# Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 177 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Philip Gale' 'Peter R. Edwards' 'Jennifer R. Hiscock' 'Mark Light' _publ_contact_author_name 'Philip Gale' _publ_contact_author_email PHILIP.GALE@SOTON.AC.UK _publ_section_title ; Carbamate complexation by urea-based receptors: studies in solution and the solid state ; # Attachment '2008sot1042.cif' data_2008sot1042 _database_code_depnum_ccdc_archive 'CCDC 745012' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; 2(C27 H32 N6 O3), 2(C12 H24 O6), 2(C4 H10 N2 O2), 0.5(C2 H6 O S) ; _chemical_formula_sum 'C87 H135 N16 O22.50 S0.50' _chemical_formula_weight 1781.14 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' 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 12.626(7) _cell_length_b 14.165(9) _cell_length_c 27.564(17) _cell_angle_alpha 84.204(10) _cell_angle_beta 77.246(8) _cell_angle_gamma 72.121(9) _cell_volume 4573(5) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 941 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 28.43 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.294 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1914 _exptl_absorpt_coefficient_mu 0.105 _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 120(2) _diffrn_radiation_wavelength 0.6889 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Diamond beamline I19' _diffrn_radiation_monochromator 'silicon double crystal' _diffrn_measurement_device_type 'Rigaku Saturn 724+ detector on Crystal Logics diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34055 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0861 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 24.21 _reflns_number_total 14794 _reflns_number_gt 10644 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Rigaku CrystalClear' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^ > 2\s(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^)+(0.1142P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14794 _refine_ls_number_parameters 1151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0854 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.1936 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.17596(18) 0.26998(18) 0.32451(7) 0.0410(6) Uani 1 1 d . . . O2 O 0.69193(19) 0.43785(17) 0.22800(8) 0.0384(5) Uani 1 1 d . . . O3 O 0.59503(19) 0.14049(16) -0.00523(7) 0.0395(5) Uani 1 1 d . . . N1 N 0.1216(2) 0.26756(18) 0.40837(9) 0.0326(6) Uani 1 1 d . . . H1 H 0.1335 0.2814 0.4360 0.039 Uiso 1 1 calc R . . N2 N 0.3377(2) 0.36225(17) 0.32757(8) 0.0265(5) Uani 1 1 d . . . H2 H 0.3267 0.3612 0.2980 0.032 Uiso 1 1 calc R . . N3 N 0.5104(2) 0.43251(17) 0.25738(8) 0.0280(6) Uani 1 1 d . . . H3 H 0.4482 0.4382 0.2479 0.034 Uiso 1 1 calc R . . N4 N 0.5872(2) 0.41274(18) 0.17521(9) 0.0312(6) Uani 1 1 d . . . H4 H 0.5213 0.4093 0.1735 0.037 Uiso 1 1 calc R . . N5 N 0.5894(2) 0.29402(17) 0.09336(8) 0.0290(6) Uani 1 1 d . . . H5 H 0.5337 0.2905 0.1172 0.035 Uiso 1 1 calc R . . N6 N 0.4630(2) 0.17645(18) 0.06514(8) 0.0321(6) Uani 1 1 d . . . H6 H 0.4399 0.2071 0.0927 0.038 Uiso 1 1 calc R . . C1 C 0.1467(3) -0.0563(3) 0.44541(13) 0.0455(9) Uani 1 1 d . . . H1A H 0.1586 -0.0511 0.4781 0.068 Uiso 1 1 calc R . . H1B H 0.2076 -0.1089 0.4286 0.068 Uiso 1 1 calc R . . H1C H 0.0759 -0.0703 0.4480 0.068 Uiso 1 1 calc R . . C2 C 0.1435(3) 0.0415(2) 0.41596(12) 0.0397(8) Uani 1 1 d . . . H2A H 0.2138 0.0570 0.4147 0.048 Uiso 1 1 calc R . . H2B H 0.1376 0.0344 0.3821 0.048 Uiso 1 1 calc R . . C3 C 0.0441(3) 0.1263(2) 0.43928(11) 0.0330(7) Uani 1 1 d . . . H3A H 0.0536 0.1357 0.4723 0.040 Uiso 1 1 calc R . . H3B H -0.0251 0.1076 0.4431 0.040 Uiso 1 1 calc R . . C4 C 0.0305(3) 0.2239(2) 0.40990(11) 0.0354(7) Uani 1 1 d . . . H4A H 0.0270 0.2136 0.3761 0.042 Uiso 1 1 calc R . . H4B H -0.0411 0.2705 0.4245 0.042 Uiso 1 1 calc R . . C5 C 0.1878(2) 0.2872(2) 0.36578(10) 0.0283(7) Uani 1 1 d . . . C6 C 0.2760(2) 0.3316(2) 0.37046(10) 0.0267(7) Uani 1 1 d . . . C7 C 0.3165(3) 0.3450(2) 0.41049(10) 0.0290(7) Uani 1 1 d . . . H7 H 0.2889 0.3305 0.4437 0.035 Uiso 1 1 calc R . . C8 C 0.4086(3) 0.3852(2) 0.39197(10) 0.0274(7) Uani 1 1 d . . . C9 C 0.4841(3) 0.4128(2) 0.41403(11) 0.0342(7) Uani 1 1 d . . . H9 H 0.4780 0.4078 0.4484 0.041 Uiso 1 1 calc R . . C10 C 0.5671(3) 0.4474(2) 0.38377(12) 0.0360(7) Uani 1 1 d . . . H10 H 0.6172 0.4664 0.3981 0.043 