# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2006 data_global _journal_name_full 'New J.Chem.(Nouv.J.Chim.)' _journal_coden_Cambridge 0440 _publ_contact_author_name A.W.Coleman _publ_contact_author_address ; CNRS Institute de Biologie et Chimie des Proteines (IBCP) 7, Passage du Vercors Lyon Cedex 7 69367 FRANCE ; _publ_contact_author_email AW.COLEMAN@IBCP.FR _publ_section_title ; Conformational Extremes in the Supramolecular Assemblies of para-sulfonato-Calix[8]arene ; loop_ _publ_author_name A.W.Coleman 'Vanessa Bonnard' 'Oksana Danylyuk' 'Florent Perret' 'Kinga Suwinska' # Attachment 'compound 1A.cif' data_1a _database_code_depnum_ccdc_archive 'CCDC 294462' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;para-sulfonatocalix(8)arene / 1,4-hexanediammonium cation complex ; _chemical_melting_point ? _chemical_formula_moiety 'C56 H48 O32 S8 . 3(C4 H16 N2) . 2(H2 O) . C H3 O H' _chemical_formula_sum 'C69 H64 N6 O35 S8' _chemical_formula_weight 1793.81 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 24.3724(9) _cell_length_b 22.2422(8) _cell_length_c 23.340(1) _cell_angle_alpha 90.000(2) _cell_angle_beta 119.279(2) _cell_angle_gamma 90.000(3) _cell_volume 11035.9(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3664 _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.411 0.250 0.661 1090.1 48.8 2 -0.086 0.750 0.664 1090.1 48.8 _platon_squeeze_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.1 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16344 _diffrn_reflns_av_R_equivalents 0.0635 _diffrn_reflns_av_sigmaI/netI 0.0443 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 18.79 _reflns_number_total 4256 _reflns_number_gt 3518 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo / Scalepak (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo / Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Johnson & Burnet, 1996)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4256 _refine_ls_number_parameters 362 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.2058 _refine_ls_R_factor_gt 0.1892 _refine_ls_wR_factor_ref 0.4992 _refine_ls_wR_factor_gt 0.4826 _refine_ls_goodness_of_fit_ref 2.196 _refine_ls_restrained_S_all 2.205 _refine_ls_shift/su_max 0.278 _refine_ls_shift/su_mean 0.047 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 C20 C 0.2386(6) 0.4314(6) 0.0387(7) 0.065(4) Uiso 1 1 d . . . C21 C 0.1752(6) 0.4181(6) 0.0017(7) 0.065(4) Uiso 1 1 d . . . H21 H 0.1527 0.4336 -0.0417 0.078 Uiso 1 1 calc R . . C22 C 0.1441(6) 0.3846(6) 0.0240(7) 0.063(4) Uiso 1 1 d . . . C23 C 0.1745(7) 0.3594(7) 0.0873(8) 0.081(4) Uiso 1 1 d . . . H23 H 0.1523 0.3360 0.1033 0.098 Uiso 1 1 calc R . . C24 C 0.2691(6) 0.4050(5) 0.1014(6) 0.052(3) Uiso 1 1 d . . . C25 C 0.2399(7) 0.3705(6) 0.1261(7) 0.071(4) Uiso 1 1 d . . . C26 C 0.2745(8) 0.3391(7) 0.1947(8) 0.088(5) Uiso 1 1 d . . . H26A H 0.3185 0.3305 0.2062 0.106 Uiso 1 1 calc R . . H26B H 0.2536 0.3004 0.1928 0.106 Uiso 1 1 calc R . . C27 C 0.2737(6) 0.3800(6) 0.2485(7) 0.065(4) Uiso 1 1 d . . . C28 C 0.3234(6) 0.4169(6) 0.2870(7) 0.064(4) Uiso 1 1 d . . . C29 C 0.3264(6) 0.4483(5) 0.3387(6) 0.054(3) Uiso 1 1 d . . . C30 C 0.2780(7) 0.4438(7) 0.3529(8) 0.081(4) Uiso 1 1 d . A . H30 H 0.2780 0.4679 0.3865 0.097 Uiso 1 1 calc R . . C31 C 0.2263(7) 0.4017(7) 0.3156(8) 0.079(4) Uiso 1 1 d . . . C32 C 0.2249(8) 0.3734(7) 0.2628(9) 0.094(5) Uiso 1 1 d . A . H32 H 0.1899 0.3487 0.2354 0.112 Uiso 1 1 calc R . . C33 C 0.3817(6) 0.4877(6) 0.3828(6) 0.069(4) Uiso 1 1 d . . . H33A H 0.3666 0.5232 0.3966 0.083 Uiso 1 1 calc R . . H33B H 0.4026 0.5021 0.3581 0.083 Uiso 1 1 calc R . . C34 C 0.4736(6) 0.4142(5) 0.4406(7) 0.057(4) Uiso 1 1 d . . . C35 C 0.4302(6) 0.4522(5) 0.4450(6) 0.053(3) Uiso 1 1 d . . . C36 C 0.4259(6) 0.4552(6) 0.5028(6) 0.058(4) Uiso 1 1 d . . . H36 H 0.3963 0.4814 0.5053 0.070 Uiso 1 1 calc R . . C37 C 0.5066(6) 0.3810(6) 0.5519(7) 0.067(4) Uiso 1 1 d . . . H37 H 0.5322 0.3563 0.5885 0.081 Uiso 1 1 calc R . . C38 C 0.5123(6) 0.3769(5) 0.4947(6) 0.055(4) Uiso 1 1 d . . . C39 C 0.4648(6) 0.4201(6) 0.5558(7) 0.059(4) Uiso 1 1 d . . . C40 C 0.5594(6) 0.3363(6) 0.4927(7) 0.065(4) Uiso 1 1 d . . . H40A H 0.5463 0.3270 0.4463 0.078 Uiso 1 1 calc R . . H40B H 0.5599 0.2981 0.5146 0.078 Uiso 1 1 calc R . . C41 C 0.6434(6) 0.3975(6) 0.4941(7) 0.057(4) Uiso 1 1 d . . . C42 C 0.6243(6) 0.3611(6) 0.5245(6) 0.059(4) Uiso 1 1 d . . . C43 C 0.6678(6) 0.3470(6) 0.5930(7) 0.069(4) Uiso 1 1 d . . . H43 H 0.6558 0.3200 0.6164 0.083 Uiso 1 1 calc R . . C44 C 0.7249(7) 0.3726(6) 0.6228(7) 0.070(4) Uiso 1 1 d . . . C45 C 0.7442(7) 0.4063(6) 0.5923(7) 0.067(4) Uiso 1 1 d . . . H45 H 0.7863 0.4206 0.6145 0.081 Uiso 1 1 calc R . . C46 C 0.2969(7) 0.4239(6) -0.0234(8) 0.079(4) Uiso 1 1 d . . . C47 C 0.2719(7) 0.4662(7) 0.0107(7) 0.080(4) Uiso 1 1 d . . . H47A H 0.3074 0.4885 0.0462 0.096 Uiso 1 1 calc R . . H47B H 0.2427 0.4957 -0.0215 0.096 Uiso 1 1 calc R . . S1 S 0.0616(2) 0.3692(3) -0.0245(3) 0.109(2) Uani 1 1 d . . . O5A O 0.0472(12) 0.3125(13) -0.0029(13) 0.119(8) Uiso 0.50 1 d P . . O6A O 0.0441(16) 0.3763(18) -0.0915(19) 0.157(12) Uiso 0.50 1 d P . . O7B O 0.0322(11) 0.4141(11) -0.0110(12) 0.110(7) Uiso 0.50 1 d P . . O5B O 0.0356(11) 0.4137(12) -0.0746(13) 0.106(7) Uiso 0.50 1 d P . . O6B O 0.0397(15) 0.3602(15) 0.0196(16) 0.147(10) Uiso 0.50 1 d P . . O7A O 0.0570(12) 0.3146(12) -0.0614(14) 0.127(8) Uiso 0.50 1 d P . . S2A S 0.1603(5) 0.4120(7) 0.3301(6) 0.097(3) Uiso 0.50 1 d P A 1 O14A O 0.1951(19) 0.388(2) 0.402(2) 0.168(15) Uiso 0.50 1 d P A 1 O15A O 0.1131(13) 0.3831(14) 0.2820(14) 0.109(9) Uiso 0.50 1 d P A 1 O16A O 0.1606(13) 0.4612(14) 0.3596(15) 0.126(9) Uiso 0.50 1 d P A 1 S2B