# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 _publ_contact_author_name 'Colin L. Raston' _publ_contact_author_address ; Department of Chemistry University of Western Australia Crawley Perth WA6909 Australia ; _publ_contact_author_phone '+44 (0)113 2336555' _publ_contact_author_fax '+44 (0)113 2336401' _publ_contact_author_email clraston@chem.uwa.edu.au _publ_requested_journal 'Chem. Comm.' _publ_section_title ; Conformation perturbation of p-sulfonatocalix[5]arene via complexation of 1,4-diazabicyclo[2.2.2]octane ; loop_ _publ_author_name _publ_author_address 'Colin L. Raston' ; Department of Chemistry University of Western Australia Crawley Perth WA6909 Australia ; 'Scott J. Dalgarno' ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Michaele J. Hardie' ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; #================================================================= data_dabcocalix5 _database_code_depnum_ccdc_archive 'CCDC 244468' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[{(DABCO+2H+)}Ì (p-sulfonatocalix[5]arene+H+)][DABCO+2H+].H2O9.25' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H74.50 N5 O29.25 S5' _chemical_formula_weight 1373.95 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 12.7511(2) _cell_length_b 15.9188(3) _cell_length_c 16.7800(4) _cell_angle_alpha 85.7950(10) _cell_angle_beta 79.5540(10) _cell_angle_gamma 74.4390(10) _cell_volume 3225.72(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.593 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68394 _diffrn_reflns_av_R_equivalents 0.0941 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _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 2.66 _diffrn_reflns_theta_max 27.34 _reflns_number_total 14404 _reflns_number_gt 9211 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; XSeed (Barbour, 2001) ; _computing_publication_material 'local program' _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^)+(0.1000P)^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 0.0025(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14404 _refine_ls_number_parameters 913 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1426 _refine_ls_R_factor_gt 0.0977 _refine_ls_wR_factor_ref 0.2862 _refine_ls_wR_factor_gt 0.2649 _refine_ls_goodness_of_fit_ref 1.751 _refine_ls_restrained_S_all 1.756 _refine_ls_shift/su_max 0.010 _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 S1 S 0.96077(9) 0.12345(7) 0.19907(6) 0.0319(3) Uani 1 1 d . . . O1 O 0.9569(3) 0.0790(2) 0.27826(19) 0.0433(8) Uani 1 1 d . . . N1 N 0.8458(10) 0.3804(9) 0.3657(7) 0.122(4) Uiso 0.75 1 d PD A 1 C1 C 1.0821(3) -0.0954(3) 0.0680(3) 0.0298(9) Uani 1 1 d . . . S2 S 1.19092(10) 0.28180(7) -0.22503(7) 0.0394(3) Uani 1 1 d . . . O2 O 0.8515(2) 0.1513(2) 0.17617(19) 0.0391(7) Uani 1 1 d . . . N2 N 0.8301(9) 0.2465(7) 0.4501(6) 0.111(3) Uiso 0.75 1 d P . . C2 C 1.0161(3) -0.0320(3) 0.1211(3) 0.0305(9) Uani 1 1 d . . . H2 H 0.9509 -0.0417 0.1533 0.037 Uiso 1 1 calc R . . S3 S 1.62111(10) -0.25447(8) -0.01207(7) 0.0412(3) Uani 1 1 d . . . O3 O 1.0150(3) 0.1938(2) 0.1945(2) 0.0432(8) Uani 1 1 d . . . N3 N 0.9429(6) 0.5067(5) 0.0987(5) 0.0362(17) Uani 0.50 1 d PD . . C3 C 1.0442(3) 0.0459(3) 0.1279(2) 0.0282(9) Uani 1 1 d . . . S4 S 1.71881(11) -0.09344(9) -0.45992(7) 0.0462(3) Uani 1 1 d . . . O4 O 1.2428(2) -0.14417(18) -0.02723(18) 0.0335(7) Uani 1 1 d . . . H57 H 1.2991 -0.1295 -0.0516 0.040 Uiso 1 1 