# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name _publ_author_address 'de Mendoza, J.' ;The Institute of Chemical Research of Catalonia (ICIQ) Avgda. Pa\=isos Catalans 16 E-43007 Tarragona, Spain ; P.Blondeau ;The Institute of Chemical Research of Catalonia (ICIQ) X-ray Diffraction Unit Avgda. Pa\=isos Catalans s/n E-43007 Tarragona, Spain ; _publ_contact_author_name 'J. de Mendoza' _publ_contact_author_address ; Institute of Chemical Research of Catalonia (ICIQ) Tarragona 43007 SPAIN ; _publ_contact_author_email JMENDOZA@ICIQ.ES _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Enthalpy driven nitrate complexation by guanidinium-based macrocycles ; _publ_contact_author ; Dr. Benet-Buchholz, Jordi The Institute of Chemical Research of Catalonia (ICIQ) X-ray Diffraction Unit Avgda. Pa\=isos Catalans 16 E-43007 Tarragona, Spain ; _publ_contact_author_fax '+34 977 920 221' _publ_contact_author_phone '+34 977 920 204' _publ_contact_letter ; ? ; _publ_requested_coeditor_name ? data_pbl105_0m _database_code_depnum_ccdc_archive 'CCDC 635651' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H36 N8 O5.08 S2' _chemical_formula_weight 618.09 _chemical_absolute_configuration rmad 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.1246(10) _cell_length_b 20.319(2) _cell_length_c 47.951(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8890.1(16) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9424 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 21.18 _exptl_crystal_description Needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.385 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3920 _exptl_absorpt_coefficient_mu 0.232 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.910154 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78274 _diffrn_reflns_av_R_equivalents 0.0952 _diffrn_reflns_av_sigmaI/netI 0.0753 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -57 _diffrn_reflns_limit_l_max 57 _diffrn_reflns_theta_min 2.48 _diffrn_reflns_theta_max 25.39 _reflns_number_total 15128 _reflns_number_gt 11345 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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. The structure described can be solved and refined in the higher symmetric orthorhombic chiral space group P212121 or in the lower symmetric monoclinic chiral space group P21 as a monoclinic twin which emulates a higher symmetric orthorhombic crystal with an beta angle close to 90 degrees. In the higher symmetric space group the three independent refined structures are partly disordered and the obtained R-values are higher (R1 = 0.0752 (Fo > 4sigmaFo)). In the lower symmetric space group which refines with better R-values applying a twin matrix (1 0 0 0 -1 0 0 0 -1, basf 0.43), six different independent molecules without disorder can be refined (R1 = 0.0654 (Fo > 4sigmaFo)). In this case the six independent molecules are showing correlation effects.In order to discuss the crystal packing and the arrangement of the NO3-anions the higher symmetrical and partly disordered structure solution was selected. ; _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^)+(0.0551P)^2^+13.4450P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.05(9) _refine_ls_number_reflns 15128 _refine_ls_number_parameters 1171 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1050 _refine_ls_R_factor_gt 0.0752 _refine_ls_wR_factor_ref 0.1787 _refine_ls_wR_factor_gt 0.1644 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.001 _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 N1A N 0.7823(6) 0.5544(2) 0.90115(8) 0.0372(11) Uani 1 1 d . . . H1NA H 0.7172 0.5257 0.8951 0.045 Uiso 1 1 calc R . . O1A O 0.5742(8) 0.3428(3) 0.80146(10) 0.101(2) Uani 1 1 d . . . S1A S 0.8502(2) 0.40536(8) 0.89450(4) 0.0559(5) Uani 1 1 d . . . C1A C 0.9342(7) 0.5336(3) 0.90408(12) 0.0447(16) Uani 1 1 d . . . H1A H 0.9542 0.5212 0.9239 0.054 Uiso 1 1 calc R . . S2A S 0.28991(19) 0.77582(7) 0.91370(3) 0.0463(4) Uani 1 1 d . . . C2A C 0.7380(7) 0.6156(3) 0.90733(9) 0.0339(13) Uani 1 1 d . . . N2A N 0.8351(6) 0.6621(2) 0.91424(9) 0.0382(12) Uani 1 1 d . . . O2A O 0.4844(5) 0.6959(2) 0.82436(9) 0.0570(12) Uani 1 1 d . . . C3A C 0.9934(7) 0.6509(3) 0.91306(11) 0.0444(15) Uani 1 1 d . . . H3A1 H 1.0317 0.6450 0.9322 0.053 Uiso 1 1 calc R . . H3A2 H 1.0419 0.6900 0.9049 0.053 Uiso 1 1 calc R . . N3A N 0.6555(8) 0.3684(3) 0.84515(11) 0.0684(19) Uani 1 1 d . . . H3AA H 0.6340 0.3920 0.8600 0.082 Uiso 1 1 calc R . . C4A C 1.0297(7) 0.5909(3) 0.89583(12) 0.0443(15) Uani 1 1 d . . . H4A1 H 1.0148 0.6009 0.8758 0.053 Uiso 1 1 calc R . . H4A2 H 1.1340 0.5791 0.8986 0.053 Uiso 1 1 calc R . . N4A N 0.4186(8) 0.3904(3) 0.83265(11) 0.0688(19) Uani 1 1 d . . . H4AA H 0.4034 0.3990 0.8504 0.083 Uiso 1 1 calc R . . N5A N 0.2626(6) 0.6465(2) 0.82540(9) 0.0411(12) Uani 1 1 d . . . H5AA H 0.1721 0.6482 0.8317 0.049 Uiso 1 1 calc R . . C5A C 0.9624(8) 0.4749(3) 0.88521(13) 0.0498(17) Uani 1 1 d . . . H5A1 H 1.0670 0.4623 0.8865 0.060 Uiso 1 1 calc R . . H5A2 H 0.9419 0.4875 0.8657 0.060 Uiso 1 1 calc R . . N6A N 0.3044(5) 0.7397(2) 0.85110(10) 0.0418(12) Uani 1 1 d . . . H6AA H 0.2175 0.7331 0.8585 0.050 Uiso 1 1 calc R . . C6A C 0.8954(9) 0.3517(3) 0.86638(15) 0.059(2) Uani 1 1 d . . . N7A N 0.5965(6) 0.6300(2) 0.90567(9) 0.0347(11) Uani 1 1 d . . . H7NA H 0.5330 0.5981 0.9027 0.042 Uiso 1 1 calc R . . C7A C 1.0282(11) 0.3204(3) 0.86683(18) 0.074(2) Uani 1 1 d . . . H7A H 1.0944 0.3302 0.8815 0.089 Uiso 1 1 calc R . . C8A C 1.0699(11) 0.2757(4) 0.8471(2) 0.081(3) Uani 1 1 d . . . H8A H 1.1636 0.2554 0.8478 0.097 Uiso 1 1 calc R . . C9A C 0.9719(14) 0.2610(4) 0.82618(18) 0.095(3) Uani 1 1 d . . . H9A H 0.9980 0.2297 0.8123 0.114 Uiso 1 1 calc R . . C10A C 0.8340(12) 0.2915(4) 0.82496(15) 0.082(3) Uani 1 1 d . . . H10A H 0.7678 0.2807 0.8104 0.098 Uiso 1 1 calc R . . C11A C 0.7938(10) 0.3374(3) 0.84505(13) 0.065(2) Uani 1 1 d . . . C12A C 0.5507(11) 0.3656(4) 0.82463(14) 0.073(3) Uani 1 1 d . . . C13A C 0.3012(10) 0.4030(4) 0.81249(14) 0.071(2) Uani 1 1 d . . . H13A H 0.2052 0.3978 0.8219 0.085 Uiso 1 1 calc R . . H13B H 0.3069 0.3701 0.7973 0.085 Uiso 1 1 calc R . . C14A C 0.3111(9) 0.4710(3) 0.80023(12) 0.0553(19) Uani 1 1 d . . . H14A H 0.2414 0.4740 0.7845 0.066 Uiso 1 1 calc R . . H14B H 0.4109 0.4773 0.7926 0.066 Uiso 1 1 calc R . . C15A C 0.2789(8) 0.5272(3) 0.82057(11) 0.0474(16) Uani 1 1 d . . . H15A H 0.1762 0.5238 0.8271 0.057 Uiso 1 1 calc R . . H15B H 0.3437 0.5231 0.8370 0.057 Uiso 1 1 calc R . . C16A C 0.3021(7) 0.5934(3) 0.80726(12) 0.0458(15) Uani 1 1 d . . . H16A H 0.4065 0.5980 0.8020 0.055 Uiso 1 1 calc R . . H16B H 0.2428 0.5962 0.7900 0.055 Uiso 1 1 calc R . . C17A C 0.3565(8) 0.6940(3) 0.83324(12) 0.0435(15) Uani 1 1 d . . . C18A C 0.3800(7) 0.7969(3) 0.85854(13) 0.0429(15) Uani 1 1 d . . . C19A C 0.4579(8) 0.8346(3) 0.83897(14) 0.0525(17) Uani 1 1 d . . . H19A H 0.4640 0.8191 0.8203 0.063 Uiso 1 1 calc R . . C20A C 0.5240(9) 0.8917(3) 0.84539(15) 