Uiso 1 1 calc R . . C11 C 0.5785(3) 0.4549(2) 0.33150(11) 0.0332(7) Uani 1 1 d . . . H11 H 0.6363 0.4780 0.3121 0.040 Uiso 1 1 calc R . . C12 C 0.5058(2) 0.4287(2) 0.30886(10) 0.0273(7) Uani 1 1 d . . . C13 C 0.4198(2) 0.3947(2) 0.33978(10) 0.0265(6) Uani 1 1 d . . . C14 C 0.6045(3) 0.4280(2) 0.22112(10) 0.0275(7) Uani 1 1 d . . . C15 C 0.6695(3) 0.4025(2) 0.13108(10) 0.0300(7) Uani 1 1 d . . . C16 C 0.7555(3) 0.4476(2) 0.12107(11) 0.0319(7) Uani 1 1 d . . . H16 H 0.7608 0.4874 0.1447 0.038 Uiso 1 1 calc R . . C17 C 0.8346(3) 0.4343(2) 0.07599(12) 0.0392(8) Uani 1 1 d . . . H17 H 0.8920 0.4647 0.0707 0.047 Uiso 1 1 calc R . . C18 C 0.8301(3) 0.3779(3) 0.03956(12) 0.0399(8) Uani 1 1 d . . . H18 H 0.8832 0.3701 0.0098 0.048 Uiso 1 1 calc R . . C19 C 0.7435(3) 0.3320(2) 0.04803(11) 0.0337(7) Uani 1 1 d . . . C20 C 0.6646(2) 0.3455(2) 0.09356(10) 0.0297(7) Uani 1 1 d . . . C21 C 0.7112(3) 0.2708(2) 0.02032(11) 0.0369(8) Uani 1 1 d . . . H21 H 0.7474 0.2494 -0.0116 0.044 Uiso 1 1 calc R . . C22 C 0.6179(3) 0.2485(2) 0.04826(10) 0.0307(7) Uani 1 1 d . . . C23 C 0.5574(3) 0.1853(2) 0.03431(10) 0.0318(7) Uani 1 1 d . . . C24 C 0.3988(3) 0.1161(2) 0.05308(11) 0.0381(8) Uani 1 1 d . . . H24A H 0.3518 0.0990 0.0835 0.046 Uiso 1 1 calc R . . H24B H 0.4513 0.0549 0.0391 0.046 Uiso 1 1 calc R . . C25 C 0.3234(3) 0.1677(2) 0.01633(11) 0.0371(8) Uani 1 1 d . . . H25A H 0.2838 0.1232 0.0096 0.044 Uiso 1 1 calc R . . H25B H 0.3710 0.1811 -0.0148 0.044 Uiso 1 1 calc R . . C26 C 0.2365(3) 0.2645(2) 0.03467(12) 0.0417(8) Uani 1 1 d . . . H26A H 0.1893 0.2513 0.0659 0.050 Uiso 1 1 calc R . . H26B H 0.2760 0.3094 0.0410 0.050 Uiso 1 1 calc R . . C27 C 0.1615(3) 0.3144(3) -0.00187(14) 0.0527(10) Uani 1 1 d . . . H27A H 0.2076 0.3284 -0.0328 0.079 Uiso 1 1 calc R . . H27B H 0.1091 0.3753 0.0114 0.079 Uiso 1 1 calc R . . H27C H 0.1200 0.2713 -0.0075 0.079 Uiso 1 1 calc R . . O4 O 0.87604(18) 0.66832(15) 0.49561(7) 0.0365(5) Uani 1 1 d . . . O5 O 0.83254(19) 1.16333(16) 0.29124(8) 0.0357(5) Uani 1 1 d . . . O6 O 1.35034(18) 0.74880(16) 0.18690(7) 0.0395(5) Uani 1 1 d . . . N7 N 1.0165(2) 0.67059(17) 0.42975(8) 0.0299(6) Uani 1 1 d . . . H7A H 1.0392 0.7019 0.4031 0.036 Uiso 1 1 calc R . . N8 N 0.9002(2) 0.87692(17) 0.41148(8) 0.0266(5) Uani 1 1 d . . . H8 H 0.9623 0.8577 0.3899 0.032 Uiso 1 1 calc R . . N9 N 0.9251(2) 1.04634(18) 0.34307(9) 0.0298(6) Uani 1 1 d . . . H9A H 0.9909 1.0084 0.3467 0.036 Uiso 1 1 calc R . . N10 N 1.0080(2) 1.05742(18) 0.26125(9) 0.0292(6) Uani 1 1 d . . . H10A H 1.0658 1.0156 0.2707 0.035 Uiso 1 1 calc R . . N11 N 1.1861(2) 0.93036(17) 0.18832(8) 0.0264(5) Uani 1 1 d . . . H11A H 1.1924 0.9051 0.2176 0.032 Uiso 1 1 calc R . . N12 N 1.4129(2) 0.76518(18) 0.10397(9) 0.0336(6) Uani 1 1 d . . . H12 H 1.4047 0.8027 0.0777 0.040 Uiso 1 1 calc R . . C28 C 1.3152(4) 0.6366(3) 0.49555(15) 0.0607(11) Uani 1 1 d . . . H28A H 1.2668 0.6720 0.5241 0.091 Uiso 1 1 calc R . . H28B H 1.3705 0.6700 0.4803 0.091 Uiso 1 1 calc R . . H28C H 1.3531 0.5703 0.5058 0.091 Uiso 1 1 calc R . . C29 C 1.2440(3) 0.6328(3) 0.45836(13) 0.0436(8) Uani 1 1 d . . . H29A H 1.2031 0.7000 0.4494 0.052 Uiso 1 1 calc R . . H29B H 1.2941 0.6025 0.4284 0.052 Uiso 1 1 calc R . . C30 C 1.1601(3) 0.5753(2) 0.47819(11) 0.0342(7) Uani 1 1 d . . . H30A H 1.1110 0.6051 0.5085 0.041 Uiso 1 1 calc R . . H30B H 1.2012 0.5079 0.4867 0.041 Uiso 1 1 calc R . . C31 C 1.0868(3) 0.5720(2) 0.44169(11) 0.0324(7) Uani 1 1 d . . . H31A H 1.1355 0.5422 0.4113 0.039 Uiso 1 1 calc R . . H31B H 1.0384 0.5306 0.4560 0.039 Uiso 1 1 calc R . . C32 C 0.9181(3) 0.7130(2) 0.45915(10) 0.0290(7) Uani 1 1 d . . . C33 C 0.8581(3) 0.8180(2) 0.44881(10) 0.0291(7) Uani 1 1 d . . . C34 C 0.7570(3) 0.8739(2) 0.47544(11) 0.0326(7) Uani 1 1 d . . . H34 H 0.7110 0.8515 0.5024 0.039 Uiso 1 1 calc R . . C35 C 0.7352(3) 0.9718(2) 0.45462(10) 0.0303(7) Uani 1 1 d . . . C36 C 0.6490(3) 1.0609(2) 0.46570(11) 0.0361(8) Uani 1 1 d . . . H36 H 0.5879 1.0637 0.4921 0.043 Uiso 1 1 calc R . . C37 C 0.6571(3) 1.1439(2) 0.43671(11) 0.0367(8) Uani 1 1 d . . . H37 H 0.6006 1.2036 0.4440 0.044 Uiso 1 1 calc R . . C38 C 0.7477(3) 1.1417(2) 0.39634(11) 0.0337(7) Uani 1 1 d . . . H38 H 0.7497 1.1997 0.3776 0.040 Uiso 1 1 calc R . . C39 C 0.8336(3) 1.0554(2) 0.38400(10) 0.0283(7) Uani 1 1 d . . . C40 C 0.8272(2) 0.9709(2) 0.41439(10) 0.0273(6) Uani 1 1 d . . . C41 C 0.9151(3) 1.0952(2) 0.29731(10) 