calc R . . N4 N 0.9305(7) 0.5938(5) 0.0035(5) 0.0392(18) Uani 0.50 1 d PD . . C4 C 1.1381(3) 0.0614(3) 0.0808(3) 0.0316(9) Uani 1 1 d . . . H4 H 1.1563 0.1147 0.0857 0.038 Uiso 1 1 calc R . . S5 S 1.20927(11) -0.41196(8) 0.27472(8) 0.0486(4) Uani 1 1 d . . . O5 O 1.1330(3) 0.3244(2) -0.1506(2) 0.0448(8) Uani 1 1 d . . . N5 N 1.2937(3) -0.1315(3) 0.2864(3) 0.0496(11) Uani 1 1 d . . . H5 H 1.2333 -0.1068 0.3252 0.059 Uiso 1 1 calc R B 1 C5 C 1.2067(3) -0.0001(3) 0.0262(2) 0.0277(9) Uani 1 1 d . . . O6 O 1.1232(4) 0.2941(2) -0.2877(2) 0.0624(11) Uani 1 1 d . . . N6 N 1.4585(4) -0.1999(3) 0.1876(3) 0.0496(11) Uani 1 1 d . . . H6 H 1.5195 -0.2251 0.1495 0.059 Uiso 1 1 calc R C 1 C6 C 1.1784(3) -0.0787(3) 0.0209(2) 0.0289(9) Uani 1 1 d . . . O7 O 1.2953(3) 0.3044(2) -0.2546(3) 0.0652(12) Uani 1 1 d . . . N7 N 0.7791(17) 0.4235(12) 0.4087(14) 0.057(5) Uiso 0.25 1 d PD D 2 C7 C 1.3101(4) 0.0180(3) -0.0249(2) 0.0310(9) Uani 1 1 d . . . H7A H 1.3326 0.0622 0.0018 0.037 Uiso 1 1 calc R . . H7B H 1.3709 -0.0362 -0.0284 0.037 Uiso 1 1 calc R . . O8 O 1.3622(2) -0.09397(18) -0.15955(17) 0.0317(7) Uani 1 1 d . . . H58 H 1.4313 -0.1042 -0.1705 0.038 Uiso 1 1 calc R . . C8 C 1.2918(3) 0.0504(3) -0.1092(3) 0.0310(9) Uani 1 1 d . . . O9 O 1.6745(3) -0.0015(3) -0.4773(2) 0.0572(10) Uani 1 1 d . . . N9 N 0.9156(16) 0.3861(11) 0.2813(11) 0.062(5) Uiso 0.25 1 d PD D 2 C9 C 1.2493(3) 0.1397(3) -0.1255(3) 0.0313(9) Uani 1 1 d . . . H9 H 1.2342 0.1804 -0.0836 0.038 Uiso 1 1 calc R . . O10 O 1.7526(4) -0.1448(3) -0.5321(2) 0.0678(12) Uani 1 1 d . . . C10 C 1.2294(4) 0.1683(3) -0.2022(3) 0.0306(9) Uani 1 1 d . . . O11 O 1.8078(3) -0.1104(3) -0.4124(2) 0.0705(13) Uani 1 1 d . . . C11 C 1.2476(4) 0.1105(3) -0.2645(3) 0.0330(10) Uani 1 1 d . . . H11 H 1.2307 0.1317 -0.3163 0.040 Uiso 1 1 calc R . . O12 O 1.3619(3) -0.22878(19) -0.26906(19) 0.0400(8) Uani 1 1 d . . . H59 H 1.3161 -0.1920 -0.2381 0.048 Uiso 1 1 calc R . . C12 C 1.2908(3) 0.0212(3) -0.2511(2) 0.0298(9) Uani 1 1 d . . . O13 O 1.5542(3) -0.1650(2) -0.0068(2) 0.0505(9) Uani 1 1 d . . . C13 C 1.3153(3) -0.0064(3) -0.1741(2) 0.0292(9) Uani 1 1 d . . . O14 O 1.7342(3) -0.2625(3) -0.0506(2) 0.0663(12) Uani 1 1 d . . . C14 C 1.3045(4) -0.0419(3) -0.3178(2) 0.0317(9) Uani 1 1 d . . . H14A H 1.2878 -0.0080 -0.3678 0.038 Uiso 1 1 calc R . . H14B H 1.2497 -0.0764 -0.3023 0.038 Uiso 1 1 calc R . . O15 O 1.6114(3) -0.2972(2) 0.0694(2) 0.0486(9) Uani 1 1 d . . . C15 C 1.4199(4) -0.1050(3) -0.3364(2) 0.0308(9) Uani 1 1 d . . . O16 O 1.4239(3) -0.4371(2) -0.2154(2) 0.0477(9) Uani 1 1 d . . . H60 H 1.3785 -0.4617 -0.1872 0.057 Uiso 1 1 calc R . . C16 C 1.5052(4) -0.0746(3) -0.3822(3) 0.0349(10) Uani 1 1 d . . . H16 H 1.4913 -0.0155 -0.4011 0.042 Uiso 1 1 calc R . . O17 O 1.3222(3) -0.4279(3) 0.2860(3) 0.0665(11) Uani 1 1 d . . . C17 C 1.6109(4) -0.1298(3) -0.4006(3) 0.0368(10) Uani 1 1 d . . . O18 O 1.1728(4) -0.4918(3) 0.2815(3) 0.0657(11) Uani 1 1 d . . . C18 C 1.6315(4) -0.2173(3) -0.3730(3) 0.0373(10) Uani 1 1 d . . . H18 H 1.7036 -0.2550 -0.3858 0.045 Uiso 1 1 calc R . . O19 O 1.1357(3) -0.3447(3) 0.3260(2) 0.0630(11) Uani 1 1 d . . . C19 C 1.5478(4) -0.2489(3) -0.3274(3) 0.0374(10) Uani 1 1 d . . . O20 O 1.2015(3) -0.29556(19) -0.0667(2) 0.0387(7) Uani 1 1 d . . . H61 H 1.1773 -0.2415 -0.0737 0.046 Uiso 1 1 calc R . . C20 C 1.4407(4) -0.1921(3) -0.3104(3) 0.0363(10) Uani 1 1 d . . . C21 C 1.5687(4) -0.3420(3) -0.2961(3) 0.0397(11) Uani 1 1 d . . . H21A H 1.6473 -0.3723 -0.3141 0.048 Uiso 1 1 calc R . . H21B H 1.5233 -0.3718 -0.3200 0.048 Uiso 1 1 calc R . . O22 O 1.1432(13) -0.6357(11) 0.2235(12) 0.052(4) Uiso 0.25 1 d P . 