602(10) 0.0738(7) Uani 0.11 1 d PD A 10 H12S H 0.8533 0.4329 0.3986 0.111 Uiso 0.11 1 calc PR A 10 H12T H 0.8546 0.4808 0.3413 0.111 Uiso 0.11 1 calc PR A 10 H12U H 0.9438 0.4193 0.3860 0.111 Uiso 0.11 1 calc PR A 10 O1A O 0.62129(8) 0.04270(6) 0.27102(6) 0.0361(2) Uani 1 1 d . . . H1A H 0.5522(16) 0.0363(10) 0.2549(11) 0.050 Uiso 1 1 d . . . O7A O 0.96192(9) 0.27822(7) 0.49221(7) 0.0535(3) Uani 1 1 d . . . C1A C 0.67810(10) 0.09702(7) 0.32039(7) 0.0272(3) Uani 1 1 d . . . C2A C 0.65034(10) 0.12035(7) 0.36540(7) 0.0272(3) Uani 1 1 d . . . C3A C 0.71585(10) 0.17304(8) 0.41812(7) 0.0300(3) Uani 1 1 d . . . H3A H 0.6986 0.1897 0.4494 0.036 Uiso 1 1 calc R . . C4A C 0.80631(11) 0.20201(8) 0.42607(7) 0.0303(3) Uani 1 1 d . . . C5A C 0.82981(10) 0.17815(8) 0.37847(7) 0.0292(3) Uani 1 1 d . . . H5A H 0.8906 0.1980 0.3831 0.035 Uiso 1 1 calc R . . C6A C 0.76606(10) 0.12638(7) 0.32506(7) 0.0272(3) Uani 1 1 d . . . C7A C 0.87852(11) 0.25762(9) 0.48306(8) 0.0361(4) Uani 1 1 d . . . C8A C 0.84914(12) 0.28787(9) 0.53049(9) 0.0386(4) Uani 1 1 d . . . H8A1 H 0.8758 0.2570 0.5746 0.046 Uiso 1 1 calc R . . H8A2 H 0.7639 0.2922 0.4957 0.046 Uiso 1 1 calc R . . C9A C 0.90429(13) 0.35663(9) 0.56472(9) 0.0434(4) Uani 1 1 d . . . H9A1 H 0.9895 0.3512 0.6053 0.052 Uiso 1 1 calc R . . H9A2 H 0.8868 0.3854 0.5217 0.052 Uiso 1 1 calc R . . C10A C 0.86230(12) 0.39176(9) 0.60245(9) 0.0377(4) Uani 1 1 d . . . H10A' H 0.7768 0.3958 0.5625 0.045 Uiso 1 1 calc R . . H10B' H 0.8825 0.3639 0.6469 0.045 Uiso 1 1 calc R . . C11A C 0.91450(14) 0.46126(9) 0.63360(9) 0.0435(4) Uani 1 1 d . . . H11A' H 1.0000 0.4576 0.6706 0.052 Uiso 1 1 calc R . . H11B' H 0.8898 0.4900 0.5885 0.052 Uiso 1 1 calc R . . C12A C 0.87974(16) 0.49485(10) 0.67638(11) 0.0543(4) Uani 1 1 d . . . H12A' H 0.7950 0.4970 0.6409 0.065 Uiso 1 1 calc R . . H12B' H 0.9117 0.5405 0.6920 0.065 Uiso 1 1 calc R . . H12C' H 0.9100 0.4688 0.7239 0.065 Uiso 1 1 calc R . . C13A C 0.54906(11) 0.09207(8) 0.35565(7) 0.0300(3) Uani 1 1 d . . . H13A H 0.5619 0.1007 0.4048 0.036 Uiso 1 1 calc R . . H13B H 0.5451 0.0428 0.3479 0.036 Uiso 1 1 calc R . . O1B O 0.39720(8) 0.03200(5) 0.20222(6) 0.0346(2) Uani 1 1 d . . . H1B H 0.3737 0.0283 0.1561 0.042 Uiso 1 1 calc R . . C1B C 0.36312(10) 0.09350(7) 0.20980(7) 0.0276(3) Uani 1 1 d . B . C2B C 0.43459(10) 0.12364(7) 0.28508(7) 0.0277(3) Uani 1 1 d . . . C3B C 0.40147(10) 0.18513(8) 0.29393(8) 0.0305(3) Uani 1 1 d . B . H3B H 0.4487 0.2061 0.3447 0.037 Uiso 1 1 calc R . . C4B C 0.29943(11) 0.21682(8) 0.22912(8) 0.0309(3) Uani 1 1 d D . . C5B C 0.23006(10) 0.18522(8) 0.15497(8) 0.0309(3) Uani 1 1 d . B . H5B H 0.1608 0.2066 0.1109 0.037 Uiso 1 1 calc R . . C6B C 0.25979(10) 0.12334(8) 0.14401(7) 0.0284(3) Uani 1 1 d . . . C13B C 0.18030(11) 0.09129(8) 0.06166(8) 0.0310(3) Uani 1 1 d . B . H13C H 0.1918 0.0419 0.0673 0.037 Uiso 1 1 calc R . . H13D H 0.0987 0.1004 0.0361 0.037 Uiso 1 1 calc R . . O1C O 0.35360(9) 0.03753(6) 0.06433(6) 0.0378(3) Uani 1 1 d . . . H1C H 0.4153 0.0324 0.0725 0.045 Uiso 1 1 calc R . . C1C C 0.29269(11) 0.09071(7) 0.01367(7) 0.0292(3) Uani 1 1 d . A . C2C C 0.20210(10) 0.11744(8) 0.00830(7) 0.0284(3) Uani 1 1 d . . . C3C C 0.13641(11) 0.16903(8) -0.04536(8) 0.0309(3) Uani 1 1 d . A . H3C H 0.0754 0.1879 -0.0496 0.037 Uiso 1 1 calc R . . C4C C 0.15763(11) 0.19419(8) -0.09376(8) 0.0324(3) Uani 1 1 d D . . C5C C 0.24951(11) 0.16698(8) -0.08560(7) 0.0316(3) Uani 1 1 d . A . H5C H 0.2651 0.1841 -0.1177 0.038 Uiso 1 1 calc R . . C6C C 0.31825(10) 0.11580(7) -0.03202(7) 0.0283(3) Uani 1 1 d . . . C13C C 0.42061(11) 0.08958(8) -0.02233(7) 0.0319(3) Uani 1 1 d . A . H13E H 0.4064 0.0974 -0.0721 0.038 Uiso 1 1 calc R . . H13F H 0.4286 0.0405 -0.0123 0.038 Uiso 1 1 calc R . . O1D O 0.58096(8) 0.03432(5) 0.13358(6) 0.0351(2) Uani 1 1 d . . . H1D H 0.6080 0.0302 0.1806 0.042 Uiso 1 1 calc R . . C1D C 0.60678(10) 0.09725(7) 0.12342(7) 0.0285(3) Uani 1 1 d . A . C2D C 0.53226(10) 0.12477(8) 0.04657(7) 0.0293(3) Uani 1 1 d . . . C3D C 0.55831(11) 0.18735(8) 0.03477(8) 0.0322(3) Uani 1 1 d . A . H3D H 0.5092 0.2062 -0.0172 0.039 Uiso 1 1 calc R . . C4D C 0.65540(11) 0.22343(8) 0.09768(8) 0.0330(3) Uani 1 1 d D . . C5D C 0.72810(11) 0.19467(8) 0.17375(8) 0.0312(3) Uani 1 1 d . A . H5D H 0.7942 0.2190 0.2168 0.037 Uiso 1 1 calc R . . C6D C 0.70584(10) 0.13153(7) 0.18779(7) 0.0279(3) Uani 1 1 d . . . C13D C 0.78924(10) 0.10222(8) 0.27167(7) 0.0293(3) Uani 1 1 d . A . H13G H 0.7834 0.0525 0.2681 0.035 Uiso 1 1 calc R . . H13H H 0.8695 0.1145 0.2964 0.035 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 O7C 0.0450(5) 0.0940(13) 0.0424(7) 0.0349(8) 0.0327(5) 0.0414(7) C7C 0.0279(6) 0.0540(12) 0.0169(7) -0.0011(7) 0.0126(5) 0.0103(7) C8C 0.0382(8) 0.0644(14) 0.0316(8) 0.0155(8) 0.0227(7) 0.0211(9) C9C 0.0613(13) 0.075(2) 0.0572(12) 0.0261(13) 0.0440(10) 0.0238(14) C10C 0.0687(15) 0.073(3) 0.0485(15) -0.0018(14) 0.0363(12) 0.0090(16) C11C 0.134(2) 0.059(3) 0.124(3) -0.020(2) 0.102(2) -0.003(2) C12C 0.100(3) 0.128(5) 0.148(4) 0.046(4) 0.077(3) -0.005(4) O7G 0.0450(5) 0.0940(13) 0.0424(7) 0.0349(8) 0.0327(5) 0.0414(7) C7G 0.0279(6) 0.0540(12) 0.0169(7) -0.0011(7) 0.0126(5) 0.0103(7) C8G 0.0382(8) 0.0644(14) 0.0316(8) 0.0155(8) 0.0227(7) 0.0211(9) C9G 0.0613(13) 0.075(2) 0.0572(12) 0.0261(13) 0.0440(10) 0.0238(14) C10G 0.0687(15) 0.073(3) 0.0485(15) -0.0018(14) 0.0363(12) 0.0090(16) C11G 0.134(2) 0.059(3) 0.124(3) -0.020(2) 0.102(2) -0.003(2) C12G 0.100(3) 0.128(5) 0.148(4) 0.046(4) 0.077(3) -0.005(4) O7H 0.0450(5) 0.0940(13) 0.0424(7) 0.0349(8) 0.0327(5) 0.0414(7) C7H 0.0279(6) 0.0540(12) 0.0169(7) -0.0011(7) 0.0126(5) 0.0103(7) C8H 0.0382(8) 0.0644(14) 0.0316(8) 0.0155(8) 0.0227(7) 0.0211(9) C9H 0.0613(13) 0.075(2) 0.0572(12) 0.0261(13) 0.0440(10) 0.0238(14) C10H 0.0687(15) 0.073(3) 0.0485(15) -0.0018(14) 0.0363(12) 0.0090(16) C11H 0.134(2) 0.059(3) 0.124(3) -0.020(2) 0.102(2) -0.003(2) C12H 0.100(3) 0.128(5) 0.148(4) 0.046(4) 0.077(3) -0.005(4) O7I 0.0450(5) 0.0940(13) 0.0424(7) 0.0349(8) 0.0327(5) 0.0414(7) C7I 0.0279(6) 0.0540(12) 0.0169(7) -0.0011(7) 0.0126(5) 0.0103(7) C8I 0.0382(8) 0.0644(14) 0.0316(8) 0.0155(8) 0.0227(7) 0.0211(9) C9I 0.0613(13) 0.075(2) 0.0572(12) 0.0261(13) 0.0440(10) 0.0238(14) C10I 0.0687(15) 0.073(3) 0.0485(15) -0.0018(14) 0.0363(12) 0.0090(16) C11I 0.134(2) 0.059(3) 0.124(3) -0.020(2) 0.102(2) -0.003(2) C12I 0.100(3) 0.128(5) 0.148(4) 0.046(4) 0.077(3) -0.005(4) O7B 0.0339(5) 0.0499(8) 0.0231(6) -0.0075(6) 0.0150(4) 0.0022(6) C7B 0.0293(5) 0.0395(8) 0.0279(7) -0.0065(6) 0.0203(5) -0.0035(6) C8B 0.0318(8) 0.0369(11) 0.0370(8) -0.0061(8) 0.0241(7) -0.0037(8) C9B 0.0457(11) 0.0474(12) 0.0339(14) -0.0047(11) 0.0207(10) 0.0090(11) C10B 0.0496(12) 0.0439(16) 0.0402(14) -0.0065(11) 0.0242(10) 0.0048(12) C11B 0.0505(14) 0.0500(17) 0.0458(14) -0.0078(12) 0.0224(11) 0.0024(13) C12B 0.0658(18) 0.055(2) 0.0586(18) 0.0005(15) 0.0288(15) 0.0035(16) O7F 0.0339(5) 0.0499(8) 0.0231(6) -0.0075(6) 0.0150(4) 0.0022(6) C7F 0.0293(5) 0.0395(8) 0.0279(7) -0.0065(6) 0.0203(5) -0.0035(6) C8F 0.0318(8) 0.0369(11) 0.0370(8) -0.0061(8) 0.0241(7) -0.0037(8) C9F 0.0457(11) 0.0474(12) 0.0339(14) -0.0047(11) 0.0207(10) 0.0090(11) C10F 0.0496(12) 0.0439(16) 0.0402(14) -0.0065(11) 0.0242(10) 0.0048(12) C11F 0.0505(14) 0.0500(17) 0.0458(14) -0.0078(12) 0.0224(11) 0.0024(13) C12F 0.0658(18) 0.055(2) 0.0586(18) 0.0005(15) 0.0288(15) 0.0035(16) O7L 0.0339(5) 0.0499(8) 0.0231(6) -0.0075(6) 0.0150(4) 0.0022(6) C7L 0.0293(5) 0.0395(8) 0.0279(7) -0.0065(6) 0.0203(5) -0.0035(6) C8L 0.0318(8) 0.0369(11) 0.0370(8) -0.0061(8) 0.0241(7) -0.0037(8) C9L 0.0457(11) 0.0474(12) 0.0339(14) -0.0047(11) 0.0207(10) 0.0090(11) C10L 0.0496(12) 0.0439(16) 0.0402(14) -0.0065(11) 0.0242(10) 0.0048(12) C11L 0.0505(14) 0.0500(17) 0.0458(14) -0.0078(12) 0.0224(11) 0.0024(13) C12L 0.0658(18) 0.055(2) 0.0586(18) 0.0005(15) 0.0288(15) 0.0035(16) O1N 0.0956(11) 0.1196(15) 0.0416(8) 0.0059(9) 0.0201(8) 0.0491(11) N1N 0.0479(6) 0.0475(9) 0.0469(7) -0.0020(6) 0.0262(5) 0.0011(7) C2N 0.0380(6) 0.0350(8) 0.0387(6) 0.0018(6) 0.0232(5) -0.0019(6) C3N 0.0502(8) 0.0448(10) 0.0476(8) 0.0097(7) 0.0278(6) 0.0094(7) C4N 0.0561(10) 0.0805(16) 0.0403(9) 0.0091(9) 0.0210(8) 0.0088(11) C5N 0.0602(9) 0.0722(14) 0.0481(8) -0.0122(9) 0.0324(7) -0.0090(10) C6N 0.0552(7) 0.0482(10) 0.0644(8) -0.0053(7) 0.0436(6) -0.0012(8) C7N 0.0394(7) 0.0437(9) 0.0481(8) 0.0054(7) 0.0255(6) 0.0045(7) O1N1 0.0829(7) 0.0370(7) 0.0703(7) -0.0063(5) 0.0510(6) -0.0011(6) O7D 0.0572(6) 0.0584(8) 0.0455(5) 0.0137(5) 0.0374(5) 0.0038(7) C7D 0.0421(6) 0.0483(10) 0.0421(6) 0.0056(6) 0.0337(5) 0.0039(7) C8D 0.0489(7) 0.0501(10) 0.0569(8) 0.0034(7) 0.0397(6) -0.0073(8) C9D 0.0572(9) 0.0510(12) 0.0620(10) -0.0032(9) 0.0407(8) -0.0044(9) C10D 0.0757(10) 0.0577(14) 0.0896(13) -0.0210(11) 0.0610(9) -0.0198(11) C11D 0.1045(12) 0.0626(15) 0.0961(13) -0.0257(11) 0.0794(10) -0.0234(13) C12D 0.0857(13) 0.0732(18) 0.0680(12) 0.0042(11) 0.0526(10) 0.0099(13) O7K 0.0572(6) 0.0584(8) 0.0455(5) 0.0137(5) 0.0374(5) 0.0038(7) C7K 0.0421(6) 0.0483(10) 0.0421(6) 0.0056(6) 0.0337(5) 0.0039(7) C8K 0.0489(7) 0.0501(10) 0.0569(8) 0.0034(7) 0.0397(6) -0.0073(8) C9K 0.0572(9) 0.0510(12) 0.0620(10) -0.0032(9) 0.0407(8) -0.0044(9) C10K 0.0757(10) 0.0577(14) 0.0896(13) -0.0210(11) 0.0610(9) -0.0198(11) C11K 0.1045(12) 0.0626(15) 0.0961(13) -0.0257(11) 0.0794(10) -0.0234(13) C12K 0.0857(13) 0.0732(18) 0.0680(12) 0.0042(11) 0.0526(10) 0.0099(13) O1A 0.0315(4) 0.0356(6) 0.0371(4) -0.0080(4) 0.0207(3) -0.0060(4) O7A 0.0392(4) 0.0792(9) 0.0499(5) -0.0323(5) 0.0325(4) -0.0294(5) C1A 0.0224(5) 0.0295(7) 0.0217(5) 0.0019(4) 0.0110(4) 0.0013(5) C2A 0.0220(4) 0.0326(7) 0.0219(5) 0.0026(5) 0.0122(4) -0.0001(5) C3A 0.0231(4) 0.0414(8) 0.0219(5) -0.0014(5) 0.0131(4) -0.0010(5) C4A 0.0219(5) 0.0399(8) 0.0228(5) -0.0030(5) 0.0119(4) -0.0034(5) C5A 0.0200(4) 0.0382(7) 0.0244(5) 0.0011(5) 0.0123(4) -0.0011(5) C6A 0.0215(4) 0.0329(7) 0.0216(5) 0.0026(5) 0.0117(4) 0.0046(5) C7A 0.0251(5) 0.0499(9) 0.0297(5) -0.0100(6) 0.0163(4) -0.0092(6) C8A 0.0320(5) 0.0495(9) 0.0353(6) -0.0130(6) 0.0224(4) -0.0109(6) C9A 0.0431(6) 0.0491(9) 0.0436(6) -0.0134(6) 0.0309(5) -0.0134(7) C10A 0.0343(5) 0.0417(8) 0.0357(6) -0.0024(6) 0.0223(5) -0.0024(6) C11A 0.0547(7) 0.0357(8) 0.0484(7) 0.0011(6) 0.0373(5) -0.0023(7) C12A 0.0738(8) 0.0388(9) 0.0668(8) -0.0011(7) 0.0533(7) 0.0006(8) C13A 0.0284(5) 0.0348(7) 0.0259(5) 0.0004(5) 0.0174(4) -0.0044(5) O1B 0.0344(4) 0.0297(5) 0.0358(4) -0.0009(4) 0.0212(3) -0.0007(4) C1B 0.0258(4) 0.0278(6) 0.0299(5) -0.0008(5) 0.0185(4) -0.0041(5) C2B 0.0234(4) 0.0349(7) 0.0258(5) 0.0002(5) 0.0166(4) -0.0057(5) C3B 0.0263(4) 0.0396(8) 0.0287(5) -0.0047(5) 0.0193(4) -0.0069(5) C4B 0.0293(4) 0.0351(7) 0.0345(5) -0.0027(5) 0.0236(4) -0.0025(5) C5B 0.0254(4) 0.0381(8) 0.0298(5) 0.0009(5) 0.0185(4) 0.0003(5) C6B 0.0236(4) 0.0352(7) 0.0268(5) -0.0020(5) 0.0167(4) -0.0039(5) C13B 0.0207(5) 0.0372(7) 0.0276(5) -0.0051(5) 0.0126(4) -0.0048(5) O1C 0.0347(4) 0.0354(6) 0.0369(4) 0.0027(4) 0.0206(3) 0.0079(4) C1C 0.0244(5) 0.0309(7) 0.0239(5) -0.0052(5) 0.0122(4) 0.0009(5) C2C 0.0214(4) 0.0338(7) 0.0228(5) -0.0068(5) 0.0112(4) -0.0032(5) C3C 0.0206(4) 0.0402(8) 0.0255(5) -0.0036(5) 0.0124(4) 0.0029(5) C4C 0.0215(5) 0.0441(8) 0.0228(5) -0.0004(5) 0.0106(4) 0.0058(5) C5C 0.0242(5) 0.0435(8) 0.0217(5) -0.0013(5) 0.0127(4) 0.0041(5) C6C 0.0220(5) 0.0346(7) 0.0202(5) -0.0063(5) 0.0102(4) 0.0024(5) C13C 0.0256(5) 0.0421(8) 0.0225(5) -0.0034(5) 0.0134(4) 0.0073(5) O1D 0.0377(4) 0.0306(5) 0.0346(4) -0.0003(4) 0.0226(3) 0.0046(4) C1D 0.0265(4) 0.0321(7) 0.0280(5) -0.0008(5) 0.0183(4) 0.0065(5) C2D 0.0244(4) 0.0385(7) 0.0251(5) -0.0022(5) 0.0163(4) 0.0070(5) C3D 0.0282(5) 0.0449(8) 0.0263(5) 0.0041(5) 0.0189(4) 0.0090(5) C4D 0.0332(5) 0.0396(8) 0.0336(5) 0.0025(5) 0.0251(4) 0.0039(5) C5D 0.0266(4) 0.0398(8) 0.0290(5) -0.0011(5) 0.0190(4) 0.0010(5) C6D 0.0244(4) 0.0363(7) 0.0251(5) 0.0009(5) 0.0172(4) 0.0062(5) C13D 0.0224(4) 0.0367(7) 0.0251(5) 0.0005(5) 0.0139(4) 0.0044(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O7C C7C 1.220(8) . ? C7C C4C 1.483(5) . ? C7C C8C 1.523(9) . ? C8C C9C 1.528(9) . ? C9C C10C 1.526(7) . ? C10C C11C 1.536(11) . ? C11C C12C 1.575(11) . ? O7G C7G 1.204(11) . ? C7G C4C 1.477(8) . ? C7G C8G 1.514(12) . ? C8G C9G 1.520(11) . ? C9G C10G 1.507(11) . ? C10G C11G 1.470(12) . ? C11G C12G 1.477(13) . ? O7H C7H 1.223(11) . ? C7H C8H 1.502(12) . ? C7H C4C 1.511(7) . ? C8H C9H 1.520(12) . ? C9H C10H 1.509(9) . ? C10H C11H 1.552(12) . ? C11H C12H 1.560(14) . ? O7I C7I 1.212(16) . ? C7I C8I 1.497(16) . ? C7I C4C 1.504(13) . ? C8I C9I 1.512(16) . ? C9I C10I 1.505(17) . ? C10I C11I 1.504(17) . ? C11I C12I 1.563(19) . ? O7B C7B 1.219(5) . ? C7B C4B 1.486(5) . ? C7B C8B 1.529(5) . ? C8B C9B 1.518(6) . ? C9B C10B 1.518(5) . ? C10B C11B 1.522(6) . ? C11B C12B 1.517(6) . ? O7F C7F 1.219(5) . ? C7F C4B 1.511(5) . ? C7F C8F 1.527(5) . ? C8F C9F 1.523(6) . ? C9F C10F 1.531(5) . ? C10F C11F 1.501(7) . ? C11F C12F 1.528(6) . ? O7L C7L 1.211(13) . ? C7L C8L 1.498(13) . ? C7L C4B 1.515(12) . ? C8L C9L 1.535(15) . ? C9L C10L 1.522(14) . ? C10L C11L 1.549(15) . ? C11L C12L 1.535(15) . ? O1N N1N 1.217(2) . ? N1N O1N1 1.208(2) . ? N1N C2N 1.471(2) . ? C2N C3N 1.373(2) . ? C2N C7N 1.381(3) . ? C3N C4N 1.383(3) . ? C4N C5N 1.388(3) . ? C5N C6N 1.370(3) . ? C6N C7N 1.375(3) . ? O7D C7D 1.228(2) . ? C7D C4D 1.487(3) . ? C7D C8D 1.506(3) . ? C8D C9D 1.540(3) . ? C9D C10D 1.525(3) . ? C10D C11D 1.515(4) . ? C11D C12D 1.488(4) . ? O7K C7K 1.203(14) . ? C7K C8K 1.473(14) . ? C7K C4D 1.496(13) . ? C8K C9K 1.456(15) . ? C9K C10K 1.542(16) . ? C10K C11K 1.512(15) . ? C11K C12K 1.550(16) . ? O1A C1A 1.3697(17) . ? O7A C7A 1.2208(19) . ? C1A C2A 1.397(2) . ? C1A C6A 1.404(2) . ? C2A C3A 1.3912(19) . ? C2A C13A 1.5212(19) . ? C3A C4A 1.396(2) . ? C4A C5A 1.404(2) . ? C4A C7A 1.488(2) . ? C5A C6A 1.3794(19) . ? C6A C13D 1.522(2) . ? C7A C8A 1.515(2) . ? C8A C9A 1.522(2) . ? C9A C10A 1.519(2) . ? C10A C11A 1.516(2) . ? C11A C12A 1.514(3) . ? C13A C2B 1.5227(17) . ? O1B C1B 1.3811(18) . ? C1B C6B 1.3994(17) . ? C1B C2B 1.4000(18) . ? C2B C3B 1.385(2) . ? C3B C4B 1.4000(18) . ? C4B C5B 1.3958(19) . ? C5B C6B 1.387(2) . ? C6B C13B 1.5238(18) . ? C13B C2C 1.518(2) . ? O1C C1C 1.3707(17) . ? C1C C6C 1.397(2) . ? C1C C2C 1.411(2) . ? C2C C3C 1.383(2) . ? C3C C4C 1.404(2) . ? C4C C5C 1.400(2) . ? C5C C6C 1.385(2) . ? C6C C13C 1.523(2) . ? C13C C2D 1.5237(18) . ? O1D C1D 1.3738(19) . ? C1D C6D 1.4018(17) . ? C1D C2D 1.4027(18) . ? C2D C3D 1.382(2) . ? C3D C4D 1.3974(19) . ? C4D C5D 1.4005(19) . ? C5D C6D 1.388(2) . ? C6D C13D 1.5263(18) . ? 