S 0.1709(4) 0.3773(5) 0.3389(4) 0.070(3) Uiso 0.50 1 d P A 2 O14B O 0.1064(15) 0.4196(17) 0.2756(16) 0.140(11) Uiso 0.50 1 d P A 2 O15B O 0.1710(10) 0.3241(11) 0.3451(11) 0.098(6) Uiso 0.50 1 d P A 2 O16B O 0.1811(13) 0.4221(16) 0.3916(15) 0.103(8) Uiso 0.50 1 d P A 2 S3 S 0.4628(2) 0.4255(2) 0.6309(2) 0.0903(18) Uani 1 1 d . . . O8A O 0.4107(10) 0.4642(11) 0.6229(10) 0.078(6) Uiso 0.50 1 d P . . O9A O 0.5210(15) 0.4472(15) 0.6790(15) 0.123(10) Uiso 0.50 1 d P . . O10A O 0.4601(13) 0.3589(10) 0.6466(12) 0.091(7) Uiso 0.50 1 d P . . O8B O 0.4939(14) 0.3731(11) 0.6711(13) 0.104(8) Uiso 0.50 1 d P . . O9B O 0.3960(9) 0.4317(10) 0.6102(9) 0.067(6) Uiso 0.50 1 d P . . O10B O 0.5093(10) 0.4791(11) 0.6670(10) 0.076(6) Uiso 0.50 1 d P . . S4 S 0.7788(3) 0.3515(3) 0.7059(2) 0.114(2) Uani 1 1 d . . . O11A O 0.7970(18) 0.4003(15) 0.7401(16) 0.135(10) Uiso 0.50 1 d P . . O12A O 0.8233(8) 0.3051(8) 0.7001(9) 0.075(5) Uiso 0.50 1 d P . . O13A O 0.7510(11) 0.3292(12) 0.7323(12) 0.080(7) Uiso 0.50 1 d P . . O11B O 0.7334(14) 0.2995(15) 0.7193(15) 0.125(11) Uiso 0.50 1 d P . . O12B O 0.7462(16) 0.3959(14) 0.7375(15) 0.148(10) Uiso 0.50 1 d P . . O13B O 0.8337(18) 0.3936(15) 0.7351(17) 0.149(11) Uiso 0.50 1 d P . . O1 O 0.3321(4) 0.4188(4) 0.1415(5) 0.071(3) Uani 1 1 d . . . H1 H 0.3528 0.4077 0.1233 0.106 Uiso 1 1 calc R . . O2 O 0.3726(4) 0.4247(4) 0.2732(4) 0.072(3) Uani 1 1 d . . . H2 H 0.3595 0.4180 0.2331 0.108 Uiso 1 1 calc R . . O3 O 0.4777(4) 0.4123(4) 0.3857(4) 0.069(3) Uani 1 1 d . . . H3 H 0.4922 0.3788 0.3830 0.104 Uiso 1 1 calc R . . O4 O 0.6036(4) 0.4133(4) 0.4283(4) 0.069(3) Uani 1 1 d . . . H4 H 0.6223 0.4077 0.4066 0.103 Uiso 1 1 calc R . . O11A' O 0.5000 0.3248(5) 0.2500 0.025(6) Uiso 0.68(3) 2 d SP . 1 C11A C 0.4495(15) 0.2808(16) 0.2032(16) 0.094(10) Uiso 0.338(15) 1 d P . 1 O12A' O 0.5000 0.2396(17) 0.2500 0.070(16) Uiso 0.32(3) 2 d SP . 2 C12A C 0.4495(15) 0.2808(16) 0.2032(16) 0.094(10) Uiso 0.162(15) 1 d P . 2 N1C N 0.3804(9) 0.2330(9) 0.1299(9) 0.164(7) Uiso 1 1 d D . . C2C C 0.3289(10) 0.2628(10) 0.0767(11) 0.165(9) Uiso 1 1 d D . . H2C1 H 0.3475 0.2870 0.0549 0.198 Uiso 1 1 calc R . . H2C2 H 0.3129 0.2920 0.0971 0.198 Uiso 1 1 calc R . . C3C C 0.2712(8) 0.2329(8) 0.0219(9) 0.123(7) Uiso 1 1 d D . . H3C1 H 0.2855 0.2046 -0.0007 0.147 Uiso 1 1 calc R . . H3C2 H 0.2511 0.2088 0.0422 0.147 Uiso 1 1 calc R . . N1B N 0.457(3) 0.1529(17) 0.303(3) 0.25(2) Uiso 0.50 1 d PD . . C2B C 0.4411(10) 0.2103(10) 0.3165(11) 0.046(6) Uiso 0.50 1 d PD . . H2B1 H 0.3953 0.2129 0.2856 0.056 Uiso 0.50 1 calc PR . . H2B2 H 0.4607 0.2381 0.2987 0.056 Uiso 0.50 1 calc PR . . C3B C 0.4483(19) 0.243(4) 0.377(3) 0.39(6) Uiso 0.50 1 d PD . . H3B1 H 0.4716 0.2175 0.4158 0.474 Uiso 0.50 1 calc PR . . H3B2 H 0.4729 0.2804 0.3831 0.474 Uiso 0.50 1 calc PR . . C4B C 0.3846(17) 0.2587(19) 0.3687(17) 0.136(14) Uiso 0.50 1 d PD . . H4B1 H 0.3693 0.2918 0.3362 0.163 Uiso 0.50 1 calc PR . . H4B2 H 0.3580 0.2236 0.3456 0.163 Uiso 0.50 1 calc PR . . C5B C 0.3641(19) 0.2762(17) 0.4174(19) 0.127(13) Uiso 0.50 1 d PD . . H5B1 H 0.4029 0.2930 0.4543 0.152 Uiso 0.50 1 calc PR . . H5B2 H 0.3365 0.3113 0.3964 0.152 Uiso 0.50 1 calc PR . . N6B N 0.335(4) 0.247(3) 0.449(4) 0.37(4) Uiso 0.50 1 d PD . . N1D N 0.6110(11) 0.3888(11) 0.7767(12) 0.087(7) Uiso 0.50 1 d PD . . C2D C 0.6632(14) 0.4235(17) 0.7888(18) 0.133(14) Uiso 0.50 1 d PD . . H2D1 H 0.6509 0.4660 0.7883 0.160 Uiso 0.50 1 calc PR . . H2D2 H 0.6698 0.4183 0.7505 0.160 Uiso 0.50 1 calc PR . . C3D C 0.7291(16) 0.416(3) 0.851(2) 0.21(2) Uiso 0.50 1 d PD . . H3D1 H 0.7240 0.4164 0.8910 0.247 Uiso 0.50 1 calc PR . . H3D2 H 0.7467 0.3760 0.8497 0.247 Uiso 0.50 1 calc PR . . C4D C 0.7752(18) 0.465(3) 0.857(4) 0.34(5) Uiso 0.50 1 d PD . . H4D1 H 0.7596 0.4803 0.8115 0.413 Uiso 0.50 1 calc PR . . H4D2 H 0.7689 0.4986 0.8813 0.413 Uiso 0.50 1 calc PR . . C5D C 0.8466(17) 0.459(2) 0.886(2) 0.19(2) Uiso 0.50 1 d PD . . H5D1 H 0.8659 0.4711 0.9331 0.228 Uiso 0.50 1 calc PR . . H5D2 H 0.8557 0.4158 0.8858 0.228 Uiso 0.50 1 calc PR . . N6D N 0.879(2) 0.491(3) 0.858(3) 0.27(3) Uiso 0.50 1 d PD . . O2W O 0.6548(14) 0.2787(13) 0.7534(15) 0.148(10) Uiso 0.50 1 d P . . O1W O 0.4793(14) 0.4376(12) 0.2367(19) 0.163(12) Uiso 0.50 1 d P . . 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 S1 0.077(3) 0.152(5) 0.093(4) -0.048(4) 0.039(3) -0.026(3) S3 0.111(4) 0.114(4) 0.080(3) 0.037(3) 0.073(3) 0.041(3) S4 0.117(4) 0.162(5) 0.063(3) 0.010(3) 0.043(3) 0.029(4) O1 0.059(6) 0.076(7) 0.078(7) -0.003(5) 0.034(5) 0.001(5) O2 0.080(6) 0.088(7) 0.065(7) -0.010(6) 0.048(6) 0.000(5) O3 0.088(7) 0.096(7) 0.049(6) -0.022(5) 0.053(5) -0.007(6) O4 0.072(6) 0.077(6) 0.055(6) 0.002(5) 0.030(5) 0.016(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 C20 C21 1.385(17) . ? C20 C24 1.403(17) . ? C20 C47 1.486(18) . ? C21 C22 1.336(16) . ? C22 C23 1.406(19) . ? C22 S1 1.793(14) . ? C23 C25 1.42(2) . ? C24 C25 1.354(17) . ? C24 O1 1.385(15) . ? C25 C26 1.56(2) . ? C26 C27 1.56(2) . ? C27 C28 1.372(17) . ? C27 C32 1.391(19) . ? C28 C29 1.366(17) . ? C28 O2 1.396(15) . ? C29 C30 1.374(17) . ? C29 C33 1.513(17) . ? C30 C31 1.47(2) . ? C31 C32 1.37(2) . ? C31 S2B 1.771(17) . ? C31 S2A 1.814(18) . ? C33 C35 1.564(17) . ? C34 O3 1.334(14) . ? C34 C35 1.396(16) . ? C34 C38 1.416(17) . ? C35 C36 1.406(16) . ? C36 C39 1.375(17) . ? C37 C39 1.375(16) . ? C37 C38 1.413(17) . ? C38 C40 1.479(17) . ? C39 S3 1.780(14) . ? C40 C42 1.486(18) . ? C41 C42 1.304(16) . ? C41 C46 1.398(18) 6_656 ? C41 O4 1.402(15) . ? C42 C43 1.454(19) . ? C43 C44 1.341(18) . ? C44 C45 1.273(17) . ? C44 S4 1.793(16) . ? C45 C46 1.47(2) 6_656 ? C46 C41 1.398(18) 6_656 ? C46 C45 1.47(2) 6_656 ? C46 C47 1.537(19) . ? S1 