0.0278(7) Uani 1 1 d . . . C42 C 1.0179(2) 1.0808(2) 0.20972(10) 0.0273(7) Uani 1 1 d . . . C43 C 0.9487(3) 1.1599(2) 0.18820(11) 0.0297(7) Uani 1 1 d . . . H43 H 0.8885 1.2038 0.2083 0.036 Uiso 1 1 calc R . . C44 C 0.9665(3) 1.1764(2) 0.13624(11) 0.0356(7) Uani 1 1 d . . . H44 H 0.9178 1.2312 0.1229 0.043 Uiso 1 1 calc R . . C45 C 1.0529(3) 1.1146(2) 0.10492(11) 0.0366(8) Uani 1 1 d . . . H45 H 1.0634 1.1268 0.0707 0.044 Uiso 1 1 calc R . . C46 C 1.1255(3) 1.0324(2) 0.12536(10) 0.0297(7) Uani 1 1 d . . . C47 C 1.1071(3) 1.0162(2) 0.17774(10) 0.0281(7) Uani 1 1 d . . . C48 C 1.2197(3) 0.9518(2) 0.10555(11) 0.0320(7) Uani 1 1 d . . . H48 H 1.2524 0.9422 0.0720 0.038 Uiso 1 1 calc R . . C49 C 1.2538(3) 0.8910(2) 0.14455(10) 0.0290(7) Uani 1 1 d . . . C50 C 1.3427(2) 0.7959(2) 0.14689(10) 0.0296(7) Uani 1 1 d . . . C51 C 1.5025(3) 0.6714(2) 0.09943(11) 0.0348(7) Uani 1 1 d . . . H51A H 1.5086 0.6418 0.1324 0.042 Uiso 1 1 calc R . . H51B H 1.5742 0.6837 0.0842 0.042 Uiso 1 1 calc R . . C52 C 1.4814(3) 0.5992(2) 0.06858(11) 0.0373(8) Uani 1 1 d . . . H52A H 1.4672 0.6319 0.0370 0.045 Uiso 1 1 calc R . . H52B H 1.5498 0.5437 0.0616 0.045 Uiso 1 1 calc R . . C53 C 1.3835(3) 0.5595(2) 0.09254(12) 0.0407(8) Uani 1 1 d . . . H53A H 1.3147 0.6147 0.0996 0.049 Uiso 1 1 calc R . . H53B H 1.3976 0.5260 0.1240 0.049 Uiso 1 1 calc R . . C54 C 1.3651(3) 0.4878(3) 0.06016(13) 0.0458(9) Uani 1 1 d . . . H54A H 1.3378 0.5233 0.0317 0.069 Uiso 1 1 calc R . . H54B H 1.3104 0.4569 0.0790 0.069 Uiso 1 1 calc R . . H54C H 1.4357 0.4379 0.0493 0.069 Uiso 1 1 calc R . . O7 O 0.35192(17) 0.37270(15) 0.22205(7) 0.0318(5) Uani 1 1 d . . . O8 O 0.39315(17) 0.28705(15) 0.15297(7) 0.0341(5) Uani 1 1 d . . . N14 N 0.4973(2) -0.03572(18) 0.24879(9) 0.0324(6) Uani 1 1 d . . . H14A H 0.5077 -0.0911 0.2334 0.049 Uiso 1 1 calc R . . H14B H 0.5058 -0.0507 0.2801 0.049 Uiso 1 1 calc R . . H14C H 0.5481 -0.0054 0.2331 0.049 Uiso 1 1 calc R . . C55 C 0.3443(2) 0.3051(2) 0.19745(10) 0.0269(6) Uani 1 1 d . . . N13 N 0.2771(2) 0.24844(17) 0.22111(8) 0.0278(6) Uani 1 1 d . . . H13 H 0.2407 0.2626 0.2510 0.033 Uiso 1 1 calc R . . C57 C 0.2637(2) 0.1661(2) 0.19890(11) 0.0297(7) Uani 1 1 d . . . H57A H 0.2514 0.1858 0.1654 0.036 Uiso 1 1 calc R . . H57B H 0.1969 0.1498 0.2179 0.036 Uiso 1 1 calc R . . C58 C 0.3659(3) 0.0742(2) 0.19683(10) 0.0286(7) Uani 1 1 d . . . H58A H 0.3564 0.0244 0.1778 0.034 Uiso 1 1 calc R . . H58B H 0.4339 0.0913 0.1798 0.034 Uiso 1 1 calc R . . C59 C 0.3808(3) 0.0313(2) 0.24832(11) 0.0335(7) Uani 1 1 d . . . H59A H 0.3647 0.0852 0.2705 0.040 Uiso 1 1 calc R . . H59B H 0.3263 -0.0054 0.2609 0.040 Uiso 1 1 calc R . . O9 O 1.16426(17) 0.88839(14) 0.28996(7) 0.0316(5) Uani 1 1 d . . . O10 O 1.10357(17) 0.79434(15) 0.35368(7) 0.0327(5) Uani 1 1 d . . . N16 N 0.9736(2) 0.60915(17) 0.24847(9) 0.0313(6) Uani 1 1 d . . . H16A H 0.9524 0.5584 0.2650 0.047 Uiso 1 1 calc R . . H16B H 0.9663 0.6110 0.2170 0.047 Uiso 1 1 calc R . . H16C H 0.9299 0.6656 0.2626 0.047 Uiso 1 1 calc R . . C60 C 1.1570(2) 0.8055(2) 0.31020(10) 0.0280(7) Uani 1 1 d . . . N15 N 1.2132(2) 0.72345(17) 0.28312(9) 0.0297(6) Uani 1 1 d . . . H15 H 1.2469 0.7317 0.2530 0.036 Uiso 1 1 calc R . . C62 C 1.2200(2) 0.6236(2) 0.30171(11) 0.0299(7) Uani 1 1 d . . . H62A H 1.2338 0.6164 0.3353 0.036 Uiso 1 1 calc R . . H62B H 1.2839 0.5779 0.2812 0.036 Uiso 1 1 calc R . . C63 C 1.1127(3) 0.5961(2) 0.30201(10) 0.0316(7) Uani 1 1 d . . . H63A H 1.1188 0.5307 0.3176 0.038 Uiso 1 1 calc R . . H63B H 1.0481 0.6431 0.3214 0.038 Uiso 1 1 calc R . . C64 C 1.0937(3) 0.5965(2) 0.24997(12) 0.0368(8) Uani 1 1 d . . . H64A H 1.1175 0.6500 0.2304 0.044 Uiso 1 1 calc R . . H64B H 1.1407 0.5345 0.2349 0.044 Uiso 1 1 calc R . . O11 O 0.00259(19) 0.52597(16) 0.15209(8) 0.0389(5) Uani 1 1 d . . . O12 O -0.01734(19) 0.41398(15) 0.24631(8) 0.0400(5) Uani 1 1 d . . . O13 O -0.15940(19) 0.51471(15) 0.33035(8) 0.0383(5) Uani 1 1 d . . . O14 O -0.17719(17) 0.71825(15) 0.33467(8) 0.0351(5) Uani 1 1 d . . . O15 O -0.13556(18) 0.82412(15) 0.24328(8) 0.0354(5) Uani 1 1 d . . . O16 O 0.00367(19) 0.72200(16) 0.15746(8) 0.0412(6) Uani 1 1 d . . . C65 C 0.0630(3) 0.4241(2) 0.15939(13) 0.0445(8) Uani 1 1 d . . . H65A H 0.1339 0.4194 0.1690 0.053 Uiso 1 1 calc R . . H65B H 0.0807 0.3900 0.1285 0.053 Uiso 1 1 calc R . . C66 C -0.0063(3) 0.3757(2) 0.19879(13) 0.0422(8) Uani 1 1 d . . . H66A H -0.0810 0.3877 0.1913 