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 O7C C7C C4C 121.8(6) . . ? O7C C7C C8C 118.2(5) . . ? C4C C7C C8C 119.9(5) . . ? C7C C8C C9C 112.2(6) . . ? C10C C9C C8C 110.9(5) . . ? C9C C10C C11C 113.1(6) . . ? C10C C11C C12C 113.9(8) . . ? O7G C7G C4C 121.2(8) . . ? O7G C7G C8G 120.2(8) . . ? C4C C7G C8G 118.5(7) . . ? C7G C8G C9G 109.8(7) . . ? C10G C9G C8G 111.8(8) . . ? C11G C10G C9G 114.3(9) . . ? C10G C11G C12G 147.9(12) . . ? O7H C7H C8H 116.5(8) . . ? O7H C7H C4C 118.6(7) . . ? C8H C7H C4C 123.5(6) . . ? C7H C8H C9H 119.5(9) . . ? C10H C9H C8H 113.7(7) . . ? C9H C10H C11H 112.9(8) . . ? C10H C11H C12H 113.6(11) . . ? O7I C7I C8I 122.6(17) . . ? O7I C7I C4C 117.7(17) . . ? C8I C7I C4C 117.0(12) . . ? C7I C8I C9I 119.8(15) . . ? C10I C9I C8I 116.8(16) . . ? C11I C10I C9I 113.9(17) . . ? C10I C11I C12I 106.6(18) . . ? O7B C7B C4B 119.8(3) . . ? O7B C7B C8B 120.0(4) . . ? C4B C7B C8B 119.5(3) . . ? C9B C8B C7B 116.5(3) . . ? C8B C9B C10B 111.2(3) . . ? C9B C10B C11B 115.2(3) . . ? C12B C11B C10B 113.8(4) . . ? O7F C7F C4B 123.2(4) . . ? O7F C7F C8F 122.1(4) . . ? C4B C7F C8F 114.7(3) . . ? C9F C8F C7F 112.3(4) . . ? C8F C9F C10F 113.4(3) . . ? C11F C10F C9F 115.6(4) . . ? C10F C11F C12F 113.1(4) . . ? O7L C7L C8L 117.1(12) . . ? O7L C7L C4B 116.2(10) . . ? C8L C7L C4B 125.0(10) . . ? C7L C8L C9L 115.9(11) . . ? C10L C9L C8L 110.4(11) . . ? C9L C10L C11L 111.0(11) . . ? C12L C11L C10L 109.0(12) . . ? O1N1 N1N O1N 123.08(18) . . ? O1N1 N1N C2N 119.33(14) . . ? O1N N1N C2N 117.53(17) . . ? C3N C2N C7N 122.67(17) . . ? C3N C2N N1N 118.57(16) . . ? C7N C2N N1N 118.75(14) . . ? C2N C3N C4N 117.58(19) . . ? C3N C4N C5N 120.72(18) . . ? C6N C5N C4N 120.1(2) . . ? C5N C6N C7N 120.3(2) . . ? C6N C7N C2N 118.62(15) . . ? O7D C7D C4D 120.18(16) . . ? O7D C7D C8D 119.4(2) . . ? C4D C7D C8D 120.36(16) . . ? C7D C8D C9D 109.84(17) . . ? C10D C9D C8D 111.28(19) . . ? C11D C10D C9D 113.2(2) . . ? C12D C11D C10D 114.4(2) . . ? O7K C7K C8K 122.5(14) . . ? O7K C7K C4D 122.5(12) . . ? C8K C7K C4D 114.6(10) . . ? C9K C8K C7K 129.4(13) . . ? C8K C9K C10K 107.1(14) . . ? C11K C10K C9K 117.9(14) . . ? C10K C11K C12K 118.1(15) . . ? O1A C1A C2A 120.39(13) . . ? O1A C1A C6A 117.37(13) . . ? C2A C1A C6A 122.22(12) . . ? C3A C2A C1A 117.75(13) . . ? C3A C2A C13A 120.06(13) . . ? C1A C2A C13A 122.14(12) . . ? C2A C3A C4A 121.52(14) . . ? C3A C4A C5A 119.00(13) . . ? C3A C4A C7A 122.27(14) . . ? C5A C4A C7A 118.73(13) . . ? C6A C5A C4A 121.11(13) . . ? C5A C6A C1A 118.35(13) . . ? C5A C6A C13D 120.92(13) . . ? C1A C6A C13D 120.72(12) . . ? O7A C7A C4A 120.07(15) . . ? O7A C7A C8A 120.18(14) . . ? C4A C7A C8A 119.74(13) . . ? C7A C8A C9A 112.68(14) . . ? C10A C9A C8A 113.19(14) . . ? C11A C10A C9A 112.68(14) . . ? C12A C11A C10A 113.15(15) . . ? C2A C13A C2B 111.60(11) . . ? O1B C1B C6B 120.29(12) . . ? O1B C1B C2B 117.63(11) . . ? C6B C1B C2B 122.08(13) . . ? C3B C2B C1B 118.44(11) . . ? C3B C2B C13A 119.77(12) . . ? C1B C2B C13A 121.73(13) . . ? C2B C3B C4B 120.96(12) . . ? C5B C4B C3B 119.06(14) . . ? C5B C4B C7B 118.70(16) . . ? C3B C4B C7B 122.23(17) . . ? C5B C4B C7F 126.97(17) . . ? C3B C4B C7F 113.96(17) . . ? C7B C4B C7F 8.4(2) . . ? C5B C4B C7L 112.1(4) . . ? C3B C4B C7L 128.8(4) . . ? C7B C4B C7L 6.7(5) . . ? C7F C4B C7L 14.9(4) . . ? C6B C5B C4B 121.61(12) . . ? C5B C6B C1B 117.83(12) . . ? C5B C6B C13B 119.16(11) . . ? C1B C6B C13B 123.01(13) . . ? C2C C13B C6B 112.74(12) . . ? O1C C1C C6C 120.70(13) . . ? O1C C1C C2C 117.36(14) . . ? C6C C1C C2C 121.92(13) . . ? C3C C2C C1C 117.94(14) . . ? C3C C2C C13B 121.45(13) . . ? C1C C2C C13B 120.59(12) . . ? C2C C3C C4C 121.64(13) . . ? C5C C4C C3C 118.54(13) . . ? C5C C4C C7G 124.0(4) . . ? C3C C4C C7G 117.0(4) . . ? C5C C4C C7C 123.6(3) . . ? C3C C4C C7C 117.8(3) . . ? C7G C4C C7C 9.4(4) . . ? C5C C4C C7I 127.8(7) . . ? C3C C4C C7I 112.7(8) . . ? C7G C4C C7I 4.8(10) . . ? C7C C4C C7I 12.8(8) . . ? C5C C4C C7H 118.1(4) . . ? C3C C4C C7H 123.1(4) . . ? C7G C4C C7H 12.7(5) . . ? C7C C4C C7H 5.7(5) . . ? C7I C4C C7H 17.0(8) . . ? C6C C5C C4C 121.72(15) . . ? C5C C6C C1C 118.20(13) . . ? C5C C6C C13C 120.16(14) . . ? C1C C6C C13C 121.61(12) . . ? C6C C13C C2D 110.71(12) . . ? O1D C1D C6D 120.55(12) . . ? O1D C1D C2D 117.66(11) . . ? C6D C1D C2D 121.78(14) . . ? C3D C2D C1D 118.52(12) . . ? C3D C2D C13C 119.57(12) . . ? C1D C2D C13C 121.81(14) . . ? C2D C3D C4D 121.34(12) . . ? C3D C4D C5D 118.81(14) . . ? C3D C4D C7D 118.92(13) . . ? C5D C4D C7D 122.25(13) . . ? C3D C4D C7K 114.8(5) . . ? C5D C4D C7K 125.6(5) . . ? C7D C4D C7K 10.5(9) . . ? C6D C5D C4D 121.57(12) . . ? C5D C6D C1D 117.96(12) . . ? C5D C6D C13D 119.26(11) . . ? C1D C6D C13D 122.77(13) . . ? C6A C13D C6D 113.52(11) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.73 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.452 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.069 data_ad3 _database_code_depnum_ccdc_archive 'CCDC 265961' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common p-hexanoyl-calix(4)arene.Methanol _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52.50 H66 O8.50' _chemical_formula_weight 833.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6164(8) _cell_length_b 13.1000(9) _cell_length_c 15.4081(11) _cell_angle_alpha 105.1650(10) _cell_angle_beta 90.1980(10) _cell_angle_gamma 91.7940(10) _cell_volume 2261.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 898 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.9604 _exptl_absorpt_correction_T_max 0.9799 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _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 27086 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.72 _reflns_number_total 11618 _reflns_number_gt 8455 _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^)+(0.1007P)^2^+0.7967P] 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 11618 _refine_ls_number_parameters 633 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0640 _refine_ls_wR_factor_ref 0.1965 _refine_ls_wR_factor_gt 0.1796 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.019 _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 O2B O -0.17018(7) 0.28576(6) 0.40912(6) 0.04219(17) Uani 0.66 1 d P A 3 C7B C -0.06969(10) 0.29427(9) 0.43678(8) 0.03690(19) Uani 0.66 1 d P A 3 C8B C -0.03320(10) 0.23724(9) 0.50523(8) 0.0406(2) Uani 0.66 1 d P A 3 H8B1 H -0.0225 0.2895 0.5643 0.049 Uiso 0.66 1 calc PR A 3 H8B2 H 0.0421 0.2052 0.4875 0.049 Uiso 0.66 1 calc PR A 3 C9B C -0.11858(12) 0.15123(10) 0.51524(9) 0.0473(2) Uani 0.66 1 d P A 3 H9B1 H -0.1260 0.0973 0.4568 0.057 Uiso 0.66 1 calc PR A 3 H9B2 H -0.1948 0.1828 0.5294 0.057 Uiso 0.66 1 calc PR A 3 C10B C -0.08713(13) 0.09636(10) 0.58717(9) 0.0496(3) Uani 0.66 1 d P A 3 H40A H -0.0077 0.0710 0.5767 0.059 Uiso 0.66 1 calc PR A 3 H40B H -0.0879 0.1486 0.6466 0.059 Uiso 0.66 1 calc PR A 3 C11B C -0.16671(16) 0.00405(12) 0.58951(11) 0.0664(4) Uani 0.66 1 d P A 3 H41A H -0.2466 0.0288 0.5963 0.080 Uiso 0.66 1 calc PR A 3 H41B H -0.1626 -0.0496 0.5310 0.080 Uiso 0.66 1 calc PR A 3 C12B C -0.1417(2) -0.04736(16) 0.66219(12) 0.0941(6) Uani 0.66 1 d P A 3 H42A H -0.0618 -0.0698 0.6578 0.113 Uiso 0.66 1 calc PR A 3 H42B H -0.1938 -0.1092 0.6562 0.113 Uiso 0.66 1 calc PR A 3 H42C H -0.1531 0.0030 0.7207 0.113 Uiso 0.66 1 calc PR A 3 O2F O -0.15631(13) 0.26516(13) 0.39512(11) 0.04219(17) Uani 0.34 1 d PD A 4 C7F C -0.06716(17) 0.28918(16) 0.43804(14) 0.03690(19) Uani 0.34 1 d PD A 4 C8F C -0.02705(19) 0.22526(16) 0.50164(14) 0.0406(2) Uani 0.34 1 d PD A 4 H8F1 H 0.0044 0.2747 0.5573 0.049 Uiso 0.34 1 calc PR A 4 H8F2 H 0.0361 0.1798 0.4729 0.049 Uiso 0.34 1 calc PR A 4 C9F C -0.1226(2) 0.15557(17) 0.52679(15) 0.0473(2) Uani 0.34 1 d PD A 4 H9F1 H -0.1405 0.0943 0.4749 0.057 Uiso 0.34 1 calc PR A 4 H9F2 H -0.1933 0.1966 0.5419 0.057 Uiso 0.34 1 calc PR A 4 C10F C -0.0849(2) 0.11626(18) 0.60749(15) 0.0496(3) Uani 0.34 1 d PD A 4 H40C H -0.0738 0.1777 0.6605 0.059 Uiso 0.34 1 calc PR A 4 H40D H -0.0101 0.0817 0.5942 0.059 Uiso 0.34 1 calc PR A 4 C11F C -0.1731(2) 0.0375(2) 0.6302(2) 0.0664(4) Uani 0.34 1 d PD A 4 H41C H -0.1934 -0.0189 0.5752 0.080 Uiso 0.34 1 calc PR A 4 H41D H -0.1393 0.0041 0.6746 0.080 Uiso 0.34 1 calc PR A 4 C12F C -0.2786(3) 0.0939(3) 0.6678(2) 0.0941(6) Uani 0.34 1 d PD A 4 H42D H -0.2587 0.1473 0.7238 0.113 Uiso 0.34 1 calc PR A 4 H42E H -0.3358 0.0430 0.6800 0.113 Uiso 0.34 1 calc PR A 4 H42F H -0.3105 0.1286 0.6243 0.113 Uiso 0.34 1 calc PR A 4 O2C O 0.53571(10) 0.16876(7) 0.50209(6) 0.0726(3) Uani 0.75 1 d PD A 1 C7C C 0.55397(10) 0.17343(8) 0.42496(7) 0.0448(3) Uani 0.75 1 d PD A 1 C8C C 0.61311(10) 0.08600(7) 0.35920(8) 0.0445(2) Uani 0.75 1 d PD A 1 H8C1 H 0.6923 0.1103 0.3492 0.053 Uiso 0.75 1 calc PR A 1 H8C2 H 0.5711 0.0689 0.3009 0.053 Uiso 0.75 1 calc PR A 1 C9C C 0.61837(10) -0.01310(8) 0.39277(7) 0.0461(3) Uani 0.75 1 d PD A 1 H9C1 H 0.6502 0.0060 0.4548 0.055 Uiso 0.75 1 calc PR A 1 H9C2 H 0.5394 -0.0432 0.3944 0.055 Uiso 0.75 1 calc PR A 1 C10C C 0.69254(10) -0.09591(8) 0.33315(8) 0.0473(3) Uani 0.75 1 d PD A 1 H10A H 0.7728 -0.0675 0.3353 0.057 Uiso 0.75 1 calc PR A 1 H10B H 0.6644 -0.1105 0.2702 0.057 Uiso 0.75 1 calc PR A 1 C11C C 0.69149(12) -0.19948(9) 0.36147(10) 0.0612(4) Uani 0.75 1 d PD A 1 H11A H 0.7203 -0.1848 0.4242 0.073 Uiso 0.75 1 calc PR A 1 H11B H 0.6111 -0.2274 0.3599 0.073 Uiso 0.75 1 calc PR A 1 C12C C 0.76386(13) -0.28262(10) 0.30221(12) 0.0741(5) Uani 0.75 1 d PD A 1 H12A H 0.7359 -0.2976 0.2399 0.089 Uiso 0.75 1 calc PR A 1 H12B H 0.7585 -0.3475 0.3226 0.089 Uiso 0.75 1 calc PR A 1 H12C H 0.8443 -0.2569 0.3056 0.089 Uiso 0.75 1 calc PR A 1 O2E O 0.4558(3) 0.1137(2) 0.44073(16) 0.0726(3) Uani 0.25 1 d PD A 2 C7E C 0.5209(2) 0.14490(18) 0.38946(19) 0.0448(3) Uani 0.25 1 d PD A 2 C8E C 0.6223(2) 0.07954(18) 0.3471(2) 0.0445(2) Uani 0.25 1 d PD A 2 H8E1 H 0.6934 0.1231 0.3671 0.053 Uiso 0.25 1 calc PR A 2 H8E2 H 0.6158 0.0687 0.2812 0.053 Uiso 0.25 1 calc PR A 2 C9E C 0.6400(3) -0.02882(19) 0.3642(2) 0.0461(3) Uani 0.25 1 d PD A 2 H9E1 H 0.6512 -0.0191 0.4297 0.055 Uiso 0.25 1 calc PR A 2 H9E2 H 0.5690 -0.0731 0.3459 0.055 Uiso 0.25 1 calc PR A 2 C10E C 0.7413(3) -0.08816(19) 0.3155(2) 0.0473(3) Uani 0.25 1 d PD A 2 H10C H 0.8090 -0.0387 0.3231 0.057 Uiso 0.25 1 calc PR A 2 H10D H 0.7225 -0.1119 0.2504 0.057 Uiso 0.25 1 calc PR A 2 C11E C 0.7742(3) -0.1849(2) 0.3480(3) 0.0612(4) Uani 0.25 1 d PD A 2 H11C H 0.8506 -0.2088 0.3241 0.073 Uiso 0.25 1 calc PR A 2 H11D H 0.7795 -0.1649 0.4145 0.073 Uiso 0.25 1 calc PR A 2 C12E C 0.6857(3) -0.2742(2) 0.3169(4) 0.0741(5) Uani 0.25 1 d PD A 2 H12D H 0.6084 -0.2474 0.3317 0.089 Uiso 0.25 1 calc PR A 2 H12E H 0.7000 -0.3298 0.3472 0.089 Uiso 0.25 1 calc PR A 2 H12F H 0.6912 -0.3034 0.2517 0.089 Uiso 0.25 1 calc PR A 2 O1 O 0.37161(14) 0.75076(10) 0.31344(9) 0.0647(4) Uani 0.50 1 d PD B 5 H1M H 0.3809 0.8141 0.3749 0.150 Uiso 0.50 1 d P C 5 C2 C 0.3837(2) 0.81482(15) 0.25476(13) 0.0677(6) Uani 0.50 1 d PD B 5 H2A H 0.3566 0.8856 0.2837 0.102 Uiso 0.50 1 calc PR B 5 H2B H 0.3381 0.7840 0.2000 0.102 Uiso 0.50 1 calc PR B 5 H2C H 0.4650 0.8200 0.2392 0.102 Uiso 0.50 1 calc PR B 5 O1A O 0.22385(5) 0.60042(4) 0.18049(4) 0.03992(14) Uani 1 1 d D . . H1A H 0.3007(6) 0.5863(14) 0.1609(6) 0.050 Uiso 0.50 1 d PD . . H77A H 0.2170(10) 0.6092(13) 0.2447(4) 0.050 Uiso 0.50 1 d PD . . O2A O -0.17864(5) 0.27955(5) -0.00347(4) 0.05279(18) Uani 1 1 d . . . C1A C 0.15215(6) 0.52156(5) 0.13025(5) 0.03196(16) Uani 1 1 d . . . C2A C 0.18603(6) 0.46627(5) 0.04417(4) 0.03170(16) Uani 1 1 d . . . C3A C 0.11074(6) 0.38871(5) -0.00647(5) 0.03306(17) Uani 1 1 d . . . H99A H 0.1326 0.3503 -0.0650 0.040 Uiso 1 1 calc R . . C4A C 0.00409(6) 0.36583(5) 0.02625(5) 0.03402(17) Uani 1 1 d . . . C5A C -0.02688(6) 0.42238(5) 0.11244(5) 0.03456(17) Uani 1 1 d . . . H5A H -0.0995 0.4073 0.1352 0.041 Uiso 1 1 calc R . . C6A C 0.04561(6) 0.49998(5) 0.16566(5) 0.03282(16) Uani 1 1 d . . . C7A C -0.07890(7) 0.28322(6) -0.02686(5) 0.04020(19) Uani 1 1 d . . . C8A C -0.03652(8) 0.20177(7) -0.10684(6) 0.0518(3) Uani 1 1 d . . . H8A1 H 0.0033 0.2375 -0.1480 0.062 Uiso 1 1 calc R . . H8A2 H -0.1029 0.1597 -0.1398 0.062 Uiso 1 1 calc R . . C9A C 0.04774(11) 0.12695(8) -0.07705(9) 