1 C22 C 1.5420(4) -0.3498(3) -0.2043(3) 0.0359(10) Uani 1 1 d . . . O23 O 1.1463(13) -0.5875(10) 0.4468(9) 0.050(4) Uiso 0.25 1 d P E 1 C23 C 1.5899(4) -0.3073(3) -0.1565(3) 0.0351(10) Uani 1 1 d . . . H23 H 1.6417 -0.2762 -0.1817 0.042 Uiso 1 1 calc R . . O24 O 1.678(3) -0.318(2) -0.5625(14) 0.059(8) Uani 0.15 1 d P F 2 C24 C 1.5626(4) -0.3100(3) -0.0726(3) 0.0346(10) Uani 1 1 d . . . O25 O 1.6264(9) -0.2540(9) -0.5793(6) 0.050(3) Uani 0.35 1 d P G 1 C25 C 1.4858(4) -0.3540(3) -0.0359(3) 0.0339(10) Uani 1 1 d . . . H25 H 1.4657 -0.3543 0.0214 0.041 Uiso 1 1 calc R . . O26 O 1.5842(14) 0.1888(7) -0.4732(7) 0.089(5) Uani 0.35 1 d P H 1 C26 C 1.4375(4) -0.3978(3) -0.0815(3) 0.0336(10) Uani 1 1 d . . . O27 O 1.5750(18) 0.2873(15) -0.4781(13) 0.044(5) Uani 0.15 1 d P I 2 C27 C 1.4676(4) -0.3963(3) -0.1656(3) 0.0347(10) Uani 1 1 d . . . O28 O 0.4321(3) 0.0825(2) 0.1586(2) 0.0471(8) Uani 1 1 d . . . C28 C 1.3525(4) -0.4442(3) -0.0391(3) 0.0373(10) Uani 1 1 d . . . H28A H 1.3081 -0.4536 -0.0786 0.045 Uiso 1 1 calc R . . H28B H 1.3910 -0.5021 -0.0187 0.045 Uiso 1 1 calc R . . O29 O 0.2333(13) 0.1309(10) 0.2477(11) 0.072(5) Uani 0.50 1 d P J 2 C29 C 1.2767(4) -0.3937(3) 0.0305(3) 0.0376(11) Uani 1 1 d . . . O30 O 0.2145(12) 0.1705(7) 0.2468(9) 0.045(3) Uani 0.50 1 d P K 1 C30 C 1.2782(4) -0.4215(3) 0.1115(3) 0.0382(11) Uani 1 1 d . . . H30 H 1.3285 -0.4747 0.1239 0.046 Uiso 1 1 calc R . . O31 O 0.7501(15) 0.1404(12) 0.5167(11) 0.068(4) Uiso 0.25 1 d P . . C31 C 1.2071(4) -0.3725(3) 0.1735(3) 0.0399(11) Uani 1 1 d . . . O32 O 0.4857(11) 0.3815(7) 0.4986(6) 0.065(3) Uani 0.35 1 d P L 1 C32 C 1.1342(4) -0.2932(3) 0.1553(3) 0.0380(10) Uani 1 1 d . . . H32 H 1.0856 -0.2595 0.1979 0.046 Uiso 1 1 calc R . . O33 O 0.341(2) 0.427(2) 0.5022(14) 0.067(8) Uani 0.15 1 d P M 2 C33 C 1.1325(3) -0.2635(3) 0.0753(3) 0.0327(10) Uani 1 1 d . . . O34 O 0.4571(10) 0.5197(6) 0.3997(5) 0.052(3) Uani 0.35 1 d P N 1 C34 C 1.2022(4) -0.3145(3) 0.0141(3) 0.0342(10) Uani 1 1 d . . . O35 O 0.3723(19) 0.5646(15) 0.4511(14) 0.045(5) Uiso 0.15 1 d P O 2 C35 C 1.0499(4) -0.1783(3) 0.0569(3) 0.0332(10) Uani 1 1 d . . . H35A H 1.0386 -0.1791 0.0001 0.040 Uiso 1 1 calc R . . H35B H 0.9782 -0.1764 0.0923 0.040 Uiso 1 1 calc R . . C36 C 0.7828(8) 0.3316(6) 0.5031(6) 0.075(2) Uiso 0.75 1 d P A 1 O37 O 0.7306(14) 0.5138(11) 0.2186(11) 0.080(4) Uiso 0.30 1 d P P 1 C37 C 0.7670(19) 0.4124(15) 0.4442(13) 0.079(6) Uiso 0.38 1 d PD A 1 H37A H 0.6897 0.4322 0.4348 0.095 Uiso 0.38 1 calc PR A 1 H37B H 0.7865 0.4612 0.4663 0.095 Uiso 0.38 1 calc PR A 1 O38 O 0.6959(6) 0.5578(4) 0.1673(4) 0.0699(17) Uani 0.70 1 d P Q 2 C38 C 0.832(2) 0.3939(15) 0.4553(9) 0.078(6) Uiso 0.38 1 d PD A 1 H38A H 0.9058 0.3888 0.4698 0.094 Uiso 0.38 1 calc PR A 1 H38B H 0.7860 0.4535 0.4681 0.094 Uiso 0.38 1 calc PR A 1 C39 C 0.7674(10) 0.2528(8) 0.3838(7) 0.098(3) Uiso 0.75 1 d P A 1 H39A H 0.6885 0.2581 0.4059 0.117 Uiso 0.75 1 calc PR A 1 H39B H 0.7961 0.2000 0.3507 0.117 Uiso 0.75 1 calc PR A 1 O40 O 0.9764(6) 0.7987(5) 0.4026(4) 0.061(2) Uani 0.50 1 d P . . C40 C 0.7801(14) 0.3339(10) 0.3317(10) 0.113(4) Uiso 0.75 1 d P A 1 H40A H 0.8165 0.3162 0.2760 0.136 Uiso 0.75 1 calc PR A 1 H40B H 0.7062 0.3733 0.3286 0.136 Uiso 0.75 1 calc PR A 1 O41 O 1.0673(13) 0.8981(10) 