0.051 Uiso 1 1 calc R . . H66B H 0.0297 0.3046 0.1995 0.051 Uiso 1 1 calc R . . C67 C -0.0812(3) 0.3671(2) 0.28462(13) 0.0427(8) Uani 1 1 d . . . H67A H -0.0418 0.2968 0.2869 0.051 Uiso 1 1 calc R . . H67B H -0.1548 0.3746 0.2770 0.051 Uiso 1 1 calc R . . C68 C -0.0962(3) 0.4130(2) 0.33258(13) 0.0438(9) Uani 1 1 d . . . H68A H -0.1357 0.3786 0.3592 0.053 Uiso 1 1 calc R . . H68B H -0.0224 0.4070 0.3397 0.053 Uiso 1 1 calc R . . C69 C -0.1744(3) 0.5628(3) 0.37535(11) 0.0396(8) Uani 1 1 d . . . H69A H -0.1011 0.5598 0.3819 0.048 Uiso 1 1 calc R . . H69B H -0.2129 0.5295 0.4029 0.048 Uiso 1 1 calc R . . C70 C -0.2430(3) 0.6677(3) 0.37048(12) 0.0405(8) Uani 1 1 d . . . H70A H -0.3123 0.6710 0.3598 0.049 Uiso 1 1 calc R . . H70B H -0.2634 0.6989 0.4023 0.049 Uiso 1 1 calc R . . C71 C -0.2369(3) 0.8192(2) 0.32656(12) 0.0360(7) Uani 1 1 d . . . H71A H -0.2616 0.8532 0.3577 0.043 Uiso 1 1 calc R . . H71B H -0.3036 0.8236 0.3134 0.043 Uiso 1 1 calc R . . C72 C -0.1604(3) 0.8667(2) 0.29054(12) 0.0363(7) Uani 1 1 d . . . H72A H -0.1968 0.9375 0.2877 0.044 Uiso 1 1 calc R . . H72B H -0.0906 0.8567 0.3022 0.044 Uiso 1 1 calc R . . C73 C -0.0547(3) 0.8609(2) 0.20865(12) 0.0384(8) Uani 1 1 d . . . H73A H 0.0183 0.8373 0.2186 0.046 Uiso 1 1 calc R . . H73B H -0.0787 0.9328 0.2085 0.046 Uiso 1 1 calc R . . C74 C -0.0433(3) 0.8274(2) 0.15818(12) 0.0404(8) Uani 1 1 d . . . H74A H -0.1171 0.8467 0.1491 0.049 Uiso 1 1 calc R . . H74B H 0.0059 0.8584 0.1343 0.049 Uiso 1 1 calc R . . C75 C 0.0072(3) 0.6817(3) 0.11195(12) 0.0481(9) Uani 1 1 d . . . H75A H 0.0474 0.7137 0.0844 0.058 Uiso 1 1 calc R . . H75B H -0.0692 0.6922 0.1069 0.058 Uiso 1 1 calc R . . C76 C 0.0669(3) 0.5740(3) 0.11472(12) 0.0475(9) Uani 1 1 d . . . H76A H 0.0778 0.5455 0.0828 0.057 Uiso 1 1 calc R . . H76B H 0.1411 0.5641 0.1223 0.057 Uiso 1 1 calc R . . O17 O 0.67515(19) 0.90540(16) 0.15539(7) 0.0371(5) Uani 1 1 d . . . O18 O 0.5818(2) 0.76620(16) 0.21285(9) 0.0430(6) Uani 1 1 d . . . O19 O 0.50668(18) 0.78023(17) 0.31891(8) 0.0417(6) Uani 1 1 d . . . O20 O 0.46359(19) 0.96665(17) 0.35533(8) 0.0412(6) Uani 1 1 d . . . O21 O 0.58093(18) 1.09316(15) 0.29774(8) 0.0384(5) Uani 1 1 d . . . O22 O 0.63214(18) 1.08953(15) 0.19147(8) 0.0368(5) Uani 1 1 d . . . C77 C 0.6608(3) 0.8242(3) 0.13412(13) 0.0475(9) Uani 1 1 d . . . H77A H 0.7178 0.8053 0.1040 0.057 Uiso 1 1 calc R . . H77B H 0.5863 0.8419 0.1258 0.057 Uiso 1 1 calc R . . C78 C 0.6734(3) 0.7406(2) 0.17204(13) 0.0470(9) Uani 1 1 d . . . H78A H 0.6737 0.6807 0.1577 0.056 Uiso 1 1 calc R . . H78B H 0.7446 0.7281 0.1829 0.056 Uiso 1 1 calc R . . C79 C 0.5737(3) 0.6850(2) 0.24661(15) 0.0513(9) Uani 1 1 d . . . H79A H 0.6441 0.6573 0.2586 0.062 Uiso 1 1 calc R . . H79B H 0.5613 0.6335 0.2298 0.062 Uiso 1 1 calc R . . C80 C 0.4783(3) 0.7193(3) 0.28909(14) 0.0482(9) Uani 1 1 d . . . H80A H 0.4104 0.7565 0.2769 0.058 Uiso 1 1 calc R . . H80B H 0.4630 0.6625 0.3089 0.058 Uiso 1 1 calc R . . C81 C 0.4179(3) 0.8166(3) 0.36027(13) 0.0498(10) Uani 1 1 d . . . H81A H 0.4038 0.7618 0.3821 0.060 Uiso 1 1 calc R . . H81B H 0.3484 0.8526 0.3489 0.060 Uiso 1 1 calc R . . C82 C 0.4534(3) 0.8835(3) 0.38731(12) 0.0478(9) Uani 1 1 d . . . H82A H 0.3973 0.9051 0.4174 0.057 Uiso 1 1 calc R . . H82B H 0.5256 0.8488 0.3966 0.057 Uiso 1 1 calc R . . C83 C 0.5026(3) 1.0340(3) 0.37697(12) 0.0444(9) Uani 1 1 d . . . H83A H 0.5791 1.0018 0.3823 0.053 Uiso 1 1 calc R . . H83B H 0.4537 1.0542 0.4089 0.053 Uiso 1 1 calc R . . C84 C 0.5013(3) 1.1221(3) 0.34298(12) 0.0431(8) Uani 1 1 d . . . H84A H 0.4258 1.1517 0.3360 0.052 Uiso 1 1 calc R . . H84B H 0.5209 1.1711 0.3586 0.052 Uiso 1 1 calc R . . C85 C 0.5893(3) 1.1776(2) 0.26591(13) 0.0394(8) Uani 1 1 d . . . H85A H 0.6130 1.2224 0.2826 0.047 Uiso 1 1 calc R . . H85B H 0.5157 1.2129 0.2581 0.047 Uiso 1 1 calc R . . C86 C 0.6729(3) 1.1450(2) 0.21940(13) 0.0388(8) Uani 1 1 d . . . H86A H 0.6861 1.2025 0.1997 0.047 Uiso 1 1 calc R . . H86B H 0.7446 1.1044 0.2274 0.047 Uiso 1 1 calc R . . C87 C 0.7091(3) 1.0598(2) 0.14586(12) 0.0418(8) Uani 1 1 d . . . H87A H 0.7850 1.0283 0.1521 0.050 Uiso 1 1 calc R . . H87B H 0.7110 1.1176 0.1239 0.050 Uiso 1 1 calc R . . C88 C 0.6723(3) 0.9894(2) 0.12196(12) 0.0413(8) Uani 1 1 d . . . H88A H 0.5960 1.0199 0.1160 0.050 Uiso 1 1 calc R . . H88B H 0.7230 0.9696 0.0904 0.050 Uiso 1 1 calc R . . C89 C 0.8914(4) 0.0427(5) 0.0141(2) 0.111(2) Uani 1 1 d . . . H89A H 