0.0744(4) Uani 1 1 d . . . H9A1 H 0.1238 0.1642 -0.0638 0.089 Uiso 1 1 calc R . . H9A2 H 0.0193 0.1137 -0.0204 0.089 Uiso 1 1 calc R . . C10A C 0.06392(9) 0.02418(8) -0.14226(8) 0.0649(3) Uani 1 1 d . . . H50A H 0.0882 0.0376 -0.1999 0.078 Uiso 1 1 calc R . . H50B H -0.0116 -0.0144 -0.1530 0.078 Uiso 1 1 calc R . . C11A C 0.15026(12) -0.04743(9) -0.11635(9) 0.0798(4) Uani 1 1 d . . . H51A H 0.2279 -0.0135 -0.1148 0.096 Uiso 1 1 calc R . . H51B H 0.1331 -0.0519 -0.0545 0.096 Uiso 1 1 calc R . . C12A C 0.15431(12) -0.15525(10) -0.17448(9) 0.0821(4) Uani 1 1 d . . . H52A H 0.0835 -0.1949 -0.1675 0.099 Uiso 1 1 calc R . . H52B H 0.2209 -0.1903 -0.1576 0.099 Uiso 1 1 calc R . . H52C H 0.1613 -0.1527 -0.2373 0.099 Uiso 1 1 calc R . . C13A C 0.01049(6) 0.55695(6) 0.26014(5) 0.03632(18) Uani 1 1 d . . . H13A H -0.0744 0.5618 0.2619 0.044 Uiso 1 1 calc R . . H13B H 0.0441 0.6299 0.2754 0.044 Uiso 1 1 calc R . . O1B O 0.22664(5) 0.60333(4) 0.35458(4) 0.04160(15) Uani 1 1 d D . . H77B H 0.3022(6) 0.5912(10) 0.3697(6) 0.050 Uiso 0.50 1 d PD . . H1B H 0.2197(10) 0.6173(9) 0.2964(5) 0.050 Uiso 0.50 1 d PD . . C1B C 0.15813(6) 0.52431(5) 0.37257(5) 0.03236(17) Uani 1 1 d . A . C2B C 0.04912(6) 0.50190(5) 0.33053(4) 0.03213(17) Uani 1 1 d . . . C3B C -0.02135(6) 0.42576(5) 0.35271(5) 0.03309(17) Uani 1 1 d . A . H99B H -0.0954 0.4101 0.3253 0.040 Uiso 1 1 calc R . . C4B C 0.01368(6) 0.37140(5) 0.41436(4) 0.03285(17) Uani 1 1 d D . . C5B C 0.12319(6) 0.39386(6) 0.45330(4) 0.03331(17) Uani 1 1 d . A . H5B H 0.1482 0.3560 0.4943 0.040 Uiso 1 1 calc R . . C6B C 0.19661(6) 0.47026(6) 0.43362(4) 0.03233(17) Uani 1 1 d . . . C13B C 0.31577(6) 0.49294(6) 0.47701(5) 0.03567(18) Uani 1 1 d . A . H13C H 0.3129 0.4807 0.5377 0.043 Uiso 1 1 calc R . . H13D H 0.3375 0.5684 0.4842 0.043 Uiso 1 1 calc R . . O1C O 0.44829(5) 0.55122(4) 0.33880(4) 0.03859(14) Uani 1 1 d D . . H77C H 0.3734(6) 0.5742(13) 0.3589(6) 0.050 Uiso 0.50 1 d PD . . H1C H 0.4593(10) 0.5510(12) 0.2772(4) 0.050 Uiso 0.50 1 d PD . . C1C C 0.46755(6) 0.45401(5) 0.35342(4) 0.03049(16) Uani 1 1 d . A . C2C C 0.40793(6) 0.42448(6) 0.42257(5) 0.03376(17) Uani 1 1 d . . . C3C C 0.43538(7) 0.33041(6) 0.44048(5) 0.0425(2) Uani 1 1 d . A . H99C H 0.3971 0.3096 0.4878 0.051 Uiso 1 1 calc R . . C4C C 0.51753(7) 0.26484(6) 0.39123(5) 0.0437(2) Uani 1 1 d D . . C5C C 0.57226(6) 0.29454(5) 0.32071(5) 0.03458(17) Uani 1 1 d . A . H5C H 0.6265 0.2491 0.2856 0.041 Uiso 1 1 calc R . . C6C C 0.54884(5) 0.38930(5) 0.30097(4) 0.02939(16) Uani 1 1 d . . . C13C C 0.60976(6) 0.41940(5) 0.22297(4) 0.03093(16) Uani 1 1 d . A . H13E H 0.6231 0.4971 0.2386 0.037 Uiso 1 1 calc R . . H13F H 0.6858 0.3863 0.2144 0.037 Uiso 1 1 calc R . . O1D O 0.44817(4) 0.55073(4) 0.16560(3) 0.03707(13) Uani 1 1 d D . . H77D H 0.4743(8) 0.5578(11) 0.2260(5) 0.050 Uiso 0.50 1 d PD . . H1D H 0.3746(6) 0.5793(10) 0.1618(8) 0.050 Uiso 0.50 1 d PD . . O2D O 0.42307(6) 0.10427(5) -0.11829(5) 0.0619(2) Uani 1 1 d . . . C1D C 0.46066(5) 0.44991(5) 0.11085(4) 0.02936(15) Uani 1 1 d . A . C2D C 0.54148(5) 0.38501(5) 0.13532(4) 0.02836(15) Uani 1 1 d . . . C3D C 0.55588(6) 0.28524(5) 0.07711(4) 0.03090(16) Uani 1 1 d . A . H99D H 0.6122 0.2409 0.0913 0.037 Uiso 1 1 calc R . . C4D C 0.49018(6) 0.24887(5) -0.00098(5) 0.03315(17) Uani 1 1 d . . . C5D C 0.40954(6) 0.31569(5) -0.02235(5) 0.03410(17) Uani 1 1 d . A . H5D H 0.3641 0.2912 -0.0755 0.041 Uiso 1 1 calc R . . C6D C 0.39410(6) 0.41674(5) 0.03196(4) 0.03120(16) Uani 1 1 d . . . C7D C 0.49994(7) 0.14036(6) -0.06285(5) 0.0399(2) Uani 1 1 d . A . C8D C 0.60338(7) 0.07674(6) -0.05530(5) 0.03800(19) Uani 1 1 d . . . H8D1 H 0.6032 0.0610 0.0041 0.046 Uiso 1 1 calc R A . H8D2 H 0.6742 0.1196 -0.0587 0.046 Uiso 1 1 calc R . . C9D C 0.60605(7) -0.02665(6) -0.12861(5) 0.0419(2) Uani 1 1 d . A . H9D1 H 0.5340 -0.0683 -0.1262 0.050 Uiso 1 1 calc R . . H9D2 H 0.6080 -0.0105 -0.1879 0.050 Uiso 1 1 calc R . . C10D C 0.70740(7) -0.09353(6) -0.12125(6) 0.0431(2) Uani 1 1 d . . . H10G H 0.7067 -0.1087 -0.0616 0.052 Uiso 1 1 calc R A . H10H H 0.7796 -0.0530 -0.1254 0.052 Uiso 1 1 calc R . . C11D C 0.70602(8) -0.19753(7) -0.19413(7) 0.0530(3) Uani 1 1 d . A . H11G H 0.6344 -0.2383 -0.1887 0.064 Uiso 1 1 calc R . . H11H H 0.7038 -0.1818 -0.2535 0.064 Uiso 1 1 calc R . . C12D C 0.80574(10) -0.26454(8) -0.19125(8) 0.0669(3) Uani 1 1 d . . . H12J H 0.8767 -0.2277 -0.2023 0.080 Uiso 1 1 calc R A . H12K H 0.7958 -0.3316 -0.2376 0.080 Uiso 1 1 calc R . . H12L H 0.8106 -0.2786 -0.1319 0.080 Uiso 1 1 calc R . . C13D C 0.30346(6) 0.48626(5) 0.00745(4) 0.03321(16) Uani 1 1 d . A . H13G H 0.3273 0.5616 0.0320 0.040 Uiso 1 1 calc R . . H13H H 0.2980 0.4719 -0.0588 0.040 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 O2B 0.0324(3) 0.0464(3) 0.0480(3) 0.0133(2) -0.0025(2) -0.0018(2) C7B 0.0346(3) 0.0394(3) 0.0362(3) 0.0089(3) 0.0019(3) 0.0020(3) C8B 0.0388(4) 0.0399(3) 0.0445(4) 0.0136(3) 0.0001(3) 0.0024(3) C9B 0.0464(4) 0.0448(4) 0.0541(4) 0.0191(3) 0.0003(4) -0.0013(3) C10B 0.0628(5) 0.0453(4) 0.0403(5) 0.0116(4) -0.0033(4) -0.0047(4) C11B 0.0814(8) 0.0608(6) 0.0620(8) 0.0268(5) -0.0029(7) -0.0134(6) C12B 0.1111(13) 0.1157(10) 0.0690(8) 0.0523(7) -0.0080(8) -0.0309(10) O2F 0.0324(3) 0.0464(3) 0.0480(3) 0.0133(2) -0.0025(2) -0.0018(2) C7F 0.0346(3) 0.0394(3) 0.0362(3) 0.0089(3) 0.0019(3) 0.0020(3) C8F 0.0388(4) 0.0399(3) 0.0445(4) 0.0136(3) 0.0001(3) 0.0024(3) C9F 0.0464(4) 0.0448(4) 0.0541(4) 0.0191(3) 0.0003(4) -0.0013(3) C10F 0.0628(5) 0.0453(4) 0.0403(5) 0.0116(4) -0.0033(4) -0.0047(4) C11F 0.0814(8) 0.0608(6) 0.0620(8) 0.0268(5) -0.0029(7) -0.0134(6) C12F 0.1111(13) 0.1157(10) 0.0690(8) 0.0523(7) -0.0080(8) -0.0309(10) O2C 0.1031(7) 0.0709(4) 0.0560(4) 0.0353(3) 0.0217(4) 0.0278(4) C7C 0.0487(5) 0.0488(4) 0.0427(5) 0.0219(3) -0.0003(4) 0.0044(4) C8C 0.0458(4) 0.0391(3) 0.0521(4) 0.0180(3) -0.0043(4) 0.0039(3) C9C 0.0590(6) 0.0374(4) 0.0439(5) 0.0129(3) 0.0047(5) 0.0117(4) C10C 0.0510(6) 0.0432(4) 0.0495(5) 0.0138(4) 0.0059(5) 0.0126(4) C11C 0.0684(7) 0.0436(5) 0.0732(7) 0.0164(5) 0.0084(6) 0.0179(5) C12C 0.0688(8) 0.0443(6) 0.1056(11) 0.0113(6) 0.0058(8) 0.0172(6) O2E 0.1031(7) 0.0709(4) 0.0560(4) 0.0353(3) 0.0217(4) 0.0278(4) C7E 0.0487(5) 0.0488(4) 0.0427(5) 0.0219(3) -0.0003(4) 0.0044(4) C8E 0.0458(4) 0.0391(3) 0.0521(4) 0.0180(3) -0.0043(4) 0.0039(3) C9E 0.0590(6) 0.0374(4) 0.0439(5) 0.0129(3) 0.0047(5) 0.0117(4) C10E 0.0510(6) 0.0432(4) 0.0495(5) 0.0138(4) 0.0059(5) 0.0126(4) C11E 0.0684(7) 0.0436(5) 0.0732(7) 0.0164(5) 0.0084(6) 0.0179(5) C12E 0.0688(8) 0.0443(6) 0.1056(11) 0.0113(6) 0.0058(8) 0.0172(6) O1 0.0901(9) 0.0561(6) 0.0530(6) 0.0269(5) -0.0150(6) -0.0260(6) C2 0.0955(14) 0.0543(8) 0.0577(9) 0.0257(7) -0.0088(10) -0.0222(9) O1A 0.0377(2) 0.0373(2) 0.0448(3) 0.01147(19) -0.0036(2) -0.0028(2) O2A 0.0357(3) 0.0567(3) 0.0637(3) 0.0130(3) -0.0046(3) -0.0098(2) C1A 0.0313(3) 0.0316(3) 0.0362(3) 0.0146(2) -0.0029(3) 0.0021(2) C2A 0.0302(3) 0.0358(3) 0.0341(3) 0.0177(2) -0.0011(2) 0.0028(2) C3A 0.0338(3) 0.0368(3) 0.0316(3) 0.0139(2) -0.0024(3) 0.0036(3) C4A 0.0312(3) 0.0372(3) 0.0375(3) 0.0167(2) -0.0059(3) 0.0007(2) C5A 0.0277(3) 0.0427(3) 0.0384(3) 0.0196(2) -0.0017(3) 0.0030(3) C6A 0.0301(3) 0.0382(3) 0.0342(3) 0.0161(2) -0.0011(2) 0.0059(2) C7A 0.0356(3) 0.0418(3) 0.0461(4) 0.0170(3) -0.0085(3) -0.0006(3) C8A 0.0415(4) 0.0517(4) 0.0553(5) 0.0024(4) -0.0092(4) -0.0021(4) C9A 0.0870(7) 0.0538(5) 0.0778(7) 0.0076(5) -0.0102(6) 0.0167(5) C10A 0.0514(5) 0.0631(5) 0.0737(6) 0.0064(5) -0.0023(5) 0.0021(4) C11A 0.0865(7) 0.0642(6) 0.0828(7) 0.0077(6) -0.0154(6) 0.0124(6) C12A 0.0793(7) 0.0782(7) 0.0845(8) 0.0116(6) 0.0029(6) 0.0173(6) C13A 0.0298(3) 0.0418(3) 0.0394(3) 0.0136(3) 0.0013(3) 0.0074(3) O1B 0.0382(3) 0.0400(2) 0.0459(3) 0.0103(2) 0.0013(2) -0.0018(2) C1B 0.0304(3) 0.0342(3) 0.0300(3) 0.0037(2) 0.0037(2) 0.0040(2) C2B 0.0294(3) 0.0369(3) 0.0291(3) 0.0061(2) 0.0028(2) 0.0070(2) C3B 0.0271(3) 0.0407(3) 0.0297(3) 0.0060(2) 0.0005(2) 0.0033(3) C4B 0.0300(3) 0.0383(3) 0.0289(3) 0.0062(2) 0.0036(2) 0.0027(3) C5B 0.0322(3) 0.0408(3) 0.0261(3) 0.0067(2) 0.0013(2) 0.0050(3) C6B 0.0290(3) 0.0403(3) 0.0245(3) 0.0026(2) 0.0011(2) 0.0030(3) C13B 0.0310(3) 0.0480(3) 0.0257(3) 0.0057(3) -0.0026(3) 0.0003(3) O1C 0.0408(3) 0.0330(2) 0.0412(2) 0.00849(19) -0.0019(2) 0.0003(2) C1C 0.0274(3) 0.0326(3) 0.0307(3) 0.0077(2) -0.0063(2) -0.0035(2) C2C 0.0267(3) 0.0445(3) 0.0295(3) 0.0090(2) -0.0044(2) -0.0007(3) C3C 0.0362(3) 0.0537(4) 0.0441(3) 0.0245(3) 0.0055(3) 0.0032(3) C4C 0.0410(4) 0.0463(3) 0.0507(4) 0.0244(3) 0.0045(3) 0.0063(3) C5C 0.0290(3) 0.0382(3) 0.0375(3) 0.0117(2) -0.0025(3) 0.0013(3) C6C 0.0248(3) 0.0339(3) 0.0286(3) 0.0073(2) -0.0043(2) -0.0045(2) C13C 0.0251(3) 0.0330(3) 0.0345(3) 0.0090(2) -0.0022(2) -0.0027(2) O1D 0.0407(2) 0.0302(2) 0.0400(2) 0.00888(18) 0.0015(2) -0.00108(19) O2D 0.0603(3) 0.0571(3) 0.0563(3) -0.0070(3) -0.0212(3) 0.0111(3) C1D 0.0272(3) 0.0312(3) 0.0319(3) 0.0127(2) 0.0038(2) -0.0034(2) C2D 0.0246(3) 0.0321(3) 0.0301(3) 0.0116(2) 0.0014(2) -0.0040(2) C3D 0.0267(3) 0.0344(3) 0.0334(3) 0.0121(2) 0.0028(2) -0.0002(2) C4D 0.0319(3) 0.0370(3) 0.0307(3) 0.0092(2) 0.0027(3) 0.0005(3) C5D 0.0320(3) 0.0417(3) 0.0295(3) 0.0111(2) 0.0006(3) -0.0003(3) C6D 0.0277(3) 0.0379(3) 0.0319(3) 0.0162(2) 0.0036(2) 0.0001(2) C7D 0.0414(4) 0.0421(3) 0.0337(3) 0.0053(3) -0.0014(3) 0.0003(3) C8D 0.0380(3) 0.0348(3) 0.0385(3) 0.0049(3) 0.0009(3) 0.0006(3) C9D 0.0445(4) 0.0379(3) 0.0392(4) 0.0026(3) 0.0031(3) 0.0009(3) C10D 0.0403(4) 0.0380(3) 0.0471(4) 0.0045(3) 0.0024(3) 0.0002(3) C11D 0.0506(4) 0.0469(4) 0.0540(5) -0.0003(4) -0.0003(4) 0.0045(4) C12D 0.0781(6) 0.0554(5) 0.0616(6) 0.0031(4) -0.0031(5) 0.0220(5) C13D 0.0328(3) 0.0384(3) 0.0329(3) 0.0175(2) 0.0008(2) 0.0005(3) _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 O2B C7B 1.2329(14) . ? C7B C4B 1.4839(14) . ? C7B C8B 1.5096(18) . ? C8B C9B 1.5163(18) . ? C9B C10B 1.519(2) . ? C10B C11B 1.507(2) . ? C11B C12B 1.482(3) . ? O2F C7F 1.215(2) . ? C7F C4B 1.523(2) . ? C7F C8F 1.526(3) . ? C8F C9F 1.530(3) . ? C9F C10F 1.532(3) . ? C10F C11F 1.536(4) . ? C11F C12F 1.490(4) . ? O2C C7C 1.2247(14) . ? C7C C4C 1.4965(14) . ? C7C C8C 1.5024(14) . ? C8C C9C 1.5208(16) . ? C9C C10C 1.5185(15) . ? C10C C11C 1.5297(17) . ? C11C C12C 1.5063(18) . ? O2E C7E 1.232(4) . ? C7E C8E 1.524(4) . ? C7E C4C 1.566(3) . ? C8E C9E 1.530(4) . ? C9E C10E 1.520(4) . ? C10E C11E 1.537(4) . ? C11E C12E 1.512(4) . ? O1 C2 1.390(3) . ? O1A C1A 1.3724(8) . ? O2A C7A 1.2178(10) . ? C1A C2A 1.3991(9) . ? C1A C6A 1.4045(10) . ? C2A C3A 1.3896(9) . ? C2A C13D 1.5199(10) . ? C3A C4A 1.3925(10) . ? C4A C5A 1.3954(9) . ? C4A C7A 1.4954(10) . ? C5A C6A 1.3858(9) . ? C6A C13A 1.5157(9) . ? C7A C8A 1.4995(11) . ? C8A C9A 1.5563(16) . ? C9A C10A 1.4720(14) . ? C10A C11A 1.5157(18) . ? C11A C12A 1.4635(16) . ? C13A C2B 1.5244(11) . ? O1B C1B 1.3718(9) . ? C1B C6B 1.3970(11) . ? C1B C2B 1.4074(9) . ? C2B C3B 1.3824(10) . ? C3B C4B 1.3944(11) . ? C4B C5B 1.3942(10) . ? C5B C6B 1.3885(10) . ? C6B C13B 1.5216(10) . ? C13B C2C 1.5254(10) . ? O1C C1C 1.3747(9) . ? C1C C6C 1.4001(9) . ? C1C C2C 1.4031(10) . ? C2C C3C 1.3779(12) . ? C3C C4C 1.3927(11) . ? C4C C5C 1.3952(12) . ? C5C C6C 1.3877(10) . ? C6C C13C 1.5286(10) . ? C13C C2D 1.5192(9) . ? O1D C1D 1.3809(7) . ? O2D C7D 1.2279(10) . ? C1D C6D 1.4001(9) . ? C1D C2D 1.4006(10) . ? C2D C3D 1.3936(8) . ? C3D C4D 1.3886(9) . ? C4D C5D 1.3972(10) . ? C4D C7D 1.4980(10) . ? C5D C6D 1.3861(9) . ? C6D C13D 1.5224(10) . ? C7D C8D 1.5048(11) . ? C8D C9D 1.5211(10) . ? C9D C10D 1.5106(12) . ? C10D C11D 1.5217(11) . ? C11D C12D 1.4826(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2B C7B C4B 121.39(11) . . ? O2B C7B C8B 120.14(11) . . ? C4B C7B C8B 117.92(9) . . ? C7B C8B C9B 113.70(10) . . ? C8B C9B C10B 114.85(11) . . ? C11B C10B C9B 113.84(12) . . ? C12B C11B C10B 114.95(15) . . ? O2F C7F C4B 118.02(19) . . ? O2F C7F C8F 120.81(19) . . ? C4B C7F C8F 120.27(16) . . ? C7F C8F C9F 113.56(19) . . ? C8F C9F C10F 110.3(2) . . ? C9F C10F C11F 112.5(2) . . ? C12F C11F C10F 109.7(2) . . ? O2C C7C C4C 122.08(9) . . ? O2C C7C C8C 121.08(10) . . ? C4C C7C C8C 116.84(9) . . ? C7C C8C C9C 111.70(9) . . ? C10C C9C C8C 111.77(10) . . ? C9C C10C C11C 112.61(10) . . ? C12C C11C C10C 113.08(12) . . ? O2E C7E C8E 120.8(3) . . ? O2E C7E C4C 117.0(2) . . ? C8E C7E C4C 120.0(2) . . ? C7E C8E C9E 119.8(3) . . ? C10E C9E C8E 114.9(3) . . ? C9E C10E C11E 114.4(3) . . ? C12E C11E C10E 110.7(3) . . ? O1A C1A C2A 119.08(6) . . ? O1A C1A C6A 119.25(6) . . ? C2A C1A C6A 121.66(6) . . ? C3A C2A C1A 118.11(6) . . ? C3A C2A C13D 120.18(6) . . ? C1A C2A C13D 121.66(6) . . ? C2A C3A C4A 121.74(6) . . ? C3A C4A C5A 118.64(6) . . ? C3A C4A C7A 122.93(6) . . ? C5A C4A C7A 118.43(6) . . ? C6A C5A C4A 121.70(6) . . ? C5A C6A C1A 118.14(6) . . ? C5A C6A C13A 120.05(6) . . ? C1A C6A C13A 121.79(6) . . ? O2A C7A C4A 120.46(7) . . ? O2A C7A C8A 120.31(7) . . ? C4A C7A C8A 119.17(7) . . ? C7A C8A C9A 110.71(8) . . ? C10A C9A C8A 115.78(10) . . ? C9A C10A C11A 116.50(10) . . ? C12A C11A C10A 116.54(11) . . ? C6A C13A C2B 112.93(6) . . ? O1B C1B C6B 119.48(6) . . ? O1B C1B C2B 118.77(7) . . ? C6B C1B C2B 121.73(7) . . ? C3B C2B C1B 118.15(7) . . ? C3B C2B C13A 120.46(6) . . ? C1B C2B C13A 121.36(6) . . ? C2B C3B C4B 121.60(6) . . ? C5B C4B C3B 118.79(7) . . ? C5B C4B C7B 123.45(8) . . ? C3B C4B C7B 117.74(7) . . ? C5B C4B C7F 121.19(10) . . ? C3B C4B C7F 