0.0608(19) Uani 1 1 d . . . H20A H 0.5782 0.9149 0.8316 0.073 Uiso 1 1 calc R . . C21A C 0.5127(8) 0.9162(3) 0.87205(15) 0.0557(19) Uani 1 1 d . . . H21A H 0.5544 0.9577 0.8765 0.067 Uiso 1 1 calc R . . C22A C 0.4396(8) 0.8798(3) 0.89249(15) 0.0526(17) Uani 1 1 d . . . H22A H 0.4332 0.8963 0.9110 0.063 Uiso 1 1 calc R . . C23A C 0.3761(7) 0.8195(3) 0.88599(13) 0.0431(15) Uani 1 1 d . . . C24A C 0.3783(7) 0.6950(3) 0.91212(12) 0.0398(14) Uani 1 1 d . . . H24A H 0.3555 0.6707 0.9295 0.048 Uiso 1 1 calc R . . H24B H 0.3360 0.6700 0.8963 0.048 Uiso 1 1 calc R . . C25A C 0.5431(6) 0.6978(3) 0.90861(11) 0.0331(13) Uani 1 1 d . . . H25A H 0.5658 0.7224 0.8911 0.040 Uiso 1 1 calc R . . C26A C 0.6285(7) 0.7292(3) 0.93257(11) 0.0379(14) Uani 1 1 d . . . H261 H 0.5987 0.7757 0.9348 0.046 Uiso 1 1 calc R . . H262 H 0.6070 0.7057 0.9502 0.046 Uiso 1 1 calc R . . C27A C 0.7889(7) 0.7254(3) 0.92636(11) 0.0417(15) Uani 1 1 d . . . H271 H 0.8148 0.7612 0.9133 0.050 Uiso 1 1 calc R . . H272 H 0.8442 0.7329 0.9438 0.050 Uiso 1 1 calc R . . S1B S 0.5000(2) 1.03919(8) 0.77133(3) 0.0541(5) Uani 1 1 d . . . O1B O 0.7175(5) 1.0631(2) 0.87271(8) 0.0537(12) Uani 1 1 d . . . N1B N 0.5238(6) 0.8846(2) 0.76872(10) 0.0456(13) Uani 1 1 d . . . H1B H 0.5992 0.9099 0.7727 0.055 Uiso 1 1 d R . . C1B C 0.3768(8) 0.9135(3) 0.77148(13) 0.0492(16) Uani 1 1 d . . . H1BB H 0.3508 0.9170 0.7917 0.059 Uiso 1 1 calc R . . S2B S 0.9548(2) 0.72354(8) 0.78650(3) 0.0502(4) Uani 1 1 d . . . C2B C 0.5521(7) 0.8235(3) 0.76062(11) 0.0385(14) Uani 1 1 d . . . O2B O 1.0052(5) 0.71219(18) 0.84968(7) 0.0376(9) Uani 1 1 d . . . N2B N 0.4445(6) 0.7802(2) 0.75844(10) 0.0459(13) Uani 1 1 d . . . C3B C 0.2926(8) 0.7987(3) 0.76366(15) 0.0562(18) Uani 1 1 d . . . H3B1 H 0.2688 0.7911 0.7835 0.067 Uiso 1 1 calc R . . H3B2 H 0.2269 0.7708 0.7523 0.067 Uiso 1 1 calc R . . N3B N 0.6451(7) 1.0484(3) 0.82700(10) 0.0526(15) Uani 1 1 d . . . H3BT H 0.6811 1.0406 0.8103 0.063 Uiso 1 1 calc R . . C4B C 0.2674(9) 0.8678(4) 0.75682(16) 0.071(2) Uani 1 1 d . . . H4B1 H 0.1665 0.8801 0.7624 0.085 Uiso 1 1 calc R . . H4B2 H 0.2757 0.8738 0.7364 0.085 Uiso 1 1 calc R . . N4B N 0.8662(7) 1.0100(2) 0.84240(10) 0.0521(15) Uani 1 1 d . . . H4BA H 0.8839 1.0015 0.8247 0.063 Uiso 1 1 calc R . . N5B N 0.8193(6) 0.7843(2) 0.85770(9) 0.0402(12) Uani 1 1 d . . . H5B H 0.7238 0.7902 0.8583 0.048 Uiso 1 1 calc R . . C5B C 0.3713(9) 0.9799(3) 0.75849(12) 0.0550(19) Uani 1 1 d . . . H5C H 0.2714 0.9978 0.7611 0.066 Uiso 1 1 calc R . . H5D H 0.3872 0.9748 0.7382 0.066 Uiso 1 1 calc R . . N6B N 0.7752(6) 0.6842(2) 0.83644(9) 0.0401(12) Uani 1 1 d . . . H6BA H 0.6812 0.6904 0.8396 0.048 Uiso 1 1 calc R . . C6B C 0.4141(8) 1.0649(3) 0.80330(12) 0.0512(18) Uani 1 1 d . . . N7B N 0.6898(6) 0.8075(2) 0.75557(9) 0.0404(12) Uani 1 1 d . . . H7NB H 0.7591 0.8366 0.7588 0.048 Uiso 1 1 calc R . . C7B C 0.2656(9) 1.0818(3) 0.80337(13) 0.0517(18) Uani 1 1 d . . . H7B H 0.2109 1.0809 0.7865 0.062 Uiso 1 1 calc R . . C8B C 0.1993(9) 1.0998(3) 0.82792(14) 0.0584(19) Uani 1 1 d . . . H8B H 0.0983 1.1111 0.8282 0.070 Uiso 1 1 calc R . . C9B C 0.2805(9) 1.1015(3) 0.85244(15) 0.063(2) Uani 1 1 d . . . H9B H 0.2344 1.1137 0.8694 0.076 Uiso 1 1 calc R . . C10B C 0.4245(9) 1.0860(3) 0.85232(13) 0.059(2) Uani 1 1 d . . . H10B H 0.4784 1.0889 0.8692 0.071 Uiso 1 1 calc R . . C11B C 0.4967(8) 1.0658(3) 0.82797(12) 0.0479(17) Uani 1 1 d . . . C12B C 0.7438(8) 1.0417(3) 0.84928(12) 0.0437(15) Uani 1 1 d . . . C13B C 0.9719(8) 0.9891(3) 0.86356(12) 0.0508(17) Uani 1 1 d . . . H13C H 0.9189 0.9727 0.8802 0.061 Uiso 1 1 calc R . . H13D H 1.0323 1.0272 0.8693 0.061 Uiso 1 1 calc R . . C14B C 1.0707(8) 0.9352(3) 0.85233(13) 0.0485(16) Uani 1 1 d . . . H14C H 1.1423 0.9230 0.8669 0.058 Uiso 1 1 calc R . . H14D H 1.1263 0.9528 0.8362 0.058 Uiso 1 1 calc R . . C15B C 0.9885(8) 0.8726(3) 0.84300(12) 0.0472(16) Uani 1 1 d . . . H15C H 0.9125 0.8849 0.8292 0.057 Uiso 1 1 calc R . . H15D H 1.0585 0.8426 0.8337 0.057 Uiso 1 1 calc R . . C16B C 0.9157(7) 0.8363(3) 0.86733(12) 0.0456(16) Uani 1 1 d . . . H16C H 0.9925 0.8171 0.8794 0.055 Uiso 1 1 calc R . . H16D H 0.8587 0.8680 0.8786 0.055 Uiso 1 1 calc R . . C17B C 0.8737(8) 0.7266(3) 0.84772(10) 0.0397(15) Uani 1 1 d . . . C18B C 0.8188(7) 0.6308(3) 0.81984(10) 0.0414(15) Uani 1 1 d . . . C19B C 0.7724(7) 0.5680(3) 0.82646(11) 0.0432(15) Uani 1 1 d . . . H19B H 0.7113 0.5619 0.8423 0.052 Uiso 1 1 calc R . . C20B C 0.8116(8) 0.5146(3) 0.81093(12) 0.0512(18) Uani 1 1 d . . . H20B H 0.7796 0.4717 0.8160 0.061 Uiso 1 1 calc R . . C21B C 0.9004(8) 0.5242(3) 0.78736(12) 0.0482(16) Uani 1 1 d . . . H21B H 0.9293 0.4878 0.7763 0.058 Uiso 1 1 calc R . . C22B C 0.9449(7) 0.5861(3) 0.78045(11) 0.0459(16) Uani 1 1 d . . . H22B H 1.0060 0.5920 0.7646 0.055 Uiso 1 1 calc R . . C23B C 0.9037(7) 0.6408(3) 0.79583(10) 0.0399(15) Uani 1 1 d . . . C24B C 0.8991(8) 0.7279(3) 0.75081(12) 0.0536(18) Uani 1 1 d . . . H24C H 0.9582 0.7625 0.7416 0.064 Uiso 1 1 calc R . . H24D H 0.9242 0.6855 0.7418 0.064 Uiso 1 1 calc R . . C25B C 0.7306(7) 0.7428(3) 0.74475(12) 0.0451(15) Uani 1 1 d . . . H25C H 0.7132 0.7417 0.7242 0.054 Uiso 1 1 calc R . . C26B C 0.6363(9) 0.6920(3) 0.75853(13) 0.0519(18) Uani 1 1 d . . . H26C H 0.6508 0.6926 0.7790 0.062 Uiso 1 1 calc R . . H26D H 0.6599 0.6475 0.7514 0.062 Uiso 1 1 calc R . . C27B C 0.4752(9) 0.7112(3) 0.75098(16) 0.063(2) Uani 1 1 d . . . H27C H 0.4594 0.7050 0.7307 0.075 Uiso 1 1 calc R . . H27D H 0.4065 0.6820 0.7611 0.075 Uiso 1 1 calc R . . S1C S 0.2464(3) 0.24551(12) 0.94677(6) 0.0927(8) Uani 1 1 d . . . N1C N 0.4745(6) 0.1576(2) 0.92005(9) 0.0374(11) Uani 1 1 d . A . H1CA H 0.4053 0.1297 0.9250 0.045 Uiso 1 1 calc R . . O1C O 0.2459(6) 0.2358(2) 1.01576(10) 0.0630(13) Uani 1 1 d . . . C1C C 0.4310(8) 0.2138(3) 0.90422(13) 0.0488(17) Uani 1 1 d . . . H1CT H 0.4305 0.2063 0.8836 0.059 Uiso 0.327(15) 1 calc PR A 2 H1CB H 0.3472 0.2005 0.8920 0.059 Uiso 0.673(15) 1 d PR A 1 C2C C 0.6130(7) 0.1436(3) 0.92803(12) 0.0407(15) Uani 1 1 d . . . S2C S 0.7281(2) -0.05734(9) 0.93194(3) 0.0607(5) Uani 1 1 d D . . N2C N 0.7241(7) 0.1826(2) 0.92109(12) 0.0576(15) Uani 1 1 d . A . O2C O 0.4541(8) -0.1280(3) 1.02416(10) 0.093(2) Uani 1 1 d . . . N3C N 0.0367(7) 0.2629(3) 0.99354(14) 0.0715(18) Uani 1 1 d . . . H3CA H -0.0547 0.2515 0.9902 0.086 Uiso 1 1 calc R . . C3C C 0.6995(10) 0.2379(4) 0.90288(19) 0.077(2) Uani 1 1 d . . . H3CB H 0.6938 0.2236 0.8832 0.092 Uiso 0.327(15) 1 calc PR A 2 H3CC H 0.7788 0.2709 0.9048 0.092 Uiso 0.327(15) 1 calc PR A 2 H3C1 H 0.7872 0.2441 0.8910 0.092 Uiso 0.673(15) 1 d PR A 1 H3C2 H 0.6877 0.2781 0.9144 0.092 Uiso 0.673(15) 1 d PR A 1 C4C C 0.5664(14) 0.2309(4) 0.8844(2) 0.061(4) Uani 0.673(15) 1 d P A 1 H4C1 H 0.5817 0.1953 0.8706 0.073 Uiso 0.673(15) 1 calc PR A 1 H4C2 H 0.5478 0.2724 0.8742 0.073 Uiso 0.673(15) 1 calc PR A 1 N4C N 0.0514(7) 0.1673(3) 1.01844(13) 0.0661(17) Uani 1 1 d . . . H4CA H -0.0434 0.1633 1.0155 0.079 Uiso 1 1 calc R . . C4C' C 0.536(3) 0.2696(10) 0.9137(4) 0.060(7) Uani 