O7B 1.35(3) . ? S1 O6B 1.38(3) . ? S1 O6A 1.41(4) . ? S1 O5B 1.42(3) . ? S1 O7A 1.46(3) . ? S1 O5A 1.46(3) . ? O5A O6B 1.23(3) . ? O5A O7A 1.50(3) . ? O6A O5B 0.98(3) . ? O6A O7A 1.50(4) . ? O7B O6B 1.36(3) . ? O7B O5B 1.53(3) . ? S2A O16A 1.29(3) . ? S2A O15A 1.32(3) . ? S2A O14A 1.56(4) . ? S2B O15B 1.19(2) . ? S2B O16B 1.51(3) . ? S2B O14B 1.81(4) . ? S3 O9A 1.40(3) . ? S3 O9B 1.462(19) . ? S3 O8B 1.46(3) . ? S3 O8A 1.47(2) . ? S3 O10A 1.54(2) . ? S3 O10B 1.57(2) . ? O8A O9B 0.80(2) . ? O9A O10B 0.77(3) . ? O9A O8B 1.75(4) . ? O10A O8B 0.80(3) . ? S4 O13A 1.22(3) . ? S4 O11A 1.29(3) . ? S4 O13B 1.50(4) . ? S4 O12A 1.552(18) . ? S4 O12B 1.65(3) . ? S4 O11B 1.73(3) . ? O11A O13B 0.97(4) . ? O11A O12B 1.21(4) . ? O13A O11B 0.77(3) . ? O13A O12B 1.50(4) . ? O11A' C11A 1.53(3) . ? O11A' C11A 1.53(3) 6_656 ? O12A' C12A 1.50(4) 6_656 ? N1C C2C 1.424(16) . ? C2C C3C 1.515(17) . ? C3C C3C 1.29(3) 7 ? N1B C2B 1.416(19) . ? C2B C3B 1.51(2) . ? C3B C4B 1.51(2) . ? C4B C5B 1.500(18) . ? C5B N6B 1.41(2) . ? N1D C2D 1.395(18) . ? C2D C3D 1.56(2) . ? C3D C4D 1.54(2) . ? C4D C5D 1.53(2) . ? C5D N6D 1.44(2) . ? O1W O1W 0.89(6) 6_656 ? 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 C21 C20 C24 115.0(12) . . ? C21 C20 C47 121.3(13) . . ? C24 C20 C47 123.4(12) . . ? C22 C21 C20 123.3(14) . . ? C21 C22 C23 121.5(13) . . ? C21 C22 S1 122.4(11) . . ? C23 C22 S1 116.1(10) . . ? C22 C23 C25 116.9(13) . . ? C25 C24 O1 118.6(12) . . ? C25 C24 C20 124.0(12) . . ? O1 C24 C20 117.3(11) . . ? C24 C25 C23 119.3(13) . . ? C24 C25 C26 123.8(13) . . ? C23 C25 C26 116.8(12) . . ? C25 C26 C27 110.6(12) . . ? C28 C27 C32 119.4(13) . . ? C28 C27 C26 121.4(12) . . ? C32 C27 C26 118.7(13) . . ? C29 C28 C27 122.2(12) . . ? C29 C28 O2 117.4(11) . . ? C27 C28 O2 120.4(12) . . ? C28 C29 C30 119.7(12) . . ? C28 C29 C33 122.8(11) . . ? C30 C29 C33 117.6(12) . . ? C29 C30 C31 119.5(13) . . ? C32 C31 C30 117.7(14) . . ? C32 C31 S2B 116.6(12) . . ? C30 C31 S2B 125.2(12) . . ? C32 C31 S2A 126.3(13) . . ? C30 C31 S2A 113.1(11) . . ? S2B C31 S2A 26.0(4) . . ? C31 C32 C27 121.2(16) . . ? C29 C33 C35 110.9(11) . . ? O3 C34 C35 120.3(12) . . ? O3 C34 C38 120.4(11) . . ? C35 C34 C38 119.3(12) . . ? C34 C35 C36 120.9(12) . . ? C34 C35 C33 119.6(11) . . ? C36 C35 C33 119.3(11) . . ? C39 C36 C35 119.6(12) . . ? C39 C37 C38 121.5(13) . . ? C37 C38 C34 118.2(11) . . ? C37 C38 C40 120.5(12) . . ? C34 C38 C40 121.3(11) . . ? C36 C39 C37 120.4(12) . . ? C36 C39 S3 120.6(10) . . ? C37 C39 S3 119.0(10) . . ? C38 C40 C42 114.3(10) . . ? C42 C41 C46 123.9(13) . 6_656 ? C42 C41 O4 120.8(12) . . ? C46 C41 O4 115.3(11) 6_656 . ? C41 C42 C43 118.0(12) . . ? C41 C42 C40 122.2(12) . . ? C43 C42 C40 119.7(12) . . ? C44 C43 C42 119.5(13) . . ? C45 C44 C43 122.3(15) . . ? C45 C44 S4 118.9(12) . . ? C43 C44 S4 118.4(11) . . ? C44 C45 C46 121.7(14) . 6_656 ? C41 C46 C45 114.4(13) 6_656 6_656 ? C41 C46 C47 125.8(14) 6_656 . ? C45 C46 C47 119.7(13) 6_656 . ? C20 C47 C46 110.4(11) . . ? O7B S1 O6B 59.7(15) . . ? O7B S1 O6A 105.5(19) . . ? O6B S1 O6A 145.1(19) . . ? O7B S1 O5B 66.7(15) . . ? O6B S1 O5B 122.2(17) . . ? O6A S1 O5B 40.6(14) . . ? O7B S1 O7A 148.7(15) . . ? O6B S1 O7A 111.8(17) . . ? O6A S1 O7A 63.0(17) . . ? O5B S1 O7A 102.6(15) . . ? O7B S1 O5A 108.4(14) . . ? O6B S1 O5A 51.3(14) . . ? O6A S1 O5A 119.0(19) . . ? O5B S1 O5A 142.9(14) . . ? O7A S1 O5A 61.6(13) . . ? O7B S1 C22 105.6(11) . . ? O6B S1 C22 106.2(14) . . ? O6A S1 C22 108.3(14) . . ? O5B S1 C22 107.3(11) . . ? O7A S1 C22 105.7(11) . . ? O5A S1 C22 109.3(12) . . ? O6B O5A S1 61(2) . . ? O6B O5A O7A 119(3) . . ? S1 O5A O7A 59.2(15) . . ? O5B O6A S1 70(3) . . ? O5B O6A O7A 128(4) . . ? S1 O6A O7A 60.0(18) . . ? S1 O7B O6B 61.3(18) . . ? S1 O7B O5B 58.9(14) . . ? O6B O7B O5B 117(3) . . ? O6A O5B S1 69(3) . . ? O6A O5B O7B 121(4) . . ? S1 O5B O7B 54.5(14) . . ? O5A O6B O7B 123(3) . . ? O5A O6B S1 68(2) . . ? O7B O6B S1 59.0(17) . . ? S1 O7A O5A 59.3(15) . . ? S1 O7A O6A 57.0(18) . . ? O5A O7A O6A 111(3) . . ? O16A S2A O15A 130(2) . . ? O16A S2A O14A 82(2) . . ? O15A S2A O14A 123(2) . . ? O16A S2A C31 115.6(14) . . ? O15A S2A C31 105.3(14) . . ? O14A S2A C31 95.2(16) . . ? O15B S2B O16B 124.6(19) . . ? O15B S2B C31 112.6(13) . . ? O16B S2B C31 101.7(12) . . ? O15B S2B O14B 124.4(18) . . ? O16B S2B O14B 93.1(19) . . ? C31 S2B O14B 94.5(12) . . ? O9A S3 O9B 139.7(15) . . ? O9A S3 O8B 75.7(18) . . ? O9B S3 O8B 115.6(14) . . ? O9A S3 O8A 112.1(17) . . ? O9B S3 O8A 31.5(9) . . ? O8B S3 O8A 134.0(13) . . ? O9A S3 O10A 106.6(18) . . ? O9B S3 O10A 89.8(13) . . ? O8B S3 O10A 31.0(11) . . ? O8A S3 O10A 117.3(13) . . ? O9A S3 O10B 29.1(13) . . ? O9B S3 O10B 119.9(12) . . ? O8B S3 O10B 104.5(15) . . ? O8A S3 O10B 88.6(13) . . ? O10A S3 O10B 134.9(14) . . ? O9A S3 C39 108.1(12) . . ? O9B S3 C39 104.1(9) . . ? O8B S3 C39 109.0(10) . . ? O8A S3 C39 110.6(9) . . ? O10A S3 C39 101.3(10) . . ? O10B S3 C39 102.7(8) . . ? O9B O8A S3 74(2) . . ? O10B O9A S3 88(4) . . ? O10B O9A O8B 141(4) . . ? S3 O9A O8B 53.7(15) . . ? O8B O10A S3 69(3) . . ? O10A O8B S3 80(3) . . ? O10A O8B O9A 131(4) . . ? S3 O8B O9A 50.6(13) . . ? O8A O9B S3 75(2) . . ? O9A O10B S3 62(3) . . ? O13A S4 O11A 98(2) . . ? O13A S4 O13B 128.0(19) . . ? O11A S4 O13B 39.7(15) . . ? O13A S4 O12A 111.0(13) . . ? O11A S4 O12A 124.7(19) . . ? O13B S4 O12A 87.0(16) . . ? O13A S4 O12B 60.7(15) . . ? O11A S4 O12B 46.8(17) . . ? O13B S4 O12B 86.6(17) . . ? O12A S4 O12B 161.4(13) . . ? O13A S4 O11B 22.7(15) . . ? O11A S4 O11B 120(2) . . ? O13B S4 O11B 147.5(17) . . ? O12A S4 O11B 96.2(12) . . ? O12B S4 O11B 80.2(15) . . ? O13A S4 C44 111.0(12) . . ? O11A S4 C44 107.4(15) . . ? O13B S4 C44 110.4(14) . . ? O12A S4 C44 104.7(8) . . ? O12B S4 C44 94.0(12) . . ? O11B S4 C44 100.1(11) . . ? O13B O11A O12B 164(5) . . ? O13B O11A S4 82(3) . . ? O12B O11A S4 82(3) . . ? O11B O13A S4 119(4) . . ? O11B O13A O12B 147(4) . . ? S4 O13A O12B 73.9(19) . . ? O13A O11B S4 38(3) . . ? O11A O12B O13A 88(3) . . ? O11A O12B S4 51(2) . . ? O13A O12B S4 45.4(13) . . ? O11A O13B S4 59(3) . . ? C11A O11A' C11A 101(3) . 