120.02(10) . . ? C7B C4B C7F 2.68(10) . . ? C6B C5B C4B 121.64(7) . . ? C5B C6B C1B 118.06(6) . . ? C5B C6B C13B 120.48(7) . . ? C1B C6B C13B 121.45(7) . . ? C6B C13B C2C 113.01(5) . . ? O1C C1C C6C 118.99(6) . . ? O1C C1C C2C 118.83(6) . . ? C6C C1C C2C 122.14(7) . . ? C3C C2C C1C 117.68(6) . . ? C3C C2C C13B 120.27(7) . . ? C1C C2C C13B 122.05(7) . . ? C2C C3C C4C 121.97(8) . . ? C3C C4C C5C 118.97(7) . . ? C3C C4C C7C 117.54(8) . . ? C5C C4C C7C 122.95(7) . . ? C3C C4C C7E 121.46(12) . . ? C5C C4C C7E 116.33(11) . . ? C7C C4C C7E 25.70(11) . . ? C6C C5C C4C 121.18(6) . . ? C5C C6C C1C 118.00(6) . . ? C5C C6C C13C 119.97(6) . . ? C1C C6C C13C 122.03(6) . . ? C2D C13C C6C 112.85(5) . . ? O1D C1D C6D 119.08(6) . . ? O1D C1D C2D 118.71(6) . . ? C6D C1D C2D 122.20(6) . . ? C3D C2D C1D 117.63(6) . . ? C3D C2D C13C 120.30(6) . . ? C1D C2D C13C 122.05(5) . . ? C4D C3D C2D 121.83(6) . . ? C3D C4D C5D 118.67(6) . . ? C3D C4D C7D 123.14(7) . . ? C5D C4D C7D 118.19(6) . . ? C6D C5D C4D 121.78(6) . . ? C5D C6D C1D 117.85(6) . . ? C5D C6D C13D 120.20(6) . . ? C1D C6D C13D 121.90(5) . . ? O2D C7D C4D 119.61(7) . . ? O2D C7D C8D 121.01(7) . . ? C4D C7D C8D 119.38(6) . . ? C7D C8D C9D 112.78(6) . . ? C10D C9D C8D 113.92(7) . . ? C9D C10D C11D 112.64(7) . . ? C12D C11D C10D 114.60(8) . . ? C2A C13D C6D 111.66(6) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.72 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.514 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.052 data_ad4 _database_code_depnum_ccdc_archive 'CCDC 265960' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common p-hexanoyl-calix(4)arene.Dimethylformamide.Methanol _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55.70 H73.80 N O9.70' _chemical_formula_weight 912.56 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' _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 10.3974(8) _cell_length_b 15.6582(12) _cell_length_c 16.6568(12) _cell_angle_alpha 90.948(2) _cell_angle_beta 107.931(2) _cell_angle_gamma 100.732(2) _cell_volume 2527.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 985 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.9607 _exptl_absorpt_correction_T_max 0.9723 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _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 23077 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.0560 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8906 _reflns_number_gt 4536 _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^)+(0.1011P)^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 8906 _refine_ls_number_parameters 823 _refine_ls_number_restraints 208 _refine_ls_R_factor_all 0.1282 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1790 _refine_ls_wR_factor_gt 0.1563 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.960 _refine_ls_shift/su_max 0.022 _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 O1A1 O 0.3237(5) 0.3033(5) 0.2989(4) 0.1178(8) Uani 0.14 1 d PD A 1 N1A1 N 0.4309(5) 0.2759(4) 0.2324(3) 0.0981(5) Uani 0.14 1 d PD A 1 C1A1 C 0.4300(7) 0.2695(6) 0.3128(4) 0.1114(12) Uani 0.14 1 d PD A 1 H1A1 H 0.4869 0.2480 0.3613 0.134 Uiso 0.14 1 calc PR A 1 C2A1 C 0.3349(8) 0.3100(6) 0.1591(4) 0.1123(12) Uani 0.14 1 d PD A 1 H2A1 H 0.2736 0.3391 0.1792 0.168 Uiso 0.14 1 calc PR A 1 H2A2 H 0.2798 0.2614 0.1176 0.168 Uiso 0.14 1 calc PR A 1 H2A3 H 0.3886 0.3518 0.1326 0.168 Uiso 0.14 1 calc PR A 1 C3A1 C 0.5487(6) 0.2499(5) 0.2257(6) 0.0896(9) Uani 0.14 1 d PDU A 1 H3A1 H 0.6299 0.2958 0.2524 0.134 Uiso 0.14 1 calc PR A 1 H3A2 H 0.5393 0.2393 0.1658 0.134 Uiso 0.14 1 calc PR A 1 H3A3 H 0.5596 0.1962 0.2542 0.134 Uiso 0.14 1 calc PR A 1 O1B1 O 0.17429(19) 0.30192(17) 0.20492(14) 0.1178(8) Uani 0.47 1 d PD B 2 N1B1 N 0.3831(2) 0.26318(17) 0.23288(15) 0.0981(5) Uani 0.47 1 d PD B 2 C1B1 C 0.2658(3) 0.2767(2) 0.25001(18) 0.1114(12) Uani 0.47 1 d PD B 2 H1B1 H 0.2600 0.2639 0.3045 0.134 Uiso 0.47 1 calc PR B 2 C2B1 C 0.3954(3) 0.2849(3) 0.15153(15) 0.1123(12) Uani 0.47 1 d PD B 2 H2B1 H 0.3771 0.2312 0.1153 0.168 Uiso 0.47 1 calc PR B 2 H2B2 H 0.4889 0.3173 0.1588 0.168 Uiso 0.47 1 calc PR B 2 H2B3 H 0.3284 0.3208 0.1252 0.168 Uiso 0.47 1 calc PR B 2 C3B1 C 0.5028(3) 0.24327(19) 0.28690(19) 0.0896(9) Uani 0.47 1 d PDU B 2 H3B1 H 0.5309 0.2791 0.3405 0.134 Uiso 0.47 1 calc PR B 2 H3B2 H 0.5762 0.2552 0.2608 0.134 Uiso 0.47 1 calc PR B 2 H3B3 H 0.4859 0.1815 0.2975 0.134 Uiso 0.47 1 calc PR B 2 O1C1 O 0.1903(4) 0.2427(3) 0.2417(3) 0.1178(8) Uani 0.23 1 d PD C 3 N1C1 N 0.3952(4) 0.2518(3) 0.2282(3) 0.0981(5) Uani 0.23 1 d PD C 3 C1C1 C 0.2662(5) 0.2660(4) 0.1954(3) 0.1114(12) Uani 0.23 1 d PD C 3 H1C1 H 0.2349 0.2909 0.1431 0.134 Uiso 0.23 1 calc PR C 3 C2C1 C 0.4941(5) 0.2579(5) 0.1835(3) 0.1123(12) Uani 0.23 1 d PD C 3 H2C1 H 0.4680 0.2934 0.1354 0.168 Uiso 0.23 1 calc PR C 3 H2C2 H 0.4962 0.1994 0.1628 0.168 Uiso 0.23 1 calc PR C 3 H2C3 H 0.5857 0.2852 0.2217 0.168 Uiso 0.23 1 calc PR C 3 C3C1 C 0.4387(6) 0.2264(4) 0.3146(3) 0.0896(9) Uani 0.23 1 d PDU C 3 H3C1 H 0.4268 0.2703 0.3529 0.134 Uiso 0.23 1 calc PR C 3 H3C2 H 0.5361 0.2221 0.3310 0.134 Uiso 0.23 1 calc PR C 3 H3C3 H 0.3826 0.1697 0.3181 0.134 Uiso 0.23 1 calc PR C 3 O1D1 O 0.2608(5) 0.3470(5) 0.2159(4) 0.1178(8) Uani 0.16 1 d PD D 4 N1D1 N 0.4079(5) 0.2662(4) 0.2315(4) 0.0981(5) Uani 0.16 1 d PD D 4 C1D1 C 0.3498(6) 0.3280(5) 0.1933(4) 0.1114(12) Uani 0.16 1 d PD D 4 H1D1 H 0.3777 0.3563 0.1496 0.134 Uiso 0.16 1 calc PR D 4 C3D1 C 0.3336(7) 0.2250(5) 0.2864(4) 0.0896(9) Uani 0.16 1 d PDU D 4 H3D1 H 0.2502 0.2488 0.2790 0.134 Uiso 0.16 1 calc PR D 4 H3D2 H 0.3928 0.2367 0.3455 0.134 Uiso 0.16 1 calc PR D 4 H3D3 H 0.3077 0.1620 0.2718 0.134 Uiso 0.16 1 calc PR D 4 C2D1 C 0.5383(6) 0.2479(7) 0.2401(5) 0.1123(12) Uani 0.16 1 d PD D 4 H2D1 H 0.5497 0.1962 0.2719 0.168 Uiso 0.16 1 calc PR D 4 H2D2 H 0.6099 0.2978 0.2706 0.168 Uiso 0.16 1 calc PR D 4 H2D3 H 0.5463 0.2369 0.1840 0.168 Uiso 0.16 1 calc PR D 4 O1M O 1.1651(4) 0.3495(3) 0.3489(2) 0.1004(9) Uani 0.18 1 d PD E -1 H1M H 1.2096 0.3704 0.3170 0.151 Uiso 0.18 1 calc PR E -1 C1M C 1.2314(6) 0.3804(4) 0.4259(2) 0.0710(11) Uani 0.18 1 d PD E -1 H1M1 H 1.2555 0.4441 0.4280 0.106 Uiso 0.18 1 calc PR E -1 H1M2 H 1.3158 0.3570 0.4465 0.106 Uiso 0.18 1 calc PR E -1 H1M3 H 1.1731 0.3635 0.4617 0.106 Uiso 0.18 1 calc PR E -1 O2M O 1.1686(8) 0.3031(2) 0.3841(5) 0.1004(9) Uani 0.10 1 d PD F -2 H2M H 1.0963 0.2839 0.3960 0.151 Uiso 0.10 1 calc PR F -2 C2M C 1.1684(11) 0.3817(3) 0.3619(6) 0.0710(11) Uani 0.10 1 d PD F -2 H2M1 H 1.0821 0.3981 0.3623 0.106 Uiso 0.10 1 calc PR F -2 H2M2 H 1.1761 0.3848 0.3048 0.106 Uiso 0.10 1 calc PR F -2 H2M3 H 1.2467 0.4217 0.4017 0.106 Uiso 0.10 1 calc PR F -2 O3M O 1.2665(5) 0.3264(5) 0.3641(3) 0.1004(9) Uani 0.12 1 d PD G -3 H3M H 1.2564 0.3695 0.3350 0.151 Uiso 0.12 1 calc PR G -3 C3M C 1.3587(7) 0.3514(6) 0.4364(3) 0.0710(11) Uani 0.12 1 d PD G -3 H3M1 H 1.4451 0.3344 0.4371 0.106 Uiso 0.12 1 calc PR G -3 H3M2 H 1.3269 0.3240 0.4812 0.106 Uiso 0.12 1 calc PR G -3 H3M3 H 1.3743 0.4150 0.4461 0.106 Uiso 0.12 1 calc PR G -3 O4M O 1.1876(3) 0.29490(18) 0.3971(2) 0.1004(9) Uani 0.30 1 d PD H -4 H4M H 1.2345 0.2569 0.4149 0.151 Uiso 0.30 1 calc PR H -4 C4M C 1.2652(4) 0.37141(19) 0.4188(3) 0.0710(11) Uani 0.30 1 d PD H -4 H4M1 H 1.2462 0.3984 0.4663 0.106 Uiso 0.30 1 calc PR H -4 H4M2 H 1.2462 0.4076 0.3708 0.106 Uiso 0.30 1 calc PR H -4 H4M3 H 1.3623 0.3663 0.4359 0.106 Uiso 0.30 1 calc PR H -4 O7C O 0.45831(14) 0.08349(8) 0.56685(8) 0.0785(3) Uani 0.58 1 d PD I 1 C7C C 0.48955(19) 0.16143(12) 0.55881(11) 0.0622(4) Uani 0.58 1 d PD I 1 C8C C 0.41875(18) 0.22496(12) 0.58859(12) 0.0718(4) Uani 0.58 1 d PD I 1 H8C1 H 0.3881 0.2627 0.5423 0.086 Uiso 0.58 1 calc PR I 1 H8C2 H 0.4878 0.2628 0.6367 0.086 Uiso 0.58 1 calc PR I 1 C9C C 0.29606(17) 0.18699(12) 0.61616(11) 0.0586(4) Uani 0.58 1 d PD I 1 H9C1 H 0.3272 0.1536 0.6660 0.070 Uiso 0.58 1 calc PR I 1 H9C2 H 0.2290 0.1458 0.5700 0.070 Uiso 0.58 1 calc PR I 1 C10C C 0.22397(17) 0.25511(11) 0.63862(10) 0.0560(4) Uani 0.58 1 d PD I 1 H10C H 0.2880 0.2926 0.6887 0.067 Uiso 0.58 1 calc PR I 1 H10D H 0.2013 0.2925 0.5910 0.067 Uiso 0.58 1 calc PR I 1 C11C C 0.09347(17) 0.21640(12) 0.65754(12) 0.0620(4) Uani 0.58 1 d PD I 1 H11C H 0.0236 0.1880 0.6044 0.074 Uiso 0.58 1 calc PR I 1 H11D H 0.1130 0.1705 0.6971 0.074 Uiso 0.58 1 calc PR I 1 C12C C 0.03271(18) 0.28068(12) 0.69534(11) 0.0630(4) Uani 0.58 1 d PD I 1 H12C H 0.0999 0.3081 0.7489 0.076 Uiso 0.58 1 calc PR I 1 H12D H -0.0513 0.2502 0.7057 0.076 Uiso 0.58 1 calc PR I 1 H12E H 0.0100 0.3255 0.6560 0.076 Uiso 0.58 1 calc PR I 1 O7G O 0.4595(2) 0.08901(12) 0.57281(12) 0.0785(3) Uani 0.42 1 d PD I 2 C7G C 0.4907(3) 0.16553(17) 0.56076(16) 0.0622(4) Uani 0.42 1 d PD I 2 C8G C 0.4125(3) 0.23070(18) 0.57988(18) 0.0718(4) Uani 0.42 1 d PD I 2 H8G1 H 0.3861 0.2652 0.5303 0.086 Uiso 0.42 1 calc PR I 2 H8G2 H 0.4746 0.2714 0.6282 0.086 Uiso 0.42 1 calc PR I 2 C9G C 0.2839(2) 0.19076(17) 0.60095(15) 0.0586(4) Uani 0.42 1 d PD I 2 H9G1 H 0.2187 0.1529 0.5514 0.070 Uiso 0.42 1 calc PR I 2 H9G2 H 0.3090 0.1536 0.6486 0.070 Uiso 0.42 1 calc PR I 2 C10G C 0.2127(2) 0.25845(17) 0.62468(15) 0.0560(4) Uani 0.42 1 d PD I 2 H10G H 0.1799 0.2916 0.5749 0.067 Uiso 0.42 1 calc PR I 2 H10H H 0.2812 0.3000 0.6700 0.067 Uiso 0.42 1 calc PR I 2 C11G C 0.0913(3) 0.22166(18) 0.65475(17) 0.0620(4) Uani 0.42 1 d PD I 2 H11G H 0.1222 0.1881 0.7046 0.074 Uiso 0.42 1 calc PR I 2 H11H H 0.0200 0.1817 0.6093 0.074 Uiso 0.42 1 calc PR I 2 C12G C 0.0306(3) 0.29631(17) 0.67836(17) 0.0630(4) Uani 0.42 1 d PD I 2 H12G H 0.0929 0.3273 0.7318 0.076 Uiso 0.42 1 calc PR I 2 H12H H -0.0595 0.2728 0.6849 0.076 Uiso 0.42 1 calc PR I 2 H12I H 0.0194 0.3367 0.6336 0.076 Uiso 0.42 1 calc PR I 2 O7H O 0.4358(7) -0.0630(5) 0.0727(3) 0.0698(3) Uani 0.10 1 d PD J 1 C7H C 0.4663(7) -0.0571(5) 0.1479(4) 0.0540(4) Uani 0.10 1 d PD J 1 C8H C 0.3918(6) -0.1055(5) 0.2039(5) 0.0633(4) Uani 0.10 1 d PD J 1 H8H1 H 0.4553 -0.1087 0.2614 0.076 Uiso 0.10 1 calc PR J 1 H8H2 H 0.3432 -0.1650 0.1789 0.076 Uiso 0.10 1 calc PR J 1 C9H C 0.2903(7) -0.0457(6) 0.2045(4) 0.0752(5) Uani 0.10 1 d PD J 1 H9H1 H 0.3322 0.0149 0.1980 0.090 Uiso 0.10 1 calc PR J 1 H9H2 H 0.2052 -0.0643 0.1558 0.090 Uiso 0.10 1 calc PR J 1 C10H C 0.2531(8) -0.0478(5) 0.2851(5) 0.0908(6) Uani 0.10 1 d PD J 1 H10A H 0.3351 -0.0554 0.3319 0.109 Uiso 0.10 1 calc PR J 1 H10B H 0.1800 -0.1000 0.2798 0.109 Uiso 0.10 1 calc PR J 1 C11H C 0.2034(7) 0.0316(5) 0.3107(5) 0.0957(6) Uani 0.10 1 d PD J 1 H11A H 0.1492 0.0570 0.2604 0.115 Uiso 0.10 1 calc PR J 1 H11B H 0.2818 0.0771 0.3448 0.115 Uiso 0.10 1 calc PR J 1 C12H C 0.1122(9) -0.0085(9) 0.3638(6) 0.1126(6) Uani 0.10 1 d PD J 1 H12A H 0.1217 -0.0691 0.3726 0.135 Uiso 0.10 1 calc PR J 1 H12B H 0.0155 -0.0070 0.3338 0.135 Uiso 0.10 1 calc PR J 1 H12C' H 0.1415 0.0251 0.4188 0.135 Uiso 0.10 1 calc PR J 1 O7D O 0.39103(8) -0.05562(6) 0.07343(5) 0.0698(3) Uani 0.90 1 d PD J 2 C7D C 0.43772(11) -0.04104(7) 0.15074(7) 0.0540(4) Uani 0.90 1 d PD J 2 C8D C 0.35147(11) -0.08244(8) 0.20193(8) 0.0633(4) Uani 0.90 1 d PD J 2 H8D1 H 0.4106 -0.1054 0.2521 0.076 Uiso 0.90 1 calc PR J 2 H8D2 H 0.2813 -0.1321 0.1676 0.076 Uiso 0.90 1 calc PR J 2 C9D C 0.27851(13) -0.01609(9) 0.23124(8) 0.0752(5) Uani 0.90 1 d PD J 2 H9D1 H 0.3487 0.0281 0.2731 0.090 Uiso 0.90 1 calc PR J 2 H9D2 H 0.2334 0.0144 0.1820 0.090 Uiso 0.90 1 calc PR J 2 C10D C 0.17057(13) -0.05844(10) 0.27075(10) 0.0908(6) Uani 0.90 1 d PD J 2 H40A H 0.0987 -0.1014 0.2284 0.109 Uiso 0.90 1 calc PR J 2 H40B H 0.2149 -0.0902 0.3191 0.109 Uiso 0.90 1 calc PR J 2 C11D C 0.10348(14) 0.00738(10) 0.30107(10) 0.0957(6) Uani 0.90 1 d PD J 2 H41A H 0.0755 0.0468 0.2558 0.115 Uiso 0.90 1 calc PR J 2 H41B H 0.0190 -0.0236 0.3119 0.115 Uiso 0.90 1 calc PR J 2 C12D C 0.19630(17) 0.06085(12) 0.38004(10) 0.1126(6) Uani 0.90 1 d PD J 2 H42A H 0.2015 0.0259 0.4288 0.135 Uiso 0.90 1 calc PR J 2 H42B H 0.1593 0.1124 0.3879 0.135 Uiso 0.90 1 calc PR J 2 H42F H 0.2888 0.0792 0.3751 0.135 Uiso 0.90 1 calc PR J 2 O7J O 0.4053(3) 0.55499(18) 0.37152(17) 0.0826(3) Uani 0.28 1 d PD K 3 C7J C 0.4402(4) 0.5390(2) 0.3101(2) 0.0743(4) Uani 0.28 1 d PD K 3 C8J C 0.3243(4) 0.5236(3) 0.2241(3) 0.0777(6) Uani 0.28 1 d PD K 3 H8J1 H 0.3640 0.5200 0.1775 0.093 Uiso 0.28 1 calc PR K 3 H8J2 H 0.2590 0.4681 0.2217 0.093 Uiso 0.28 1 calc PR K 3 C9J C 0.2483(4) 0.6002(3) 0.2144(3) 0.0881(7) Uani 0.28 1 d PD K 3 H9J1 H 0.1766 0.5865 0.2425 0.106 Uiso 0.28 1 calc PR K 3 H9J2 H 0.3155 0.6522 0.2466 0.106 Uiso 0.28 1 calc PR K 3 C10J C 0.1797(4) 0.6260(4) 0.1271(3) 0.1039(10) Uani 0.28 1 d PD K 3 H50A H 0.2066 0.5917 0.0867 0.125 Uiso 0.28 1 calc PR K 3 H50B H 0.2211 0.6879 0.1250 0.125 Uiso 0.28 1 calc PR K 3 C11J C 0.0239(4) 0.6171(3) 0.0929(3) 0.0937(9) Uani 0.28 1 d PD K 3 H51A H -0.0199 0.5544 0.0859 0.112 Uiso 0.28 1 calc PR K 3 H51B H -0.0071 0.6458 0.1350 0.112 Uiso 0.28 1 calc PR K 3 C12J C -0.0254(6) 0.6563(4) 0.0089(3) 0.1352(12) Uani 0.28 1 d PD K 3 H51A' H 0.0302 0.7149 0.0120 0.162 Uiso 0.28 1 calc PR K 3 H51B' H -0.1226 0.6600 -0.0033 0.162 Uiso 0.28 1 calc PR K 3 H51C H -0.0156 0.6195 -0.0361 0.162 Uiso 0.28 1 calc PR K 3 O7B O 0.3701(2) 0.52025(15) 0.36722(14) 0.0826(3) Uani 0.35 1 d PD K 1 C7B C 0.4270(3) 0.5237(2) 0.3115(2) 0.0743(4) Uani 0.35 1 d PD K 1 C8B C 0.3793(3) 0.5674(2) 0.2271(2) 0.0777(6) Uani 0.35 1 d PD K 1 H8B1 H 0.4443 0.6234 0.2311 0.093 Uiso 