0.327(15) 1 d PU A 2 H4CB H 0.5337 0.2758 0.9342 0.072 Uiso 0.327(15) 1 calc PR A 2 H4CC H 0.5135 0.3118 0.9044 0.072 Uiso 0.327(15) 1 calc PR A 2 N5C N 0.3041(9) -0.0733(3) 0.99515(11) 0.069(2) Uani 1 1 d . . . H5NC H 0.2922 -0.0562 0.9785 0.083 Uiso 1 1 calc R . . C5C C 0.3863(11) 0.2742(4) 0.92003(18) 0.043(3) Uani 0.659(15) 1 d P A 1 H5CE H 0.3424 0.3071 0.9073 0.052 Uiso 0.659(15) 1 calc PR A 1 H5CF H 0.4721 0.2943 0.9294 0.052 Uiso 0.659(15) 1 calc PR A 1 C5C' C 0.270(2) 0.2297(9) 0.9173(3) 0.050(7) Uani 0.341(15) 1 d P A 2 H5CC H 0.2293 0.2670 0.9064 0.060 Uiso 0.341(15) 1 calc PR A 2 H5CD H 0.2070 0.1912 0.9131 0.060 Uiso 0.341(15) 1 calc PR A 2 N6C N 0.5381(8) -0.1012(2) 0.98030(10) 0.0576(17) Uani 1 1 d . . . H6NC H 0.5124 -0.0811 0.9648 0.069 Uiso 1 1 calc R . . C6C C 0.1907(8) 0.3219(4) 0.95999(14) 0.0574(19) Uani 1 1 d . A . N7C N 0.6365(6) 0.0893(3) 0.94335(10) 0.0479(13) Uani 1 1 d . A . H7CA H 0.5593 0.0653 0.9476 0.057 Uiso 1 1 calc R . . C7C C 0.2369(8) 0.3816(4) 0.94890(13) 0.064(2) Uani 1 1 d . . . H7C H 0.3069 0.3822 0.9342 0.076 Uiso 1 1 calc R A . C8C C 0.1809(9) 0.4403(4) 0.95919(16) 0.072(2) Uani 1 1 d . A . H8C H 0.2142 0.4812 0.9520 0.086 Uiso 1 1 calc R . . C9C C 0.0768(9) 0.4385(4) 0.97988(16) 0.068(2) Uani 1 1 d . . . H9C H 0.0349 0.4784 0.9864 0.081 Uiso 1 1 calc R A . C10C C 0.0327(8) 0.3801(4) 0.99122(13) 0.0572(18) Uani 1 1 d . A . H10C H -0.0375 0.3802 1.0058 0.069 Uiso 1 1 calc R . . C11C C 0.0880(8) 0.3218(4) 0.98189(13) 0.0548(19) Uani 1 1 d . . . C12C C 0.1170(9) 0.2230(4) 1.00941(14) 0.0554(18) Uani 1 1 d . . . C13C C 0.1238(9) 0.1139(3) 1.03249(14) 0.0602(19) Uani 1 1 d . . . H13E H 0.0709 0.1042 1.0500 0.072 Uiso 1 1 calc R A . H13F H 0.2245 0.1277 1.0374 0.072 Uiso 1 1 calc R . . C14C C 0.1314(9) 0.0519(3) 1.01508(12) 0.0590(19) Uani 1 1 d . A . H14E H 0.0332 0.0424 1.0073 0.071 Uiso 1 1 calc R . . H14F H 0.1994 0.0590 0.9993 0.071 Uiso 1 1 calc R . . C15C C 0.1817(9) -0.0051(3) 1.03161(13) 0.062(2) Uani 1 1 d . . . H15E H 0.1157 -0.0108 1.0478 0.075 Uiso 1 1 calc R A . H15F H 0.2811 0.0042 1.0389 0.075 Uiso 1 1 calc R . . C16C C 0.1859(10) -0.0691(4) 1.01525(14) 0.070(2) Uani 1 1 d . A . H16E H 0.1951 -0.1061 1.0285 0.084 Uiso 1 1 calc R . . H16F H 0.0916 -0.0743 1.0053 0.084 Uiso 1 1 calc R . . C17C C 0.4302(12) -0.1027(3) 1.00140(13) 0.067(2) Uani 1 1 d . . . C18C C 0.6795(10) -0.1271(3) 0.98059(13) 0.056(2) Uani 1 1 d . . . C19C C 0.7232(12) -0.1737(3) 1.00063(14) 0.076(3) Uani 1 1 d . . . H19C H 0.6563 -0.1882 1.0145 0.091 Uiso 1 1 calc R . . C20C C 0.8674(14) -0.1986(3) 0.99987(17) 0.086(4) Uani 1 1 d . . . H20C H 0.8970 -0.2298 1.0135 0.103 Uiso 1 1 calc R A . C21C C 0.9630(12) -0.1796(3) 0.98053(17) 0.078(3) Uani 1 1 d . . . H21C H 1.0597 -0.1969 0.9805 0.093 Uiso 1 1 calc R . . C22C C 0.9210(10) -0.1346(3) 0.96041(15) 0.066(2) Uani 1 1 d . . . H22C H 0.9889 -0.1211 0.9465 0.079 Uiso 1 1 calc R A . C23C C 0.7797(10) -0.1089(3) 0.96046(13) 0.0533(19) Uani 1 1 d . . . C24C C 0.8409(9) 0.0120(3) 0.93502(14) 0.051(2) Uani 0.897(8) 1 d P A 1 H24E H 0.9371 -0.0020 0.9425 0.062 Uiso 0.897(8) 1 calc PR A 1 H24F H 0.8578 0.0305 0.9162 0.062 Uiso 0.897(8) 1 calc PRD A 1 C24' C 0.801(10) -0.0060(10) 0.9586(11) 0.090 Uiso 0.103(8) 1 d PD A 2 H24V H 0.7537 -0.0180 0.9766 0.108 Uiso 0.103(8) 1 calc PR A 2 H24W H 0.9068 -0.0149 0.9604 0.108 Uiso 0.103(8) 1 calc PR A 2 C25C C 0.7790(8) 0.0661(4) 0.95375(12) 0.0569(19) Uani 1 1 d D . . H25G H 0.7962 0.0886 0.9720 0.068 Uiso 0.103(8) 1 calc PR A 2 H25H H 0.7642 0.0474 0.9728 0.068 Uiso 0.897(8) 1 d PR A 1 C26C C 0.8753(10) 0.1252(4) 0.95606(17) 0.065(3) Uani 0.897(8) 1 d P A 1 H26G H 0.9766 0.1111 0.9604 0.077 Uiso 0.897(8) 1 calc PR A 1 H26H H 0.8406 0.1533 0.9716 0.077 Uiso 0.897(8) 1 calc PR A 1 C26' C 0.864(7) 0.107(3) 0.9307(10) 0.050 Uiso 0.103(8) 1 d PD A 2 H26I H 0.9662 0.0906 0.9311 0.060 Uiso 0.103(8) 1 calc PR A 2 H26J H 0.8228 0.0929 0.9126 0.060 Uiso 0.103(8) 1 calc PRD A 2 C27C C 0.8752(8) 0.1654(4) 0.92895(19) 0.072(2) Uani 1 1 d . . . H27G H 0.9333 0.2061 0.9316 0.087 Uiso 0.897(8) 1 calc PR A 1 H27H H 0.9211 0.1394 0.9138 0.087 Uiso 0.897(8) 1 calc PR A 1 H27I H 0.8943 0.1801 0.9476 0.087 Uiso 0.103(8) 1 d PR A 2 H27J H 0.9429 0.1871 0.9167 0.087 Uiso 0.103(8) 1 d PR A 2 N1SA N 0.4149(6) 0.4823(2) 0.89195(9) 0.0363(12) Uani 1 1 d . . . O1SA O 0.5322(6) 0.4857(2) 0.87839(10) 0.0625(13) Uani 1 1 d . . . O2SA O 0.3816(5) 0.52614(19) 0.90873(8) 0.0460(11) Uani 1 1 d . . . O3SA O 0.3321(5) 0.4347(2) 0.88791(8) 0.0498(11) Uani 1 1 d . . . N1SB N 0.8997(6) 0.9461(2) 0.77326(9) 0.0405(12) Uani 1 1 d . . . O2SB O 0.9136(5) 0.9062(2) 0.75359(8) 0.0507(11) Uani 1 1 d . . . O3SB O 0.9996(7) 0.9859(2) 0.77914(10) 0.0704(15) Uani 1 1 d . . . O1SB O 0.7881(5) 0.9449(2) 0.78813(8) 0.0482(11) Uani 1 1 d . . . N1SC N 0.2619(7) 0.0176(3) 0.93517(11) 0.0507(14) Uani 1 1 d . . . O1SC O 0.2287(5) 0.0684(2) 0.92237(10) 0.0630(13) Uani 1 1 d . . . O2SC O 0.3808(7) 0.0129(3) 0.94731(13) 0.096(2) Uani 1 1 d . . . O3SC O 0.1819(7) -0.0303(3) 0.93657(16) 0.101(2) Uani 1 1 d . . . O1W O 0.127(2) 0.6242(10) 0.7153(4) 0.064(5) Uani 0.25 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 N1A 0.027(3) 0.051(3) 0.034(2) 0.004(2) 0.003(2) 0.001(2) O1A 0.121(6) 0.130(5) 0.052(3) -0.024(3) 0.004(3) 0.055(4) S1A 0.0598(14) 0.0455(8) 0.0625(10) 0.0111(7) 0.0170(9) 0.0012(8) C1A 0.027(4) 0.065(4) 0.043(3) 0.014(3) -0.001(3) 0.003(3) S2A 0.0319(11) 0.0454(8) 0.0615(9) -0.0057(7) 0.0012(7) 0.0027(7) C2A 0.025(4) 0.050(3) 0.026(2) 0.000(2) -0.004(2) -0.003(3) N2A 0.034(4) 0.044(3) 0.037(2) -0.003(2) 0.000(2) -0.005(2) O2A 0.018(3) 0.086(3) 0.067(3) -0.001(2) -0.002(2) 0.005(2) C3A 0.023(4) 0.069(4) 0.041(3) 0.001(3) 0.000(3) -0.011(3) N3A 0.091(6) 0.067(4) 0.048(3) 0.004(3) 0.010(3) 0.039(4) C4A 0.022(4) 0.065(4) 0.046(3) 0.005(3) 0.001(3) 0.001(3) N4A 0.100(6) 0.061(4) 0.046(3) -0.009(3) -0.001(3) 0.019(4) N5A 0.019(3) 0.056(3) 0.049(3) 0.007(2) 0.004(2) 0.003(2) C5A 0.038(5) 0.051(4) 0.060(4) 0.011(3) 0.010(3) 0.014(3) N6A 0.012(3) 0.053(3) 0.061(3) 0.003(2) -0.003(2) -0.004(2) C6A 0.054(6) 0.048(4) 0.074(5) 0.015(3) 0.021(4) 0.007(4) N7A 0.023(4) 0.036(2) 0.044(2) 0.0017(19) -0.004(2) -0.002(2) C7A 0.071(7) 0.052(4) 0.099(6) 0.017(4) 0.015(5) 0.004(4) C8A 0.084(8) 0.050(4) 0.109(6) 0.003(4) 0.030(6) 0.017(4) C9A 0.121(10) 0.087(6) 0.077(5) -0.003(5) 0.025(6) 0.044(6) C10A 0.111(9) 0.081(5) 0.053(4) 0.002(4) 0.008(4) 0.039(5) C11A 0.092(7) 0.056(4) 0.047(4) 0.010(3) 0.016(4) 0.017(4) C12A 0.111(8) 0.062(4) 0.044(4) 0.004(3) 0.004(4) 0.026(5) C13A 0.089(7) 0.067(5) 0.058(4) -0.015(3) -0.006(4) -0.003(5) C14A 0.057(6) 0.070(4) 0.038(3) -0.012(3) -0.006(3) 0.007(4) C15A 0.040(5) 0.068(4) 0.034(3) -0.004(3) -0.004(3) 0.004(3) C16A 0.028(4) 0.064(4) 0.045(3) -0.004(3) -0.005(3) 0.017(3) C17A 0.021(4) 0.056(4) 0.053(3) 0.004(3) -0.009(3) 0.010(3) C18A 0.014(4) 0.053(4) 0.062(4) 0.002(3) -0.015(3) 0.004(3) C19A 0.030(5) 0.054(4) 0.074(4) 0.024(3) -0.012(3) -0.001(3) C20A 0.049(5) 0.069(5) 0.064(4) 