6_656 ? N1C C2C C3C 126.1(19) . . ? C3C C3C C2C 118(2) 7 . ? N1B C2B C3B 136(4) . . ? C4B C3B C2B 111(2) . . ? C5B C4B C3B 132(3) . . ? N6B C5B C4B 136(4) . . ? N1D C2D C3D 123(3) . . ? C4D C3D C2D 112(3) . . ? C5D C4D C3D 126(3) . . ? N6D C5D C4D 120(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C24 C20 C21 C22 2.3(19) . . . . ? C47 C20 C21 C22 176.8(12) . . . . ? C20 C21 C22 C23 -1(2) . . . . ? C20 C21 C22 S1 178.9(10) . . . . ? C21 C22 C23 C25 -1(2) . . . . ? S1 C22 C23 C25 179.3(10) . . . . ? C21 C20 C24 C25 -1.9(19) . . . . ? C47 C20 C24 C25 -176.3(12) . . . . ? C21 C20 C24 O1 -177.4(10) . . . . ? C47 C20 C24 O1 8.2(18) . . . . ? O1 C24 C25 C23 175.7(11) . . . . ? C20 C24 C25 C23 0(2) . . . . ? O1 C24 C25 C26 -7.2(19) . . . . ? C20 C24 C25 C26 177.4(12) . . . . ? C22 C23 C25 C24 1(2) . . . . ? C22 C23 C25 C26 -176.2(12) . . . . ? C24 C25 C26 C27 92.5(16) . . . . ? C23 C25 C26 C27 -90.4(15) . . . . ? C25 C26 C27 C28 -95.9(16) . . . . ? C25 C26 C27 C32 92.0(16) . . . . ? C32 C27 C28 C29 -1(2) . . . . ? C26 C27 C28 C29 -173.1(13) . . . . ? C32 C27 C28 O2 -179.3(13) . . . . ? C26 C27 C28 O2 9(2) . . . . ? C27 C28 C29 C30 -1(2) . . . . ? O2 C28 C29 C30 177.6(12) . . . . ? C27 C28 C29 C33 178.2(12) . . . . ? O2 C28 C29 C33 -3.4(18) . . . . ? C28 C29 C30 C31 5(2) . . . . ? C33 C29 C30 C31 -174.1(12) . . . . ? C29 C30 C31 C32 -7(2) . . . . ? C29 C30 C31 S2B 164.4(12) . . . . ? C29 C30 C31 S2A -169.1(12) . . . . ? C30 C31 C32 C27 6(2) . . . . ? S2B C31 C32 C27 -166.8(12) . . . . ? S2A C31 C32 C27 164.8(13) . . . . ? C28 C27 C32 C31 -2(2) . . . . ? C26 C27 C32 C31 170.6(14) . . . . ? C28 C29 C33 C35 -94.3(14) . . . . ? C30 C29 C33 C35 84.7(14) . . . . ? O3 C34 C35 C36 -179.2(11) . . . . ? C38 C34 C35 C36 2.0(18) . . . . ? O3 C34 C35 C33 6.2(17) . . . . ? C38 C34 C35 C33 -172.5(11) . . . . ? C29 C33 C35 C34 81.4(14) . . . . ? C29 C33 C35 C36 -93.2(13) . . . . ? C34 C35 C36 C39 -0.3(18) . . . . ? C33 C35 C36 C39 174.3(11) . . . . ? C39 C37 C38 C34 0.0(18) . . . . ? C39 C37 C38 C40 177.5(11) . . . . ? O3 C34 C38 C37 179.4(11) . . . . ? C35 C34 C38 C37 -1.9(17) . . . . ? O3 C34 C38 C40 1.9(18) . . . . ? C35 C34 C38 C40 -179.4(11) . . . . ? C35 C36 C39 C37 -1.7(19) . . . . ? C35 C36 C39 S3 177.1(9) . . . . ? C38 C37 C39 C36 1.8(19) . . . . ? C38 C37 C39 S3 -177.0(10) . . . . ? C37 C38 C40 C42 -80.3(15) . . . . ? C34 C38 C40 C42 97.1(15) . . . . ? C46 C41 C42 C43 0(2) 6_656 . . . ? O4 C41 C42 C43 -179.3(10) . . . . ? C46 C41 C42 C40 176.9(12) 6_656 . . . ? O4 C41 C42 C40 -2.3(19) . . . . ? C38 C40 C42 C41 -83.1(16) . . . . ? C38 C40 C42 C43 93.8(14) . . . . ? C41 C42 C43 C44 1.4(19) . . . . ? C40 C42 C43 C44 -175.7(11) . . . . ? C42 C43 C44 C45 -4(2) . . . . ? C42 C43 C44 S4 -176.9(9) . . . . ? C43 C44 C45 C46 5(2) . . . 6_656 ? S4 C44 C45 C46 178.1(10) . . . 6_656 ? C21 C20 C47 C46 -87.8(16) . . . . ? C24 C20 C47 C46 86.2(17) . . . . ? C41 C46 C47 C20 -91.8(17) 6_656 . . . ? C45 C46 C47 C20 86.0(16) 6_656 . . . ? C21 C22 S1 O7B -90.0(16) . . . . ? C23 C22 S1 O7B 90.0(15) . . . . ? C21 C22 S1 O6B -152.3(18) . . . . ? C23 C22 S1 O6B 27.6(18) . . . . ? C21 C22 S1 O6A 23(2) . . . . ? C23 C22 S1 O6A -157(2) . . . . ? C21 C22 S1 O5B -20.1(17) . . . . ? C23 C22 S1 O5B 159.9(15) . . . . ? C21 C22 S1 O7A 88.8(16) . . . . ? C23 C22 S1 O7A -91.2(15) . . . . ? C21 C22 S1 O5A 153.6(15) . . . . ? C23 C22 S1 O5A -26.4(16) . . . . ? O7B S1 O5A O6B -19(2) . . . . ? O6A S1 O5A O6B -139(2) . . . . ? O5B S1 O5A O6B -94(3) . . . . ? O7A S1 O5A O6B -167(2) . . . . ? C22 S1 O5A O6B 96(2) . . . . ? O7B S1 O5A O7A 147.6(17) . . . . ? O6B S1 O5A O7A 167(2) . . . . ? O6A S1 O5A O7A 27(2) . . . . ? O5B S1 O5A O7A 72(3) . . . . ? C22 S1 O5A O7A -97.8(14) . . . . ? O7B S1 O6A O5B 17(3) . . . . ? O6B S1 O6A O5B 76(4) . . . . ? O7A S1 O6A O5B 166(3) . . . . ? O5A S1 O6A O5B 139(2) . . . . ? C22 S1 O6A O5B -95(2) . . . . ? O7B S1 O6A O7A -148.6(16) . . . . ? O6B S1 O6A O7A -90(4) . . . . ? O5B S1 O6A O7A -166(3) . . . . ? O5A S1 O6A O7A -27(2) . . . . ? C22 S1 O6A O7A 98.7(15) . . . . ? O6A S1 O7B O6B 146(2) . . . . ? O5B S1 O7B O6B 158(2) . . . . ? O7A S1 O7B O6B 82(3) . . . . ? O5A S1 O7B O6B 17(2) . . . . ? C22 S1 O7B O6B -99.9(17) . . . . ? O6B S1 O7B O5B -158(2) . . . . ? O6A S1 O7B O5B -12(2) . . . . ? O7A S1 O7B O5B -75(3) . . . . ? O5A S1 O7B O5B -140.5(16) . . . . ? C22 S1 O7B O5B 102.4(13) . . . . ? O7A O6A O5B S1 16(3) . . . . ? S1 O6A O5B O7B -17(3) . . . . ? O7A O6A O5B O7B -2(6) . . . . ? O7B S1 O5B O6A -162(3) . . . . ? O6B S1 O5B O6A -139(3) . . . . ? O7A S1 O5B O6A -13(3) . . . . ? O5A S1 O5B O6A -72(4) . . . . ? C22 S1 O5B O6A 98(3) . . . . ? O6B S1 O5B O7B 23(2) . . . . ? O6A S1 O5B O7B 162(3) . . . . ? O7A S1 O5B O7B 149.0(15) . . . . ? O5A S1 O5B O7B 90(3) . . . . ? C22 S1 O5B O7B -100.0(13) . . . . ? S1 O7B O5B O6A 20(3) . . . . ? O6B O7B O5B O6A -2(5) . . . . ? O6B O7B O5B S1 -22(2) . . . . ? S1 O5A O6B O7B 21(3) . . . . ? O7A O5A O6B O7B 8(5) . . . . ? O7A O5A O6B S1 -13(2) . . . . ? S1 O7B O6B O5A -23(3) . . . . ? O5B O7B O6B O5A -2(4) . . . . ? O5B O7B O6B S1 21(2) . . . . ? O7B S1 O6B O5A 159(3) . . . . ? O6A S1 O6B O5A 86(4) . . . . ? O5B S1 O6B O5A 135(2) . . . . ? O7A S1 O6B O5A 13(2) . . . . ? C22 S1 O6B O5A -102.0(18) . . . . ? O6A S1 O6B O7B -73(4) . . . . ? O5B S1 O6B O7B -24(2) . . . . ? O7A