0.35 1 calc PR K 1 H8B2 H 0.3852 0.5294 0.1808 0.093 Uiso 0.35 1 calc PR K 1 C9B C 0.2354(3) 0.5847(3) 0.2041(2) 0.0881(7) Uani 0.35 1 d PD K 1 H9B1 H 0.1826 0.5389 0.2284 0.106 Uiso 0.35 1 calc PR K 1 H9B2 H 0.2428 0.6405 0.2357 0.106 Uiso 0.35 1 calc PR K 1 C10B C 0.1463(4) 0.5903(3) 0.1165(2) 0.1039(10) Uani 0.35 1 d PD K 1 H60A H 0.0846 0.5326 0.0962 0.125 Uiso 0.35 1 calc PR K 1 H60B H 0.2060 0.6016 0.0801 0.125 Uiso 0.35 1 calc PR K 1 C11B C 0.0581(4) 0.6585(3) 0.1040(2) 0.0937(9) Uani 0.35 1 d PD K 1 H61A H 0.1171 0.7176 0.1138 0.112 Uiso 0.35 1 calc PR K 1 H61B H 0.0051 0.6532 0.1445 0.112 Uiso 0.35 1 calc PR K 1 C12B C -0.0417(5) 0.6438(4) 0.0118(3) 0.1352(12) Uani 0.35 1 d PD K 1 H62A H -0.0061 0.6088 -0.0226 0.162 Uiso 0.35 1 calc PR K 1 H62B H -0.0492 0.7003 -0.0118 0.162 Uiso 0.35 1 calc PR K 1 H62C H -0.1330 0.6130 0.0116 0.162 Uiso 0.35 1 calc PR K 1 O7F O 0.4138(2) 0.55353(15) 0.38086(14) 0.0826(3) Uani 0.37 1 d PD K 2 C7F C 0.4484(3) 0.5450(2) 0.3185(2) 0.0743(4) Uani 0.37 1 d PD K 2 C8F C 0.3625(3) 0.5747(2) 0.2351(2) 0.0777(6) Uani 0.37 1 d PD K 2 H8F1 H 0.3352 0.5264 0.1903 0.093 Uiso 0.37 1 calc PR K 2 H8F2 H 0.4201 0.6242 0.2179 0.093 Uiso 0.37 1 calc PR K 2 C9F C 0.2320(3) 0.6029(2) 0.2423(2) 0.0881(7) Uani 0.37 1 d PD K 2 H9F1 H 0.1695 0.5523 0.2541 0.106 Uiso 0.37 1 calc PR K 2 H9F2 H 0.2577 0.6483 0.2897 0.106 Uiso 0.37 1 calc PR K 2 C10F C 0.1586(4) 0.6386(3) 0.1602(2) 0.1039(10) Uani 0.37 1 d PD K 2 H70A H 0.0864 0.6667 0.1700 0.125 Uiso 0.37 1 calc PR K 2 H70B H 0.2262 0.6847 0.1467 0.125 Uiso 0.37 1 calc PR K 2 C11F C 0.0927(4) 0.5754(2) 0.0846(2) 0.0937(9) Uani 0.37 1 d PD K 2 H71A H 0.0500 0.5198 0.1017 0.112 Uiso 0.37 1 calc PR K 2 H71B H 0.1640 0.5636 0.0604 0.112 Uiso 0.37 1 calc PR K 2 C12F C -0.0163(5) 0.6100(3) 0.0180(3) 0.1352(12) Uani 0.37 1 d PD K 2 H72A H -0.1053 0.5929 0.0280 0.162 Uiso 0.37 1 calc PR K 2 H72B H -0.0234 0.5858 -0.0381 0.162 Uiso 0.37 1 calc PR K 2 H72C H 0.0092 0.6737 0.0211 0.162 Uiso 0.37 1 calc PR K 2 O7A O 0.42630(13) 0.38805(7) -0.08558(7) 0.0895(4) Uani 0.70 1 d PD L 1 C7A C 0.48143(18) 0.32518(10) -0.06831(9) 0.0707(4) Uani 0.70 1 d PD L 1 C8A C 0.42742(18) 0.24414(10) -0.12995(9) 0.0713(5) Uani 0.70 1 d PD L 1 H8A1 H 0.5069 0.2233 -0.1383 0.086 Uiso 0.70 1 calc PR L 1 H8B1' H 0.3722 0.2603 -0.1853 0.086 Uiso 0.70 1 calc PR L 1 C9A C 0.33670(17) 0.16788(12) -0.10067(12) 0.0895(7) Uani 0.70 1 d PD L 1 H9A1 H 0.2972 0.1216 -0.1477 0.107 Uiso 0.70 1 calc PR L 1 H9B1' H 0.3980 0.1432 -0.0528 0.107 Uiso 0.70 1 calc PR L 1 C10A C 0.2248(2) 0.18825(14) -0.07467(14) 0.1081(8) Uani 0.70 1 d PD L 1 H80A H 0.1589 0.2093 -0.1230 0.130 Uiso 0.70 1 calc PR L 1 H80B H 0.2619 0.2357 -0.0287 0.130 Uiso 0.70 1 calc PR L 1 C11A C 0.1487(2) 0.10945(17) -0.04373(16) 0.1431(10) Uani 0.70 1 d PD L 1 H81A H 0.1159 0.0616 -0.0893 0.172 Uiso 0.70 1 calc PR L 1 H81B H 0.2155 0.0897 0.0052 0.172 Uiso 0.70 1 calc PR L 1 C12A C 0.0294(2) 0.1233(2) -0.0181(2) 0.1744(13) Uani 0.70 1 d PD L 1 H82A H 0.0617 0.1470 0.0411 0.209 Uiso 0.70 1 calc PR L 1 H82B H -0.0353 0.0676 -0.0243 0.209 Uiso 0.70 1 calc PR L 1 H82C H -0.0171 0.1644 -0.0542 0.209 Uiso 0.70 1 calc PR L 1 O7E O 0.4114(3) 0.38437(17) -0.06495(17) 0.0895(4) Uani 0.30 1 d PD L 2 C7E C 0.4696(4) 0.3239(2) -0.0589(2) 0.0707(4) Uani 0.30 1 d PD L 2 C8E C 0.3938(4) 0.2399(2) -0.1114(2) 0.0713(5) Uani 0.30 1 d PD L 2 H8E1 H 0.4592 0.2122 -0.1298 0.086 Uiso 0.30 1 calc PR L 2 H8E2 H 0.3225 0.2521 -0.1625 0.086 Uiso 0.30 1 calc PR L 2 C9E C 0.3228(4) 0.1755(3) -0.0572(3) 0.0895(7) Uani 0.30 1 d PD L 2 H9E1 H 0.3861 0.1373 -0.0286 0.107 Uiso 0.30 1 calc PR L 2 H9E2 H 0.3040 0.2097 -0.0130 0.107 Uiso 0.30 1 calc PR L 2 C10E C 0.1944(4) 0.1225(3) -0.1118(3) 0.1081(8) Uani 0.30 1 d PD L 2 H10E H 0.2135 0.0870 -0.1549 0.130 Uiso 0.30 1 calc PR L 2 H10F H 0.1321 0.1607 -0.1415 0.130 Uiso 0.30 1 calc PR L 2 C11E C 0.1264(5) 0.0640(4) -0.0603(3) 0.1431(10) Uani 0.30 1 d PD L 2 H11E H 0.1764 0.0158 -0.0443 0.172 Uiso 0.30 1 calc PR L 2 H11F H 0.0309 0.0381 -0.0957 0.172 Uiso 0.30 1 calc PR L 2 C12E C 0.1217(6) 0.1108(5) 0.0212(4) 0.1744(13) Uani 0.30 1 d PD L 2 H12E' H 0.1661 0.0813 0.0705 0.209 Uiso 0.30 1 calc PR L 2 H12F H 0.0255 0.1092 0.0177 0.209 Uiso 0.30 1 calc PR L 2 H12G' H 0.1707 0.1716 0.0269 0.209 Uiso 0.30 1 calc PR L 2 O1A O 0.94395(8) 0.34500(5) 0.22210(5) 0.0764(3) Uani 1 1 d D . . H1A H 1.0238(7) 0.3191(6) 0.2238(6) 0.050 Uiso 0.50 1 d PD . . H77A H 0.9502(9) 0.3666(8) 0.2780(5) 0.050 Uiso 0.50 1 d PD . . O1B O 0.94135(7) 0.42675(5) 0.36361(4) 0.0672(3) Uani 1 1 d D . . H1B H 0.9558(11) 0.4218(8) 0.3094(4) 0.050 Uiso 0.50 1 d PD . . H77B H 0.9329(14) 0.3722(5) 0.3886(5) 0.050 Uiso 0.50 1 d PD . . O1C O 0.93267(7) 0.27382(5) 0.43404(4) 0.0658(2) Uani 1 1 d D . . H1C H 0.9529(15) 0.3347(4) 0.4311(8) 0.050 Uiso 0.50 1 d PD . . H77C H 0.9408(12) 0.2402(5) 0.3869(5) 0.050 Uiso 0.50 1 d PD . . O1D O 0.94999(7) 0.18549(5) 0.29964(4) 0.0640(2) Uani 1 1 d D . . H1D H 0.9949(14) 0.1936(8) 0.3595(4) 0.050 Uiso 0.50 1 d PD . . H77D H 0.9302(13) 0.2406(5) 0.2780(6) 0.050 Uiso 0.50 1 d PD . . C1A C 0.82901(10) 0.33621(7) 0.15333(6) 0.0569(3) Uani 1 1 d . L . C2A C 0.76472(10) 0.40847(6) 0.13716(6) 0.0567(3) Uani 1 1 d . . . C3A C 0.65127(11) 0.40285(6) 0.06597(6) 0.0588(3) Uani 1 1 d . L . H3A H 0.6072 0.4513 0.0542 0.071 Uiso 1 1 calc R . . C4A C 0.59973(11) 0.32722(7) 0.01078(6) 0.0583(3) Uani 1 1 d D . . C5A C 0.66485(10) 0.25584(6) 0.02958(6) 0.0551(3) Uani 1 1 d . L . H5A H 0.6309 0.2043 -0.0076 0.066 Uiso 1 1 calc R . . C6A C 0.77762(10) 0.25902(6) 0.10128(6) 0.0534(3) Uani 1 1 d . . . C13D C 0.83593(10) 0.17657(7) 0.12127(6) 0.0571(3) Uani 1 1 d . L . H13D H 0.8210 0.1418 0.0679 0.069 Uiso 1 1 calc R . . H13E H 0.9366 0.1927 0.1506 0.069 Uiso 1 1 calc R . . C1B C 0.81756(10) 0.45242(6) 0.34859(6) 0.0557(3) Uani 1 1 d . K . C2B C 0.75826(10) 0.44714(6) 0.41406(6) 0.0556(3) Uani 1 1 d . . . C3B C 0.63600(11) 0.47507(6) 0.40067(6) 0.0607(3) Uani 1 1 d . K . H3B H 0.5963 0.4736 0.4451 0.073 Uiso 1 1 calc R . . C4B C 0.56840(11) 0.50556(7) 0.32374(7) 0.0639(4) Uani 1 1 d D . . C5B C 0.63001(11) 0.50878(7) 0.25997(7) 0.0646(4) Uani 1 1 d . K . H5B H 0.5852 0.5295 0.2074 0.078 Uiso 1 1 calc R . . C6B C 0.75342(11) 0.48302(6) 0.27059(6) 0.0576(3) Uani 1 1 d . . . C13A C 0.81654(11) 0.48962(7) 0.19857(6) 0.0644(4) Uani 1 1 d . K . H13A H 0.7939 0.5409 0.1673 0.077 Uiso 1 1 calc R . . H13B H 0.9182 0.4989 0.2229 0.077 Uiso 1 1 calc R . . C1C C 0.82017(10) 0.24937(7) 0.46143(6) 0.0536(3) Uani 1 1 d . I . C2C C 0.76382(10) 0.15996(7) 0.45551(6) 0.0525(3) Uani 1 1 d . . . C3C C 0.65675(10) 0.13456(7) 0.48811(6) 0.0536(3) Uani 1 1 d . I . H3C H 0.6188 0.0742 0.4863 0.064 Uiso 1 1 calc R . . C4C C 0.60266(10) 0.19492(7) 0.52368(6) 0.0568(3) Uani 1 1 d D . . C5C C 0.65819(10) 0.28374(7) 0.52520(6) 0.0579(3) Uani 1 1 d . I . H5C H 0.6206 0.3256 0.5479 0.070 Uiso 1 1 calc R . . C6C C 0.76692(10) 0.31173(7) 0.49422(6) 0.0539(3) Uani 1 1 d . . . C13B C 0.82370(11) 0.40955(7) 0.49653(6) 0.0621(4) Uani 1 1 d . I . H13A' H 0.8062 0.4403 0.5433 0.075 Uiso 1 1 calc R . . H13B' H 0.9248 0.4196 0.5080 0.075 Uiso 1 1 calc R . . C1D C 0.82511(9) 0.13108(6) 0.26556(6) 0.0499(3) Uani 1 1 d . J . C2D C 0.76663(9) 0.12190(6) 0.17700(6) 0.0490(3) Uani 1 1 d . . . C3D C 0.64261(10) 0.06523(6) 0.14214(6) 0.0502(3) Uani 1 1 d . J . H3D H 0.6030 0.0578 0.0823 0.060 Uiso 1 1 calc R . . C4D C 0.57273(10) 0.01808(6) 0.19199(6) 0.0517(3) Uani 1 1 d D . . C5D C 0.63412(10) 0.02961(6) 0.27984(6) 0.0523(3) Uani 1 1 d . J . H5D H 0.5879 -0.0020 0.3146 0.063 Uiso 1 1 calc R . . C6D C 0.75884(9) 0.08494(6) 0.31796(6) 0.0489(3) Uani 1 1 d . . . C13C C 0.81862(10) 0.09355(7) 0.41405(6) 0.0562(3) Uani 1 1 d . J . H13A'' H 0.9203 0.1110 0.4304 0.067 Uiso 1 1 calc R . . H13B'' H 0.7964 0.0360 0.4357 0.067 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 O1A1 0.0907(9) 0.1538(19) 0.1212(12) 0.0062(12) 0.0518(8) 0.0238(11) N1A1 0.1044(9) 0.0913(9) 0.0827(8) 0.0045(7) 0.0165(7) 0.0033(8) C1A1 0.0964(15) 0.179(3) 0.0557(15) 0.0166(19) 0.0255(13) 0.0187(17) C2A1 0.1090(16) 0.174(3) 0.0849(12) 0.0256(15) 0.0722(11) 0.0334(17) C3A1 0.0859(14) 0.0830(12) 0.0882(15) 0.0157(12) 0.0040(11) 0.0277(11) O1B1 0.0907(9) 0.1538(19) 0.1212(12) 0.0062(12) 0.0518(8) 0.0238(11) N1B1 0.1044(9) 0.0913(9) 0.0827(8) 0.0045(7) 0.0165(7) 0.0033(8) C1B1 0.0964(15) 0.179(3) 0.0557(15) 0.0166(19) 0.0255(13) 0.0187(17) C2B1 0.1090(16) 0.174(3) 0.0849(12) 0.0256(15) 0.0722(11) 0.0334(17) C3B1 0.0859(14) 0.0830(12) 0.0882(15) 0.0157(12) 0.0040(11) 0.0277(11) O1C1 0.0907(9) 0.1538(19) 0.1212(12) 0.0062(12) 0.0518(8) 0.0238(11) N1C1 0.1044(9) 0.0913(9) 0.0827(8) 0.0045(7) 0.0165(7) 0.0033(8) C1C1 0.0964(15) 0.179(3) 0.0557(15) 0.0166(19) 0.0255(13) 0.0187(17) C2C1 0.1090(16) 0.174(3) 0.0849(12) 0.0256(15) 0.0722(11) 0.0334(17) C3C1 0.0859(14) 0.0830(12) 0.0882(15) 0.0157(12) 0.0040(11) 0.0277(11) O1D1 0.0907(9) 0.1538(19) 0.1212(12) 0.0062(12) 0.0518(8) 0.0238(11) N1D1 0.1044(9) 0.0913(9) 0.0827(8) 0.0045(7) 0.0165(7) 0.0033(8) C1D1 0.0964(15) 0.179(3) 0.0557(15) 0.0166(19) 0.0255(13) 0.0187(17) C3D1 0.0859(14) 0.0830(12) 0.0882(15) 0.0157(12) 0.0040(11) 0.0277(11) C2D1 0.1090(16) 0.174(3) 0.0849(12) 0.0256(15) 0.0722(11) 0.0334(17) O1M 0.0819(10) 0.1051(17) 0.1207(15) 0.0072(12) 0.0551(10) -0.0040(12) C1M 0.0705(19) 0.0518(14) 0.0822(17) -0.0110(14) 0.0093(15) 0.0185(14) O2M 0.0819(10) 0.1051(17) 0.1207(15) 0.0072(12) 0.0551(10) -0.0040(12) C2M 0.0705(19) 0.0518(14) 0.0822(17) -0.0110(14) 0.0093(15) 0.0185(14) O3M 0.0819(10) 0.1051(17) 0.1207(15) 0.0072(12) 0.0551(10) -0.0040(12) C3M 0.0705(19) 0.0518(14) 0.0822(17) -0.0110(14) 0.0093(15) 0.0185(14) O4M 0.0819(10) 0.1051(17) 0.1207(15) 0.0072(12) 0.0551(10) -0.0040(12) C4M 0.0705(19) 0.0518(14) 0.0822(17) -0.0110(14) 0.0093(15) 0.0185(14) O7C 0.1131(5) 0.0493(4) 0.0929(4) 0.0186(4) 0.0610(4) 0.0154(4) C7C 0.0854(6) 0.0487(6) 0.0571(6) 0.0116(5) 0.0298(5) 0.0119(5) C8C 0.0950(6) 0.0537(6) 0.0879(7) 0.0245(5) 0.0530(5) 0.0239(5) C9C 0.0793(6) 0.0549(6) 0.0491(6) 0.0167(5) 0.0298(5) 0.0150(5) C10C 0.0728(6) 0.0557(6) 0.0429(6) 0.0162(5) 0.0203(5) 0.0166(5) C11C 0.0647(6) 0.0615(7) 0.0566(6) 0.0013(5) 0.0182(5) 0.0067(5) C12C 0.0775(7) 0.0559(8) 0.0606(7) 0.0195(6) 0.0287(6) 0.0128(6) O7G 0.1131(5) 0.0493(4) 0.0929(4) 0.0186(4) 0.0610(4) 0.0154(4) C7G 0.0854(6) 0.0487(6) 0.0571(6) 0.0116(5) 0.0298(5) 0.0119(5) C8G 0.0950(6) 0.0537(6) 0.0879(7) 0.0245(5) 0.0530(5) 0.0239(5) C9G 0.0793(6) 0.0549(6) 0.0491(6) 0.0167(5) 0.0298(5) 0.0150(5) C10G 0.0728(6) 0.0557(6) 0.0429(6) 0.0162(5) 0.0203(5) 0.0166(5) C11G 0.0647(6) 0.0615(7) 0.0566(6) 0.0013(5) 0.0182(5) 0.0067(5) C12G 0.0775(7) 0.0559(8) 0.0606(7) 0.0195(6) 0.0287(6) 0.0128(6) O7H 0.0758(5) 0.0687(5) 0.0576(4) -0.0075(4) 0.0168(4) 0.0049(4) C7H 0.0703(6) 0.0420(6) 0.0551(6) -0.0002(5) 0.0230(5) 0.0190(5) C8H 0.0690(7) 0.0519(7) 0.0703(7) -0.0026(6) 0.0218(6) 0.0164(6) C9H 0.0900(7) 0.0666(8) 0.0762(8) 0.0037(7) 0.0385(6) 0.0130(7) C10H 0.0671(7) 0.0769(9) 0.1365(11) 0.0178(8) 0.0472(7) 0.0075(7) C11H 0.0775(8) 0.0944(10) 0.1317(11) 0.0225(9) 0.0514(7) 0.0253(8) C12H 0.1346(10) 0.1497(13) 0.0766(9) 0.0209(9) 0.0375(8) 0.0776(9) O7D 0.0758(5) 0.0687(5) 0.0576(4) -0.0075(4) 0.0168(4) 0.0049(4) C7D 0.0703(6) 0.0420(6) 0.0551(6) -0.0002(5) 0.0230(5) 0.0190(5) C8D 0.0690(7) 0.0519(7) 0.0703(7) -0.0026(6) 0.0218(6) 0.0164(6) C9D 0.0900(7) 0.0666(8) 0.0762(8) 0.0037(7) 0.0385(6) 0.0130(7) C10D 0.0671(7) 0.0769(9) 0.1365(11) 0.0178(8) 0.0472(7) 0.0075(7) C11D 0.0775(8) 0.0944(10) 0.1317(11) 0.0225(9) 0.0514(7) 0.0253(8) C12D 0.1346(10) 0.1497(13) 0.0766(9) 0.0209(9) 0.0375(8) 0.0776(9) O7J 0.1200(5) 0.0617(7) 0.0919(5) 0.0049(5) 0.0622(4) 0.0329(5) C7J 0.1108(7) 0.0458(7) 0.0858(7) 0.0037(6) 0.0534(6) 0.0259(6) C8J 0.0914(9) 0.0684(12) 0.0864(9) -0.0017(9) 0.0382(7) 0.0315(8) C9J 0.1076(10) 0.0874(11) 0.0938(15) 0.0153(10) 0.0546(10) 0.0400(9) C10J 0.1126(13) 0.129(2) 0.0796(16) 0.0008(14) 0.0280(12) 0.0512(13) C11J 0.1049(14) 0.0901(19) 0.0950(13) 0.0206(13) 0.0387(11) 0.0285(12) C12J 0.1417(15) 0.156(3) 0.1202(14) 0.0569(16) 0.0459(12) 0.0477(17) O7B 0.1200(5) 0.0617(7) 0.0919(5) 0.0049(5) 0.0622(4) 0.0329(5) C7B 0.1108(7) 0.0458(7) 0.0858(7) 0.0037(6) 0.0534(6) 0.0259(6) C8B 0.0914(9) 0.0684(12) 0.0864(9) -0.0017(9) 0.0382(7) 0.0315(8) C9B 0.1076(10) 0.0874(11) 0.0938(15) 0.0153(10) 0.0546(10) 0.0400(9) C10B 0.1126(13) 0.129(2) 0.0796(16) 0.0008(14) 0.0280(12) 0.0512(13) C11B 0.1049(14) 0.0901(19) 0.0950(13) 0.0206(13) 0.0387(11) 0.0285(12) C12B 0.1417(15) 0.156(3) 0.1202(14) 0.0569(16) 0.0459(12) 0.0477(17) O7F 0.1200(5) 0.0617(7) 0.0919(5) 0.0049(5) 0.0622(4) 0.0329(5) C7F 0.1108(7) 0.0458(7) 0.0858(7) 0.0037(6) 0.0534(6) 0.0259(6) C8F 0.0914(9) 0.0684(12) 0.0864(9) -0.0017(9) 0.0382(7) 0.0315(8) C9F 0.1076(10) 0.0874(11) 0.0938(15) 0.0153(10) 0.0546(10) 0.0400(9) C10F 0.1126(13) 0.129(2) 0.0796(16) 0.0008(14) 0.0280(12) 0.0512(13) C11F 0.1049(14) 0.0901(19) 0.0950(13) 0.0206(13) 0.0387(11) 0.0285(12) C12F 0.1417(15) 0.156(3) 0.1202(14) 0.0569(16) 0.0459(12) 0.0477(17) O7A 0.1538(7) 0.0692(5) 0.0551(6) 0.0173(4) 0.0268(5) 0.0555(5) C7A 0.1162(8) 0.0533(6) 0.0512(6) 0.0156(5) 0.0332(6) 0.0259(6) C8A 0.1111(10) 0.0709(8) 0.0425(7) 0.0152(6) 0.0303(7) 0.0330(7) C9A 0.0927(10) 0.0821(11) 0.0903(14) -0.0204(11) 0.0306(10) 0.0089(9) C10A 0.1088(12) 0.0892(14) 0.1216(15) -0.0135(12) 0.0292(11) 