0.023(3) -0.015(4) -0.003(4) C21A 0.047(5) 0.036(3) 0.084(5) 0.016(3) -0.021(4) -0.003(3) C22A 0.035(5) 0.049(4) 0.074(4) 0.006(3) -0.018(3) 0.004(3) C23A 0.022(4) 0.038(3) 0.069(4) 0.005(3) -0.011(3) 0.001(3) C24A 0.036(4) 0.034(3) 0.050(3) 0.000(2) 0.000(3) -0.002(3) C25A 0.020(4) 0.039(3) 0.040(3) 0.002(2) 0.001(2) 0.002(2) C26A 0.035(4) 0.039(3) 0.040(3) -0.007(2) -0.002(3) -0.001(3) C27A 0.039(4) 0.051(3) 0.035(3) -0.002(2) -0.010(3) -0.010(3) S1B 0.0680(14) 0.0509(8) 0.0434(8) 0.0127(7) 0.0076(8) 0.0196(9) O1B 0.059(4) 0.059(3) 0.043(2) -0.0074(19) 0.006(2) 0.012(2) N1B 0.028(4) 0.046(3) 0.062(3) -0.009(2) -0.010(2) 0.001(2) C1B 0.033(5) 0.062(4) 0.053(3) -0.009(3) -0.005(3) 0.008(3) S2B 0.0381(12) 0.0576(9) 0.0550(9) 0.0136(7) 0.0048(7) 0.0019(8) C2B 0.033(5) 0.046(3) 0.037(3) 0.003(2) -0.003(3) -0.002(3) O2B 0.017(3) 0.048(2) 0.048(2) 0.0023(17) -0.0006(17) 0.0066(18) N2B 0.031(4) 0.045(3) 0.061(3) -0.003(2) 0.004(2) 0.001(3) C3B 0.032(5) 0.065(4) 0.072(4) -0.017(3) -0.003(3) -0.005(3) N3B 0.053(4) 0.060(3) 0.044(3) -0.005(2) 0.004(3) 0.017(3) C4B 0.040(6) 0.084(5) 0.088(5) -0.019(4) -0.023(4) 0.015(4) N4B 0.057(4) 0.059(3) 0.040(3) -0.002(2) 0.000(3) 0.013(3) N5B 0.021(3) 0.051(3) 0.049(3) 0.003(2) 0.005(2) 0.012(2) C5B 0.053(5) 0.072(4) 0.040(3) -0.001(3) -0.005(3) 0.024(4) N6B 0.013(3) 0.061(3) 0.047(3) 0.002(2) 0.002(2) 0.002(2) C6B 0.059(6) 0.044(3) 0.051(3) 0.011(3) 0.004(3) 0.014(3) N7B 0.035(4) 0.037(2) 0.049(3) 0.000(2) 0.003(2) -0.003(2) C7B 0.056(6) 0.038(3) 0.061(4) 0.008(3) 0.003(3) 0.012(3) C8B 0.066(6) 0.045(4) 0.065(4) -0.003(3) 0.010(4) 0.010(3) C9B 0.062(6) 0.062(4) 0.066(4) -0.023(3) 0.003(4) 0.018(4) C10B 0.055(6) 0.068(4) 0.054(4) -0.017(3) -0.002(3) 0.023(4) C11B 0.054(5) 0.035(3) 0.054(3) 0.002(3) -0.003(3) 0.011(3) C12B 0.046(5) 0.040(3) 0.045(3) 0.002(3) 0.002(3) 0.009(3) C13B 0.045(5) 0.058(4) 0.049(3) 0.005(3) -0.001(3) 0.005(3) C14B 0.045(5) 0.043(3) 0.058(4) 0.004(3) 0.007(3) 0.007(3) C15B 0.037(5) 0.045(3) 0.060(4) 0.012(3) 0.006(3) 0.010(3) C16B 0.035(5) 0.048(3) 0.053(3) 0.005(3) 0.001(3) 0.013(3) C17B 0.037(5) 0.050(3) 0.032(3) 0.007(2) 0.006(3) -0.005(3) C18B 0.026(4) 0.067(4) 0.031(3) 0.006(3) -0.006(2) -0.003(3) C19B 0.039(4) 0.059(4) 0.032(3) 0.002(3) -0.003(3) -0.010(3) C20B 0.046(5) 0.058(4) 0.050(4) -0.001(3) -0.010(3) -0.011(3) C21B 0.039(5) 0.060(4) 0.045(3) -0.008(3) -0.018(3) 0.002(3) C22B 0.020(4) 0.079(4) 0.039(3) 0.000(3) -0.002(2) -0.012(3) C23B 0.017(4) 0.067(4) 0.036(3) 0.009(3) -0.003(2) 0.001(3) C24B 0.059(6) 0.059(4) 0.043(3) 0.007(3) 0.011(3) -0.004(4) C25B 0.037(5) 0.048(3) 0.050(3) -0.008(3) 0.009(3) 0.000(3) C26B 0.069(6) 0.033(3) 0.054(3) -0.005(3) 0.000(3) -0.004(3) C27B 0.043(6) 0.056(4) 0.090(5) -0.003(3) -0.001(4) -0.007(4) S1C 0.0417(16) 0.0915(15) 0.145(2) -0.0655(14) 0.0229(13) -0.0105(11) N1C 0.030(4) 0.034(2) 0.048(3) 0.0030(19) 0.006(2) -0.003(2) O1C 0.028(4) 0.082(3) 0.078(3) 0.003(3) -0.005(2) -0.003(3) C1C 0.056(5) 0.035(3) 0.055(3) 0.000(3) 0.003(3) 0.000(3) C2C 0.030(4) 0.040(3) 0.052(3) -0.011(3) 0.011(3) -0.003(3) S2C 0.0681(15) 0.0579(10) 0.0560(9) 0.0127(8) -0.0085(9) 0.0001(9) N2C 0.037(4) 0.040(3) 0.095(4) 0.001(3) 0.006(3) -0.005(3) O2C 0.121(6) 0.105(4) 0.053(3) 0.031(3) -0.011(3) -0.019(4) N3C 0.030(4) 0.075(4) 0.110(5) -0.005(4) -0.008(4) -0.005(3) C3C 0.050(6) 0.066(5) 0.115(6) 0.014(4) 0.007(5) -0.022(4) C4C 0.089(11) 0.024(4) 0.069(6) 0.006(4) 0.023(6) 0.000(5) N4C 0.036(4) 0.073(4) 0.090(4) 0.007(3) -0.002(3) -0.009(3) C4C' 0.048(15) 0.067(12) 0.066(11) 0.009(9) -0.006(10) -0.007(10) N5C 0.102(7) 0.062(4) 0.042(3) 0.014(3) -0.001(3) -0.024(4) C5C 0.035(8) 0.032(5) 0.062(6) 0.001(4) -0.001(4) -0.006(4) C5C' 0.068(17) 0.054(11) 0.028(8) 0.006(7) -0.002(9) 0.014(10) N6C 0.086(6) 0.047(3) 0.040(3) 0.011(2) -0.012(3) -0.023(3) C6C 0.033(5) 0.075(5) 0.064(4) -0.017(4) -0.006(3) 0.011(4) N7C 0.035(4) 0.060(3) 0.049(3) 0.005(2) -0.007(2) -0.008(3) C7C 0.037(5) 0.105(6) 0.048(4) -0.004(4) -0.002(3) 0.017(4) C8C 0.046(6) 0.088(6) 0.081(5) 0.021(4) -0.014(4) 0.014(5) C9C 0.045(6) 0.078(5) 0.079(5) -0.012(4) -0.012(4) 0.021(4) C10C 0.039(5) 0.082(5) 0.051(4) -0.007(3) -0.005(3) 0.016(4) C11C 0.022(4) 0.089(5) 0.053(4) -0.018(4) -0.009(3) 0.013(4) C12C 0.032(5) 0.073(5) 0.061(4) -0.012(4) -0.006(3) -0.001(4) C13C 0.044(5) 0.076(5) 0.061(4) 0.001(4) 0.001(3) -0.017(4) C14C 0.057(5) 0.077(5) 0.043(3) 0.007(3) -0.005(3) -0.022(4) C15C 0.065(6) 0.077(5) 0.045(3) 0.006(3) 0.001(3) -0.029(4) C16C 0.077(7) 0.072(5) 0.061(4) 0.006(4) 0.008(4) -0.040(4) C17C 0.105(8) 0.053(4) 0.043(4) 0.013(3) -0.007(4) -0.031(4) C18C 0.089(7) 0.034(3) 0.045(3) 0.002(3) -0.024(4) -0.017(4) C19C 0.130(9) 0.039(4) 0.058(4) 0.009(3) -0.044(5) -0.018(5) C20C 0.157(11) 0.026(3) 0.076(5) 0.012(3) -0.070(6) -0.003(5) C21C 0.113(9) 0.039(4) 0.082(5) 0.008(4) -0.044(6) 0.010(4) C22C 0.084(7) 0.040(4) 0.074(5) -0.012(3) -0.028(4) -0.007(4) C23C 0.081(6) 0.029(3) 0.050(3) 0.000(2) -0.020(4) -0.003(3) C24C 0.056(6) 0.054(4) 0.044(4) 0.010(3) -0.001(3) 0.003(4) C25C 0.040(5) 0.088(5) 0.042(3) -0.017(3) -0.006(3) 0.009(4) C26C 0.058(7) 0.049(4) 0.087(6) -0.016(4) -0.031(5) 0.008(4) C27C 0.019(5) 0.065(5) 0.133(7) -0.014(5) -0.006(4) 0.000(3) N1SA 0.029(4) 0.040(3) 0.040(2) 0.001(2) -0.005(2) 0.001(2) O1SA 0.029(3) 0.084(3) 0.075(3) -0.033(2) 0.010(2) -0.007(3) O2SA 0.033(3) 0.050(2) 0.056(2) -0.012(2) 0.008(2) -0.005(2) O3SA 0.045(3) 0.050(2) 0.054(2) -0.0043(19) 0.001(2) -0.013(2) N1SB 0.034(4) 0.046(3) 0.042(3) -0.002(2) 0.008(2) -0.002(2) O2SB 0.052(3) 0.050(2) 0.050(2) -0.0104(19) 0.012(2) -0.005(2) O3SB 0.064(4) 0.074(3) 0.074(3) -0.020(2) 0.023(3) -0.022(3) O1SB 0.034(3) 0.060(3) 0.051(2) -0.0096(19) 0.004(2) -0.003(2) N1SC 0.029(4) 0.056(3) 0.067(3) 0.015(3) 0.008(3) -0.002(3) O1SC 0.037(3) 0.053(3) 0.099(4) 0.013(2) -0.004(3) -0.002(2) O2SC 0.054(5) 0.112(5) 0.123(5) 0.071(4) -0.030(4) -0.035(3) O3SC 0.055(5) 0.062(3) 0.185(6) 0.043(4) -0.018(4) -0.019(3) O1W 0.034(13) 0.092(14) 0.067(11) -0.017(10) 0.010(9) 0.035(11) _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 N1A C2A 1.341(7) . ? N1A C1A 1.456(8) . ? O1A C12A 1.222(8) . ? S1A C6A 1.783(7) . ? S1A C5A 1.801(7) . ? C1A C4A 1.508(9) . ? C1A C5A 1.519(9) . ? S2A C23A 1.781(6) . ? S2A C24A 1.830(6) . ? C2A N7A 1.327(7) . ? C2A N2A 1.337(7) . ? N2A C3A 1.464(8) . ? N2A C27A 1.473(7) . ? O2A C17A 1.243(8) . ? C3A C4A 1.510(8) . ? N3A C12A 1.373(11) . ? N3A C11A 1.410(10) . ? N4A C12A 1.362(11) . ? N4A C13A 1.465(10) . ? N5A C17A 1.344(8) . ? N5A C16A 1.432(7) . ? N6A C17A 1.350(8) . ? N6A C18A 1.398(8) . ? C6A C7A 1.369(11) . ? C6A C11A 1.410(11) . ? N7A C25A 1.469(7) . ? C7A C8A 1.364(11) . ? C8A C9A 1.379(13) . ? C9A C10A 1.403(13) . ? C10A C11A 1.391(10) . ? C13A C14A 1.504(10) . ? C14A C15A 1.530(8) . ? C15A C16A 1.504(9) . ? C18A C23A 1.395(8) . ? C18A C19A 1.405(9) . ? C19A C20A 1.342(10) . ? C20A C21A 1.376(9) . ? C21A C22A 1.397(10) . ? C22A C23A 1.389(8) . ? C24A C25A 1.514(9) . ? C25A C26A 1.528(7) . ? C26A C27A 1.495(9) . ? S1B