0.3127(9) 0.018(3) Uiso 0.15 1 d P R 2 C41 C 0.9463(10) 0.2431(8) 0.4097(7) 0.095(3) Uiso 0.75 1 d P A 1 H41A H 0.9708 0.1953 0.3705 0.114 Uiso 0.75 1 calc PR A 1 H41B H 0.9946 0.2280 0.4515 0.114 Uiso 0.75 1 calc PR A 1 O42 O 1.0774(7) 0.9397(6) 0.3532(5) 0.0358(19) Uiso 0.35 1 d P S 1 C42 C 0.9652(13) 0.3333(11) 0.3615(10) 0.130(6) Uiso 0.75 1 d PD A 1 H42A H 1.0046 0.3639 0.3905 0.156 Uiso 0.75 1 calc PR A 1 H42B H 1.0040 0.3228 0.3050 0.156 Uiso 0.75 1 calc PR A 1 O43 O 1.1785(10) 0.8976(7) 0.4581(7) 0.093(3) Uiso 0.50 1 d P . . C43 C 0.9367(7) 0.4088(6) 0.1281(5) 0.039(2) Uani 0.50 1 d PD . 2 H43A H 0.9535 0.3960 0.1837 0.046 Uiso 0.50 1 calc PR . 2 H43B H 0.8624 0.4012 0.1272 0.046 Uiso 0.50 1 calc PR . 2 O44 O 0.8734(9) 0.6067(7) -0.1752(7) 0.088(3) Uiso 0.50 1 d P . . C44 C 0.9774(10) 0.4599(7) -0.0439(7) 0.049(3) Uani 0.50 1 d P . 1 H44A H 0.9333 0.4227 -0.0587 0.058 Uiso 0.50 1 calc PR . 1 H44B H 1.0070 0.4889 -0.0938 0.058 Uiso 0.50 1 calc PR . 1 O45 O 1.1099(17) -0.6461(12) 0.2620(13) 0.071(5) Uiso 0.25 1 d P . 2 C45 C 0.9440(8) 0.4815(7) -0.0924(7) 0.043(2) Uani 0.50 1 d P . 2 H45A H 0.9454 0.4193 -0.0812 0.052 Uiso 0.50 1 calc PR . 2 H45B H 0.9164 0.4997 -0.1442 0.052 Uiso 0.50 1 calc PR . 2 O46 O 1.186(2) -0.5642(19) 0.4530(16) 0.112(8) Uiso 0.25 1 d P T 2 C46 C 0.8687(9) 0.5366(7) -0.0243(8) 0.046(2) Uani 0.50 1 d P U 2 H46A H 0.8016 0.5729 -0.0437 0.055 Uiso 0.50 1 calc PR U 2 H46B H 0.8459 0.4986 0.0211 0.055 Uiso 0.50 1 calc PR U 2 C47 C 0.9041(10) 0.5296(8) 0.0186(7) 0.051(3) Uani 0.50 1 d P . . H47A H 0.9112 0.5885 -0.0003 0.061 Uiso 0.50 1 calc PR V 1 H47B H 0.8255 0.5294 0.0241 0.061 Uiso 0.50 1 calc PR V 1 C48 C 0.9832(10) 0.6462(5) -0.0723(7) 0.073(5) Uani 0.50 1 d PD . 2 H48A H 0.9234 0.6808 -0.1007 0.088 Uiso 0.50 1 calc PR . 2 H48B H 1.0173 0.6875 -0.0518 0.088 Uiso 0.50 1 calc PR . 2 C49 C 1.2664(11) -0.1021(10) 0.2073(7) 0.059(3) Uiso 0.50 1 d P W 1 H49A H 1.2450 -0.0375 0.2037 0.071 Uiso 0.50 1 calc PR W 1 H49B H 1.2039 -0.1234 0.1976 0.071 Uiso 0.50 1 calc PR W 1 C50 C 1.3696(9) -0.1386(9) 0.1442(7) 0.051(3) Uiso 0.50 1 d P W 1 H50A H 1.3980 -0.0902 0.1162 0.061 Uiso 0.50 1 calc PR W 1 H50B H 1.3506 -0.1711 0.1031 0.061 Uiso 0.50 1 calc PR W 1 C51 C 1.2670(9) -0.1411(9) 0.1983(7) 0.048(3) Uiso 0.50 1 d P W 2 H51A H 1.2123 -0.1758 0.2028 0.057 Uiso 0.50 1 calc PR W 2 H51B H 1.2345 -0.0826 0.1757 0.057 Uiso 0.50 1 calc PR W 2 C52 C 1.3642(12) -0.1824(12) 0.1454(9) 0.074(4) Uiso 0.50 1 d P W 2 H52A H 1.3759 -0.1443 0.0971 0.089 Uiso 0.50 1 calc PR W 2 H52B H 1.3564 -0.2378 0.1270 0.089 Uiso 0.50 1 calc PR W 2 C53 C 1.3828(5) -0.0891(4) 0.2901(4) 0.0693(18) Uani 1 1 d . W . H53A H 1.4003 -0.0952 0.3456 0.083 Uiso 1 1 calc R . . H53B H 1.3583 -0.0262 0.2761 0.083 Uiso 1 1 calc R . . C54 C 1.4841(5) -0.1320(4) 0.2308(5) 0.0715(19) Uani 1 1 d . W . H54A H 1.5060 -0.0878 0.1914 0.086 Uiso 1 1 calc R . . H54B H 1.5462 -0.1586 0.2601 0.086 Uiso 1 1 calc R . . C55 C 1.3311(5) -0.2257(4) 0.3068(4) 0.0591(15) Uani 1 1 d . W . H55A H 1.2704 -0.2537 0.3070 0.071 Uiso 1 1 calc R . . H55B H 1.3516 -0.2335 0.3615 0.071 Uiso 1 1 calc R . . C56 C 1.4293(6) -0.2678(4) 0.2451(5) 0.077(2) Uani 1 1 d . W . H56A H 1.4925 -0.2969 0.2725 0.092 Uiso 1 1 calc R . . H56B H 1.4111 -0.3124 0.2157 0.092 Uiso 1 1 calc R . . C57 C 0.8868(19) 0.3815(16) 0.4357(14) 0.063(7) Uiso 0.25 1 d PD D 2 H57A H 0.9325 0.4223 0.4383 0.075 Uiso 0.25 1 calc PR D 2 H57B H 0.8801 0.3461 0.4865 