0.0229(12) C11A 0.1298(12) 0.127(2) 0.1683(15) -0.0435(16) 0.0854(10) -0.0441(15) C12A 0.1233(18) 0.182(2) 0.228(2) -0.0234(19) 0.0936(14) -0.0047(19) O7E 0.1538(7) 0.0692(5) 0.0551(6) 0.0173(4) 0.0268(5) 0.0555(5) C7E 0.1162(8) 0.0533(6) 0.0512(6) 0.0156(5) 0.0332(6) 0.0259(6) C8E 0.1111(10) 0.0709(8) 0.0425(7) 0.0152(6) 0.0303(7) 0.0330(7) C9E 0.0927(10) 0.0821(11) 0.0903(14) -0.0204(11) 0.0306(10) 0.0089(9) C10E 0.1088(12) 0.0892(14) 0.1216(15) -0.0135(12) 0.0292(11) 0.0229(12) C11E 0.1298(12) 0.127(2) 0.1683(15) -0.0435(16) 0.0854(10) -0.0441(15) C12E 0.1233(18) 0.182(2) 0.228(2) -0.0234(19) 0.0936(14) -0.0047(19) O1A 0.0830(4) 0.0828(5) 0.0646(4) -0.0105(4) 0.0234(3) 0.0206(4) O1B 0.0657(4) 0.0639(5) 0.0693(4) -0.0034(4) 0.0289(3) -0.0052(4) O1C 0.0652(4) 0.0693(5) 0.0636(4) -0.0055(4) 0.0255(3) 0.0073(4) O1D 0.0615(4) 0.0674(4) 0.0609(4) 0.0023(4) 0.0168(3) 0.0121(3) C1A 0.0735(5) 0.0514(6) 0.0524(5) 0.0015(5) 0.0342(4) 0.0046(5) C2A 0.0869(6) 0.0399(5) 0.0546(5) 0.0031(4) 0.0447(4) 0.0022(5) C3A 0.0965(6) 0.0397(5) 0.0549(5) 0.0137(4) 0.0435(4) 0.0155(5) C4A 0.0911(6) 0.0461(6) 0.0475(5) 0.0115(4) 0.0348(4) 0.0152(5) C5A 0.0864(6) 0.0387(5) 0.0478(5) 0.0054(4) 0.0346(4) 0.0081(5) C6A 0.0759(5) 0.0429(5) 0.0523(5) 0.0044(4) 0.0359(4) 0.0117(5) C13D 0.0722(6) 0.0517(6) 0.0554(5) 0.0028(5) 0.0285(4) 0.0176(5) C1B 0.0665(5) 0.0382(5) 0.0595(5) -0.0091(5) 0.0278(4) -0.0088(5) C2B 0.0738(6) 0.0356(5) 0.0558(5) -0.0064(4) 0.0291(4) -0.0068(5) C3B 0.0872(6) 0.0428(6) 0.0605(5) -0.0038(5) 0.0415(4) 0.0034(5) C4B 0.0967(6) 0.0422(6) 0.0650(6) -0.0003(5) 0.0415(5) 0.0169(5) C5B 0.0994(7) 0.0410(5) 0.0614(6) 0.0034(5) 0.0346(5) 0.0181(5) C6B 0.0865(6) 0.0326(5) 0.0576(5) -0.0043(4) 0.0371(4) -0.0019(5) C13A 0.0945(6) 0.0427(6) 0.0646(6) 0.0048(5) 0.0441(5) 0.0026(5) C1C 0.0559(5) 0.0622(6) 0.0398(5) 0.0027(5) 0.0131(4) 0.0085(5) C2C 0.0616(5) 0.0536(6) 0.0396(5) 0.0069(4) 0.0094(4) 0.0160(5) C3C 0.0685(6) 0.0474(5) 0.0444(5) 0.0117(4) 0.0158(4) 0.0132(5) C4C 0.0729(6) 0.0508(6) 0.0500(5) 0.0103(5) 0.0237(4) 0.0129(5) C5C 0.0756(6) 0.0548(6) 0.0484(5) 0.0070(5) 0.0266(4) 0.0133(5) C6C 0.0632(6) 0.0530(6) 0.0412(5) -0.0006(5) 0.0142(4) 0.0058(5) C13B 0.0785(6) 0.0561(6) 0.0525(5) -0.0042(5) 0.0298(4) 0.0009(5) C1D 0.0551(5) 0.0430(5) 0.0544(5) 0.0041(4) 0.0178(4) 0.0155(4) C2D 0.0635(5) 0.0425(5) 0.0480(5) 0.0057(4) 0.0210(4) 0.0215(4) C3D 0.0688(5) 0.0415(5) 0.0424(5) 0.0026(4) 0.0153(4) 0.0203(4) C4D 0.0662(5) 0.0401(5) 0.0507(5) 0.0034(4) 0.0180(4) 0.0165(4) C5D 0.0718(5) 0.0405(5) 0.0515(5) 0.0093(4) 0.0244(4) 0.0191(4) C6D 0.0579(5) 0.0452(5) 0.0456(5) 0.0055(4) 0.0135(4) 0.0201(4) C13C 0.0659(5) 0.0569(6) 0.0475(5) 0.0110(5) 0.0147(4) 0.0213(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1A1 C1A1 1.272(9) . ? N1A1 C1A1 1.348(8) . ? N1A1 C3A1 1.396(9) . ? N1A1 C2A1 1.496(9) . ? O1B1 C1B1 1.155(4) . ? N1B1 C3B1 1.385(3) . ? N1B1 C1B1 1.387(4) . ? N1B1 C2B1 1.440(4) . ? O1C1 C1C1 1.275(7) . ? N1C1 C1C1 1.345(6) . ? N1C1 C2C1 1.435(7) . ? N1C1 C3C1 1.456(6) . ? O1D1 C1D1 1.184(9) . ? N1D1 C1D1 1.307(9) . ? N1D1 C2D1 1.401(8) . ? N1D1 C3D1 1.456(9) . ? O1M C1M 1.290(4) . ? O2M C2M 1.291(6) . ? O3M C3M 1.288(5) . ? O4M C4M 1.290(4) . ? O7C C7C 1.224(2) . ? C7C C4C 1.485(2) . ? C7C C8C 1.503(3) . ? C8C C9C 1.510(3) . ? C9C C10C 1.516(3) . ? C10C C11C 1.507(3) . ? C11C C12C 1.506(3) . ? O7G C7G 1.218(3) . ? C7G C4C 1.484(3) . ? C7G C8G 1.503(4) . ? C8G C9G 1.513(4) . ? C9G C10G 1.511(4) . ? C10G C11G 1.518(4) . ? C11G C12G 1.527(4) . ? O7H C7H 1.192(7) . ? C7H C4D 1.461(6) . ? C7H C8H 1.514(10) . ? C8H C9H 1.538(10) . ? C9H C10H 1.506(10) . ? C10H C11H 1.534(11) . ? C11H C12H 1.546(12) . ? O7D C7D 1.2288(13) . ? C7D C4D 1.4835(13) . ? C7D C8D 1.4914(18) . ? C8D C9D 1.549(2) . ? C9D C10D 1.525(2) . ? C10D C11D 1.507(2) . ? C11D C12D 1.498(2) . ? O7J C7J 1.223(5) . ? C7J C4B 1.477(4) . ? C7J C8J 1.543(5) . ? C8J C9J 1.539(6) . ? C9J C10J 1.508(6) . ? C10J C11J 1.521(6) . ? C11J C12J 1.517(7) . ? O7B C7B 1.241(4) . ? C7B C4B 1.502(4) . ? C7B C8B 1.555(5) . ? C8B C9B 1.504(5) . ? C9B C10B 1.482(5) . ? C10B C11B 1.510(6) . ? C11B C12B 1.551(5) . ? O7F C7F 1.212(4) . ? C7F C4B 1.473(4) . ? C7F C8F 1.535(4) . ? C8F C9F 1.541(5) . ? C9F C10F 1.519(5) . ? C10F C11F 1.486(5) . ? C11F C12F 1.509(6) . ? O7A C7A 1.224(2) . ? C7A C4A 1.4952(17) . ? C7A C8A 1.522(2) . ? C8A C9A 1.561(2) . ? C9A C10A 1.445(3) . ? C10A C11A 1.524(3) . ? C11A C12A 1.480(4) . ? O7E C7E 1.205(5) . ? C7E C4A 1.478(4) . ? C7E C8E 1.506(5) . ? C8E C9E 1.593(6) . ? C9E C10E 1.454(5) . ? C10E C11E 1.494(7) . ? C11E C12E 1.551(8) . ? O1A C1A 1.3601(11) . ? O1B C1B 1.3706(13) . ? O1C C1C 1.3750(13) . ? O1D C1D 1.3609(10) . ? C1A C6A 1.3919(13) . ? C1A C2A 1.4074(15) . ? C2A C3A 1.3791(13) . ? C2A C13A 1.5210(14) . ? C3A C4A 1.3996(13) . ? C4A C5A 1.4030(15) . ? C5A C6A 1.3848(12) . ? C6A C13D 1.5254(15) . ? C13D C2D 1.5240(15) . ? C1B C6B 1.4031(14) . ? C1B C2B 1.4050(16) . ? C2B C3B 1.3757(16) . ? C2B C13B 1.5155(14) . ? C3B C4B 1.3981(14) . ? C4B C5B 1.3962(17) . ? C5B C6B 1.3770(16) . ? C6B C13A 1.5310(17) . ? C1C C6C 1.3886(16) . ? C1C C2C 1.4026(14) . ? C2C C3C 1.3810(15) . ? C2C C13C 1.5238(16) . ? C3C C4C 1.3947(16) . ? C4C C5C 1.3997(14) . ? C5C C6C 1.3850(16) . ? C6C C13B 1.5309(15) . ? C1D C6D 1.4016(15) . ? C1D C2D 1.4051(13) . ? C2D C3D 1.3722(12) . ? C3D C4D 1.3980(15) . ? C4D C5D 1.3980(13) . ? C5D C6D 1.3754(12) . ? C6D C13C 1.5217(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1A1 N1A1 C3A1 108.4(6) . . ? C1A1 N1A1 C2A1 130.3(7) . . ? C3A1 N1A1 C2A1 121.2(6) . . ? O1A1 C1A1 N1A1 92.3(6) . . ? C3B1 N1B1 C1B1 129.4(3) . . ? C3B1 N1B1 C2B1 112.6(3) . . ? C1B1 N1B1 C2B1 117.3(2) . . ? O1B1 C1B1 N1B1 126.8(3) . . ? C1C1 N1C1 C2C1 124.8(5) . . ? C1C1 N1C1 C3C1 118.6(5) . . ? C2C1 N1C1 C3C1 116.6(4) . . ? O1C1 C1C1 N1C1 113.3(5) . . ? C1D1 N1D1 C2D1 130.0(7) . . ? C1D1 N1D1 C3D1 110.7(6) . . ? C2D1 N1D1 C3D1 117.8(6) . . ? O1D1 C1D1 N1D1 116.7(7) . . ? O7C C7C C4C 120.47(18) . . ? O7C C7C C8C 120.29(18) . . ? C4C C7C C8C 119.16(14) . . ? C7C C8C C9C 116.90(16) . . ? C8C C9C C10C 113.52(15) . . ? C11C C10C C9C 113.22(15) . . ? C12C C11C C10C 114.85(15) . . ? O7G C7G C4C 120.3(3) . . ? O7G C7G C8G 120.5(3) . . ? C4C C7G C8G 119.1(2) . . ? C7G C8G C9G 114.3(2) . . ? C10G C9G C8G 112.7(2) . . ? C9G C10G C11G 114.6(2) . . ? C10G C11G C12G 109.4(2) . . ? O7H C7H C4D 116.1(6) . . ? O7H C7H C8H 128.9(6) . . ? C4D C7H C8H 113.7(5) . . ? C7H C8H C9H 99.8(6) . . ? C10H C9H C8H 112.0(6) . . ? C9H C10H C11H 117.1(7) . . ? C10H C11H C12H 102.1(8) . . ? O7D C7D C4D 121.50(11) . . ? O7D C7D C8D 117.64(9) . . ? C4D C7D C8D 120.82(9) . . ? C7D C8D C9D 111.04(10) . . ? C10D C9D C8D 113.02(11) . . ? C11D C10D C9D 112.28(12) . . ? C12D C11D C10D 112.96(12) . . ? O7J C7J C4B 118.6(3) . . ? O7J C7J C8J 115.8(4) . . ? C4B C7J C8J 121.9(3) . . ? C9J C8J C7J 108.3(3) . . ? C10J C9J C8J 119.5(4) . . ? C9J C10J C11J 120.9(4) . . ? C12J C11J C10J 113.7(4) . . ? O7B C7B C4B 124.7(3) . . ? O7B C7B C8B 124.9(3) . . ? C4B C7B C8B 109.1(3) . . ? C9B C8B C7B 115.0(3) . . ? C10B C9B C8B 124.6(4) . . ? C9B C10B C11B 116.6(4) . . ? C10B C11B C12B 107.9(4) . . ? O7F C7F C4B 119.9(3) . . ? O7F C7F C8F 118.3(3) . . ? C4B C7F C8F 121.8(3) . . ? C7F C8F C9F 112.4(3) . . ? C10F C9F C8F 109.6(3) . . ? C11F C10F C9F 117.1(3) . . ? C10F C11F C12F 111.4(4) . . ? O7A C7A C4A 121.44(13) . . ? O7A C7A C8A 118.35(13) . . ? C4A C7A C8A 120.21(14) . . ? C7A C8A C9A 114.17(14) . . ? C10A C9A C8A 117.23(17) . . ? C9A C10A C11A 112.03(19) . . ? C12A C11A C10A 116.0(2) . . ? O7E C7E C4A 119.6(3) . . ? O7E C7E C8E 118.5(3) . . ? C4A C7E C8E 120.8(3) . . ? C7E C8E C9E 109.8(3) . . ? C10E C9E C8E 110.1(3) . . ? C9E C10E C11E 109.9(4) . . ? C10E C11E C12E 113.8(5) . . ? O1A C1A C6A 121.29(10) . . ? O1A C1A C2A 117.11(9) . . ? C6A C1A C2A 121.61(8) . . ? C3A C2A C1A 118.49(9) . . ? C3A C2A C13A 120.92(10) . . ? C1A C2A C13A 120.56(8) . . ? C2A C3A C4A 121.32(10) . . ? C3A C4A C5A 118.70(8) . . ? C3A C4A C7E 117.39(17) . . ? C5A C4A C7E 123.52(16) . . ? C3A C4A C7A 119.85(11) . . ? C5A C4A C7A 121.39(10) . . ? C7E C4A C7A 8.7(2) . . ? C6A C5A C4A 121.31(9) . . ? C5A C6A C1A 118.49(10) . . ? C5A C6A C13D 118.33(8) . . ? C1A C6A C13D 123.14(8) . . ? C2D C13D C6A 110.81(9) . . ? O1B C1B C6B 120.81(10) . . ? O1B C1B C2B 117.56(9) . . ? C6B C1B C2B 121.63(10) . . ? C3B C2B C1B 118.13(9) . . ? C3B C2B C13B 120.28(10) . . ? C1B C2B C13B 121.57(10) . . ? C2B C3B C4B 122.01(11) . . ? C5B C4B C3B 118.02(11) . . ? C5B C4B C7F 122.90(16) . . ? C3B C4B C7F 118.39(16) . . ? C5B C4B C7J 119.56(18) . . ? C3B C4B C7J 122.32(18) . . ? C7F C4B C7J 6.14(19) . . ? C5B C4B C7B 123.81(15) . . ? C3B C4B C7B 117.84(16) . . ? C7F C4B C7B 13.85(17) . . ? C7J C4B C7B 9.9(2) . . ? C6B C5B C4B 122.30(10) . . ? C5B C6B C1B 117.88(11) . . ? C5B C6B C13A 119.65(9) . . ? C1B C6B C13A 122.46(10) . . ? C2A C13A C6B 112.52(8) . . ? O1C C1C C6C 120.42(9) . . ? O1C C1C C2C 117.36(10) . . ? C6C C1C C2C 122.22(10) . . ? C3C C2C C1C 117.62(10) . . ? C3C C2C C13C 121.40(9) . . ? C1C C2C C13C 120.98(10) . . ? C2C C3C C4C 121.93(9) . . ? C3C C4C C5C 118.57(10) . . ? C3C C4C C7G 120.71(13) . . ? C5C C4C C7G 120.70(14) . . ? C3C C4C C7C 118.13(11) . . ? C5C C4C C7C 123.29(12) . . ? C7G C4C C7C 2.66(13) . . ? C6C C5C C4C 121.19(11) . . ? C5C C6C C1C 118.37(10) . . ? C5C C6C C13B 119.42(10) . . ? C1C C6C C13B 122.21(10) . . ? C2B C13B C6C 111.99(7) . . ? O1D C1D C6D 120.38(8) . . ? O1D C1D C2D 118.08(9) . . ? C6D C1D C2D 121.53(8) . . ? C3D C2D C1D 118.36(9) . . ? C3D C2D C13D 120.78(8) . . ? C1D C2D C13D 120.80(8) . . ? C2D C3D C4D 122.03(9) . . ? C3D C4D C5D 117.74(8) . . ? C3D C4D C7H 115.5(3) . . ? C5D C4D C7H 124.0(3) . . ? C3D C4D C7D 119.59(9) . . ? C5D C4D C7D 122.67(10) . . ? C7H C4D C7D 17.0(3) . . ? C6D C5D C4D 122.56(10) . . ? C5D C6D C1D 117.77(9) . . ? C5D C6D C13C 119.22(9) . . ? C1D C6D C13C 123.01(8) . . ? C6D C13C C2C 112.96(8) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.237 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.038 data_a6 _database_code_depnum_ccdc_archive 'CCDC 265962' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common p-hexanoyl-calix(4)arene.Dimehylsulfoxyde.Methanol _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H74 O10 S' _chemical_formula_weight 927.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 10.2460(8) _cell_length_b 15.8637(13) _cell_length_c 16.5907(14) _cell_angle_alpha 83.700(2) _cell_angle_beta 107.745(2) _cell_angle_gamma 99.412(2) _cell_volume 2528.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.218 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.9530 _exptl_absorpt_correction_T_max 0.9820 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _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 30252 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 28.74 _reflns_number_total 12951 _reflns_number_gt 7730 _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^)+(0.1646P)^2^+0.1798P] 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 12951 _refine_ls_number_parameters 739 _refine_ls_number_restraints 122 _refine_ls_R_factor_all 0.1253 _refine_ls_R_factor_gt 0.0785 _refine_ls_wR_factor_ref 0.2652 _refine_ls_wR_factor_gt 0.2272 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.125 _refine_ls_shift/su_mean 0.005 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 S1N S -0.34693(7) 0.22733(4) 0.30863(4) 0.06914(11) Uani 0.41 1 d PD A -1 O1N O -0.49626(17) 0.21714(13) 0.26687(11) 0.0773(4) Uani 0.41 1 d PD A -1 C1N C -0.2582(2) 0.24084(15) 0.23055(12) 0.0606(5) Uani 0.41 1 d PD A -1 H1N1 H -0.2770 0.1880 0.2010 0.091 Uiso 0.41 1 calc PR A -1 H1N2 H -0.1586 0.2540 0.2578 0.091 Uiso 0.41 1 calc PR A -1 H1N3 H -0.2901 0.2880 0.1897 0.091 Uiso 0.41 1 calc PR A -1 C2N C -0.3050(3) 0.33342(15) 0.34233(16) 0.0739(5) Uani 0.41 1 d PD A -1 H2N1 H -0.3425 0.3733 0.2946 0.111 Uiso 0.41 1 calc PR A -1 H2N2 H -0.2042 0.3480 0.3629 0.111 Uiso 0.41 1 calc PR A -1 H2N3 H -0.3451 0.3375 0.3881 0.111 Uiso 0.41 1 calc PR A -1 S1N1 S -0.3502(2) 0.22834(12) 0.30424(12) 0.06914(11) Uani 0.14 1 d PD B -2 O1N1 O -0.2365(5) 0.2931(3) 0.3366(3) 0.0773(4) Uani 0.14 1 d PD B -2 C1N1 C -0.3096(6) 0.2134(4) 0.2105(3) 0.0606(5) Uani 0.14 1 d PD B -2 H1N4 H -0.3375 0.2603 0.1681 0.091 Uiso 0.14 1 calc PR B -2 H1N5 H -0.3591 0.1588 0.1879 0.091 Uiso 0.14 1 calc PR B -2 H1N6 H -0.2097 0.2130 0.2236 0.091 Uiso 0.14 1 calc PR B -2 C2N1 C -0.5075(5) 0.2689(4) 0.2731(5) 0.0739(5) Uani 0.14 1 d PD B -2 H2N4 H -0.5534 0.2543 0.3176 0.111 Uiso 0.14 1 calc PR B -2 H2N5 H -0.5667 0.2439 0.2205 0.111 Uiso 0.14 1 calc PR B -2 H2N6 H -0.4909 0.3313 0.2635 0.111 Uiso 0.14 1 calc PR B -2 S1N2 S -0.34602(12) 0.22693(7) 0.31019(7) 0.06914(11) Uani 0.27 1 d PD C -3 O1N2 O -0.4923(3) 0.2145(2) 0.26190(18) 0.0773(4) Uani 0.27 1 d PD C -3 C1N2 C -0.2241(3) 0.2492(2) 0.24912(19) 0.0606(5) Uani 0.27 1 d PD C -3 H1N7 H -0.2161 0.1961 0.2269 0.091 Uiso 0.27 1 calc PR C -3 H1N8 H -0.1335 0.2728 0.2855 0.091 Uiso 0.27 1 calc PR C -3 H1N9 H -0.2565 0.2907 0.2018 0.091 Uiso 0.27 1 calc PR C -3 C2N2 C -0.3273(4) 0.3348(2) 0.3384(3) 0.0739(5) Uani 0.27 1 d PD C -3 H2N7 H -0.3124 0.3743 0.2914 0.111 Uiso 0.27 1 calc PR C -3 H2N8 H -0.2478 0.3447 0.3889 0.111 Uiso 0.27 1 calc PR C -3 H2N9 H -0.4113 0.3445 0.3505 0.111 Uiso 0.27 1 calc PR C -3 S1N3 S -0.3343(5) 0.2998(3) 0.2526(4) 0.06914(11) Uani 0.03 