C5B 1.791(8) . ? S1B C6B 1.799(6) . ? O1B C12B 1.227(6) . ? N1B C2B 1.325(7) . ? N1B C1B 1.470(8) . ? C1B C5B 1.487(9) . ? C1B C4B 1.534(10) . ? S2B C24B 1.788(6) . ? S2B C23B 1.800(6) . ? C2B N7B 1.321(8) . ? C2B N2B 1.322(8) . ? O2B C17B 1.238(7) . ? N2B C3B 1.458(9) . ? N2B C27B 1.473(8) . ? C3B C4B 1.459(10) . ? N3B C11B 1.400(9) . ? N3B C12B 1.404(8) . ? N4B C12B 1.331(8) . ? N4B C13B 1.464(8) . ? N5B C17B 1.361(7) . ? N5B C16B 1.450(8) . ? N6B C17B 1.357(8) . ? N6B C18B 1.404(8) . ? C6B C7B 1.398(10) . ? C6B C11B 1.403(9) . ? N7B C25B 1.462(7) . ? C7B C8B 1.373(9) . ? C8B C9B 1.390(10) . ? C9B C10B 1.351(10) . ? C10B C11B 1.402(9) . ? C13B C14B 1.516(9) . ? C14B C15B 1.542(9) . ? C15B C16B 1.532(8) . ? C18B C19B 1.380(8) . ? C18B C23B 1.403(8) . ? C19B C20B 1.365(9) . ? C20B C21B 1.405(9) . ? C21B C22B 1.362(9) . ? C22B C23B 1.385(9) . ? C24B C25B 1.594(10) . ? C25B C26B 1.497(9) . ? C26B C27B 1.564(11) . ? S1C C5C' 1.467(15) . ? S1C C6C 1.751(7) . ? S1C C5C 1.901(10) . ? N1C C2C 1.351(8) . ? N1C C1C 1.428(7) . ? O1C C12C 1.242(9) . ? C1C C5C 1.499(10) . ? C1C C4C' 1.55(2) . ? C1C C4C 1.596(12) . ? C1C C5C' 1.63(2) . ? C2C N2C 1.329(8) . ? C2C N7C 1.343(8) . ? S2C C24C 1.752(8) . ? S2C C24' 1.78(2) . ? S2C C23C 1.786(6) . ? N2C C3C 1.441(9) . ? N2C C27C 1.472(10) . ? O2C C17C 1.226(8) . ? N3C C12C 1.332(9) . ? N3C C11C 1.402(10) . ? C3C C4C 1.509(14) . ? C3C C4C' 1.70(3) . ? N4C C12C 1.352(9) . ? N4C C13C 1.437(9) . ? N5C C17C 1.330(11) . ? N5C C16C 1.449(10) . ? N6C C18C 1.394(10) . ? N6C C17C 1.412(10) . ? C6C C7C 1.390(10) . ? C6C C11C 1.408(10) . ? N7C C25C 1.470(9) . ? C7C C8C 1.388(11) . ? C8C C9C 1.374(11) . ? C9C C10C 1.365(10) . ? C10C C11C 1.363(9) . ? C13C C14C 1.513(9) . ? C14C C15C 1.478(10) . ? C15C C16C 1.518(10) . ? C18C C23C 1.380(11) . ? C18C C19C 1.407(9) . ? C19C C20C 1.410(14) . ? C20C C21C 1.331(14) . ? C21C C22C 1.385(10) . ? C22C C23C 1.390(11) . ? C24C C25C 1.527(10) . ? C24' C25C 1.50(2) . ? C25C C26C 1.493(11) . ? C25C C26' 1.59(2) . ? C26C C27C 1.535(11) . ? C26' C27C 1.19(5) . ? N1SA O2SA 1.239(6) . ? N1SA O3SA 1.241(6) . ? N1SA O1SA 1.254(6) . ? N1SB O1SB 1.244(6) . ? N1SB O2SB 1.250(6) . ? N1SB O3SB 1.251(7) . ? N1SC O3SC 1.218(7) . ? N1SC O2SC 1.235(7) . ? N1SC O1SC 1.239(7) . ? 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 C2A N1A C1A 122.3(5) . . ? C6A S1A C5A 99.3(3) . . ? N1A C1A C4A 107.5(5) . . ? N1A C1A C5A 109.4(5) . . ? C4A C1A C5A 110.6(5) . . ? C23A S2A C24A 102.8(3) . . ? N7A C2A N2A 120.2(5) . . ? N7A C2A N1A 119.0(5) . . ? N2A C2A N1A 120.7(6) . . ? C2A N2A C3A 122.3(5) . . ? C2A N2A C27A 121.7(5) . . ? C3A N2A C27A 115.7(5) . . ? N2A C3A C4A 111.3(5) . . ? C12A N3A C11A 127.1(6) . . ? C1A C4A C3A 110.7(5) . . ? C12A N4A C13A 121.7(6) . . ? C17A N5A C16A 123.4(6) . . ? C1A C5A S1A 111.8(4) . . ? C17A N6A C18A 124.1(6) . . ? C7A C6A C11A 119.9(7) . . ? C7A C6A S1A 118.5(7) . . ? C11A C6A S1A 121.5(6) . . ? C2A N7A C25A 121.6(5) . . ? C8A C7A C6A 123.1(9) . . ? C7A C8A C9A 117.9(9) . . ? C8A C9A C10A 121.1(8) . . ? C11A C10A C9A 120.2(9) . . ? C10A C11A N3A 122.5(8) . . ? C10A C11A C6A 117.9(8) . . ? N3A C11A C6A 119.6(6) . . ? O1A C12A N4A 123.5(8) . . ? O1A C12A N3A 123.0(9) . . ? N4A C12A N3A 113.5(6) . . ? N4A C13A C14A 112.0(7) . . ? C13A C14A C15A 115.2(5) . . ? C16A C15A C14A 111.7(5) . . ? N5A C16A C15A 112.4(5) . . ? O2A C17A N5A 121.7(6) . . ? O2A C17A N6A 121.8(6) . . ? N5A C17A N6A 116.5(6) . . ? C23A C18A N6A 120.2(6) . . ? C23A C18A C19A 117.6(6) . . ? N6A C18A C19A 122.2(6) . . ? C20A C19A C18A 123.1(7) . . ? C19A C20A C21A 119.5(7) . . ? C20A C21A C22A 119.7(6) . . ? C23A C22A C21A 120.5(6) . . ? C22A C23A C18A 119.4(6) . . ? C22A C23A S2A 117.1(5) . . ? C18A C23A S2A 123.4(5) . . ? C25A C24A S2A 114.1(4) . . ? N7A C25A C24A 107.7(5) . . ? N7A C25A C26A 107.1(4) . . ? C24A C25A C26A 116.0(5) . . ? C27A C26A C25A 109.2(4) . . ? N2A C27A C26A 113.8(5) . . ? C5B S1B C6B 101.7(3) . . ? C2B N1B C1B 125.3(5) . . ? N1B C1B C5B 110.8(6) . . ? N1B C1B C4B 108.1(5) . . ? C5B C1B C4B 109.6(6) . . ? C24B S2B C23B 102.1(3) . . ? N7B C2B N2B 121.8(5) . . ? N7B C2B N1B 118.0(6) . . ? N2B C2B N1B 120.1(6) . . ? C2B N2B C3B 121.4(5) . . ? C2B N2B C27B 120.8(6) . . ? C3B N2B C27B 117.9(5) . . ? N2B C3B C4B 111.1(6) . . ? C11B N3B C12B 128.2(5) . . ? C3B C4B C1B 112.1(6) . . ? C12B N4B C13B 121.5(5) . . ? C17B N5B C16B 121.2(5) . . ? C1B C5B S1B 116.4(5) . . ? C17B N6B C18B 121.9(5) . . ? C7B C6B C11B 121.0(6) . . ? C7B C6B S1B 119.7(5) . . ? C11B C6B S1B 119.3(6) . . ? C2B N7B C25B 122.0(5) . . ? C8B C7B C6B 119.7(7) . . ? C7B C8B C9B 119.8(8) . . ? C10B C9B C8B 120.6(7) . . ? C9B C10B C11B 121.9(7) . . ? N3B C11B C10B 123.8(6) . . ? N3B C11B C6B 119.2(6) . . ? C10B C11B C6B 117.0(7) . . ? O1B C12B N4B 124.2(6) . . ? O1B C12B N3B 122.5(6) . . ? N4B C12B N3B 113.3(5) . . ? N4B C13B C14B 110.8(5) . . ? C13B C14B C15B 114.2(6) . . ? C16B C15B C14B 112.8(5) . . ? N5B C16B C15B 111.8(5) . . ? O2B C17B N6B 121.5(6) . . ? O2B C17B N5B 122.0(6) . . ? N6B C17B N5B 116.4(6) . . ? C19B C18B C23B 119.5(6) . . ? C19B C18B N6B 119.8(5) . . ? C23B C18B N6B 120.6(5) . . ? C20B C19B C18B 121.9(6) . . ? C19B C20B C21B 118.6(6) . . ? C22B C21B C20B 119.8(6) . . ? C21B C22B C23B 122.0(6) . . ? C22B C23B C18B 118.0(6) . . ? C22B C23B S2B 123.1(4) . . ? C18B C23B S2B 118.9(5) . . ? C25B C24B S2B 117.3(4) . . ? N7B C25B C26B 108.5(5) . . ? N7B C25B C24B 110.6(5) . . ? C26B C25B C24B 110.1(5) . . ? C25B C26B C27B 105.4(5) . . ? N2B C27B C26B 111.1(6) . . ? C5C' S1C C6C 125.8(8) . . ? C5C' S1C C5C 47.1(9) . . ? C6C S1C C5C 99.6(4) . . ? C2C N1C C1C 125.3(5) . . ? N1C C1C C5C 117.5(6) . . ? N1C C1C C4C' 104.9(10) . . ? C5C C1C C4C' 54.7(10) . . ? N1C C1C C4C 106.0(6) . . ? C5C C1C C4C 109.5(6) . . ? C4C' C1C C4C 62.5(10) . . ? N1C C1C C5C' 101.8(7) . . ? C5C C1C C5C' 53.0(8) . . ? C4C' C1C C5C' 107.5(12) . . ? C4C C1C C5C' 152.0(8) . . ? N2C C2C N7C 120.4(6) . . ? N2C C2C N1C 121.1(6) . . ? N7C C2C N1C 118.5(5) . . ? C24C S2C C24' 41(3) . . ? C24C S2C C23C 104.6(3) . . ? C24' S2C C23C 72.2(10) . . ? C2C N2C C3C 119.9(6) . . ? C2C N2C C27C 120.5(6) . . ? C3C N2C C27C 119.1(6) . . ? C12C N3C C11C 124.3(7) . . ? N2C C3C C4C 114.0(6) . . ? N2C C3C C4C' 104.2(9) . . ? C4C C3C C4C' 60.7(9) . . ? C3C C4C C1C 107.1(7) . . ? C12C N4C C13C 125.3(7) . . ? C1C C4C' C3C 100.1(13) . . ? C17C N5C C16C 121.4(6) . . ? C1C C5C S1C 105.8(5) . . ? S1C C5C' C1C 122.9(13) . . ? C18C N6C C17C 129.1(6) . . ? C7C C6C C11C 119.2(6) . . ? C7C C6C S1C 123.2(6) . . ? C11C C6C S1C 117.6(6) . . ? C2C N7C C25C 126.1(6) . . ? C8C C7C C6C 120.2(7) . . ? C9C C8C C7C 119.2(8) . . ? C10C C9C C8C 121.0(7) . . ? C11C C10C C9C 121.0(7) . . ? C10C C11C N3C 119.2(7) . . ? C10C C11C C6C 119.4(7) . . ? N3C C11C C6C 121.3(6) . . ? O1C C12C N3C 122.3(7) . . ? O1C C12C N4C 121.1(7) . . ? N3C C12C N4C 116.6(7) . . ? N4C C13C C14C 113.0(6) . . ? C15C C14C C13C 111.8(5) . . ? C14C C15C C16C 113.7(6) . . ? N5C C16C C15C 114.5(6) . . ? O2C C17C N5C 122.8(8) . . ? O2C C17C