S1 O6B O7B -146.3(18) . . . . ? O5A S1 O6B O7B -159(3) . . . . ? C22 S1 O6B O7B 98.9(15) . . . . ? O7B S1 O7A O5A -78(3) . . . . ? O6B S1 O7A O5A -11(2) . . . . ? O6A S1 O7A O5A -153(2) . . . . ? O5B S1 O7A O5A -143.9(16) . . . . ? C22 S1 O7A O5A 103.8(14) . . . . ? O7B S1 O7A O6A 75(3) . . . . ? O6B S1 O7A O6A 142(2) . . . . ? O5B S1 O7A O6A 9(2) . . . . ? O5A S1 O7A O6A 153(2) . . . . ? C22 S1 O7A O6A -102.9(17) . . . . ? O6B O5A O7A S1 13(2) . . . . ? O6B O5A O7A O6A -10(4) . . . . ? S1 O5A O7A O6A -24(2) . . . . ? O5B O6A O7A S1 -17(4) . . . . ? O5B O6A O7A O5A 8(5) . . . . ? S1 O6A O7A O5A 25(2) . . . . ? C32 C31 S2A O16A -146(2) . . . . ? C30 C31 S2A O16A 13(2) . . . . ? S2B C31 S2A O16A 137(2) . . . . ? C32 C31 S2A O15A 4(2) . . . . ? C30 C31 S2A O15A 164.1(19) . . . . ? S2B C31 S2A O15A -72.1(19) . . . . ? C32 C31 S2A O14A 130(2) . . . . ? C30 C31 S2A O14A -70(2) . . . . ? S2B C31 S2A O14A 53.7(18) . . . . ? C32 C31 S2B O15B 50.7(19) . . . . ? C30 C31 S2B O15B -121.2(18) . . . . ? S2A C31 S2B O15B 169(2) . . . . ? C32 C31 S2B O16B -173.7(19) . . . . ? C30 C31 S2B O16B 14(2) . . . . ? S2A C31 S2B O16B -54.9(17) . . . . ? C32 C31 S2B O14B -79.6(18) . . . . ? C30 C31 S2B O14B 108.5(17) . . . . ? S2A C31 S2B O14B 39.2(15) . . . . ? C36 C39 S3 O9A -115.5(18) . . . . ? C37 C39 S3 O9A 63.3(19) . . . . ? C36 C39 S3 O9B 40.0(14) . . . . ? C37 C39 S3 O9B -141.2(13) . . . . ? C36 C39 S3 O8B 163.9(16) . . . . ? C37 C39 S3 O8B -17.4(17) . . . . ? C36 C39 S3 O8A 7.6(16) . . . . ? C37 C39 S3 O8A -173.6(14) . . . . ? C36 C39 S3 O10A 132.7(15) . . . . ? C37 C39 S3 O10A -48.5(15) . . . . ? C36 C39 S3 O10B -85.8(14) . . . . ? C37 C39 S3 O10B 93.0(13) . . . . ? O9A S3 O8A O9B -156(2) . . . . ? O8B S3 O8A O9B -65(3) . . . . ? O10A S3 O8A O9B -32(3) . . . . ? O10B S3 O8A O9B -174(2) . . . . ? C39 S3 O8A O9B 83(2) . . . . ? O9B S3 O9A O10B -58(4) . . . . ? O8B S3 O9A O10B -171(3) . . . . ? O8A S3 O9A O10B -39(3) . . . . ? O10A S3 O9A O10B -168(3) . . . . ? C39 S3 O9A O10B 84(3) . . . . ? O9B S3 O9A O8B 113(2) . . . . ? O8A S3 O9A O8B 132.1(14) . . . . ? O10A S3 O9A O8B 2.5(16) . . . . ? O10B S3 O9A O8B 171(3) . . . . ? C39 S3 O9A O8B -105.7(12) . . . . ? O9A S3 O10A O8B -5(3) . . . . ? O9B S3 O10A O8B -147(3) . . . . ? O8A S3 O10A O8B -131(3) . . . . ? O10B S3 O10A O8B -13(3) . . . . ? C39 S3 O10A O8B 108(3) . . . . ? S3 O10A O8B O9A 5(3) . . . . ? O9A S3 O8B O10A 175(3) . . . . ? O9B S3 O8B O10A 37(3) . . . . ? O8A S3 O8B O10A 68(3) . . . . ? O10B S3 O8B O10A 171(2) . . . . ? C39 S3 O8B O10A -80(3) . . . . ? O9B S3 O8B O9A -138.7(16) . . . . ? O8A S3 O8B O9A -107(2) . . . . ? O10A S3 O8B O9A -175(3) . . . . ? O10B S3 O8B O9A -4.7(16) . . . . ? C39 S3 O8B O9A 104.6(13) . . . . ? O10B O9A O8B O10A 9(8) . . . . ? S3 O9A O8B O10A -6(4) . . . . ? O10B O9A O8B S3 15(5) . . . . ? O9A S3 O9B O8A 36(4) . . . . ? O8B S3 O9B O8A 134(2) . . . . ? O10A S3 O9B O8A 152(2) . . . . ? O10B S3 O9B O8A 7(3) . . . . ? C39 S3 O9B O8A -107(2) . . . . ? O8B O9A O10B S3 -12(4) . . . . ? O9B S3 O10B O9A 141(3) . . . . ? O8B S3 O10B O9A 9(3) . . . . ? O8A S3 O10B O9A 145(3) . . . . ? O10A S3 O10B O9A 16(4) . . . . ? C39 S3 O10B O9A -104(3) . . . . ? C45 C44 S4 O13A 167.0(16) . . . . ? C43 C44 S4 O13A -20.0(18) . . . . ? C45 C44 S4 O11A 61(2) . . . . ? C43 C44 S4 O11A -126(2) . . . . ? C45 C44 S4 O13B 19(2) . . . . ? C43 C44 S4 O13B -167.8(18) . . . . ? C45 C44 S4 O12A -73.2(14) . . . . ? C43 C44 S4 O12A 99.9(13) . . . . ? C45 C44 S4 O12B 106.9(16) . . . . ? C43 C44 S4 O12B -80.0(16) . . . . ? C45 C44 S4 O11B -172.3(15) . . . . ? C43 C44 S4 O11B 0.7(16) . . . . ? O13A S4 O11A O13B 144(3) . . . . ? O12A S4 O11A O13B 21(4) . . . . ? O12B S4 O11A O13B 180(4) . . . . ? O11B S4 O11A O13B 145(3) . . . . ? C44 S4 O11A O13B -101(3) . . . . ? O13A S4 O11A O12B -36(2) . . . . ? O13B S4 O11A O12B -180(4) . . . . ? O12A S4 O11A O12B -158.6(19) . . . . ? O11B S4 O11A O12B -35(3) . . . . ? C44 S4 O11A O12B 79(2) . . . . ? O11A S4 O13A O11B 177(4) . . . . ? O13B S4 O13A O11B -155(4) . . . . ? O12A S4 O13A O11B -52(4) . . . . ? O12B S4 O13A O11B 147(5) . . . . ? C44 S4 O13A O11B 64(4) . . . . ? O11A S4 O13A O12B 30(2) . . . . ? O13B S4 O13A O12B 58(2) . . . . ? O12A S4 O13A O12B 161.5(15) . . . . ? O11B S4 O13A O12B -147(5) . . . . ? C44 S4 O13A O12B -82.5(16) . . . . ? O12B O13A O11B S4 106(8) . . . . ? O11A S4 O11B O13A -4(5) . . . . ? O13B S4 O11B O13A 39(6) . . . . ? O12A S4 O11B O13A 133(4) . . . . ? O12B S4 O11B O13A -29(4) . . . . ? C44 S4 O11B O13A -121(4) . . . . ? O13B O11A O12B O13A 28(17) . . . . ? S4 O11A O12B O13A 28.6(18) . . . . ? O13B O11A O12B S4 0(16) . . . . ? O11B O13A O12B O11A -151(8) . . . . ? S4 O13A O12B O11A -31(2) . . . . ? O11B O13A O12B S4 -119(8) . . . . ? O13A S4 O12B O11A 138(3) . . . . ? O13B S4 O12B O11A 0(3) . . . . ? O12A S4 O12B O11A 70(5) . . . . ? O11B S4 O12B O11A 150(3) . . . . ? C44 S4 O12B O11A -110(2) . . . . ? O11A S4 O12B O13A -138(3) . . . . ? O13B S4 O12B O13A -137.8(19) . . . . ? O12A S4 O12B O13A -68(5) . . . . ? O11B S4 O12B O13A 12.3(18) . . . . ? C44 S4 O12B O13A 111.9(15) . . . . ? O12B O11A O13B S4 0(16) . . . . ? O13A S4 O13B O11A -48(4) . . . . ? O12A S4 O13B O11A -163(3) . . . . ? O12B S4 O13B O11A 0(3) . . . . ? O11B S4 O13B O11A -66(5) . . . . ? C44 S4 O13B O11A 93(3) . . . . ? N1C C2C C3C C3C 179(3) . . . 7 ? N1B C2B C3B C4B -118(6) . . . . ? C2B C3B C4B C5B 162(4) . . . . ? C3B C4B C5B N6B -101(10) . . . . ? N1D C2D C3D C4D -172(4) . . . . ? C2D C3D C4D C5D -148(6) . . . . ? C3D C4D C5D N6D 144(7) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 18.79 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.927 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.139 # Attachment 'compound 1B.cif' data_1b _database_code_depnum_ccdc_archive 'CCDC 294463' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;para-sulfonatocalix(8)arene / 1,2-cis-cyclohexanediammonium cation ; _chemical_melting_point ? _chemical_formula_moiety 'C56 H48 O32 S8 . 