1 d PD D -4 O1N3 O -0.2945(16) 0.3528(5) 0.3268(5) 0.0773(4) Uani 0.03 1 d PD D -4 C1N3 C -0.4760(7) 0.2238(6) 0.2558(11) 0.0606(5) Uani 0.03 1 d PD D -4 H1N7' H -0.4976 0.2019 0.2622 0.060 Uiso 0.03 1 d P E -4 H1N8' H -0.5549 0.2922 0.2454 0.060 Uiso 0.03 1 d P F -4 H1N9' H -0.4584 0.2652 0.3373 0.060 Uiso 0.03 1 d P G -4 C2N3 C -0.1968(6) 0.2511(6) 0.2490(9) 0.0739(5) Uani 0.03 1 d PD D -4 H2NX H -0.1531 0.2256 0.3054 0.111 Uiso 0.03 1 calc PR D -4 H2NY H -0.1289 0.2939 0.2311 0.111 Uiso 0.03 1 calc PR D -4 H2NZ H -0.2305 0.2063 0.2084 0.111 Uiso 0.03 1 calc PR D -4 S1N4 S -0.4617(5) 0.3022(2) 0.2010(3) 0.06914(11) Uani 0.04 1 d PD H -5 O1N4 O -0.3943(13) 0.3602(5) 0.2723(5) 0.0773(4) Uani 0.04 1 d PD H -5 C1N4 C -0.3246(6) 0.2544(6) 0.1922(7) 0.0606(5) Uani 0.04 1 d PD H -5 H1NX H -0.2464 0.2987 0.1906 0.091 Uiso 0.04 1 calc PR H -5 H1NY H -0.3545 0.2239 0.1399 0.091 Uiso 0.04 1 calc PR H -5 H1NZ H -0.2961 0.2138 0.2411 0.091 Uiso 0.04 1 calc PR H -5 C2N4 C -0.5699(8) 0.2195(6) 0.2381(7) 0.0739(5) Uani 0.04 1 d PD H -5 H2NA H -0.6556 0.2404 0.2363 0.111 Uiso 0.04 1 calc PR H -5 H2NB H -0.5226 0.2009 0.2966 0.111 Uiso 0.04 1 calc PR H -5 H2NC H -0.5917 0.1711 0.2020 0.111 Uiso 0.04 1 calc PR H -5 S1N5 S -0.3430(3) 0.26762(15) 0.32251(16) 0.06914(11) Uani 0.11 1 d PD I -6 O1N5 O -0.4805(6) 0.2102(3) 0.2301(4) 0.0773(4) Uani 0.11 1 d PD I -6 C1N5 C -0.2275(5) 0.2529(5) 0.2696(4) 0.0606(5) Uani 0.11 1 d PD I -6 H1NA H -0.2458 0.1938 0.2527 0.091 Uiso 0.11 1 calc PR I -6 H1NB H -0.1328 0.2641 0.3071 0.091 Uiso 0.11 1 calc PR I -6 H1NC H -0.2385 0.2924 0.2190 0.091 Uiso 0.11 1 calc PR I -6 C2N5 C -0.4408(6) 0.3468(4) 0.3067(6) 0.0739(5) Uani 0.11 1 d PD I -6 H2ND H -0.5151 0.3401 0.2532 0.111 Uiso 0.11 1 calc PR I -6 H2NE H -0.3832 0.4022 0.3040 0.111 Uiso 0.11 1 calc PR I -6 H2NF H -0.4811 0.3443 0.3536 0.111 Uiso 0.11 1 calc PR I -6 O1C O -0.00220(19) 0.38547(9) 0.57954(9) 0.0705(2) Uani 0.41 1 d PD J -12 C1C C 0.0384(2) 0.32334(12) 0.56357(11) 0.0475(3) Uani 0.41 1 d PD J -12 C2C C 0.0497(2) 0.24585(12) 0.62746(11) 0.0454(3) Uani 0.41 1 d PD J -12 H2C1 H 0.0441 0.2629 0.6818 0.054 Uiso 0.41 1 calc PR J -12 H2C2 H 0.1411 0.2267 0.6381 0.054 Uiso 0.41 1 calc PR J -12 C3C C -0.0645(2) 0.17111(13) 0.59630(13) 0.0497(4) Uani 0.41 1 d PD J -12 H3C1 H -0.0508 0.1497 0.5460 0.060 Uiso 0.41 1 calc PR J -12 H3C2 H -0.0545 0.1240 0.6412 0.060 Uiso 0.41 1 calc PR J -12 C4C C -0.2104(2) 0.19297(15) 0.57302(14) 0.0551(4) Uani 0.41 1 d PD J -12 H4C1 H -0.2233 0.2173 0.6221 0.066 Uiso 0.41 1 calc PR J -12 H4C2 H -0.2231 0.2374 0.5255 0.066 Uiso 0.41 1 calc PR J -12 C5C C -0.3179(2) 0.11713(17) 0.54784(18) 0.0697(6) Uani 0.41 1 d PD J -12 H5C1 H -0.3078 0.0744 0.5968 0.084 Uiso 0.41 1 calc PR J -12 H5C2 H -0.3001 0.0907 0.5015 0.084 Uiso 0.41 1 calc PR J -12 C6C C -0.4649(2) 0.1362(2) 0.5188(2) 0.0950(8) Uani 0.41 1 d PD J -12 H6C1 H -0.4801 0.1698 0.5606 0.114 Uiso 0.41 1 calc PR J -12 H6C2 H -0.5284 0.0824 0.5132 0.114 Uiso 0.41 1 calc PR J -12 H6C3 H -0.4818 0.1690 0.4639 0.114 Uiso 0.41 1 calc PR J -12 O1G O 0.00687(17) 0.40202(8) 0.57551(8) 0.0705(2) Uani 0.48 1 d PD K -7 C1G C 0.03258(19) 0.33592(10) 0.55845(10) 0.0475(3) Uani 0.48 1 d PD K -7 C2G C -0.00133(17) 0.25285(11) 0.60708(10) 0.0454(3) Uani 0.48 1 d PD K -7 H2G1 H -0.0142 0.2658 0.6610 0.054 Uiso 0.48 1 calc PR K -7 H2G2 H 0.0771 0.2194 0.6211 0.054 Uiso 0.48 1 calc PR K -7 C3G C -0.13369(18) 0.19881(11) 0.55535(10) 0.0497(4) Uani 0.48 1 d PD K -7 H3G1 H -0.2053 0.2366 0.5288 0.060 Uiso 0.48 1 calc PR K -7 H3G2 H -0.1130 0.1736 0.5093 0.060 Uiso 0.48 1 calc PR K -7 C4G C -0.18965(19) 0.12799(13) 0.60912(11) 0.0551(4) Uani 0.48 1 d PD K -7 H4G1 H -0.2215 0.1539 0.6502 0.066 Uiso 0.48 1 calc PR K -7 H4G2 H -0.1134 0.0957 0.6420 0.066 Uiso 0.48 1 calc PR K -7 C5G C -0.3084(2) 0.06546(15) 0.55964(15) 0.0697(6) Uani 0.48 1 d PD K -7 H5G1 H -0.3330 0.0188 0.5994 0.084 Uiso 0.48 1 calc PR K -7 H5G2 H -0.2771 0.0395 0.5184 0.084 Uiso 0.48 1 calc PR K -7 C6G C -0.4375(2) 0.1070(2) 0.5120(2) 0.0950(8) Uani 0.48 1 d PD K -7 H6G1 H -0.4519 0.1479 0.5477 0.114 Uiso 0.48 1 calc PR K -7 H6G2 H -0.5183 0.0627 0.4984 0.114 Uiso 0.48 1 calc PR K -7 H6G3 H -0.4252 0.1371 0.4594 0.114 Uiso 0.48 1 calc PR K -7 O1K O -0.0362(6) 0.3845(3) 0.5568(3) 0.0705(2) Uani 0.11 1 d PD L -8 C1K C 0.0160(5) 0.3218(3) 0.5539(3) 0.0475(3) Uani 0.11 1 d PD L -8 C2K C 0.0339(5) 0.2505(3) 0.6238(3) 0.0454(3) Uani 0.11 1 d PD L -8 H2K1 H 0.0646 0.2753 0.6799 0.054 Uiso 0.11 1 calc PR L -8 H2K2 H 0.1054 0.2169 0.6206 0.054 Uiso 0.11 1 calc PR L -8 C3K C -0.1054(6) 0.1912(4) 0.6136(3) 0.0497(4) Uani 0.11 1 d PD L -8 H3K1 H -0.0952 0.1512 0.6646 0.060 Uiso 0.11 1 calc PR L -8 H3K2 H -0.1760 0.2272 0.6131 0.060 Uiso 0.11 1 calc PR L -8 C4K C -0.1602(5) 0.1398(4) 0.5380(3) 0.0551(4) Uani 0.11 1 d PD L -8 H4K1 H -0.0881 0.1064 0.5355 0.066 Uiso 0.11 1 calc PR L -8 H4K2 H -0.1797 0.1791 0.4865 0.066 Uiso 0.11 1 calc PR L -8 C5K C -0.2924(5) 0.0780(4) 0.5376(6) 0.0697(6) Uani 0.11 1 d PD L -8 H5K1 H -0.3171 0.0417 0.4888 0.084 Uiso 0.11 1 calc PR L -8 H5K2 H -0.2745 0.0400 0.5901 0.084 Uiso 0.11 1 calc PR L -8 C6K C -0.4130(6) 0.1247(6) 0.5317(8) 0.0950(8) Uani 0.11 1 d PD L -8 H6K1 H -0.3879 0.1622 0.5789 0.114 Uiso 0.11 1 calc PR L -8 H6K2 H -0.4935 0.0830 0.5346 0.114 Uiso 0.11 1 calc PR L -8 H6K3 H -0.4355 0.1592 0.4778 0.114 Uiso 0.11 1 calc PR L -8 O1D O -0.46169(7) 0.55965(4) 0.11418(5) 0.0514(2) Uani 0.83 1 d PD M -9 C1D C -0.36043(10) 0.55298(6) 0.17558(6) 0.0435(3) Uani 0.83 1 d PD M -9 C2D C -0.35527(11) 0.58495(7) 0.25863(7) 0.0558(3) Uani 0.83 1 d PD M -9 H2D1 H -0.2753 0.6305 0.2746 0.067 Uiso 0.83 1 calc PR M -9 H2D2 H -0.3393 0.5374 0.3028 0.067 Uiso 0.83 1 calc PR M -9 C3D C -0.48407(13) 0.61994(10) 0.25815(8) 0.0762(4) Uani 0.83 1 d PD M -9 H3D1 H -0.5645 0.5747 0.2418 0.091 Uiso 0.83 1 calc PR M -9 H3D2 H -0.4995 0.6682 0.2147 0.091 Uiso 0.83 1 calc PR M -9 C4D C -0.47642(16) 0.65098(11) 0.34399(9) 0.0925(5) Uani 0.83 1 d PD M -9 H4D1 H -0.3887 0.6899 0.3640 0.111 Uiso 0.83 1 calc PR M -9 H4D2 H -0.5533 0.6847 0.3357 0.111 Uiso 0.83 1 calc PR M -9 C5D C -0.48360(15) 0.58456(12) 0.40859(9) 0.0919(6) Uani 0.83 1 d PD M -9 H5D1 H -0.3934 0.5627 0.4312 0.110 Uiso 0.83 1 calc PR M -9 H5D2 H -0.5547 0.5365 0.3844 0.110 Uiso 0.83 1 calc PR M -9 C6D C -0.52189(19) 0.62087(18) 0.48345(11) 0.1422(10) Uani 0.83 1 d PD M -9 H6D1 H -0.4657 0.6764 0.4977 0.171 Uiso 0.83 1 calc PR M -9 H6D2 H -0.5033 0.5806 0.5335 0.171 Uiso 0.83 1 calc PR M -9 H6D3 H -0.6201 0.6279 0.4651 0.171 Uiso 0.83 1 calc PR M -9 O1H O -0.4737(3) 0.5376(2) 0.1324(2) 0.0514(2) Uani 0.17 1 d PD N -10 C1H C -0.3650(4) 0.5389(3) 0.1896(2) 0.0435(3) Uani 0.17 1 d PD N -10 C2H C -0.3331(4) 0.5791(3) 0.2732(2) 0.0558(3) Uani 0.17 1 d PD N -10 H2H1 H -0.2753 0.6352 0.2707 0.067 Uiso 0.17 1 calc PR N -10 H2H2 H -0.2782 0.5422 0.3187 0.067 Uiso 0.17 1 calc PR N -10 C3H C -0.4614(4) 0.5923(4) 0.2964(3) 0.0762(4) Uani 0.17 1 d PD N -10 H3H1 H -0.5135 0.6321 0.2530 0.091 Uiso 0.17 1 calc PR N -10 H3H2 H -0.5220 0.5368 0.2959 0.091 Uiso 0.17 1 calc PR N -10 C4H C -0.4261(5) 0.6278(5) 0.3826(3) 0.0925(5) Uani 0.17 1 d PD N -10 H4H1 H -0.3641 0.6828 0.3846 0.111 Uiso 0.17 1 calc PR N -10 H4H2 H -0.3783 0.5872 0.4272 0.111 Uiso 0.17 1 calc PR N -10 C5H C -0.5611(5) 0.6411(5) 0.3974(3) 0.0919(6) Uani 0.17 1 d PD N -10 H5H1 H -0.6291 0.5888 0.3849 0.110 Uiso 0.17 1 calc PR N -10 H5H2 H -0.6002 0.6889 0.3589 0.110 Uiso 0.17 1 calc PR N -10 C6H C -0.5335(9) 0.6616(8) 0.4900(3) 0.1422(10) Uani 0.17 1 d PD N -10 H6H1 H -0.4707 0.6238 0.5275 0.171 Uiso 0.17 1 calc PR N -10 H6H2 H -0.6211 0.6527 0.5042 0.171 Uiso 0.17 1 calc PR N -10 H6H3 H -0.4913 0.7214 0.4974 0.171 Uiso 0.17 1 calc PR N -10 O1A O -0.61054(5) 0.08632(3) -0.06773(4) 0.04697(17) Uani 1 1 d D O -11 C1A C -0.57078(7) 0.16142(4) -0.05466(4) 0.0357(2) Uani 1 1 d D O -11 C2A C -0.67090(8) 0.22562(5) -0.07388(6) 0.0474(2) Uani 1 1 d D O -11 H2A1 H -0.6485 0.2694 -0.1167 0.057 Uiso 1 1 calc R O -11 H2A2 H -0.6573 0.2549 -0.0216 0.057 Uiso 1 1 calc R O -11 C3A C -0.82172(7) 0.18855(5) -0.10630(5) 0.0408(2) Uani 1 1 d D O -11 H3A1 H -0.8476 0.1491 -0.0615 0.049 Uiso 1 1 calc R O -11 H3A2 H -0.8348 0.1549 -0.1557 0.049 Uiso 1 1 calc R O -11 C4A C -0.91636(7) 0.25713(5) -0.13214(5) 0.0378(2) Uani 1 1 d D O -11 H4A1 H -0.8935 0.2946 -0.1791 0.045 Uiso 1 1 calc R O -11 H4A2 H -0.8989 0.2928 -0.0836 0.045 Uiso 1 1 calc R O -11 C5A C -1.06881(7) 0.22117(5) -0.16029(5) 0.0391(2) Uani 1 1 d D O -11 H5A1 H -1.0843 0.1804 -0.2044 0.047 Uiso 1 1 calc R O -11 H5A2 H -1.0941 0.1890 -0.1114 0.047 Uiso 1 1 calc R O -11 C6A C -1.16280(8) 0.28951(6) -0.19525(6) 0.0504(3) Uani 1 1 d D O -11 H6A1 H -1.1388 0.3347 -0.1553 0.061 Uiso 1 1 calc R O -11 H6A2 H -1.2593 0.2639 -0.2032 0.061 Uiso 1 1 calc R O -11 H6A3 H -1.1510 0.3141 -0.2498 0.061 Uiso 1 1 calc R O -11 O1 O 0.00493(5) 0.26293(3) 0.06222(3) 0.03976(15) Uani 1 1 d . P 20 H1 H 0.0252 0.3160 0.0537 0.048 Uiso 1 1 calc R P 20 O2 O 0.14998(5) 0.18050(3) 0.20176(3) 0.03747(14) Uani 1 1 d . P 20 H2 H 0.1231 0.1804 0.1486 0.045 Uiso 1 1 calc R P 20 O3 O 0.22705(5) 0.33291(4) 0.27606(3) 0.04401(16) Uani 1 1 d . P 20 H3 H 0.2522 0.2858 0.2733 0.053 Uiso 1 1 calc R P 20 O4 O 0.08513(5) 0.41392(3) 0.13385(3) 0.04178(16) Uani 1 1 d . P 20 H4 H 0.1547 0.4200 0.1767 0.050 Uiso 1 1 calc R P 20 C1 C -0.13628(7) 0.24187(4) 0.03838(4) 0.03064(18) Uani 1 1 d . P 20 C2 C -0.22268(7) 0.30432(4) 0.00622(4) 0.03160(18) Uani 1 1 d . P 20 C3 C -0.36513(7) 0.27826(4) -0.02107(4) 0.03448(19) Uani 1 1 d . P 20 H3A H -0.4260 0.3201 -0.0421 0.041 Uiso 1 1 calc R P 20 C4 C -0.41951(7) 0.19175(4) -0.01798(4) 0.03274(19) Uani 1 1 d D P 20 C5 C -0.33002(7) 0.13081(4) 0.01599(4) 0.03083(18) Uani 1 1 d . P 20 H5 H -0.3670 0.0720 0.0188 0.037 Uiso 1 1 calc R P 20 C6 C -0.18784(7) 0.15458(4) 0.04582(4) 0.03047(17) Uani 1 1 d . P 20 C7 C -0.09277(7) 0.08745(4) 0.08533(4) 0.03205(18) Uani 1 1 d . P 20 H7A H -0.0061 0.1031 0.0692 0.038 Uiso 1 1 calc R P 20 H7B H -0.1379 0.0315 0.0623 0.038 Uiso 1 1 calc R P 20 C8 C 0.05922(6) 0.12546(4) 0.23460(4) 0.03022(17) Uani 1 1 d . P 20 C9 C -0.05758(6) 0.07861(4) 0.18170(4) 0.02934(17) Uani 1 1 d . P 20 C10 C -0.14494(7) 0.02347(4) 0.21979(4) 0.03076(18) Uani 1 1 d . P 20 H10 H -0.2256 -0.0080 0.1850 0.037 Uiso 1 1 calc R P 20 C11 C -0.11721(7) 0.01313(4) 0.30805(4) 0.03248(19) Uani 1 1 d . P 20 C12 C 0.00140(7) 0.06041(4) 0.35878(4) 0.03213(18) Uani 1 1 d . P 20 H12 H 0.0215 0.0533 0.4187 0.039 Uiso 1 1 calc R P 20 C13 C 0.08955(6) 0.11699(4) 0.32358(4) 0.03002(17) Uani 1 1 d . P 20 C14 C 0.21331(7) 0.17123(4) 0.37907(4) 0.03425(19) Uani 1 1 d . P 20 H14A H 0.2866 0.1848 0.3503 0.041 Uiso 1 1 calc R P 20 H14B H 0.2509 0.1384 0.4333 0.041 Uiso 1 1 calc R P 20 C15 C 0.17662(7) 0.32873(4) 0.34389(4) 0.03403(19) Uani 1 1 d . P 20 C16 C 0.17373(7) 0.25424(4) 0.39721(4) 0.03232(18) Uani 1 1 d . P 20 C17 C 0.12776(7) 0.25540(5) 0.46709(4) 0.0368(2) Uani 1 1 d . P 20 H17 H 0.1266 0.2055 0.5043 0.044 Uiso 1 1 calc R P 20 C18 C 0.08305(8) 0.32784(5) 0.48448(4) 0.0403(2) Uani 1 1 d D P 20 C19 C 0.08496(8) 0.40115(5) 0.42942(5) 0.0402(2) Uani 1 1 d . P 20 H19 H 0.0544 0.4507 0.4409 0.048 Uiso 1 1 calc R P 20 C20 C 0.13020(7) 0.40305(4) 0.35879(4) 0.0361(2) Uani 1 1 d . P 20 C21 C 0.12669(8) 0.48200(5) 0.29782(5) 0.0389(2) Uani 1 1 d . P 20 H21A H 0.2058 0.4873 0.2743 0.047 Uiso 1 1 calc R P 20 H21B H 0.1380 0.5333 0.3295 0.047 Uiso 1 1 calc R P 20 C22 C -0.02304(7) 0.44485(4) 0.14811(4) 0.0349(2) Uani 1 1 d . P 20 C23 C -0.00684(7) 0.47977(4) 0.22483(5) 0.0366(2) Uani 1 1 d . P 20 C24 C -0.11824(8) 0.51250(4) 0.23465(5) 0.0394(2) Uani 1 1 d . P 20 H24 H -0.1098 0.5354 0.2868 0.047 Uiso 1 1 calc R P 20 C25 C -0.24283(7) 0.51248(4) 0.16942(5) 0.0382(2) Uani 1 1 d D P 20 C26 C -0.25531(7) 0.47671(4) 0.09346(5) 0.0370(2) Uani 1 1 d . P 20 H26 H -0.3396 0.4762 0.0489 0.044 Uiso 1 1 calc R P 20 C27 C -0.14803(7) 0.44234(4) 0.08215(4) 0.03410(19) Uani 1 1 d . P 20 C28 C -0.16659(8) 0.39971(4) 0.00028(4) 0.0364(2) Uani 1 1 d . P 20 H28A H -0.0764 0.4063 -0.0117 0.044 Uiso 1 1 calc R P 20 H28B H -0.2313 0.4289 -0.0474 0.044 Uiso 1 1 calc R P 20 O1B O -0.17214(7) -0.06256(4) 0.42643(3) 0.0567(2) Uani 1 1 d . P 20 C1B C -0.20787(8) -0.04776(5) 0.34993(5) 0.0382(2) Uani 1 1 d . P 20 C2B C -0.34707(8) -0.08777(5) 0.29726(5) 0.0423(2) Uani 1 1 d . P 20 H2B1 H -0.3829 -0.1369 0.3304 0.051 Uiso 1 1 calc R P 20 H2B2 H -0.3371 -0.1095 0.2460 0.051 Uiso 1 1 calc R P 20 C3B C -0.45069(8) -0.02242(5) 0.27053(6) 0.0464(2) Uani 1 1 d . P 20 H3B1 H -0.4498 0.0053 0.3214 0.056 Uiso 1 1 calc R P 20 H3B2 H -0.4205 0.0227 0.2313 0.056 Uiso 1 1 calc R P 20 C4B C -0.59827(9) -0.06259(6) 0.22733(6) 0.0539(3) Uani 1 1 d . P 20 H4B1 H -0.5984 -0.0930 0.1783 0.065 Uiso 1 1 calc R P 20 H4B2 H -0.6304 -0.1054 0.2677 0.065 Uiso 1 1 calc R P 20 C5B C -0.69843(9) 0.00255(7) 0.19695(7) 0.0612(3) Uani 1 1 d . P 20 H5B1 H -0.7941 -0.0279 0.1817 0.073 Uiso 1 1 calc R P 20 H5B2 H -0.6877 0.0390 0.2439 0.073 Uiso 1 1 calc R P 20 C6B C -0.67713(10) 0.05887(7) 0.12154(6) 0.0614(3) Uani 1 1 d . P 20 H6B1 H -0.5851 0.0927 0.1374 0.074 Uiso 1 1 calc R P 20 H6B2 H -0.7477 0.0974 0.1028 0.074 Uiso 1 1 calc R P 20 H6B3 H -0.6847 0.0231 0.0753 0.074 Uiso 1 1 calc R P 20 O1M O 0.31710(7) 0.29208(5) 0.12381(5) 0.0671(3) Uani 0.93 1 d PD Q -22 H1M H 0.3715 0.2667 0.1640 0.101 Uiso 0.93 1 calc PR Q -22 C1M C 