N6C 121.5(9) . . ? N5C C17C N6C 115.6(6) . . ? C23C C18C N6C 120.4(6) . . ? C23C C18C C19C 118.1(9) . . ? N6C C18C C19C 121.5(8) . . ? C18C C19C C20C 119.3(9) . . ? C21C C20C C19C 121.7(7) . . ? C20C C21C C22C 119.8(9) . . ? C21C C22C C23C 120.2(9) . . ? C18C C23C C22C 121.0(6) . . ? C18C C23C S2C 121.2(6) . . ? C22C C23C S2C 117.6(6) . . ? C25C C24C S2C 114.2(6) . . ? C25C C24' S2C 114.4(16) . . ? N7C C25C C26C 106.7(6) . . ? N7C C25C C24' 119(3) . . ? C26C C25C C24' 134(3) . . ? N7C C25C C24C 111.0(5) . . ? C26C C25C C24C 113.9(7) . . ? C24' C25C C24C 49(3) . . ? N7C C25C C26' 92(3) . . ? C26C C25C C26' 49(2) . . ? C24' C25C C26' 124(4) . . ? C24C C25C C26' 78(2) . . ? C25C C26C C27C 111.4(6) . . ? C27C C26' C25C 128(4) . . ? C26' C27C N2C 100(3) . . ? C26' C27C C26C 54(3) . . ? N2C C27C C26C 110.1(7) . . ? O2SA N1SA O3SA 120.8(5) . . ? O2SA N1SA O1SA 120.4(5) . . ? O3SA N1SA O1SA 118.8(5) . . ? O1SB N1SB O2SB 120.2(5) . . ? O1SB N1SB O3SB 118.6(5) . . ? O2SB N1SB O3SB 121.0(5) . . ? O3SC N1SC O2SC 116.0(6) . . ? O3SC N1SC O1SC 123.1(6) . . ? O2SC N1SC O1SC 120.9(6) . . ? 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 C2A N1A C1A C4A -36.8(6) . . . . ? C2A N1A C1A C5A -156.9(5) . . . . ? C1A N1A C2A N7A -176.2(4) . . . . ? C1A N1A C2A N2A 5.8(7) . . . . ? N7A C2A N2A C3A -172.4(5) . . . . ? N1A C2A N2A C3A 5.5(7) . . . . ? N7A C2A N2A C27A 14.3(7) . . . . ? N1A C2A N2A C27A -167.8(4) . . . . ? C2A N2A C3A C4A 16.4(7) . . . . ? C27A N2A C3A C4A -169.9(4) . . . . ? N1A C1A C4A C3A 56.2(6) . . . . ? C5A C1A C4A C3A 175.5(5) . . . . ? N2A C3A C4A C1A -47.5(7) . . . . ? N1A C1A C5A S1A -61.8(6) . . . . ? C4A C1A C5A S1A 179.9(4) . . . . ? C6A S1A C5A C1A 173.5(5) . . . . ? C5A S1A C6A C7A 75.9(6) . . . . ? C5A S1A C6A C11A -108.8(6) . . . . ? N2A C2A N7A C25A 6.0(7) . . . . ? N1A C2A N7A C25A -172.0(4) . . . . ? C11A C6A C7A C8A 0.9(11) . . . . ? S1A C6A C7A C8A 176.4(6) . . . . ? C6A C7A C8A C9A -1.1(12) . . . . ? C7A C8A C9A C10A 0.6(14) . . . . ? C8A C9A C10A C11A 0.0(14) . . . . ? C9A C10A C11A N3A -178.5(8) . . . . ? C9A C10A C11A C6A -0.3(12) . . . . ? C12A N3A C11A C10A -9.2(12) . . . . ? C12A N3A C11A C6A 172.6(7) . . . . ? C7A C6A C11A C10A -0.2(10) . . . . ? S1A C6A C11A C10A -175.5(6) . . . . ? C7A C6A C11A N3A 178.1(6) . . . . ? S1A C6A C11A N3A 2.8(9) . . . . ? C13A N4A C12A O1A -11.6(12) . . . . ? C13A N4A C12A N3A 168.6(6) . . . . ? C11A N3A C12A O1A -11.1(13) . . . . ? C11A N3A C12A N4A 168.8(7) . . . . ? C12A N4A C13A C14A -88.5(8) . . . . ? N4A C13A C14A C15A -68.4(9) . . . . ? C13A C14A C15A C16A 175.7(7) . . . . ? C17A N5A C16A C15A 121.5(6) . . . . ? C14A C15A C16A N5A 175.9(6) . . . . ? C16A N5A C17A O2A 2.4(9) . . . . ? C16A N5A C17A N6A -178.1(5) . . . . ? C18A N6A C17A O2A 8.3(9) . . . . ? C18A N6A C17A N5A -171.3(5) . . . . ? C17A N6A C18A C23A -140.6(6) . . . . ? C17A N6A C18A C19A 41.5(9) . . . . ? C23A C18A C19A C20A -1.9(10) . . . . ? N6A C18A C19A C20A 176.0(6) . . . . ? C18A C19A C20A C21A -2.0(11) . . . . ? C19A C20A C21A C22A 3.5(11) . . . . ? C20A C21A C22A C23A -1.1(10) . . . . ? C21A C22A C23A C18A -2.9(9) . . . . ? C21A C22A C23A S2A 178.3(5) . . . . ? N6A C18A C23A C22A -173.7(6) . . . . ? C19A C18A C23A C22A 4.3(9) . . . . ? N6A C18A C23A S2A 5.1(8) . . . . ? C19A C18A C23A S2A -176.9(5) . . . . ? C24A S2A C23A C22A -126.3(5) . . . . ? C24A S2A C23A C18A 54.8(6) . . . . ? C23A S2A C24A C25A 44.9(5) . . . . ? C2A N7A C25A C24A -167.6(5) . . . . ? C2A N7A C25A C26A -42.1(6) . . . . ? S2A C24A C25A N7A -176.0(3) . . . . ? S2A C24A C25A C26A 64.0(6) . . . . ? N7A C25A C26A C27A 57.2(6) . . . . ? C24A C25A C26A C27A 177.6(5) . . . . ? C2A N2A C27A C26A 5.6(7) . . . . ? C3A N2A C27A C26A -168.1(5) . . . . ? C25A C26A C27A N2A -41.5(6) . . . . ? C2B N1B C1B C5B -133.8(6) . . . . ? C2B N1B C1B C4B -13.6(8) . . . . ? C1B N1B C2B N7B 171.1(5) . . . . ? C1B N1B C2B N2B -10.6(9) . . . . ? N7B C2B N2B C3B -179.1(5) . . . . ? N1B C2B N2B C3B 2.7(8) . . . . ? N7B C2B N2B C27B 1.7(9) . . . . ? N1B C2B N2B C27B -176.6(5) . . . . ? C2B N2B C3B C4B 29.7(8) . . . . ? C27B N2B C3B C4B -151.1(6) . . . . ? N2B C3B C4B C1B -53.1(8) . . . . ? N1B C1B C4B C3B 44.8(8) . . . . ? C5B C1B C4B C3B 165.7(7) . . . . ? N1B C1B C5B S1B -57.0(6) . . . . ? C4B C1B C5B S1B -176.2(5) . . . . ? C6B S1B C5B C1B -78.9(6) . . . . ? C5B S1B C6B C7B -48.0(6) . . . . ? C5B S1B C6B C11B 130.2(5) . . . . ? N2B C2B N7B C25B 5.9(8) . . . . ? N1B C2B N7B C25B -175.8(5) . . . . ? C11B C6B C7B C8B 0.1(9) . . . . ? S1B C6B C7B C8B 178.4(5) . . . . ? C6B C7B C8B C9B 0.5(10) . . . . ? C7B C8B C9B C10B 0.4(11) . . . . ? C8B C9B C10B C11B -2.0(12) . . . . ? C12B N3B C11B C10B 6.4(10) . . . . ? C12B N3B C11B C6B -175.3(6) . . . . ? C9B C10B C11B N3B -179.1(7) . . . . ? C9B C10B C11B C6B 2.6(10) . . . . ? C7B C6B C11B N3B 179.9(6) . . . . ? S1B C6B C11B N3B 1.7(8) . . . . ? C7B C6B C11B C10B -1.6(9) . . . . ? S1B C6B C11B C10B -179.8(5) . . . . ? C13B N4B C12B O1B 9.4(10) . . . . ? C13B N4B C12B N3B -170.2(5) . . . . ? C11B N3B C12B O1B -14.5(10) . . . . ? C11B N3B C12B N4B 165.1(6) . . . . ? C12B N4B C13B C14B 160.2(6) . . . . ? N4B C13B C14B C15B -60.0(7) . . . . ? C13B C14B C15B C16B -66.3(7) . . . . ? C17B N5B C16B C15B 75.2(6) . . . . ? C14B C15B C16B N5B 170.3(5) . . . . ? C18B N6B C17B O2B -17.5(8) . . . . ? C18B N6B C17B N5B 165.0(5) . . . . ? C16B N5B C17B O2B 9.5(8) . . . . ? C16B N5B C17B N6B -173.0(5) . . . . ? C17B N6B C18B C19B 126.2(6) . . . . ? C17B N6B C18B C23B -56.8(7) . . . . ? C23B C18B C19B C20B 2.8(9) . . . . ? N6B C18B C19B C20B 179.9(6) . . . . ? C18B C19B C20B C21B -0.8(10) . . . . ? C19B C20B C21B C22B -0.2(10) . . . . ? C20B C21B C22B C23B -0.9(10) . . . . ? C21B C22B C23B C18B 2.7(9) . . . . ? C21B C22B C23B S2B -177.5(5) . . . . ? C19B C18B C23B C22B -3.6(9) . . . . ? N6B C18B C23B C22B 179.3(5) . . . . ? C19B C18B C23B S2B 176.6(5) . . . . ? N6B C18B C23B S2B -0.5(8) . . . . ? C24B S2B C23B C22B 51.7(6) . . . . ? C24B S2B C23B C18B -128.6(5) . . . . ? C23B S2B C24B C25B 81.8(5) . . . . ? C2B N7B C25B C26B -39.0(7) . . . . ? C2B N7B C25B C24B -159.8(5) . . . . ? S2B C24B C25B N7B 62.5(6) . . . . ? S2B C24B C25B C26B -57.3(6) . . . . ? N7B C25B C26B C27B 59.4(6) . . . . ? C24B C25B C26B C27B -179.5(5) . . . . ? C2B N2B C27B C26B 23.8(8) . . . . ? C3B N2B C27B C26B -155.5(6) . . . . ? C25B C26B C27B N2B -53.5(7) . . . . ? C2C N1C C1C C5C -91.3(8) . . . . ? C2C N1C C1C C4C' -33.7(11) . . . . ? C2C N1C C1C C4C 31.4(8) . . . . ? C2C N1C C1C C5C' -145.6(8) . . . . ? C1C N1C C2C N2C -0.9(8) . . . . ? C1C N1C C2C N7C 178.8(5) . . . . ? N7C C2C N2C C3C 175.2(6) . . . . ? N1C C2C N2C C3C -5.2(9) . . . . ? N7C C2C N2C C27C 2.9(9) . . . . ? N1C C2C N2C C27C -177.5(6) . . . . ? C2C N2C C3C C4C -23.6(10) . . . . ? C27C N2C C3C C4C 148.9(7) . . . . ? C2C N2C C3C C4C' 40.4(11) . . . . ? C27C N2C C3C C4C' -147.2(10) . . . . ? N2C C3C C4C C1C 52.7(9) . . . . ? C4C' C3C C4C C1C -40.7(9) . . . . ? N1C C1C C4C C3C -54.0(7) . . . . ? C5C C1C C4C C3C 