0.8946 0.0389 -0.0208 0.166 Uiso 1 1 calc R . . H89B H 0.8969 0.1063 0.0204 0.166 Uiso 1 1 calc R . . H89C H 0.8208 0.0346 0.0327 0.166 Uiso 1 1 calc R . . S1 S 0.99520(19) -0.04346(15) 0.03062(7) 0.0539(5) Uani 0.50 1 d P . . O23 O 0.9687(6) -0.1331(4) 0.0209(2) 0.0785(19) Uani 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 O1 0.0360(14) 0.0669(15) 0.0236(11) -0.0082(10) 0.0008(9) -0.0229(12) O2 0.0296(14) 0.0523(14) 0.0353(12) 0.0006(10) -0.0060(10) -0.0161(11) O3 0.0421(14) 0.0463(13) 0.0242(11) -0.0038(9) 0.0005(10) -0.0086(11) N1 0.0320(16) 0.0408(14) 0.0265(13) -0.0001(10) -0.0029(11) -0.0152(12) N2 0.0241(14) 0.0296(13) 0.0233(12) -0.0014(9) -0.0029(10) -0.0053(11) N3 0.0199(14) 0.0341(13) 0.0305(13) 0.0021(10) -0.0079(10) -0.0076(11) N4 0.0233(15) 0.0398(14) 0.0288(13) -0.0007(10) -0.0024(11) -0.0091(12) N5 0.0264(15) 0.0359(13) 0.0217(12) 0.0025(10) -0.0020(10) -0.0081(11) N6 0.0358(16) 0.0401(14) 0.0211(12) -0.0034(10) -0.0033(11) -0.0133(12) C1 0.042(2) 0.045(2) 0.052(2) 0.0062(15) -0.0080(17) -0.0205(17) C2 0.036(2) 0.050(2) 0.0355(17) 0.0043(14) -0.0037(15) -0.0208(16) C3 0.0265(18) 0.0484(19) 0.0281(15) 0.0031(13) -0.0062(13) -0.0177(15) C4 0.0258(19) 0.0493(19) 0.0332(16) -0.0039(13) -0.0032(13) -0.0154(15) C5 0.0214(17) 0.0304(15) 0.0276(16) -0.0012(11) -0.0006(12) -0.0026(13) C6 0.0215(17) 0.0236(14) 0.0282(15) -0.0001(11) 0.0013(12) -0.0017(12) C7 0.0316(18) 0.0299(15) 0.0209(14) -0.0001(11) -0.0008(12) -0.0057(13) C8 0.0265(18) 0.0249(14) 0.0283(15) -0.0035(11) -0.0056(12) -0.0031(13) C9 0.035(2) 0.0350(16) 0.0317(16) -0.0025(12) -0.0085(14) -0.0076(15) C10 0.034(2) 0.0386(17) 0.0395(18) -0.0019(13) -0.0120(15) -0.0132(15) C11 0.0312(19) 0.0366(17) 0.0319(16) 0.0013(12) -0.0046(13) -0.0119(14) C12 0.0280(18) 0.0250(14) 0.0287(15) 0.0000(11) -0.0053(13) -0.0083(13) C13 0.0228(17) 0.0242(14) 0.0302(15) -0.0030(11) -0.0048(12) -0.0034(12) C14 0.0242(19) 0.0258(15) 0.0297(15) 0.0015(11) -0.0027(13) -0.0059(13) C15 0.0266(18) 0.0298(15) 0.0276(15) 0.0049(12) -0.0043(13) -0.0022(13) C16 0.0282(18) 0.0319(16) 0.0347(16) 0.0099(12) -0.0088(13) -0.0092(14) C17 0.0303(19) 0.0483(19) 0.0385(18) 0.0127(14) -0.0041(14) -0.0172(16) C18 0.031(2) 0.057(2) 0.0305(17) 0.0107(14) -0.0030(14) -0.0159(16) C19 0.0284(19) 0.0441(18) 0.0260(15) 0.0089(13) -0.0059(13) -0.0097(15) C20 0.0234(18) 0.0339(16) 0.0274(15) 0.0059(12) -0.0043(13) -0.0048(13) C21 0.033(2) 0.0510(19) 0.0222(15) 0.0013(13) -0.0015(13) -0.0093(15) C22 0.0313(19) 0.0361(16) 0.0215(14) 0.0026(11) -0.0051(13) -0.0064(14) C23 0.0323(19) 0.0371(16) 0.0203(14) 0.0028(12) -0.0037(13) -0.0042(14) C24 0.048(2) 0.0403(18) 0.0269(16) -0.0028(13) -0.0044(14) -0.0158(16) C25 0.040(2) 0.0448(18) 0.0286(16) -0.0049(13) -0.0019(14) -0.0174(16) C26 0.040(2) 0.0461(19) 0.0408(19) -0.0086(14) -0.0073(16) -0.0139(16) C27 0.040(2) 0.060(2) 0.056(2) -0.0046(18) -0.0066(18) -0.0123(19) O4 0.0409(14) 0.0396(12) 0.0263(11) 0.0032(9) 0.0015(9) -0.0149(10) O5 0.0326(14) 0.0344(12) 0.0340(12) 0.0016(9) -0.0045(10) -0.0036(11) O6 0.0359(14) 0.0477(13) 0.0269(11) 0.0046(9) -0.0024(10) -0.0054(11) N7 0.0325(15) 0.0321(13) 0.0217(12) 0.0026(10) -0.0016(11) -0.0083(11) N8 0.0260(14) 0.0314(13) 0.0206(11) -0.0029(9) -0.0029(10) -0.0064(11) N9 0.0240(15) 0.0327(13) 0.0310(13) 0.0006(10) -0.0062(11) -0.0058(11) N10 0.0252(15) 0.0305(13) 0.0310(13) 0.0008(10) -0.0063(11) -0.0071(11) N11 0.0280(15) 0.0304(13) 0.0218(12) 0.0010(9) -0.0040(10) -0.0115(11) N12 0.0314(16) 0.0383(14) 0.0264(13) 0.0002(10) -0.0022(11) -0.0065(12) C28 0.059(3) 0.065(3) 0.066(3) -0.010(2) -0.027(2) -0.017(2) C29 0.044(2) 0.0421(19) 0.047(2) 0.0004(15) -0.0168(17) -0.0112(16) C30 0.042(2) 0.0306(16) 0.0245(15) 0.0026(11) -0.0088(14) -0.0022(14) C31 0.038(2) 0.0293(15) 0.0272(15) 0.0024(12) -0.0050(13) -0.0088(14) C32 0.0328(19) 0.0361(16) 0.0208(14) 0.0005(12) -0.0054(13) -0.0143(14) C33 0.0300(18) 0.0352(16) 0.0217(14) -0.0035(11) -0.0017(12) -0.0107(14) C34 0.0295(19) 0.0403(17) 0.0254(15) -0.0008(12) -0.0030(13) -0.0087(14) C35 0.0282(18) 0.0379(17) 0.0242(15) -0.0071(12) -0.0044(13) -0.0075(14) C36 0.0290(19) 0.0474(19) 0.0253(15) -0.0073(13) -0.0006(13) -0.0032(15) C37 0.034(2) 0.0397(18) 0.0307(16) -0.0135(13) -0.0044(14) -0.0007(15) C38 0.043(2) 0.0301(16) 0.0288(16) -0.0043(12) -0.0106(14) -0.0085(15) C39 0.0325(18) 0.0303(15) 0.0222(14) -0.0081(11) -0.0030(12) -0.0087(13) C40 0.0269(18) 