0.38087(12) 0.37284(7) 0.10766(9) 0.0778(4) Uani 0.93 1 d PD Q -22 H1M1 H 0.4120 0.4039 0.1596 0.117 Uiso 0.93 1 calc PR Q -22 H1M2 H 0.3153 0.4039 0.0635 0.117 Uiso 0.93 1 calc PR Q -22 H1M3 H 0.4607 0.3682 0.0884 0.117 Uiso 0.93 1 calc PR Q -22 O1M1 O 0.3268(6) 0.35410(12) 0.1585(3) 0.0671(3) Uani 0.07 1 d PRD Q -23 H1M4 H 0.3564 0.4052 0.1703 0.101 Uiso 0.07 1 calc PR Q -23 C1M1 C 0.42735(17) 0.31753(15) 0.1489(3) 0.0778(4) Uani 0.07 1 d PRD Q -23 H1M5 H 0.4660 0.3515 0.1064 0.117 Uiso 0.07 1 calc PR Q -23 H1M6 H 0.3907 0.2597 0.1300 0.117 Uiso 0.07 1 calc PR Q -23 H1M7 H 0.5001 0.3143 0.2031 0.117 Uiso 0.07 1 calc PR Q -23 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 S1N 0.07803(18) 0.05279(17) 0.07104(17) 0.00222(14) 0.01698(15) 0.00658(15) O1N 0.0615(5) 0.0851(7) 0.0676(6) 0.0051(6) 0.0075(5) -0.0116(5) C1N 0.0722(8) 0.0650(8) 0.0435(8) -0.0225(7) 0.0058(6) 0.0154(7) C2N 0.0754(9) 0.0689(8) 0.0789(8) -0.0286(6) 0.0277(7) -0.0120(8) S1N1 0.07803(18) 0.05279(17) 0.07104(17) 0.00222(14) 0.01698(15) 0.00658(15) O1N1 0.0615(5) 0.0851(7) 0.0676(6) 0.0051(6) 0.0075(5) -0.0116(5) C1N1 0.0722(8) 0.0650(8) 0.0435(8) -0.0225(7) 0.0058(6) 0.0154(7) C2N1 0.0754(9) 0.0689(8) 0.0789(8) -0.0286(6) 0.0277(7) -0.0120(8) S1N2 0.07803(18) 0.05279(17) 0.07104(17) 0.00222(14) 0.01698(15) 0.00658(15) O1N2 0.0615(5) 0.0851(7) 0.0676(6) 0.0051(6) 0.0075(5) -0.0116(5) C1N2 0.0722(8) 0.0650(8) 0.0435(8) -0.0225(7) 0.0058(6) 0.0154(7) C2N2 0.0754(9) 0.0689(8) 0.0789(8) -0.0286(6) 0.0277(7) -0.0120(8) S1N3 0.07803(18) 0.05279(17) 0.07104(17) 0.00222(14) 0.01698(15) 0.00658(15) O1N3 0.0615(5) 0.0851(7) 0.0676(6) 0.0051(6) 0.0075(5) -0.0116(5) C1N3 0.0722(8) 0.0650(8) 0.0435(8) -0.0225(7) 0.0058(6) 0.0154(7) C2N3 0.0754(9) 0.0689(8) 0.0789(8) -0.0286(6) 0.0277(7) -0.0120(8) S1N4 0.07803(18) 0.05279(17) 0.07104(17) 0.00222(14) 0.01698(15) 0.00658(15) O1N4 0.0615(5) 0.0851(7) 0.0676(6) 0.0051(6) 0.0075(5) -0.0116(5) C1N4 0.0722(8) 0.0650(8) 0.0435(8) -0.0225(7) 0.0058(6) 0.0154(7) C2N4 0.0754(9) 0.0689(8) 0.0789(8) -0.0286(6) 0.0277(7) -0.0120(8) S1N5 0.07803(18) 0.05279(17) 0.07104(17) 0.00222(14) 0.01698(15) 0.00658(15) O1N5 0.0615(5) 0.0851(7) 0.0676(6) 0.0051(6) 0.0075(5) -0.0116(5) C1N5 0.0722(8) 0.0650(8) 0.0435(8) -0.0225(7) 0.0058(6) 0.0154(7) C2N5 0.0754(9) 0.0689(8) 0.0789(8) -0.0286(6) 0.0277(7) -0.0120(8) O1C 0.1339(5) 0.0441(3) 0.0466(3) -0.0052(3) 0.0340(3) 0.0331(3) C1C 0.0653(5) 0.0391(4) 0.0365(3) -0.0106(3) 0.0095(3) 0.0074(4) C2C 0.0492(7) 0.0514(5) 0.0335(4) -0.0091(4) 0.0050(4) 0.0101(5) C3C 0.0584(7) 0.0512(7) 0.0428(6) 0.0010(5) 0.0184(5) 0.0124(6) C4C 0.0547(6) 0.0650(8) 0.0471(6) 0.0056(6) 0.0152(5) 0.0181(6) C5C 0.0460(6) 0.0763(12) 0.0844(9) -0.0035(10) 0.0152(6) 0.0103(8) C6C 0.0489(9) 0.1206(17) 0.1045(11) 0.0138(12) 0.0082(8) 0.0218(10) O1G 0.1339(5) 0.0441(3) 0.0466(3) -0.0052(3) 0.0340(3) 0.0331(3) C1G 0.0653(5) 0.0391(4) 0.0365(3) -0.0106(3) 0.0095(3) 0.0074(4) C2G 0.0492(7) 0.0514(5) 0.0335(4) -0.0091(4) 0.0050(4) 0.0101(5) C3G 0.0584(7) 0.0512(7) 0.0428(6) 0.0010(5) 0.0184(5) 0.0124(6) C4G 0.0547(6) 0.0650(8) 0.0471(6) 0.0056(6) 0.0152(5) 0.0181(6) C5G 0.0460(6) 0.0763(12) 0.0844(9) -0.0035(10) 0.0152(6) 0.0103(8) C6G 0.0489(9) 0.1206(17) 0.1045(11) 0.0138(12) 0.0082(8) 0.0218(10) O1K 0.1339(5) 0.0441(3) 0.0466(3) -0.0052(3) 0.0340(3) 0.0331(3) C1K 0.0653(5) 0.0391(4) 0.0365(3) -0.0106(3) 0.0095(3) 0.0074(4) C2K 0.0492(7) 0.0514(5) 0.0335(4) -0.0091(4) 0.0050(4) 0.0101(5) C3K 0.0584(7) 0.0512(7) 0.0428(6) 0.0010(5) 0.0184(5) 0.0124(6) C4K 0.0547(6) 0.0650(8) 0.0471(6) 0.0056(6) 0.0152(5) 0.0181(6) C5K 0.0460(6) 0.0763(12) 0.0844(9) -0.0035(10) 0.0152(6) 0.0103(8) C6K 0.0489(9) 0.1206(17) 0.1045(11) 0.0138(12) 0.0082(8) 0.0218(10) O1D 0.0486(3) 0.0347(3) 0.0633(4) 0.0046(3) 0.0025(3) 0.0162(2) C1D 0.0463(4) 0.0267(3) 0.0531(4) 0.0030(3) 0.0102(3) 0.0048(3) C2D 0.0515(4) 0.0528(5) 0.0630(5) -0.0045(4) 0.0132(4) 0.0132(4) C3D 0.0693(6) 0.0943(8) 0.0740(7) -0.0128(6) 0.0238(5) 0.0260(6) C4D 0.0972(8) 0.1164(11) 0.0799(7) -0.0157(7) 0.0424(5) 0.0217(8) C5D 0.0655(7) 0.1327(12) 0.0729(8) -0.0220(8) 0.0059(7) 0.0177(8) C6D 0.0915(10) 0.239(3) 0.0773(9) -0.0117(13) 0.0227(8) -0.0276(14) O1H 0.0486(3) 0.0347(3) 0.0633(4) 0.0046(3) 0.0025(3) 0.0162(2) C1H 0.0463(4) 0.0267(3) 0.0531(4) 0.0030(3) 0.0102(3) 0.0048(3) C2H 0.0515(4) 0.0528(5) 0.0630(5) -0.0045(4) 0.0132(4) 0.0132(4) C3H 0.0693(6) 0.0943(8) 0.0740(7) -0.0128(6) 0.0238(5) 0.0260(6) C4H 0.0972(8) 0.1164(11) 0.0799(7) -0.0157(7) 0.0424(5) 0.0217(8) C5H 0.0655(7) 0.1327(12) 0.0729(8) -0.0220(8) 0.0059(7) 0.0177(8) C6H 0.0915(10) 0.239(3) 0.0773(9) -0.0117(13) 0.0227(8) -0.0276(14) O1A 0.0395(3) 0.0315(2) 0.0581(3) -0.0087(2) -0.0037(2) 0.0022(2) C1A 0.0328(3) 0.0310(3) 0.0374(3) -0.0041(3) 0.0021(3) 0.0024(3) C2A 0.0343(3) 0.0347(3) 0.0644(5) -0.0100(3) 0.0004(3) 0.0024(3) C3A 0.0339(3) 0.0324(3) 0.0502(4) -0.0029(3) 0.0042(3) 0.0027(3) C4A 0.0357(3) 0.0350(3) 0.0394(3) -0.0055(3) 0.0062(3) 0.0026(3) C5A 0.0340(3) 0.0424(4) 0.0389(3) -0.0002(3) 0.0095(3) 0.0038(3) C6A 0.0398(3) 0.0588(5) 0.0538(4) -0.0014(4) 0.0137(3) 0.0114(3) O1 0.0318(2) 0.0436(3) 0.0396(2) 0.0019(2) 0.00849(18) -0.0001(2) O2 0.0343(2) 0.0400(2) 0.0384(2) -0.0009(2) 0.01207(17) 0.0042(2) O3 0.0424(2) 0.0456(3) 0.0435(2) -0.0005(2) 0.0113(2) 0.0086(2) O4 0.0334(2) 0.0420(3) 0.0449(3) 0.0009(2) 0.0073(2) 0.0013(2) C1 0.0302(3) 0.0358(3) 0.0246(3) -0.0022(2) 0.0065(2) 0.0038(2) C2 0.0359(3) 0.0283(3) 0.0262(3) -0.0005(2) 0.0048(2) 0.0011(3) C3 0.0356(3) 0.0291(3) 0.0326(3) -0.0020(3) 0.0003(3) 0.0056(3) C4 0.0332(3) 0.0302(3) 0.0304(3) -0.0044(2) 0.0026(2) 0.0032(3) C5 0.0351(3) 0.0272(3) 0.0288(3) -0.0042(2) 0.0060(2) 0.0049(2) C6 0.0352(3) 0.0337(3) 0.0225(2) -0.0039(2) 0.0064(2) 0.0071(2) C7 0.0362(3) 0.0311(3) 0.0301(3) -0.0065(2) 0.0081(2) 0.0083(2) C8 0.0271(3) 0.0286(3) 0.0350(3) -0.0030(2) 0.0067(2) 0.0076(2) C9 0.0306(3) 0.0278(3) 0.0297(3) -0.0039(2) 0.0046(2) 0.0109(2) C10 0.0303(3) 0.0268(3) 0.0327(3) -0.0056(2) 0.0031(2) 0.0062(2) C11 0.0347(3) 0.0267(3) 0.0327(3) -0.0013(2) 0.0038(2) 0.0070(2) C12 0.0359(3) 0.0284(3) 0.0278(3) -0.0012(2) 0.0007(2) 0.0092(2) C13 0.0289(3) 0.0270(3) 0.0315(3) -0.0033(2) 0.0011(2) 0.0102(2) C14 0.0293(3) 0.0345(3) 0.0326(3) -0.0026(3) -0.0013(2) 0.0062(3) C15 0.0278(3) 0.0346(3) 0.0331(3) -0.0057(3) -0.0006(2) 0.0015(3) C16 0.0286(3) 0.0305(3) 0.0309(3) -0.0043(2) -0.0009(2) 0.0011(3) C17 0.0378(3) 0.0322(3) 0.0323(3) -0.0058(3) 0.0000(3) -0.0009(3) C18 0.0455(4) 0.0373(3) 0.0337(3) -0.0101(3) 0.0035(3) 0.0037(3) C19 0.0436(4) 0.0314(3) 0.0392(3) -0.0116(3) -0.0006(3) 0.0059(3) C20 0.0321(3) 0.0291(3) 0.0360(3) -0.0054(3) -0.0047(3) -0.0009(3) C21 0.0374(3) 0.0284(3) 0.0410(3) -0.0042(3) -0.0010(3) -0.0005(3) C22 0.0354(3) 0.0251(3) 0.0354(3) 0.0035(3) 0.0024(3) -0.0014(3) C23 0.0380(3) 0.0237(3) 0.0387(3) 0.0012(3) 0.0016(3) -0.0023(3) C24 0.0456(4) 0.0257(3) 0.0402(3) -0.0020(3) 0.0045(3) 0.0019(3) C25 0.0369(3) 0.0266(3) 0.0452(4) 0.0003(3) 0.0040(3) 0.0048(3) C26 0.0382(3) 0.0240(3) 0.0388(3) 0.0035(3) 0.0009(3) 0.0000(3) C27 0.0364(3) 0.0239(3) 0.0339(3) 0.0031(3) 0.0037(3) -0.0029(3) C28 0.0409(3) 0.0294(3) 0.0310(3) 0.0029(3) 0.0028(3) 0.0010(3) O1B 0.0616(3) 0.0586(3) 0.0357(3) 0.0098(3) 0.0057(2) -0.0069(3) C1B 0.0420(3) 0.0313(3) 0.0381(3) 0.0031(3) 0.0083(3) 0.0057(3) C2B 0.0432(4) 0.0330(3) 0.0462(4) 0.0022(3) 0.0113(3) -0.0010(3) C3B 0.0438(4) 0.0381(4) 0.0568(4) -0.0035(3) 0.0143(3) 0.0049(3) C4B 0.0411(4) 0.0472(4) 0.0711(5) -0.0030(4) 0.0150(4) 0.0028(3) C5B 0.0403(4) 0.0618(5) 0.0825(6) -0.0043(5) 0.0179(4) 0.0101(4) C6B 0.0609(4) 0.0718(5) 0.0551(4) -0.0116(4) 0.0101(4) 0.0279(4) O1M 0.0593(4) 0.0581(4) 0.0752(4) 0.0034(3) 0.0174(3) -0.0075(3) C1M 0.0762(6) 0.0537(6) 0.1116(8) -0.0037(6) 0.0463(5) -0.0034(5) O1M1 0.0593(4) 0.0581(4) 0.0752(4) 0.0034(3) 0.0174(3) -0.0075(3) C1M1 0.0762(6) 0.0537(6) 0.1116(8) -0.0037(6) 0.0463(5) -0.0034(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1N O1N 1.4645(18) . ? S1N C1N 1.773(3) . ? S1N C2N 1.776(3) . ? S1N1 O1N1 1.431(5) . ? S1N1 C2N1 1.743(6) . ? S1N1 C1N1 1.777(6) . ? S1N2 O1N2 1.461(3) . ? S1N2 C2N2 1.788(4) . ? S1N2 C1N2 1.806(4) . ? S1N3 O1N3 1.482(9) . ? S1N3 C2N3 1.733(10) . ? S1N3 C1N3 1.738(9) . ? S1N4 O1N4 1.502(8) . ? S1N4 C1N4 1.752(9) . ? S1N4 C2N4 1.757(9) . ? S1N5 C2N5 1.683(7) . ? S1N5 C1N5 1.730(7) . ? S1N5 O1N5 1.933(6) . ? O1C C1C 1.214(3) . ? C1C C2C 1.528(2) . ? C2C C3C 1.535(3) . ? C3C C4C 1.513(3) . ? C4C C5C 1.494(3) . ? C5C C6C 1.505(3) . ? O1G C1G 1.204(2) . ? C1G C2G 1.515(2) . ? C2G C3G 1.543(2) . ? C3G C4G 1.506(3) . ? C4G C5G 1.521(3) . ? C5G C6G 1.531(3) . ? O1K C1K 1.215(7) . ? C1K C2K 1.521(6) . ? C2K C3K 1.548(7) . ? C3K C4K 1.483(7) . ? C4K C5K 1.536(7) . ? C5K C6K 1.515(9) . ? O1D C1D 1.2220(11) . ? C1D C2D 1.5029(16) . ? C2D C3D 1.5105(19) . ? C3D C4D 1.533(2) . ? C4D C5D 1.428(2) . ? C5D C6D 1.599(3) . ? O1H C1H 1.221(4) . ? C1H C2H 1.513(6) . ? C2H C3H 1.528(7) . ? C3H C4H 1.513(7) . ? C4H C5H 1.527(7) . ? C5H C6H 1.536(8) . ? O1A C1A 1.2150(8) . ? C1A C2A 1.5040(11) . ? C2A C3A 1.5128(10) . ? C3A C4A 1.5154(11) . ? C4A C5A 1.5184(9) . ? C5A C6A 1.5172(12) . ? O1 C1 1.3724(8) . ? O2 C8 1.3649(8) . ? O3 C15 1.3656(10) . ? O4 C22 1.3742(10) . ? C1 C2 1.3901(10) . ? C1 C6 1.4053(9) . ? C2 C3 1.3954(9) . ? C2 C28 1.5320(9) . ? C3 C4 1.3959(9) . ? C4 C5 1.3959(10) . ? C5 C6 1.3897(9) . ? C6 C7 1.5197(10) . ? C7 C9 1.5237(9) . ? C8 C9 1.4025(8) . ? C8 C13 1.4087(9) . ? C9 C10 1.3903(9) . ? C10 C11 1.4003(9) . ? C11 C12 1.4017(8) . ? C11 C1B 1.4937(10) . ? C12 C13 1.3798(10) . ? C13 C14 1.5170(8) . ? C14 C16 1.5249(11) . ? C15 C16 1.3982(9) . ? C15 C20 1.4129(11) . ? C16 C17 1.3809(11) . ? C17 C18 1.3926(12) . ? C18 C19 1.3991(10) . ? C19 C20 1.3813(12) . ? C20 C21 1.5190(10) . ? C21 C23 1.5242(9) . ? C22 C23 1.3965(11) . ? C22 C27 1.4064(9) . ? C23 C24 1.3874(12) . ? C24 C25 1.3995(9) . ? C25 C26 1.4005(11) . ? C26 C27 1.3729(12) . ? C27 C28 1.5298(11) . ? O1B C1B 1.2163(9) . ? C1B C2B 1.5056(10) . ? C2B C3B 1.5398(12) . ? C3B C4B 1.5267(11) . ? C4B C5B 1.5140(14) . ? C5B C6B 1.5061(15) . ? O1M C1M 1.3776(13) . ? O1M1 C1M1 1.3192 . ? 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 O1N S1N C1N 109.24(11) . . ? O1N S1N C2N 104.95(13) . . ? C1N S1N C2N 98.21(13) . . ? O1N1 S1N1 C2N1 111.6(3) . . ? O1N1 S1N1 C1N1 97.3(3) . . ? C2N1 S1N1 C1N1 107.3(3) . . ? O1N2 S1N2 C2N2 100.4(2) . . ? O1N2 S1N2 C1N2 116.35(17) . . ? C2N2 S1N2 C1N2 95.0(2) . . ? O1N3 S1N3 C2N3 111.0(7) . . ? O1N3 S1N3 C1N3 110.0(9) . . ? C2N3 S1N3 C1N3 110.8(6) . . ? O1N4 S1N4 C1N4 103.5(6) . . ? O1N4 S1N4 C2N4 106.9(6) . . ? C1N4 S1N4 C2N4 105.7(5) . . ? C2N5 S1N5 C1N5 128.6(4) . . ? C2N5 S1N5 O1N5 89.2(3) . . ? C1N5 S1N5 O1N5 84.6(3) . . ? O1C C1C C2C 118.24(19) . . ? C1C C2C C3C 112.28(14) . . ? C4C C3C C2C 114.74(18) . . ? C5C C4C C3C 112.8(2) . . ? C4C C5C C6C 115.0(2) . . ? O1G C1G C2G 120.01(18) . . ? C1G C2G C3G 111.53(12) . . ? C4G C3G C2G 112.42(13) . . ? C3G C4G C5G 114.64(16) . . ? C4G C5G C6G 113.4(2) . . ? O1K C1K C2K 122.3(5) . . ? C1K C2K C3K 109.5(4) . . ? C4K C3K C2K 117.9(5) . . ? C3K C4K C5K 113.7(6) . . ? C6K C5K C4K 112.2(5) . . ? O1D C1D C2D 119.64(10) . . ? C1D C2D C3D 114.55(9) . . ? C2D C3D C4D 113.33(10) . . ? C5D C4D C3D 114.87(15) . . ? C4D C5D C6D 109.78(17) . . ? O1H C1H C2H 125.8(4) . . ? C1H C2H C3H 114.0(3) . . ? C4H C3H C2H 112.6(3) . . ? C3H C4H C5H 107.9(4) . . ? C4H C5H C6H 109.7(5) . . ? O1A C1A C2A 121.25(6) . . ? C1A C2A C3A 114.92(6) . . ? C2A C3A C4A 112.40(6) . . ? C3A C4A C5A 113.31(6) . . ? C6A C5A C4A 113.30(6) . . ? O1 C1 C2 120.96(6) . . ? O1 C1 C6 116.74(6) . . ? C2 C1 C6 122.27(6) . . ? C1 C2 C3 118.19(6) . . ? C1 C2 C28 122.25(6) . . ? C3 C2 C28 119.56(6) . . ? C2 C3 C4 121.02(6) . . ? C3 C4 C5 119.30(6) . . ? C6 C5 C4 121.24(6) . . ? C5 C6 C1 117.89(6) . . ? C5 C6 C7 120.34(6) . . ? C1 C6 C7 121.77(6) . . ? C6 C7 C9 112.60(6) . . ? O2 C8 C9 121.11(6) . . ? O2 C8 C13 117.04(5) . . ? C9 C8 C13 121.84(6) . . ? C10 C9 C8 117.83(6) . . ? C10 C9 C7 119.56(5) . . ? C8 C9 C7 122.60(6) . . ? C9 C10 C11 121.74(5) . . ? C10 C11 C12 118.70(6) . . ? C10 C11 C1B 122.33(5) . . ? C12 C11 C1B 118.96(6) . . ? C13 C12 C11 121.47(6) . . ? C12 C13 C8 118.41(5) . . ? C12 C13 C14 120.89(6) . . ? C8 C13 C14 120.66(6) . . ? C13 C14 C16 111.26(6) . . ? O3 C15 C16 121.09(7) . . ? O3 C15 C20 117.34(6) . . ? C16 C15 C20 121.56(7) . . ? C17 C16 C15 118.32(7) . . ? C17 C16 C14 119.02(6) . . ? C15 C16 C14 122.62(7) . . ? C16 C17 C18 121.73(7) . . ? C17 C18 C19 118.84(8) . . ? C20 C19 C18 121.50(8) . . ? C19 C20 C15 118.03(6) . . ? C19 C20 C21 120.90(7) . . ? C15 C20 C21 121.05(7) . . ? C20 C21 C23 113.20(6) . . ? O4 C22 C23 120.60(6) . . ? O4 C22 C27 117.73(7) . . ? C23 C22 C27 121.65(7) . . ? C24 C23 C22 118.07(6) . . ? C24 C23 C21 119.23(7) . . ? C22 C23 C21 122.69(7) . . ? C23 C24 C25 121.49(7) . . ? C24 C25 C26 118.78(8) . . ? C27 C26 C25 121.27(6) . . ? C26 C27 C22 118.72(7) . . ? C26 C27 C28 120.27(6) . . ? C22 C27 C28 120.99(7) . . ? C27 C28 C2 111.91(6) . . ? O1B C1B C11 120.43(6) . . ? O1B C1B C2B 120.00(7) . . ? C11 C1B C2B 119.51(6) . . ? C1B C2B C3B 111.01(6) . . ? C4B C3B C2B 113.08(7) . . ? C5B C4B C3B 112.93(7) . . ? C6B C5B C4B 113.08(9) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 28.74 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.687 _refine_diff_density_min -1.378 _refine_diff_density_rms 0.074