73.7(8) . . . . ? C4C' C1C C4C C3C 44.7(11) . . . . ? C5C' C1C C4C C3C 119.8(18) . . . . ? N1C C1C C4C' C3C 63.3(11) . . . . ? C5C C1C C4C' C3C 176.8(15) . . . . ? C4C C1C C4C' C3C -37.2(8) . . . . ? C5C' C1C C4C' C3C 171.2(9) . . . . ? N2C C3C C4C' C1C -69.3(11) . . . . ? C4C C3C C4C' C1C 40.6(8) . . . . ? N1C C1C C5C S1C -50.4(8) . . . . ? C4C' C1C C5C S1C -139.6(12) . . . . ? C4C C1C C5C S1C -171.3(6) . . . . ? C5C' C1C C5C S1C 33.7(7) . . . . ? C5C' S1C C5C C1C -42.4(11) . . . . ? C6C S1C C5C C1C -173.1(6) . . . . ? C6C S1C C5C' C1C 112.3(12) . . . . ? C5C S1C C5C' C1C 45.1(12) . . . . ? N1C C1C C5C' S1C 60.1(15) . . . . ? C5C C1C C5C' S1C -55.5(13) . . . . ? C4C' C1C C5C' S1C -49.8(17) . . . . ? C4C C1C C5C' S1C -113.7(17) . . . . ? C5C' S1C C6C C7C -37.1(13) . . . . ? C5C S1C C6C C7C 6.1(7) . . . . ? C5C' S1C C6C C11C 139.3(12) . . . . ? C5C S1C C6C C11C -177.5(6) . . . . ? N2C C2C N7C C25C -0.7(9) . . . . ? N1C C2C N7C C25C 179.7(5) . . . . ? C11C C6C C7C C8C -0.6(11) . . . . ? S1C C6C C7C C8C 175.7(6) . . . . ? C6C C7C C8C C9C -1.7(11) . . . . ? C7C C8C C9C C10C 2.9(12) . . . . ? C8C C9C C10C C11C -1.6(11) . . . . ? C9C C10C C11C N3C -178.2(7) . . . . ? C9C C10C C11C C6C -0.8(10) . . . . ? C12C N3C C11C C10C -112.0(8) . . . . ? C12C N3C C11C C6C 70.7(9) . . . . ? C7C C6C C11C C10C 1.9(10) . . . . ? S1C C6C C11C C10C -174.6(5) . . . . ? C7C C6C C11C N3C 179.2(7) . . . . ? S1C C6C C11C N3C 2.7(9) . . . . ? C11C N3C C12C O1C 1.5(11) . . . . ? C11C N3C C12C N4C -178.5(6) . . . . ? C13C N4C C12C O1C -8.8(11) . . . . ? C13C N4C C12C N3C 171.2(6) . . . . ? C12C N4C C13C C14C -111.4(8) . . . . ? N4C C13C C14C C15C -169.8(7) . . . . ? C13C C14C C15C C16C 178.0(7) . . . . ? C17C N5C C16C C15C 95.4(8) . . . . ? C14C C15C C16C N5C 72.9(9) . . . . ? C16C N5C C17C O2C 0.5(11) . . . . ? C16C N5C C17C N6C -177.7(5) . . . . ? C18C N6C C17C O2C 1.5(10) . . . . ? C18C N6C C17C N5C 179.8(6) . . . . ? C17C N6C C18C C23C -166.1(6) . . . . ? C17C N6C C18C C19C 16.0(9) . . . . ? C23C C18C C19C C20C 1.6(9) . . . . ? N6C C18C C19C C20C 179.6(6) . . . . ? C18C C19C C20C C21C -0.6(10) . . . . ? C19C C20C C21C C22C -0.4(11) . . . . ? C20C C21C C22C C23C 0.4(10) . . . . ? N6C C18C C23C C22C -179.7(5) . . . . ? C19C C18C C23C C22C -1.7(9) . . . . ? N6C C18C C23C S2C -5.1(8) . . . . ? C19C C18C C23C S2C 172.9(4) . . . . ? C21C C22C C23C C18C 0.7(9) . . . . ? C21C C22C C23C S2C -174.0(5) . . . . ? C24C S2C C23C C18C 120.1(5) . . . . ? C24' S2C C23C C18C 94(4) . . . . ? C24C S2C C23C C22C -65.2(5) . . . . ? C24' S2C C23C C22C -91(4) . . . . ? C24' S2C C24C C25C -48(3) . . . . ? C23C S2C C24C C25C -87.7(6) . . . . ? C24C S2C C24' C25C 50(4) . . . . ? C23C S2C C24' C25C -170(7) . . . . ? C2C N7C C25C C26C 25.7(8) . . . . ? C2C N7C C25C C24' -152(3) . . . . ? C2C N7C C25C C24C -98.9(7) . . . . ? C2C N7C C25C C26' -21(2) . . . . ? S2C C24' C25C N7C 43(7) . . . . ? S2C C24' C25C C26C -134(3) . . . . ? S2C C24' C25C C24C -51(3) . . . . ? S2C C24' C25C C26' -71(7) . . . . ? S2C C24C C25C N7C -59.1(7) . . . . ? S2C C24C C25C C26C -179.5(5) . . . . ? S2C C24C C25C C24' 52(4) . . . . ? S2C C24C C25C C26' -146(3) . . . . ? N7C C25C C26C C27C -50.8(8) . . . . ? C24' C25C C26C C27C 127(4) . . . . ? C24C C25C C26C C27C 72.0(8) . . . . ? C26' C25C C26C C27C 26(3) . . . . ? N7C C25C C26' C27C 69(6) . . . . ? C26C C25C C26' C27C -42(5) . . . . ? C24' C25C C26' C27C -164(5) . . . . ? C24C C25C C26' C27C 180(7) . . . . ? C25C C26' C27C N2C -70(6) . . . . ? C25C C26' C27C C26C 37(4) . . . . ? C2C N2C C27C C26' 26(2) . . . . ? C3C N2C C27C C26' -147(2) . . . . ? C2C N2C C27C C26C -29.5(9) . . . . ? C3C N2C C27C C26C 158.0(6) . . . . ? C25C C26C C27C C26' -33(4) . . . . ? C25C C26C C27C N2C 54.8(9) . . . . ? _diffrn_measured_fraction_theta_max 0.947 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.947 _refine_diff_density_max 1.278 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.067 #===END data_pbl152az2 _database_code_depnum_ccdc_archive 'CCDC 635652' _ccdc_compound_id 1 _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ? _ccdc_disorder 1 _ccdc_comments ? _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H38 N8 O5 S2' _chemical_formula_weight 630.78 _chemical_absolute_configuration rmad 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 P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.8570(15) _cell_length_b 12.4706(16) _cell_length_c 12.9263(16) _cell_angle_alpha 98.088(3) _cell_angle_beta 112.786(3) _cell_angle_gamma 107.966(3) _cell_volume 1465.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8979 _cell_measurement_theta_min 3.79 _cell_measurement_theta_max 39.40 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.892350 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38109 _diffrn_reflns_av_R_equivalents 0.0804 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 39.44 _reflns_number_total 22507 _reflns_number_gt 20146 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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. The different data obtained for the described compound corresponded always to the overlap of the reflections of more than one crystal. The best R1-value (Fo > 4sigmaFo) reached was not lower than 0.11. Using the program Gemini (Gemini, Autoindexing Program for Twinned Crystals, Vers. 10.02 Release 5 2000; Bruker AXS Inc., Madison, Wisconsin (USA)) the overlapped data of two crystals could be first separated for integration and later refined as one data set taking in account the overlapping reflections. If only the reflections with not overlap were considered the R1-value (Fo > 4sigmaFo) reached for 6182 independent reflections was of 0.0686. If a factor was included for reflections overlapping more than 50 percent a R1-value (Fo > 4sigmaFo) of 0.812 (20146 reflections) was reached. If different factors were applied in correlation with the different degrees of overlapping of the reflections a R1-value (Fo > 4sigmaFo) of 0.931 (35238 reflections) could be reached. For the structure description the refinement model with one overlapping factor was used. Additionlly to the described overlapping of crystals the structure shows pseudosymmetry from P1 to P-1, being, for a chiral structure, the correct space group P1. ; _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^)+(0.1822P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.07(4) _refine_ls_number_reflns 22507 _refine_ls_number_parameters 776 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0812 _refine_ls_wR_factor_ref 0.2213 _refine_ls_wR_factor_gt 0.2163 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.000 _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 S1A S -0.54435(8) -0.38706(5) -0.71936(5) 0.01315(12) Uani 1 1 d . . . N1A N -0.1398(3) -0.30598(19) -0.33789(19) 0.0152(4) Uani 1 1 d . . . C1A C -0.1560(3) -0.2284(2) -0.3972(2) 0.0129(4) Uani 1 1 d . . . O1A O -0.7508(3) -0.1424(2) -0.9788(2) 0.0295(7) Uani 1 1 d . . . S2A S 0.17110(8) 0.11990(5) -0.23236(5) 