0.0291(15) 0.0250(14) -0.0077(11) -0.0068(12) -0.0041(13) C41 0.0286(19) 0.0288(16) 0.0305(15) -0.0038(12) -0.0065(13) -0.0135(15) C42 0.0283(18) 0.0286(15) 0.0300(15) 0.0025(11) -0.0063(13) -0.0163(13) C43 0.0309(19) 0.0269(15) 0.0339(16) 0.0000(12) -0.0046(13) -0.0139(14) C44 0.038(2) 0.0314(16) 0.0362(17) 0.0057(13) -0.0070(15) -0.0112(14) C45 0.042(2) 0.0414(18) 0.0294(16) 0.0060(13) -0.0084(14) -0.0185(16) C46 0.0352(19) 0.0298(15) 0.0270(15) 0.0024(11) -0.0052(13) -0.0156(14) C47 0.0265(18) 0.0311(16) 0.0291(15) 0.0022(12) -0.0049(13) -0.0132(14) C48 0.0339(19) 0.0359(16) 0.0287(15) 0.0001(12) -0.0041(13) -0.0160(14) C49 0.0273(18) 0.0370(16) 0.0244(14) 0.0003(12) -0.0019(12) -0.0146(14) C50 0.0224(18) 0.0400(17) 0.0262(15) 0.0011(12) -0.0025(12) -0.0113(14) C51 0.0255(19) 0.0430(18) 0.0307(16) -0.0022(13) -0.0027(13) -0.0041(14) C52 0.034(2) 0.0388(18) 0.0298(16) -0.0016(13) -0.0045(14) 0.0015(15) C53 0.040(2) 0.0368(17) 0.0407(18) -0.0050(14) -0.0071(15) -0.0044(15) C54 0.045(2) 0.0394(19) 0.047(2) -0.0064(15) -0.0134(17) -0.0001(16) O7 0.0324(13) 0.0348(11) 0.0310(11) -0.0031(8) -0.0058(9) -0.0137(10) O8 0.0328(13) 0.0449(12) 0.0247(11) -0.0024(9) 0.0016(9) -0.0164(10) N14 0.0340(16) 0.0318(13) 0.0310(13) 0.0001(10) -0.0096(11) -0.0074(12) C55 0.0229(17) 0.0334(16) 0.0236(15) 0.0012(11) -0.0057(12) -0.0072(13) N13 0.0291(15) 0.0338(13) 0.0205(12) -0.0036(9) 0.0019(10) -0.0133(11) C57 0.0242(18) 0.0354(16) 0.0292(15) -0.0008(12) -0.0047(13) -0.0090(14) C58 0.0305(18) 0.0349(16) 0.0230(14) 0.0008(11) -0.0066(12) -0.0132(14) C59 0.0289(19) 0.0361(16) 0.0341(16) 0.0016(13) -0.0058(14) -0.0088(14) O9 0.0370(13) 0.0297(11) 0.0273(10) 0.0010(8) -0.0063(9) -0.0092(9) O10 0.0301(13) 0.0379(12) 0.0245(10) 0.0011(8) -0.0005(9) -0.0062(10) N16 0.0386(17) 0.0285(13) 0.0302(13) -0.0006(10) -0.0103(11) -0.0125(12) C60 0.0216(17) 0.0343(16) 0.0289(15) 0.0023(12) -0.0077(13) -0.0086(13) N15 0.0285(15) 0.0328(13) 0.0243(12) -0.0022(10) 0.0009(10) -0.0081(11) C62 0.0257(18) 0.0305(15) 0.0307(15) 0.0003(12) -0.0053(13) -0.0048(13) C63 0.0341(19) 0.0301(15) 0.0296(15) 0.0028(12) -0.0058(13) -0.0096(14) C64 0.0258(19) 0.0441(18) 0.0389(18) -0.0066(14) -0.0070(14) -0.0059(15) O11 0.0383(14) 0.0378(12) 0.0375(12) -0.0065(9) -0.0059(10) -0.0063(10) O12 0.0424(14) 0.0348(12) 0.0499(13) 0.0017(10) -0.0164(11) -0.0174(11) O13 0.0396(14) 0.0365(12) 0.0419(13) 0.0076(9) -0.0155(10) -0.0133(10) O14 0.0286(13) 0.0355(12) 0.0399(12) 0.0000(9) -0.0036(10) -0.0101(10) O15 0.0348(13) 0.0342(11) 0.0403(12) -0.0030(9) -0.0056(10) -0.0155(10) O16 0.0457(15) 0.0388(12) 0.0355(12) 0.0038(9) -0.0077(10) -0.0090(11) C65 0.040(2) 0.0398(19) 0.052(2) -0.0150(15) -0.0136(17) -0.0018(16) C66 0.043(2) 0.0292(16) 0.058(2) -0.0112(14) -0.0197(17) -0.0057(15) C67 0.040(2) 0.0283(16) 0.064(2) 0.0095(15) -0.0184(17) -0.0145(15) C68 0.037(2) 0.0379(18) 0.059(2) 0.0167(16) -0.0208(17) -0.0127(16) C69 0.038(2) 0.055(2) 0.0312(17) 0.0070(14) -0.0102(14) -0.0217(17) C70 0.034(2) 0.056(2) 0.0353(17) -0.0033(14) -0.0053(15) -0.0189(17) C71 0.0291(19) 0.0331(17) 0.0433(18) -0.0129(13) -0.0078(14) -0.0015(14) C72 0.036(2) 0.0287(16) 0.0453(19) -0.0061(13) -0.0138(15) -0.0055(14) C73 0.037(2) 0.0333(17) 0.0500(19) 0.0038(14) -0.0113(16) -0.0167(15) C74 0.038(2) 0.0323(17) 0.048(2) 0.0103(14) -0.0089(16) -0.0099(15) C75 0.055(2) 0.052(2) 0.0324(18) 0.0002(15) -0.0028(16) -0.0130(18) C76 0.048(2) 0.057(2) 0.0335(18) -0.0062(15) 0.0008(16) -0.0146(18) O17 0.0426(14) 0.0392(12) 0.0294(11) -0.0014(9) -0.0086(10) -0.0108(10) O18 0.0430(15) 0.0318(12) 0.0553(14) -0.0023(10) -0.0118(12) -0.0112(11) O19 0.0310(14) 0.0461(13) 0.0500(14) 0.0076(10) -0.0099(11) -0.0160(11) O20 0.0405(14) 0.0471(13) 0.0327(12) -0.0002(9) -0.0086(10) -0.0077(11) O21 0.0369(14) 0.0328(12) 0.0429(13) -0.0090(9) -0.0085(10) -0.0038(10) O22 0.0295(13) 0.0375(12) 0.0423(12) 0.0000(9) -0.0058(10) -0.0097(10) C77 0.049(2) 0.048(2) 0.047(2) -0.0164(16) -0.0127(17) -0.0089(18) C78 0.053(2) 0.0336(18) 0.053(2) -0.0160(15) -0.0108(18) -0.0068(17) C79 0.060(3) 0.0315(18) 0.068(2) 0.0012(16) -0.021(2) -0.0167(18) C80 0.053(2) 0.0402(19) 0.065(2) 0.0120(16) -0.0251(19) -0.0293(18) C81 0.033(2) 0.066(2) 0.048(2) 0.0163(17) -0.0046(17) -0.0198(18) C82 0.038(2) 0.065(2) 0.0352(18) 0.0090(16) -0.0048(16) -0.0138(18) C83 0.042(2) 0.050(2) 0.0359(18) -0.0146(15) -0.0093(16) -0.0006(17) C84 0.040(2) 