4(C6 H14 N2) . 8(H2 O)' _chemical_formula_sum 'C80 H104 N8 O40 S8' _chemical_formula_weight 2074.19 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' S S 0.1246 0.1234 '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/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 12.5225(1) _cell_length_b 25.6792(3) _cell_length_c 14.5478(2) _cell_angle_alpha 90.000(1) _cell_angle_beta 102.421(1) _cell_angle_gamma 90.000(1) _cell_volume 4568.14(9) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 0.293 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 9.1 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21233 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.92 _reflns_number_total 10809 _reflns_number_gt 7548 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Denzo / Scalepak (Otwinowski & Minor, 1997)' _computing_data_reduction 'Denzo / Scalepak (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Johnson & Burnet, 1996)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.013(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10809 _refine_ls_number_parameters 592 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2641 _refine_ls_R_factor_gt 0.2350 _refine_ls_wR_factor_ref 0.6225 _refine_ls_wR_factor_gt 0.6173 _refine_ls_goodness_of_fit_ref 2.689 _refine_ls_restrained_S_all 2.689 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C -0.0602(10) -0.0994(5) 0.4257(8) 0.016(3) Uani 1 1 d . . . C2 C -0.1014(10) -0.0497(5) 0.4300(8) 0.014(3) Uani 1 1 d . . . H2 H -0.0940 -0.0247 0.3836 0.017 Uiso 1 1 calc R . . C3 C -0.1535(10) -0.0359(5) 0.5019(9) 0.016(3) Uani 1 1 d . . . C4 C -0.1618(10) -0.0739(5) 0.5690(8) 0.011(2) Uani 1 1 d . . . C5 C -0.1227(10) -0.1254(5) 0.5634(8) 0.013(2) Uani 1 1 d . . . C6 C -0.0714(10) -0.1372(5) 0.4905(8) 0.016(3) Uani 1 1 d . . . H6 H -0.0440 -0.1713 0.4851 0.020 Uiso 1 1 calc R . . C7 C -0.1384(10) -0.1659(5) 0.6349(8) 0.016(3) Uani 1 1 d . . . H7A H -0.2076 -0.1580 0.6545 0.019 Uiso 1 1 calc R . . H7B H -0.1477 -0.2001 0.6029 0.019 Uiso 1 1 calc R . . C8 C 0.0128(10) -0.1582(5) 0.8909(8) 0.014(2) Uiso 1 1 d . . . C9 C -0.0615(11) -0.1490(5) 0.8084(8) 0.016(3) Uani 1 1 d . . . H9 H -0.1224 -0.1271 0.8096 0.019 Uiso 1 1 calc R . . C10 C -0.0509(9) -0.1711(4) 0.7210(8) 0.006(2) Uiso 1 1 d . . . C11 C 0.0441(11) -0.1984(5) 0.7208(9) 0.017(3) Uani 1 1 d . . . C12 C 0.1207(9) -0.2095(4) 0.8043(8) 0.010(2) Uani 1 1 d . . . C13 C 0.1086(10) -0.1868(5) 0.8876(9) 0.016(3) Uani 1 1 d . . . H13 H 0.1646 -0.1904 0.9428 0.019 Uiso 1 1 calc R . . C14 C 0.2227(10) -0.2451(4) 0.8041(8) 0.008(2) Uiso 1 1 d . . . H14A H 0.2357 -0.2673 0.8610 0.010 Uiso 1 1 calc R . . H14B H 0.2059 -0.2683 0.7485 0.010 Uiso 1 1 calc R . . C15 C 0.4970(10) -0.1769(5) 0.8854(8) 0.011(2) Uiso 1 1 d . . . C16 C 0.4001(10) -0.2063(5) 0.8872(9) 0.017(3) Uani 1 1 d . . . H16 H 0.3858 -0.2195 0.9444 0.020 Uiso 1 1 calc R . . C17 C 0.3285(10) -0.2148(5) 0.8020(9) 0.015(3) Uani 1 1 d . . . C18 C 0.3490(10) -0.1973(4) 0.7186(9) 0.014(3) Uani 1 1 d . . . C19 C 0.4474(9) -0.1728(4) 0.7154(7) 0.004(2) Uiso 1 1 d . . . C20 C 0.5195(10) -0.1616(5) 0.8010(8) 0.014(3) Uani 1 1 d . . . H20 H 0.5852 -0.1431 0.8006 0.017 Uiso 1 1 calc R . . C21 C 0.4769(10) -0.1542(5) 0.6249(9) 0.015(3) Uani 1 1 d . . . H21A H 0.4376 -0.1756 0.5716 0.018 Uiso 1 1 calc R . . H21B H 0.5564 -0.1589 0.6295 0.018 Uiso 1 1 calc R . . C22 C 0.4901(10) -0.0061(5) 0.6320(9) 0.013(2) Uani 1 1 d . . . C23 C 0.5208(10) -0.0580(5) 0.6434(9) 0.016(3) Uani 1 1 d . . . H23 H 0.5923 -0.0669 0.6769 0.019 Uiso 1 1 calc R . . C24 C 0.4470(9) -0.0969(4) 0.6060(8) 0.010(2) Uani 1 1 d . . . C25 C 0.3415(10) -0.0812(5) 0.5585(8) 0.014(3) Uani 1 1 d . . . C26 C 0.3103(10) -0.0293(5) 0.5433(8) 0.014(2) Uani 1 1 d . . . C27 C 0.3873(10) 0.0088(5) 0.5831(9) 0.017(3) Uani 1 1 d . . . H27 H 0.3688 0.0447 0.5765 0.020 Uiso 1 1 calc R . . C28 C 0.1939(10) -0.0191(5) 0.4935(9) 0.016(3) Uani 1 1 d . . . H28A H 0.1458 -0.0425 0.5204 0.019 Uiso 1 1 calc R . . H28B H 0.1860 -0.0286 0.4265 0.019 Uiso 1 1 calc R . . C29 C 0.1651(10) -0.0011(5) 0.9143(9) 0.014(3) Uiso 1 1 d . . . H29 H 0.0987 -0.0016 0.9420 0.017 Uiso 1 1 calc R . . C30 C 0.2640(11) -0.0178(5) 0.9877(10) 0.021(3) Uani 1 1 d . . . H30 H 0.2458 -0.0527 1.0106 0.026 Uiso 1 1 calc R . . C31 C 0.3673(11) -0.0250(5) 0.9516(12) 0.028(3) Uani 1 1 d . . . H31A H 0.3920 0.0090 0.9316 0.034 Uiso 1 1 calc R . . H31B H 0.4258 -0.0391 1.0024 0.034 Uiso 1 1 calc R . . C32 C 0.3464(14) -0.0622(6) 0.8692(11) 0.032(4) Uani 1 1 d . . . H32A H 0.3313 -0.0972 0.8919 0.038 Uiso 1 1 calc R . . H32B H 0.4134 -0.0647 0.8436 0.038 Uiso 1 1 calc R . . C33 C 0.2510(12) -0.0461(6) 0.7901(10) 0.028(3) Uani 1 1 d . . . H33A H 0.2683 -0.0128 0.7621 0.034 Uiso 1 1 calc R . . H33B H 0.2386 -0.0730 0.7402 0.034 Uiso 1 1 calc R . . C34 C 0.1493(11) -0.0398(5) 0.8291(10) 0.022(3) Uani 1 1 d . . . H34A H 0.1276 -0.0742 0.8496 0.026 Uiso 1 1 calc R . . H34B H 0.0891 -0.0270 0.7785 0.026 Uiso 1 1 calc R . . C35 C -0.4549(11) -0.1848(5) 0.2873(9) 0.020(3) Uani 1 1 d . . . H35 H -0.4237 -0.1497 0.3069 0.024 Uiso 1 1 calc R . . C36 C -0.3649(11) -0.2150(5) 0.2523(9) 0.016(3) Uani 1 1 d . . . H36 H -0.3426 -0.1943 0.2014 0.019 Uiso 1 1 calc R . . C37 C -0.2661(10) -0.2213(6) 0.3328(9) 0.020(3) Uani 1 1 d . . . H37A H -0.2324 -0.1868 0.3498 0.024 Uiso 1 1 calc R . . H37B H -0.2112 -0.2436 