0.075 Uiso 0.25 1 calc PR D 2 C58 C 0.919(3) 0.3310(16) 0.3636(12) 0.063(7) Uiso 0.25 1 d PD D 2 H58A H 0.8693 0.2921 0.3661 0.075 Uiso 0.25 1 calc PR D 2 H58B H 0.9947 0.2936 0.3630 0.075 Uiso 0.25 1 calc PR D 2 C59 C 0.723(2) 0.3646(18) 0.3712(15) 0.072(7) Uiso 0.25 1 d PD D 2 H59A H 0.7168 0.3118 0.4047 0.087 Uiso 0.25 1 calc PR D 2 H59B H 0.6513 0.3962 0.3558 0.087 Uiso 0.25 1 calc PR D 2 C60 C 0.819(2) 0.347(2) 0.2990(19) 0.089(10) Uiso 0.25 1 d PD D 2 H60A H 0.8517 0.2831 0.3003 0.106 Uiso 0.25 1 calc PR D 2 H60B H 0.7839 0.3600 0.2500 0.106 Uiso 0.25 1 calc PR D 2 C61 C 0.7830(17) 0.5018(13) 0.3552(12) 0.055(5) Uiso 0.25 1 d PD D 2 H61A H 0.7899 0.5488 0.3878 0.066 Uiso 0.25 1 calc PR D 2 H61B H 0.7125 0.5225 0.3341 0.066 Uiso 0.25 1 calc PR D 2 C62 C 0.8771(19) 0.4848(13) 0.2847(13) 0.060(6) Uiso 0.25 1 d PD D 2 H62A H 0.9372 0.5095 0.2939 0.072 Uiso 0.25 1 calc PR D 2 H62B H 0.8518 0.5104 0.2337 0.072 Uiso 0.25 1 calc PR D 2 O100 O 0.9370(5) 0.5174(4) 0.2997(4) 0.0413(16) Uani 0.50 1 d P X 1 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 0.0322(6) 0.0281(6) 0.0351(6) -0.0016(4) -0.0071(4) -0.0063(4) O1 0.048(2) 0.0450(19) 0.0359(17) -0.0006(14) -0.0102(14) -0.0078(16) C1 0.029(2) 0.027(2) 0.037(2) 0.0065(17) -0.0147(18) -0.0097(18) S2 0.0483(7) 0.0240(6) 0.0434(7) -0.0031(5) -0.0055(5) -0.0061(5) O2 0.0338(17) 0.0354(18) 0.0456(18) 0.0023(14) -0.0083(14) -0.0045(14) C2 0.025(2) 0.030(2) 0.037(2) 0.0017(18) -0.0100(17) -0.0059(18) S3 0.0440(7) 0.0493(7) 0.0381(6) -0.0029(5) -0.0094(5) -0.0230(6) O3 0.0438(19) 0.0343(18) 0.053(2) -0.0098(15) 0.0003(15) -0.0157(15) N3 0.035(4) 0.030(4) 0.043(4) -0.006(3) -0.005(3) -0.008(3) C3 0.030(2) 0.027(2) 0.029(2) 0.0020(16) -0.0091(17) -0.0071(17) S4 0.0431(7) 0.0552(8) 0.0353(6) 0.0036(5) -0.0036(5) -0.0074(6) O4 0.0325(16) 0.0272(16) 0.0423(17) -0.0019(13) -0.0026(13) -0.0127(13) N4 0.051(5) 0.025(4) 0.046(5) -0.001(3) -0.004(4) -0.020(4) C4 0.033(2) 0.028(2) 0.036(2) -0.0005(17) -0.0118(18) -0.0069(18) S5 0.0492(8) 0.0401(7) 0.0543(8) 0.0104(6) -0.0160(6) -0.0059(6) O5 0.047(2) 0.0330(18) 0.051(2) -0.0124(14) -0.0051(16) -0.0046(15) N5 0.038(2) 0.055(3) 0.050(3) 0.007(2) 0.0018(19) -0.010(2) C5 0.031(2) 0.028(2) 0.026(2) 0.0032(16) -0.0085(17) -0.0094(17) O6 0.090(3) 0.037(2) 0.056(2) -0.0021(16) -0.033(2) 0.0044(19) N6 0.041(2) 0.063(3) 0.044(2) -0.004(2) 0.0002(18) -0.017(2) C6 0.032(2) 0.026(2) 0.031(2) 0.0027(17) -0.0122(17) -0.0071(18) O7 0.064(3) 0.038(2) 0.086(3) 0.0011(19) 0.017(2) -0.0217(19) C7 0.034(2) 0.029(2) 0.033(2) -0.0011(17) -0.0068(18) -0.0128(18) O8 0.0357(17) 0.0225(15) 0.0364(16) 0.0004(12) -0.0068(13) -0.0064(12) C8 0.029(2) 0.029(2) 0.036(2) -0.0027(18) -0.0034(17) -0.0087(18) O9 0.051(2) 0.057(2) 0.057(2) 0.0127(18) -0.0042(18) -0.0106(18) C9 0.033(2) 0.028(2) 0.035(2) -0.0038(17) -0.0053(18) -0.0108(18) O10 0.075(3) 0.079(3) 0.037(2) -0.0038(19) 0.0085(18) -0.010(2) C10 0.034(2) 0.025(2) 0.033(2) 0.0004(17) -0.0047(18) -0.0091(18) O11 0.043(2) 0.110(4) 0.057(2) 0.022(2) -0.0131(18) -0.022(2) C11 0.037(2) 0.028(2) 0.033(2) 0.0018(17) -0.0060(18) -0.0066(19) O12 0.0447(19) 0.0244(16) 0.0471(19) -0.0028(13) -0.0040(15) -0.0046(14) C12 0.031(2) 0.025(2) 0.032(2) -0.0012(17) -0.0042(17) -0.0068(17) O13 0.072(3) 0.0365(19) 0.050(2) -0.0042(15) -0.0169(18) -0.0215(18) C13 0.033(2) 0.024(2) 0.033(2) -0.0012(17) -0.0055(17) -0.0097(17) O14 0.051(2) 0.106(3) 0.053(2) -0.017(2) -0.0013(18) -0.042(2) C14 