0.0442(19) 0.0415(19) -0.0145(15) -0.0120(16) -0.0002(16) C85 0.035(2) 0.0277(16) 0.056(2) -0.0085(14) -0.0130(16) -0.0060(14) C86 0.032(2) 0.0273(16) 0.058(2) 0.0048(14) -0.0123(16) -0.0099(14) C87 0.039(2) 0.0413(18) 0.0379(18) 0.0076(14) -0.0006(15) -0.0086(16) C88 0.039(2) 0.0448(19) 0.0336(17) 0.0054(14) -0.0087(15) -0.0042(16) C89 0.063(4) 0.141(6) 0.105(4) -0.023(4) 0.005(3) -0.006(4) S1 0.0686(14) 0.0519(11) 0.0432(10) 0.0052(8) -0.0139(9) -0.0207(10) O23 0.132(6) 0.061(4) 0.059(4) 0.009(3) -0.026(4) -0.052(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C5 1.236(4) . ? O2 C14 1.212(4) . ? O3 C23 1.242(4) . ? N1 C5 1.340(3) . ? N1 C4 1.455(4) . ? N2 C13 1.369(4) . ? N2 C6 1.375(3) . ? N3 C14 1.362(4) . ? N3 C12 1.403(4) . ? N4 C14 1.379(4) . ? N4 C15 1.402(4) . ? N5 C20 1.364(4) . ? N5 C22 1.383(4) . ? N6 C23 1.335(4) . ? N6 C24 1.449(4) . ? C1 C2 1.527(4) . ? C2 C3 1.518(5) . ? C3 C4 1.513(4) . ? C5 C6 1.471(4) . ? C6 C7 1.366(4) . ? C7 C8 1.422(4) . ? C8 C9 1.401(4) . ? C8 C13 1.411(4) . ? C9 C10 1.371(4) . ? C10 C11 1.413(4) . ? C11 C12 1.371(4) . ? C12 C13 1.402(4) . ? C15 C16 1.386(4) . ? C15 C20 1.398(4) . ? C16 C17 1.400(4) . ? C17 C18 1.365(5) . ? C18 C19 1.401(4) . ? C19 C20 1.409(4) . ? C19 C21 1.411(5) . ? C21 C22 1.364(4) . ? C22 C23 1.466(4) . ? C24 C25 1.522(5) . ? C25 C26 1.520(5) . ? C26 C27 1.509(5) . ? O4 C32 1.239(3) . ? O5 C41 1.214(4) . ? O6 C50 1.237(3) . ? N7 C32 1.325(4) . ? N7 C31 1.457(4) . ? N8 C40 1.366(4) . ? N8 C33 1.377(3) . ? N9 C41 1.388(4) . ? N9 C39 1.410(4) . ? N10 C41 1.363(4) . ? N10 C42 1.412(4) . ? N11 C47 1.367(4) . ? N11 C49 1.373(4) . ? N12 C50 1.334(4) . ? N12 C51 1.452(4) . ? C28 C29 1.519(5) . ? C29 C30 1.506(4) . ? C30 C31 1.522(4) . ? C32 C33 1.478(4) . ? C33 C34 1.370(4) . ? C34 C35 1.415(4) . ? C35 C36 1.399(4) . ? C35 C40 1.416(4) . ? C36 C37 1.370(4) . ? C37 C38 1.404(4) . ? C38 C39 1.376(4) . ? C39 C40 1.402(4) . ? C42 C43 1.366(4) . ? C42 C47 1.405(4) . ? C43 C44 1.407(4) . ? C44 C45 1.361(4) . ? C45 C46 1.398(4) . ? C46 C47 1.417(4) . ? C46 C48 1.421(4) . ? C48 C49 1.369(4) . ? C49 C50 1.471(4) . ? C51 C52 1.511(5) . ? C52 C53 1.507(5) . ? C53 C54 1.517(5) . ? O7 C55 1.266(3) . ? O8 C55 1.258(3) . ? N14 C59 1.488(4) . ? C55 N13 1.362(3) . ? N13 C57 1.440(4) . ? C57 C58 1.522(4) . ? C58 C59 1.514(4) . ? O9 C60 1.268(3) . ? O10 C60 1.260(3) . ? N16 C64 1.481(4) . ? C60 N15 1.359(4) . ? N15 C62 1.438(4) . ? C62 C63 1.518(4) . ? C63 C64 1.505(4) . ? O11 C76 1.419(4) . ? O11 C65 1.428(4) . ? O12 C67 1.420(4) . ? O12 C66 1.430(4) . ? O13 C68 1.420(4) . ? O13 C69 1.423(4) . ? O14 C71 1.418(4) . ? O14 C70 1.427(4) . ? O15 C73 1.421(4) . ? O15 C72 1.421(4) . ? O16 C75 1.416(4) . ? O16 C74 1.428(4) . ? C65 C66 1.487(5) . ? C67 C68 1.481(5) . ? C69 C70 1.483(5) . ? C71 C72 1.487(4) . ? C73 C74 1.478(5) . ? C75 C76 1.482(5) . ? O17 C77 1.418(4) . ? O17 C88 1.425(4) . ? O18 C78 1.409(4) . ? O18 C79 1.419(4) . ? O19 C80 1.419(4) . ? O19 C81 1.422(4) . ? O20 C82 1.420(4) . ? O20 C83 1.429(4) . ? O21 C84 1.425(4) . ? O21 C85 1.427(4) . ? O22 C87 1.421(4) . ? O22 C86 1.421(4) . ? C77 C78 1.493(5) . ? C79 C80 1.480(5) . ? C81 C82 1.485(5) . ? C83 C84 1.480(5) . ? C85 C86 1.481(5) . ? C87 C88 1.483(5) . ? C89 S1 1.608(6) . ? S1 O23 1.471(6) . ? S1 C89 1.672(6) 2_755 ? 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 C5 N1 C4 122.9(3) . . ? C13 N2 C6 108.7(2) . . ? C14 N3 C12 125.9(3) . . ? C14 N4 C15 124.6(3) . . ? C20 N5 C22 108.4(2) . . ? C23 N6 C24 121.2(3) . . ? C3 C2 C1 111.6(3) . . ? C2 C3 C4 114.5(2) . . ? N1 C4 C3 113.7(3) . . ? O1 C5 N1 122.6(3) . . ? O1 C5 C6 121.0(2) . . ? N1 C5 C6 116.3(3) . . ? C7 C6 N2 109.5(3) . . ? C7 C6 C5 132.3(2) . . ? N2 C6 C5 118.0(3) . . ? C6 C7 C8 107.2(2) . . ? C9 C8 C13 119.2(3) . . ? C9 C8 C7 134.2(3) . . ? C13 C8 C7 106.6(3) . . ? C10 C9 C8 118.4(3) . . ? C9 C10 C11 121.8(3) . . ? C12 C11 C10 121.1(3) . . ? C11 C12 C13 117.2(3) . . ? C11 C12 N3 125.5(3) . . ? C13 C12 N3 117.3(3) . . ? N2 C13 C12 129.8(3) . . ? N2 C13 C8 107.9(2) . . ? C12 C13 C8 122.3(3) . . ? O2 C14 N3 124.4(3) . . ? O2 C14 N4 124.0(3) . . ? N3 C14 N4 111.6(3) . . ? C16 C15 C20 116.6(3) . . ? C16 C15 N4 124.4(3) . . ? C20 C15 N4 119.0(3) . . ? C15 C16 C17 121.2(3) . . ? C18 C17 C16 122.0(3) . . ? C17 C18 C19 118.5(3) . . ? C18 C19 C20 119.2(3) . . ? C18 C19 C21 134.9(3) . . ? C20 C19 C21 105.9(3) . . ? N5 C20 C15 128.9(3) . . ? N5 C20 C19 