0.3120 0.024 Uiso 1 1 calc R . . C38 C -0.2964(11) -0.2456(5) 0.4194(9) 0.016(3) Uani 1 1 d . . . H38A H -0.2306 -0.2480 0.4711 0.019 Uiso 1 1 calc R . . H38B H -0.3248 -0.2813 0.4043 0.019 Uiso 1 1 calc R . . C39 C -0.3839(13) -0.2123(6) 0.4510(9) 0.026(3) Uani 1 1 d . . . H39A H -0.4035 -0.2282 0.5071 0.032 Uiso 1 1 calc R . . H39B H -0.3542 -0.1770 0.4685 0.032 Uiso 1 1 calc R . . C40 C -0.4857(11) -0.2080(5) 0.3719(9) 0.018(3) Uani 1 1 d . . . H40A H -0.5178 -0.2430 0.3565 0.022 Uiso 1 1 calc R . . H40B H -0.5409 -0.1858 0.3923 0.022 Uiso 1 1 calc R . . N1 N 0.1816(9) 0.0537(4) 0.8781(8) 0.018(2) Uani 1 1 d . . . H1A H 0.1746 0.0775 0.9226 0.027 Uiso 1 1 calc R . . H1B H 0.1304 0.0599 0.8245 0.027 Uiso 1 1 calc R . . H1C H 0.2496 0.0561 0.8656 0.027 Uiso 1 1 calc R . . N2 N 0.2846(10) 0.0179(5) 1.0729(8) 0.026(3) Uani 1 1 d . . . H2AN H 0.2986 0.0507 1.0550 0.040 Uiso 1 1 calc R . . H2BN H 0.3432 0.0060 1.1162 0.040 Uiso 1 1 calc R . . H2CN H 0.2246 0.0183 1.0987 0.040 Uiso 1 1 calc R . . N3 N -0.5538(9) -0.1755(4) 0.2098(8) 0.019(2) Uani 1 1 d . . . H3A H -0.5778 -0.2063 0.1821 0.028 Uiso 1 1 calc R . . H3B H -0.5358 -0.1537 0.1662 0.028 Uiso 1 1 calc R . . H3C H -0.6076 -0.1607 0.2343 0.028 Uiso 1 1 calc R . . N4 N -0.4071(9) -0.2661(5) 0.2129(8) 0.022(3) Uani 1 1 d . . . H4A H -0.3506 -0.2889 0.2179 0.033 Uiso 1 1 calc R . . H4B H -0.4404 -0.2621 0.1512 0.033 Uiso 1 1 calc R . . H4C H -0.4562 -0.2785 0.2454 0.033 Uiso 1 1 calc R . . O1 O -0.2112(8) -0.0643(4) 0.6420(6) 0.022(2) Uani 1 1 d . . . H1 H -0.1724 -0.0763 0.6919 0.032 Uiso 1 1 calc R . . O2 O 0.0540(7) -0.2188(3) 0.6365(6) 0.0161(19) Uani 1 1 d . . . H2A H 0.1147 -0.2102 0.6254 0.024 Uiso 1 1 calc R . . O3 O 0.2709(7) -0.2053(3) 0.6375(6) 0.017(2) Uani 1 1 d . . . H3 H 0.2729 -0.2365 0.6206 0.026 Uiso 1 1 calc R . . O4 O 0.2721(8) -0.1232(3) 0.5262(6) 0.020(2) Uani 1 1 d . . . H4 H 0.2244 -0.1257 0.5587 0.030 Uiso 1 1 calc R . . O5 O -0.0496(7) -0.1625(4) 0.2865(6) 0.020(2) Uani 1 1 d . . . O6 O -0.0054(8) -0.0708(4) 0.2706(7) 0.024(2) Uani 1 1 d . . . O7 O 0.1213(7) -0.1266(4) 0.3733(6) 0.018(2) Uani 1 1 d . . . O8 O -0.0926(8) -0.0973(4) 0.9792(6) 0.021(2) Uani 1 1 d . . . O9 O 0.1004(8) -0.1078(4) 1.0426(7) 0.025(2) Uani 1 1 d . . . O10 O -0.0220(8) -0.1778(4) 1.0553(6) 0.023(2) Uani 1 1 d . . . O11 O 0.5103(8) -0.1368(4) 1.0442(9) 0.034(3) Uani 1 1 d . . . O12 O 0.6247(8) -0.2124(4) 1.0360(7) 0.029(2) Uani 1 1 d . . . O13 O 0.6670(8) -0.1273(4) 0.9746(7) 0.028(2) Uani 1 1 d . . . O14 O 0.5675(8) 0.0390(4) 0.7896(6) 0.021(2) Uani 1 1 d . . . O15 O 0.6937(7) 0.0222(4) 0.6899(7) 0.021(2) Uani 1 1 d . . . O16 O 0.5555(8) 0.0906(4) 0.6472(6) 0.022(2) Uani 1 1 d . . . S1 S 0.0060(2) -0.11606(12) 0.3311(2) 0.0138(8) Uani 1 1 d . . . S2 S -0.0025(2) -0.13349(13) 0.9997(2) 0.0146(8) Uani 1 1 d . . . S3 S 0.5829(3) -0.16243(12) 0.9935(2) 0.0154(8) Uani 1 1 d . . . S4 S 0.5844(2) 0.04055(12) 0.6918(2) 0.0137(8) Uani 1 1 d . . . O1W O -0.2743(7) -0.3541(4) 0.2132(6) 0.020(2) Uani 1 1 d . . . O2W O 0.8344(8) -0.2439(4) 1.1083(9) 0.027(3) Uani 1 1 d . . . O3W O 0.1030(9) -0.0126(4) 1.1378(7) 0.028(2) Uani 1 1 d . . . O4W O 0.3633(8) 0.0800(4) 0.8054(7) 0.023(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.013(6) 0.025(7) 0.009(6) 0.004(5) 0.000(5) -0.005(5) C2 0.017(6) 0.013(6) 0.011(6) 0.005(5) -0.001(5) -0.007(5) C3 0.009(6) 0.019(6) 0.015(6) 0.005(5) -0.008(5) 0.001(5) C4 0.013(6) 0.009(6) 0.015(6) 0.009(5) 0.008(5) 0.002(5) C5 0.015(6) 0.014(6) 0.011(6) -0.005(5) 0.006(5) -0.001(5) C6 0.012(6) 0.025(7) 0.010(6) -0.004(5) -0.004(5) -0.001(5) C7 0.018(6) 0.015(6) 0.012(6) 0.001(5) -0.003(5) 0.005(5) C9 0.027(7) 0.008(6) 0.014(6) 0.004(5) 0.009(5) 0.001(5) C11 0.023(7) 0.008(6) 0.018(6) 0.002(5) 0.001(5) -0.008(5) C12 0.010(5) 0.003(5) 0.016(6) 0.000(4) 0.004(4) 0.001(4) C13 0.018(6) 0.010(6) 0.018(6) -0.002(5) 0.002(5) -0.005(5) C16 0.013(6) 0.015(6) 0.021(7) -0.002(5) 0.000(5) 0.000(5) C17 0.009(6) 0.019(7) 0.017(6) -0.002(5) 0.002(5) 0.008(5) C18 0.018(6) 0.006(5) 0.014(6) 0.001(5) -0.002(5) 0.003(5) C20 0.011(6) 0.016(6) 0.015(6) -0.006(5) 0.002(5) -0.007(5) C21 0.009(6) 0.020(7) 0.014(6) 0.000(5) -0.002(5) 0.012(5) C22 0.014(6) 0.013(6) 0.013(6) 0.000(5) 0.008(5) 0.007(5) C23 0.006(5) 0.027(7) 0.014(6) 0.007(5) 0.004(4) 0.008(5) C24 0.013(6) 0.009(5) 0.009(5) -0.005(4) 0.007(4) 0.000(4) C25 0.011(6) 0.017(6) 0.014(6) 0.013(5) 0.004(5) -0.001(5) C26 0.017(6) 0.014(6) 0.006(5) 0.003(5) -0.004(4) 0.007(5) C27 0.020(7) 0.011(6) 0.020(7) 0.000(5) 0.006(5) 0.005(5) C28 0.013(6) 0.017(6) 0.018(6) 0.000(5) 0.001(5) -0.004(5) C30 0.018(7) 0.018(7) 0.026(7) 0.001(6) 0.001(5) -0.002(5) C31 0.014(7) 0.013(7) 0.055(10) 0.014(7) 0.005(6) 0.004(5) C32 0.041(9) 0.017(7) 0.041(9) 0.003(7) 0.020(7) 0.010(7) C33 0.033(8) 0.032(8) 0.025(8) -0.009(6) 0.017(6) 0.009(7) C34 0.024(7) 0.018(7) 0.022(7) 0.000(5) 0.000(6) -0.005(5) C35 0.022(7) 0.016(7) 0.019(7) -0.006(5) 0.000(5) 0.001(5) C36 0.020(6) 0.015(6) 0.014(6) 0.003(5) 0.004(5) 0.001(5) C37 0.008(6) 0.038(8) 0.015(6) 0.001(6) 0.004(5) -0.001(5) C38 0.010(6) 0.028(8) 0.012(6) 0.001(5) 0.004(5) 0.000(5) C39 0.047(9) 0.021(7) 0.011(6) 0.001(5) 0.007(6) -0.001(7) C40 0.028(7) 0.014(6) 0.015(6) -0.001(5) 0.009(5) -0.001(5) N1 0.019(6) 0.016(5) 0.018(6) 0.003(4) 0.001(4) 0.004(4) N2 0.034(7) 0.022(6) 0.021(6) 0.002(5) 0.001(5) -0.005(5) N3 0.023(6) 0.017(6) 0.020(6) 0.002(5) 0.012(5) 0.002(5) N4 0.014(6) 0.040(7) 0.014(5) 0.011(5) 0.007(4) -0.005(5) O1 0.028(5) 0.026(5) 0.014(5) -0.001(4) 0.012(4) 0.003(4) O2 0.018(5) 0.014(4) 0.015(4) 0.000(4) 0.000(3) 0.000(4) O3 0.010(4) 0.015(5) 0.027(5) -0.003(4) 0.003(4) 0.002(3) O4 0.021(5) 0.015(5) 0.020(5) 