0.039(2) 0.027(2) 0.029(2) -0.0020(17) -0.0076(18) -0.0072(18) O15 0.055(2) 0.056(2) 0.0410(19) 0.0019(16) -0.0177(16) -0.0192(18) C15 0.035(2) 0.027(2) 0.030(2) -0.0048(17) -0.0095(17) -0.0027(18) O16 0.054(2) 0.042(2) 0.055(2) -0.0076(16) -0.0181(17) -0.0189(17) C16 0.043(3) 0.028(2) 0.031(2) -0.0026(17) -0.0088(19) -0.0026(19) O17 0.057(2) 0.069(3) 0.073(3) 0.018(2) -0.030(2) -0.009(2) C17 0.042(3) 0.039(3) 0.030(2) -0.0056(18) -0.0097(19) -0.008(2) O18 0.073(3) 0.049(2) 0.073(3) 0.021(2) -0.011(2) -0.019(2) C18 0.038(3) 0.039(3) 0.031(2) -0.0028(19) -0.0060(19) 0.000(2) O19 0.066(3) 0.058(2) 0.056(2) 0.0005(19) -0.0169(19) 0.004(2) C19 0.048(3) 0.030(2) 0.031(2) -0.0070(18) -0.011(2) 0.000(2) O20 0.0415(18) 0.0239(16) 0.053(2) 0.0045(14) -0.0152(15) -0.0089(13) C20 0.043(3) 0.034(2) 0.031(2) -0.0061(18) -0.0062(19) -0.008(2) C21 0.051(3) 0.024(2) 0.040(3) -0.0052(18) -0.011(2) 0.001(2) C22 0.040(3) 0.024(2) 0.041(2) -0.0007(18) -0.012(2) 0.0008(19) C23 0.037(3) 0.029(2) 0.040(2) 0.0014(19) -0.0099(19) -0.0081(19) O24 0.09(2) 0.09(2) 0.025(12) 0.016(13) -0.015(12) -0.074(19) C24 0.036(2) 0.029(2) 0.041(3) -0.0002(18) -0.0112(19) -0.0089(19) O25 0.048(6) 0.085(9) 0.032(5) -0.030(6) 0.025(5) -0.056(6) C25 0.034(2) 0.029(2) 0.040(2) 0.0015(18) -0.0142(19) -0.0061(18) O26 0.179(14) 0.037(6) 0.060(7) -0.016(5) -0.091(9) 0.006(7) C26 0.032(2) 0.022(2) 0.047(3) 0.0001(18) -0.0143(19) -0.0026(17) O27 0.044(13) 0.056(14) 0.039(12) 0.012(10) 0.000(10) -0.034(11) C27 0.037(2) 0.021(2) 0.048(3) -0.0032(18) -0.018(2) -0.0028(18) O28 0.0410(19) 0.0383(19) 0.062(2) 0.0004(16) -0.0165(16) -0.0063(15) C28 0.035(2) 0.024(2) 0.055(3) 0.002(2) -0.012(2) -0.0080(18) O29 0.030(5) 0.120(14) 0.053(6) -0.006(10) -0.019(4) 0.011(9) C29 0.033(2) 0.022(2) 0.061(3) 0.003(2) -0.015(2) -0.0104(18) O30 0.033(7) 0.058(7) 0.036(4) 0.001(5) 0.000(4) -0.002(5) C30 0.033(2) 0.024(2) 0.058(3) 0.006(2) -0.016(2) -0.0057(19) C31 0.035(3) 0.031(2) 0.056(3) 0.006(2) -0.013(2) -0.010(2) O32 0.111(10) 0.041(6) 0.044(6) -0.007(5) -0.029(6) -0.012(6) C32 0.036(3) 0.028(2) 0.053(3) 0.002(2) -0.011(2) -0.0128(19) O33 0.059(16) 0.11(2) 0.027(12) 0.001(13) -0.006(11) -0.017(16) C33 0.027(2) 0.025(2) 0.050(3) 0.0022(19) -0.0112(19) -0.0105(18) O34 0.094(8) 0.053(6) 0.026(5) 0.004(4) -0.045(5) -0.026(6) C34 0.032(2) 0.026(2) 0.050(3) 0.0062(19) -0.014(2) -0.0129(18) C35 0.032(2) 0.026(2) 0.046(3) 0.0019(18) -0.0129(19) -0.0106(18) O38 0.089(5) 0.076(4) 0.065(4) -0.014(3) -0.009(3) -0.055(4) O40 0.039(4) 0.071(5) 0.054(4) -0.029(4) -0.006(3) 0.023(4) C43 0.021(4) 0.060(6) 0.030(4) -0.012(4) -0.015(3) 0.007(4) C44 0.070(8) 0.038(6) 0.039(6) 0.001(4) -0.007(5) -0.019(5) C45 0.038(5) 0.051(6) 0.041(6) -0.011(5) -0.004(4) -0.012(5) C46 0.034(6) 0.040(6) 0.066(7) -0.012(5) 0.000(5) -0.018(5) C47 0.053(7) 0.049(7) 0.046(6) -0.010(5) -0.022(5) 0.007(5) C48 0.123(11) 0.002(4) 0.117(10) -0.003(5) -0.104(9) 0.000(5) C53 0.066(4) 0.059(4) 0.085(5) -0.017(3) 0.010(3) -0.031(3) C54 0.041(3) 0.044(3) 0.126(6) -0.008(3) 0.004(3) -0.015(3) C55 0.064(4) 0.057(4) 0.058(3) 0.002(3) 0.001(3) -0.027(3) C56 0.070(4) 0.056(4) 0.097(5) 0.012(3) 0.013(4) -0.028(3) O100 0.037(4) 0.017(3) 0.064(4) 0.007(3) 0.001(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S1 O3 1.457(3) . ? S1 O2 1.457(3) . ? S1 O1 1.458(3) . ? S1 C3 1.770(4) . ? N1 C40 1.464(17) . ? N1 C42 1.497(14) . ? N1 C38 1.507(15) . ? N1 C37 1.533(16) . ? C1 C2 1.387(6) . ? C1 