108.6(3) . . ? C15 C20 C19 122.5(3) . . ? C22 C21 C19 108.4(3) . . ? C21 C22 N5 108.7(3) . . ? C21 C22 C23 126.8(3) . . ? N5 C22 C23 124.5(2) . . ? O3 C23 N6 121.4(3) . . ? O3 C23 C22 120.0(3) . . ? N6 C23 C22 118.7(3) . . ? N6 C24 C25 113.1(3) . . ? C24 C25 C26 113.5(3) . . ? C27 C26 C25 113.0(3) . . ? C32 N7 C31 121.4(2) . . ? C40 N8 C33 108.8(2) . . ? C41 N9 C39 123.7(3) . . ? C41 N10 C42 125.9(3) . . ? C47 N11 C49 109.0(2) . . ? C50 N12 C51 123.2(3) . . ? C30 C29 C28 112.9(3) . . ? C29 C30 C31 113.6(2) . . ? N7 C31 C30 111.9(2) . . ? O4 C32 N7 122.2(3) . . ? O4 C32 C33 118.9(3) . . ? N7 C32 C33 118.8(2) . . ? C34 C33 N8 109.0(3) . . ? C34 C33 C32 126.9(3) . . ? N8 C33 C32 124.1(3) . . ? C33 C34 C35 107.8(3) . . ? C36 C35 C34 134.7(3) . . ? C36 C35 C40 119.0(3) . . ? C34 C35 C40 106.2(3) . . ? C37 C36 C35 118.3(3) . . ? C36 C37 C38 122.2(3) . . ? C39 C38 C37 121.3(3) . . ? C38 C39 C40 116.7(3) . . ? C38 C39 N9 124.7(3) . . ? C40 C39 N9 118.6(3) . . ? N8 C40 C39 129.4(3) . . ? N8 C40 C35 108.1(2) . . ? C39 C40 C35 122.5(3) . . ? O5 C41 N10 125.3(3) . . ? O5 C41 N9 122.8(3) . . ? N10 C41 N9 111.9(3) . . ? C43 C42 C47 117.2(3) . . ? C43 C42 N10 126.0(3) . . ? C47 C42 N10 116.8(3) . . ? C42 C43 C44 121.4(3) . . ? C45 C44 C43 122.0(3) . . ? C44 C45 C46 118.6(3) . . ? C45 C46 C47 119.2(3) . . ? C45 C46 C48 134.9(3) . . ? C47 C46 C48 105.9(3) . . ? N11 C47 C42 130.1(3) . . ? N11 C47 C46 108.2(2) . . ? C42 C47 C46 121.7(3) . . ? C49 C48 C46 107.9(3) . . ? C48 C49 N11 109.1(3) . . ? C48 C49 C50 132.4(3) . . ? N11 C49 C50 118.4(2) . . ? O6 C50 N12 123.1(3) . . ? O6 C50 C49 120.7(3) . . ? N12 C50 C49 116.2(2) . . ? N12 C51 C52 112.5(3) . . ? C53 C52 C51 114.7(3) . . ? C52 C53 C54 112.8(3) . . ? O8 C55 O7 124.9(3) . . ? O8 C55 N13 117.9(3) . . ? O7 C55 N13 117.1(2) . . ? C55 N13 C57 123.7(2) . . ? N13 C57 C58 113.0(2) . . ? C59 C58 C57 111.8(2) . . ? N14 C59 C58 112.6(2) . . ? O10 C60 O9 124.5(3) . . ? O10 C60 N15 118.3(2) . . ? O9 C60 N15 117.1(2) . . ? C60 N15 C62 124.1(2) . . ? N15 C62 C63 112.7(2) . . ? C64 C63 C62 111.1(2) . . ? N16 C64 C63 112.8(2) . . ? C76 O11 C65 111.6(3) . . ? C67 O12 C66 111.2(2) . . ? C68 O13 C69 112.3(2) . . ? C71 O14 C70 112.7(2) . . ? C73 O15 C72 111.5(2) . . ? C75 O16 C74 113.5(2) . . ? O11 C65 C66 110.4(3) . . ? O12 C66 C65 110.3(3) . . ? O12 C67 C68 109.3(3) . . ? O13 C68 C67 110.0(3) . . ? O13 C69 C70 109.0(3) . . ? O14 C70 C69 108.5(3) . . ? O14 C71 C72 108.9(2) . . ? O15 C72 C71 109.4(3) . . ? O15 C73 C74 110.4(3) . . ? O16 C74 C73 109.3(3) . . ? O16 C75 C76 107.6(3) . . ? O11 C76 C75 110.1(3) . . ? C77 O17 C88 113.2(3) . . ? C78 O18 C79 113.1(3) . . ? C80 O19 C81 112.4(3) . . ? C82 O20 C83 112.8(3) . . ? C84 O21 C85 111.0(2) . . ? C87 O22 C86 111.5(2) . . ? O17 C77 C78 107.0(3) . . ? O18 C78 C77 108.8(3) . . ? O18 C79 C80 109.5(3) . . ? O19 C80 C79 109.5(3) . . ? O19 C81 C82 108.1(3) . . ? O20 C82 C81 108.1(3) . . ? O20 C83 C84 109.0(3) . . ? O21 C84 C83 109.6(3) . . ? O21 C85 C86 109.6(2) . . ? O22 C86 C85 110.2(3) . . ? O22 C87 C88 109.4(3) . . ? O17 C88 C87 106.7(3) . . ? O23 S1 C89 101.4(4) . . ? O23 S1 C89 103.1(4) . 2_755 ? C89 S1 C89 105.3(2) . 2_755 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N13 H13 O1 0.86 2.01 2.860(3) 168.7 . N15 H15 O6 0.86 2.03 2.885(3) 170.1 . N2 H2 O7 0.86 2.04 2.866(4) 159.8 . N3 H3 O7 0.86 2.01 2.782(3) 148.2 . N4 H4 O7 0.86 2.43 3.163(3) 143.5 . N5 H5 O8 0.86 1.84 2.677(3) 163.2 . N6 H6 O8 0.86 1.98 2.840(3) 174.7 . N7 H7A O10 0.86 2.01 2.846(3) 164.7 . N8 H8 O10 0.86 1.84 2.688(3) 167.5 . N9 H9A O9 0.86 2.62 3.291(3) 135.6 . N10 H10A O9 0.86 1.95 2.767(3) 158.7 . N11 H11A O9 0.86 1.95 2.775(3) 160.6 . N1 H1 O4 0.86 2.05 2.893(4) 167.1 2_666 N12 H12 O3 0.86 2.08 2.916(4) 165.4 2_765 N14 H14A O18 0.89 2.03 2.872(4) 157.6 1_545 N14 H14B O20 0.89 2.04 2.875(4) 154.9 1_545 N14 H14B O19 0.89 2.52 3.073(4) 120.9 1_545 N14 H14C O22 0.89 2.07 2.940(3) 166.1 1_545 N14 H14C O17 0.89 2.56 3.016(3) 112.7 1_545 N16 H16A O12 0.89 2.06 2.738(4) 132.1 1_655 N16 H16A O13 0.89 2.19 2.966(3) 144.8 1_655 N16 H16B O11 0.89 2.14 2.919(4) 145.2 1_655 N16 H16B O16 0.89 2.23 2.852(3) 126.5 1_655 N16 H16C O15 0.89 2.20 2.935(4) 140.1 1_655 N16 H16C O14 0.89 2.20 2.932(3) 139.6 1_655 _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 24.21 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 0.283 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.064