0.005(4) -0.004(4) -0.003(4) O5 0.019(5) 0.024(5) 0.016(5) -0.008(4) 0.001(4) -0.005(4) O6 0.027(5) 0.028(6) 0.020(5) 0.004(4) 0.009(4) 0.002(4) O7 0.015(5) 0.027(5) 0.012(4) -0.005(4) 0.002(3) 0.005(4) O8 0.027(5) 0.030(5) 0.008(4) -0.003(4) 0.007(4) 0.003(4) O9 0.027(5) 0.032(6) 0.018(5) -0.010(4) 0.008(4) -0.011(4) O10 0.028(5) 0.031(6) 0.014(5) 0.003(4) 0.015(4) 0.002(4) O11 0.017(5) 0.018(5) 0.074(9) -0.015(5) 0.027(5) -0.001(4) O12 0.028(6) 0.032(6) 0.023(5) 0.003(4) 0.000(4) -0.004(5) O13 0.015(5) 0.040(6) 0.027(5) 0.007(5) -0.001(4) -0.014(4) O14 0.027(5) 0.022(5) 0.015(5) -0.008(4) 0.002(4) 0.001(4) O15 0.010(4) 0.023(5) 0.030(5) -0.009(4) 0.006(4) 0.002(4) O16 0.026(5) 0.025(5) 0.015(5) 0.003(4) 0.004(4) 0.010(4) S1 0.0128(15) 0.0163(16) 0.0118(15) 0.0010(12) 0.0018(11) 0.0017(12) S2 0.0139(16) 0.0182(17) 0.0115(15) -0.0021(12) 0.0024(11) 0.0018(12) S3 0.0149(16) 0.0170(16) 0.0135(15) 0.0012(12) 0.0013(11) -0.0019(12) S4 0.0140(15) 0.0130(15) 0.0138(15) -0.0016(11) 0.0024(11) -0.0008(11) O1W 0.018(5) 0.019(5) 0.021(5) -0.004(4) 0.003(4) 0.004(4) O2W 0.007(5) 0.025(6) 0.046(7) 0.011(5) 0.001(4) 0.000(4) O3W 0.030(6) 0.026(5) 0.030(6) 0.001(4) 0.013(5) -0.006(4) O4W 0.028(5) 0.025(5) 0.024(5) -0.009(4) 0.021(4) -0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.381(18) . ? C1 C2 1.384(18) . ? C1 S1 1.803(13) . ? C2 C3 1.393(18) . ? C3 C4 1.400(16) . ? C3 C28 1.506(18) 3_556 ? C4 O1 1.362(14) . ? C4 C5 1.418(17) . ? C5 C6 1.387(17) . ? C5 C7 1.513(17) . ? C7 C10 1.483(15) . ? C8 C9 1.371(17) . ? C8 C13 1.416(18) . ? C8 S2 1.753(13) . ? C9 C10 1.424(16) . ? C10 C11 1.382(17) . ? C11 O2 1.364(16) . ? C11 C12 1.405(17) . ? C12 C13 1.383(17) . ? C12 C14 1.571(16) . ? C14 C17 1.542(17) . ? C15 C20 1.375(17) . ? C15 C16 1.435(17) . ? C15 S3 1.744(12) . ? C16 C17 1.381(17) . ? C17 C18 1.368(18) . ? C18 O3 1.376(14) . ? C18 C19 1.393(17) . ? C19 C20 1.402(15) . ? C19 C21 1.519(16) . ? C21 C24 1.529(16) . ? C22 C27 1.384(17) . ? C22 C23 1.385(17) . ? C22 S4 1.774(13) . ? C23 C24 1.391(17) . ? C24 C25 1.411(16) . ? C25 C26 1.394(17) . ? C25 O4 1.402(15) . ? C26 C27 1.409(18) . ? C26 C28 1.504(17) . ? C28 C3 1.506(18) 3_556 ? C29 C30 1.512(18) . ? C29 N1 1.531(16) . ? C29 C34 1.566(18) . ? C30 C31 1.510(19) . ? C30 N2 1.518(18) . ? C31 C32 1.51(2) . ? C32 C33 1.53(2) . ? C33 C34 1.511(19) . ? C35 C40 1.491(18) . ? C35 N3 1.503(16) . ? C35 C36 1.542(18) . ? C36 N4 1.482(18) . ? C36 C37 1.518(17) . ? C37 C38 1.525(18) . ? C38 C39 1.54(2) . ? C39 C40 1.526(19) . ? O5 S1 1.461(9) . ? O6 S1 1.447(10) . ? O7 S1 1.468(9) . ? O8 S2 1.444(10) . ? O9 S2 1.462(10) . ? O10 S2 1.446(10) . ? O11 S3 1.446(10) . ? O12 S3 1.471(11) . ? O13 S3 1.457(10) . ? O14 S4 1.483(10) . ? O15 S4 1.453(9) . ? O16 S4 1.450(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 121.6(12) . . ? C6 C1 S1 119.0(10) . . ? C2 C1 S1 119.4(9) . . ? C1 C2 C3 120.5(11) . . ? C2 C3 C4 117.6(12) . . ? C2 C3 C28 119.2(11) . 3_556 ? C4 C3 C28 123.2(12) . 3_556 ? O1 C4 C3 122.1(11) . . ? O1 C4 C5 115.7(10) . . ? C3 C4 C5 122.2(11) . . ? C6 C5 C4 118.1(11) . . ? C6 C5 C7 121.6(11) . . ? C4 C5 C7 120.3(10) . . ? C1 C6 C5 120.0(12) . . ? C10 C7 C5 117.4(11) . . ? C9 C8 C13 118.7(11) . . ? C9 C8 S2 122.9(10) . . ? C13 C8 S2 118.4(9) . . ? C8 C9 C10 122.4(12) . . ? C11 C10 C9 116.8(11) . . ? C11 C10 C7 121.6(11) . . ? C9 C10 C7 121.6(11) . . ? O2 C11 C10 116.2(11) . . ? O2 C11 C12 121.6(12) . . ? C10 C11 C12 121.9(12) . . ? C13 C12 C11 119.3(11) . . ? C13 C12 C14 119.3(10) . . ? C11 C12 C14 121.3(11) . . ? C12 C13 C8 120.1(11) . . ? C17 C14 C12 114.1(9) . . ? C20 C15 C16 120.2(11) . . ? C20 C15 S3 122.6(9) . . ? C16 C15 S3 117.1(9) . . ? C17 C16 C15 117.0(12) . . ? C18 C17 C16 122.3(12) . . ? C18 C17 C14 120.6(11) . . ? C16 C17 C14 117.1(11) . . ? C17 C18 O3 118.4(11) . . ? C17 C18 C19 120.9(11) . . ? O3 C18 C19 120.6(11) . . ? C18 C19 C20 117.9(10) . . ? C18 C19 C21 123.6(10) . . ? C20 C19 C21 118.4(10) . . ? C15 C20 C19 121.2(11) . . ? C19 C21 C24 111.2(9) . . ? C27 C22 C23 122.2(12) . . ? C27 C22 S4 120.7(9) . . ? C23 C22 S4 116.9(9) . . ? C22 C23 C24 119.9(11) . . ? C23 C24 C25 117.4(11) . . ? C23 C24 C21 120.3(10) . . ? C25 C24 C21 122.0(10) . . ? C26 C25 O4 123.4(11) . . ? C26 C25 C24 123.5(11) . . ? O4 C25 C24 113.1(10) . . ? C25 C26 C27 117.1(11) . . ? C25 C26 C28 116.9(11) . . ? C27 C26 C28 125.7(11) . . ? C22 C27 C26 119.8(11) . . ? C26 C28 C3 116.2(10) . 3_556 ? C30 C29 N1 110.6(10) . . ? C30 C29 C34 108.9(11) . . ? N1 C29 C34 108.3(10) . . ? C31 C30 C29 115.0(12) . . ? C31 C30 N2 110.5(12) . . ? C29 C30 N2 112.1(11) . . ? C32 C31 C30 109.8(12) . . ? C31 C32 C33 113.7(12) . . ? C34 C33 C32 109.4(12) . . ? C33 C34 C29 113.1(11) . . ? C40 C35 N3 111.5(11) . . ? C40 C35 C36 114.1(11) . . ? N3 C35 C36 112.1(10) . . ? N4 C36 C37 111.6(11) . . ? N4 C36 C35 110.3(11) . . ? C37 C36 C35 109.4(10) . . ? C36 C37 C38 112.0(11) . . ? C37 C38 C39 109.8(11) . . ? C40 C39 C38 110.4(11) . . ? C35 C40 C39 109.2(11) . . ? O6 S1 O5 114.3(6) . . ? O6 S1 O7 111.2(6) . . ? O5 S1 O7 111.5(5) . . ? O6 S1 C1 105.8(6) . . ? O5 S1 C1 106.3(6) . . ? O7 S1 C1 107.3(5) . . ? O8 S2 O10 113.8(6) . . ? O8 S2 O9 112.0(6) . . ? O10 S2 O9 110.8(6) . . ? O8 S2 C8 106.2(5) . . ? O10 S2 C8 106.5(6) . . ? O9 S2 C8 107.0(6) . . ? O11 S3 O13 111.9(6) . . ? O11 S3 O12 112.9(7) . . ? O13 S3 O12 114.4(6) . . ? O11 S3 C15 102.9(6) . . ? O13 S3 C15 107.0(6) . . ? O12 S3 C15 106.7(6) . . ? O16 S4 O15 115.1(6) . . ? O16 S4 O14 112.4(5) . . ? O15 S4 O14 109.8(6) . . ? O16 S4 C22 107.7(6) . . ? O15 S4 C22 107.6(5) . . ? O14 S4 C22 103.6(6) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 6.063 _refine_diff_density_min -1.384 _refine_diff_density_rms 0.425