C6 1.412(6) . ? C1 C35 1.518(6) . ? S2 O5 1.444(3) . ? S2 O6 1.448(4) . ? S2 O7 1.462(4) . ? S2 C10 1.772(4) . ? N2 C39 1.466(15) . ? N2 C41 1.502(14) . ? N2 C36 1.593(14) . ? C2 C3 1.397(6) . ? S3 O14 1.445(4) . ? S3 O13 1.450(4) . ? S3 O15 1.482(3) . ? S3 C24 1.769(4) . ? N3 C45 1.488(12) 2_765 ? N3 C47 1.503(13) . ? N3 C43 1.618(11) . ? C3 C4 1.381(6) . ? S4 O10 1.444(4) . ? S4 O9 1.449(4) . ? S4 O11 1.459(4) . ? S4 C17 1.750(5) . ? O4 C6 1.356(5) . ? N4 C44 1.495(14) 2_765 ? N4 C46 1.500(13) . ? N4 C48 1.614(13) . ? C4 C5 1.394(6) . ? S5 O17 1.439(4) . ? S5 O19 1.439(4) . ? S5 O18 1.457(4) . ? S5 C31 1.770(5) . ? N5 C49 1.445(13) . ? N5 C55 1.480(7) . ? N5 C53 1.481(7) . ? N5 C51 1.602(12) . ? C5 C6 1.405(6) . ? C5 C7 1.521(6) . ? N6 C52 1.458(15) . ? N6 C56 1.474(7) . ? N6 C54 1.480(8) . ? N6 C50 1.539(12) . ? N7 C61 1.488(17) . ? N7 C57 1.491(18) . ? N7 C59 1.546(18) . ? C7 C8 1.506(6) . ? O8 C13 1.385(5) . ? C8 C13 1.404(6) . ? C8 C9 1.405(6) . ? N9 C60 1.495(18) . ? N9 C62 1.518(17) . ? N9 C58 1.581(17) . ? C9 C10 1.379(6) . ? C10 C11 1.390(6) . ? C11 C12 1.397(6) . ? O12 C20 1.355(5) . ? C12 C13 1.397(6) . ? C12 C14 1.512(6) . ? C14 C15 1.535(6) . ? C15 C16 1.390(6) . ? C15 C20 1.393(6) . ? O16 C27 1.369(5) . ? C16 C17 1.392(6) . ? C17 C18 1.406(7) . ? C18 C19 1.383(7) . ? C19 C20 1.413(7) . ? C19 C21 1.507(6) . ? O20 C34 1.368(5) . ? C21 C22 1.519(6) . ? O22 O44 0.932(16) 2_755 ? C22 C27 1.398(6) . ? C22 C23 1.398(6) . ? C23 C24 1.388(6) . ? C24 C25 1.384(6) . ? C25 C26 1.389(6) . ? C26 C27 1.393(7) . ? C26 C28 1.517(6) . ? C28 C29 1.502(7) . ? C29 C30 1.399(7) . ? C29 C34 1.404(6) . ? C30 C31 1.382(7) . ? O31 O43 1.087(18) 2_766 ? C31 C32 1.402(6) . ? C32 C33 1.392(6) . ? C33 C34 1.380(7) . ? C33 C35 1.528(6) . ? C36 C38 1.44(2) . ? C36 C37 1.55(3) . ? C39 C40 1.534(18) . ? C41 C42 1.650(19) . ? O43 O31 1.087(18) 2_766 ? C43 C48 1.406(15) 2_765 ? O44 O22 0.932(16) 2_755 ? O44 O45 1.54(2) 2_755 ? C44 N4 1.495(14) 2_765 ? C44 C47 1.569(15) . ? O45 O44 1.54(2) 2_755 ? C45 N3 1.488(12) 2_765 ? C45 C46 1.514(14) . ? C48 C43 1.406(15) 2_765 ? C49 C50 1.539(17) . ? C51 C52 1.416(19) . ? C53 C54 1.511(9) . ? C55 C56 1.507(9) . ? C57 C58 1.436(18) . ? C59 C60 1.541(19) . ? C61 C62 1.507(18) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 S1 O2 113.21(19) . . ? O3 S1 O1 112.0(2) . . ? O2 S1 O1 111.13(19) . . ? O3 S1 C3 106.22(19) . . ? O2 S1 C3 107.10(19) . . ? O1 S1 C3 106.75(19) . . ? C40 N1 C42 115.0(13) . . ? C40 N1 C38 122.7(14) . . ? C42 N1 C38 91.7(15) . . ? C40 N1 C37 100.1(13) . . ? C42 N1 C37 124.2(14) . . ? C38 N1 C37 32.7(10) . . ? C2 C1 C6 118.0(4) . . ? C2 C1 C35 121.6(4) . . ? C6 C1 C35 120.3(4) . . ? O5 S2 O6 113.3(2) . . ? O5 S2 O7 112.7(2) . . ? O6 S2 O7 111.7(3) . . ? O5 S2 C10 107.0(2) . . ? O6 S2 C10 106.8(2) . . ? O7 S2 C10 104.7(2) . . ? C39 N2 C41 105.5(9) . . ? C39 N2 C36 109.7(9) . . ? C41 N2 C36 109.0(9) . . ? C1 C2 C3 121.0(4) . . ? O14 S3 O13 113.5(3) . . ? O14 S3 O15 113.2(2) . . ? O13 S3 O15 109.2(2) . . ? O14 S3 C24 107.1(2) . . ? O13 S3 C24 107.3(2) . . ? O15 S3 C24 106.1(2) . . ? C45 N3 C47 109.6(8) 2_765 . ? C45 N3 C43 112.3(7) 2_765 . ? C47 N3 C43 110.5(7) . . ? C4 C3 C2 120.2(4) . . ? C4 C3 S1 120.1(3) . . ? C2 C3 S1 119.7(3) . . ? O10 S4 O9 112.6(2) . . ? O10 S4 O11 110.7(3) . . ? O9 S4 O11 113.2(3) . . ? O10 S4 C17 106.5(2) . . ? O9 S4 C17 106.6(2) . . ? O11 S4 C17 106.8(2) . . ? C44 N4 C46 110.4(8) 2_765 . ? C44 N4 C48 108.0(7) 2_765 . ? C46 N4 C48 110.6(8) . . ? C3 C4 C5 121.0(4) . . ? O17 S5 O19 112.5(3) . . ? O17 S5 O18 112.2(2) . . ? O19 S5 O18 112.5(3) . . ? O17 S5 C31 105.5(2) . . ? O19 S5 C31 106.9(2) . . ? O18 S5 C31 106.7(2) . . ? C49 N5 C55 121.0(7) . . ? C49 N5 C53 101.3(7) . . ? C55 N5 C53 109.5(5) . . ? C49 N5 C51 23.8(6) . . ? C55 N5 C51 97.6(6) . . ? C53 N5 C51 116.8(6) . . ? C4 C5 C6 118.2(4) . . ? C4 C5 C7 120.2(4) . . ? C6 C5 C7 121.6(4) . . ? C52 N6 C56 98.1(8) . . ? C52 N6 C54 122.8(8) . . ? C56 N6 C54 110.6(5) . . ? C52 N6 C50 27.5(7) . . ? C56 N6 C50 119.8(6) . . ? C54 N6 C50 97.2(6) . . ? O4 C6 C5 122.5(4) . . ? O4 C6 C1 115.8(4) . . ? C5 C6 C1 121.6(4) . . ? C61 N7 C57 112.7(19) . . ? C61 N7 C59 109.7(19) . . ? C57 N7 C59 117.6(19) . . ? C8 C7 C5 111.9(3) . . ? C13 C8 C9 117.4(4) . . ? C13 C8 C7 122.1(4) . . ? C9 C8 C7 120.5(4) . . ? C60 N9 C62 111(2) . . ? C60 N9 C58 70(2) . . ? C62 N9 C58 118.7(17) . . ? C10 C9 C8 120.1(4) . . ? C9 C10 C11 121.6(4) . . ? C9 C10 S2 119.6(3) . . ? C11 C10 S2 118.6(3) . . ? C10 C11 C12 120.2(4) . . ? C13 C12 C11 117.5(4) . . ? C13 C12 C14 122.6(4) . . ? C11 C12 C14 119.9(4) . . ? O8 C13 C12 119.1(4) . . ? O8 C13 C8 117.8(4) . . ? C12 C13 C8 123.1(4) . . ? C12 C14 C15 114.7(4) . . ? C16 C15 C20 119.2(4) . . ? C16 C15 C14 118.9(4) . . ? C20 C15 C14 121.9(4) . . ? C15 C16 C17 120.7(4) . . ? C16 C17 C18 119.7(4) . . ? C16 C17 S4 121.4(4) . . ? C18 C17 S4 118.9(4) . . ? C19 C18 C17 120.6(4) . . ? C18 C19 C20 118.8(4) . . ? C18 C19 C21 121.4(4) . . ? C20 C19 C21 119.8(4) . . ? O12 C20 C15 123.6(4) . . ? O12 C20 C19 115.4(4) . . ? C15 C20 C19 121.0(4) . . ? C19 C21 C22 113.1(4) . . ? C27 C22 C23 118.5(4) . . ? C27 C22 C21 121.8(4) . . ? C23 C22 C21 119.7(4) . . ? C24 C23 C22 120.6(4) . . ? C25 C24 C23 119.7(4) . . ? C25 C24 S3 119.6(3) . . ? C23 C24 S3 120.7(3) . . ? C24 C25 C26 121.1(4) . . ? C25 C26 C27 118.6(4) . . ? C25 C26 C28 119.5(4) . . ? C27 C26 C28 121.9(4) . . ? O16 C27 C26 122.6(4) . . ? O16 C27 C22 115.9(4) . . ? C26 C27 C22 121.4(4) . . ? C29 C28 C26 112.4(4) . . ? C30 C29 C34 118.3(4) . . ? C30 C29 C28 122.8(4) . . ? C34 C29 C28 118.9(4) . . ? C31 C30 C29 120.7(4) . . ? C30 C31 C32 119.8(4) . . ? C30 C31 S5 119.0(3) . . ? C32 C31 S5 121.2(4) . . ? C33 C32 C31 120.6(5) . . ? C34 C33 C32 118.8(4) . . ? C34 C33 C35 121.6(4) . . ? C32 C33 C35 119.6(4) . . ? O20 C34 C33 124.0(4) . . ? O20 C34 C29 114.1(4) . . ? C33 C34 C29 121.9(4) . . ? C1 C35 C33 115.7(3) . . ? C38 C36 C37 33.0(11) . . ? C38 C36 N2 102.4(11) . . ? C37 C36 N2 108.0(9) . . ? N1 C37 C36 104.6(14) . . ? C36 C38 N1 112.2(15) . . ? N2 C39 C40 107.7(11) . . ? N1 C40 C39 111.0(12) . . ? N2 C41 C42 115.8(10) . . ? N1 C42 C41 97.1(12) . . ? C48 C43 N3 105.2(7) 2_765 . ? O22 O44 O45 20.0(13) 2_755 2_755 ? N4 C44 C47 106.8(9) 2_765 . ? N3 C45 C46 108.7(8) 2_765 . ? N4 C46 C45 108.4(8) . . ? N3 C47 C44 108.0(8) . . ? C43 C48 N4 113.2(7) 2_765 . ? N5 C49 C50 107.4(9) . . ? C49 C50 N6 108.9(8) . . ? C52 C51 N5 110.8(9) . . ? C51 C52 N6 109.5(11) . . ? N5 C53 C54 109.0(5) . . ? N6 C54 C53 108.9(5) . . ? N5 C55 C56 109.5(4) . . ? N6 C56 C55 108.7(5) . . ? C58 C57 N7 89(2) . . ? C57 C58 N9 115(2) . . ? C60 C59 N7 90.3(19) . . ? N9 C60 C59 128(2) . . ? N7 C61 C62 113.3(18) . . ? C61 C62 N9 104.2(17) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.34 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.955 _refine_diff_density_min -0.632 _refine_diff_density_rms 0.146