0.01462(12) Uani 1 1 d . . . N2A N -0.2889(3) -0.23664(19) -0.4701(2) 0.0157(4) Uani 1 1 d . . . H2AA H -0.2963 -0.1921 -0.5174 0.019 Uiso 1 1 calc R . . C2A C -0.2654(4) -0.4013(2) -0.3439(2) 0.0171(5) Uani 1 1 d . . . H2AB H -0.2823 -0.3767 -0.2761 0.020 Uiso 1 1 calc R . . H2AC H -0.2440 -0.4726 -0.3393 0.020 Uiso 1 1 calc R . . O2A O 0.2842(3) 0.30042(19) -0.55101(18) 0.0191(4) Uani 1 1 d . . . N3A N -0.6491(3) -0.21046(19) -0.82196(19) 0.0160(4) Uani 1 1 d . . . H3AA H -0.5738 -0.1901 -0.7528 0.019 Uiso 1 1 calc R . . C3A C -0.4010(4) -0.4304(2) -0.4570(2) 0.0183(5) Uani 1 1 d . . . H3AB H -0.4869 -0.4855 -0.4543 0.022 Uiso 1 1 calc R . . H3AC H -0.3916 -0.4692 -0.5243 0.022 Uiso 1 1 calc R . . N4A N -0.5202(3) -0.0334(2) -0.83392(19) 0.0178(5) Uani 1 1 d . . . H4AA H -0.4550 -0.0244 -0.7629 0.021 Uiso 1 1 calc R . . C4A C -0.4215(3) -0.3177(2) -0.4731(2) 0.0147(5) Uani 1 1 d . . . H4AB H -0.4313 -0.2810 -0.4044 0.018 Uiso 1 1 calc R . . N5A N 0.0428(3) 0.2195(2) -0.60627(19) 0.0154(4) Uani 1 1 d . . . H5AA H -0.0277 0.1763 -0.5932 0.019 Uiso 1 1 calc R . . C5A C -0.5547(4) -0.3345(2) -0.5847(2) 0.0164(5) Uani 1 1 d . . . H5AB H -0.5655 -0.2583 -0.5824 0.020 Uiso 1 1 calc R . . H5AC H -0.6425 -0.3918 -0.5864 0.020 Uiso 1 1 calc R . . N6A N 0.2046(3) 0.2105(2) -0.43054(18) 0.0151(4) Uani 1 1 d . . . H6AA H 0.1255 0.1665 -0.4281 0.018 Uiso 1 1 calc R . . C6A C -0.7247(3) -0.4129(2) -0.8189(2) 0.0134(4) Uani 1 1 d . . . N7A N -0.0403(3) -0.1401(2) -0.3892(2) 0.0172(4) Uani 1 1 d . . . H7AA H -0.0576 -0.0904 -0.4293 0.021 Uiso 1 1 calc R . . C7A C -0.8359(4) -0.5261(2) -0.8568(2) 0.0170(5) Uani 1 1 d . . . H7AB H -0.8121 -0.5873 -0.8293 0.020 Uiso 1 1 calc R . . C8A C -0.9777(4) -0.5498(3) -0.9323(3) 0.0199(5) Uani 1 1 d . . . H8AA H -1.0502 -0.6276 -0.9597 0.024 Uiso 1 1 calc R . . C9A C -1.0147(4) -0.4589(3) -0.9688(2) 0.0187(5) Uani 1 1 d . . . H9AA H -1.1134 -0.4741 -1.0182 0.022 Uiso 1 1 calc R . . C10A C -0.9068(4) -0.3458(2) -0.9328(2) 0.0169(5) Uani 1 1 d . . . H10A H -0.9324 -0.2843 -0.9581 0.020 Uiso 1 1 calc R . . C11A C -0.7620(3) -0.3225(2) -0.8602(2) 0.0138(4) Uani 1 1 d . . . C12A C -0.6482(4) -0.1292(2) -0.8861(2) 0.0159(5) Uani 1 1 d . . . C13A C -0.4881(4) 0.0550(2) -0.8929(2) 0.0159(5) Uani 1 1 d . . . H13A H -0.4432 0.1347 -0.8362 0.019 Uiso 1 1 calc R . . H13B H -0.5803 0.0478 -0.9573 0.019 Uiso 1 1 calc R . . C14A C -0.3848(4) 0.0421(2) -0.9436(2) 0.0164(5) Uani 1 1 d . . . H14A H -0.4223 -0.0414 -0.9895 0.020 Uiso 1 1 calc R . . H14B H -0.3863 0.0901 -0.9985 0.020 Uiso 1 1 calc R . . C15A C -0.2274(4) 0.0792(2) -0.8520(2) 0.0154(5) Uani 1 1 d . . . H15A H -0.1723 0.0570 -0.8907 0.019 Uiso 1 1 calc R . . H15B H -0.2255 0.0361 -0.7930 0.019 Uiso 1 1 calc R . . C16A C -0.1528(4) 0.2127(2) -0.7894(2) 0.0156(5) Uani 1 1 d . . . H16A H -0.1700 0.2546 -0.8498 0.019 Uiso 1 1 calc R . . H16B H -0.2004 0.2318 -0.7419 0.019 Uiso 1 1 calc R . . C17A C 0.0091(4) 0.2605(2) -0.7101(2) 0.0178(5) Uani 1 1 d . . . H17A H 0.0571 0.2355 -0.7545 0.021 Uiso 1 1 calc R . . H17B H 0.0488 0.3479 -0.6851 0.021 Uiso 1 1 calc R . . C18A C 0.1838(3) 0.2485(2) -0.5301(2) 0.0137(5) Uani 1 1 d . . . C19A C 0.3372(3) 0.2345(2) -0.3341(2) 0.0125(4) Uani 1 1 d . . . C20A C 0.4743(4) 0.2963(2) -0.3289(2) 0.0156(5) Uani 1 1 d . . . H20A H 0.4781 0.3215 -0.3940 0.019 Uiso 1 1 calc R . . C21A C 0.6026(4) 0.3203(2) -0.2301(2) 0.0180(5) Uani 1 1 d . . . H21A H 0.6933 0.3605 -0.2290 0.022 Uiso 1 1 calc R . . C22A C 0.6007(4) 0.2863(2) -0.1325(2) 0.0180(5) Uani 1 1 d . . . H22A H 0.6890 0.3054 -0.0640 0.022 Uiso 1 1 calc R . . C23A C 0.4683(3) 0.2244(2) -0.1368(2) 0.0140(4) Uani 1 1 d . . . H23A H 0.4665 0.2004 -0.0706 0.017 Uiso 1 1 calc R . . C24A C 0.3366(3) 0.19612(19) -0.2363(2) 0.0131(4) Uani 1 1 d . . . C25A C 0.1872(4) -0.0169(2) -0.2081(2) 0.0164(5) Uani 1 1 d . . . H25A H 0.2917 -0.0023 -0.1686 0.020 Uiso 1 1 calc R . . H25B H 0.1460 -0.0389 -0.1542 0.020 Uiso 1 1 calc R . . C26A C 0.1112(4) -0.1206(2) -0.3195(2) 0.0164(5) Uani 1 1 d . . . H26A H 0.1631 -0.1025 -0.3681 0.020 Uiso 1 1 calc R . . C27A C 0.1176(4) -0.2344(3) -0.2903(3) 0.0214(6) Uani 1 1 d . . . H27A H 0.0992 -0.2923 -0.3610 0.026 Uiso 1 1 calc R . . H27B H 0.2162 -0.2170 -0.2281 0.026 Uiso 1 1 calc R . . C28A C 0.0061(4) -0.2870(2) -0.2491(2) 0.0194(5) Uani 1 1 d . . . H28A H 0.0074 -0.3631 -0.2361 0.023 Uiso 1 1 calc R . . H28B H 0.0304 -0.2330 -0.1737 0.023 Uiso 1 1 calc R . . S1B S -0.44211(8) -0.02066(5) -0.24418(5) 0.01429(12) Uani 1 1 d . . . N1B N -0.8308(3) -0.06420(17) -0.65877(18) 0.0124(4) Uani 1 1 d . . . C1B C -0.8154(3) -0.14319(19) -0.59961(19) 0.0117(4) Uani 1 1 d . . . O1B O -0.2425(3) -0.2681(2) -0.00306(19) 0.0230(5) Uani 1 1 d . . . S2B S -1.17514(8) -0.51211(5) -0.75616(5) 0.01262(12) Uani 1 1 d . . . N2B N -0.6869(3) -0.11966(18) -0.50823(18) 0.0131(4) Uani 1 1 d . . . H2BA H -0.6720 -0.1746 -0.4753 0.016 Uiso 1 1 calc R . . C2B C -0.7065(4) 0.0339(2) -0.6506(2) 0.0158(5) Uani 1 1 d . . . H2BB H -0.7106 0.1096 -0.6208 0.019 Uiso 1 1 calc R . . H2BC H -0.7137 0.0284 -0.7301 0.019 Uiso 1 1 calc R . . O2B O -1.2805(3) -0.6829(2) -0.43206(18) 0.0185(4) Uani 1 1 d . . . N3B N -0.3387(3) -0.20574(19) -0.16441(19) 0.0155(4) Uani 1 1 d . . . H3BA H -0.4098 -0.2273 -0.2361 0.019 Uiso 1 1 calc R . . C3B C -0.5619(4) 0.0328(2) -0.5702(2) 0.0155(5) Uani 1 1 d . . . H3BB H -0.4831 0.1119 -0.5442 0.019 Uiso 1 1 calc R . . H3BC H -0.5392 -0.0248 -0.6126 0.019 Uiso 1 1 calc R . . N4B N -0.4707(3) -0.3817(2) -0.1512(2) 0.0171(5) Uani 1 1 d . . . H4BA H -0.5322 -0.3951 -0.2248 0.020 Uiso 1 1 calc R . . C4B C -0.5721(3) -0.00111(19) -0.4642(2) 0.0128(4) Uani 1 1 d . . . H4BB H -0.6008 0.0552 -0.4252 0.015 Uiso 1 1 calc R . . N5B N -1.0387(3) -0.5983(2) -0.37710(19) 0.0154(4) Uani 1 1 d . . . H5BA H -0.9685 -0.5520 -0.3885 0.018 Uiso 1 1 calc R . . C5B C -0.4274(3) 0.0033(2) -0.3755(2) 0.0156(5) Uani 1 1 d . . . H5BB H -0.3490 0.0811 -0.3550 0.019 Uiso 1 1 calc R . . H5BC H -0.4031 -0.0584 -0.4098 0.019 Uiso 1 1 calc R . . N6B N -1.2051(3) -0.59876(19) -0.55621(18) 0.0137(4) Uani 1 1 d . . . H6BA H -1.1276 -0.5523 -0.5590 0.016 Uiso 1 1 calc R . . C6B C -0.2593(3) 0.0016(2) -0.1546(2) 0.0139(4) Uani 1 1 d . . . N7B N -0.9288(3) -0.24506(17) -0.62955(18) 0.0136(4) Uani 1 1 d . . . H7BA H -0.9184 -0.2946 -0.5879 0.016 Uiso 1 1 calc R . . C7B C -0.1485(4) 0.1144(2) -0.1136(2) 0.0184(5) Uani 1 1 d . . . H7BB H -0.1721 0.1781 -0.1344 0.022 Uiso 1 1 calc R . . C8B C -0.0055(4) 0.1344(3) -0.0434(3) 0.0204(6) Uani 1 1 d . . . H8BA H 0.0687 0.2115 -0.0151 0.025 Uiso 1 1 calc R . . C9B C 0.0289(4) 0.0398(3) -0.0143(2) 0.0192(5) Uani 1 1 d . . . H9BA H 0.1273 0.0528 0.0334 0.023 Uiso 1 1 calc R . . C10B C -0.0790(4) -0.0721(2) -0.0543(2) 0.0170(5) Uani 1 1 d . . . H10B H -0.0536 -0.1356 -0.0350 0.020 Uiso 1 1 calc R . . C11B C -0.2254(3) -0.0933(2) -0.1230(2) 0.0136(4) Uani 1 1 d . . . C12B C -0.3449(4) -0.2850(2) -0.0985(2) 0.0158(5) Uani 1 1 d . . . C13B C -0.5060(4) -0.4642(2) -0.0876(3) 0.0176(5) Uani 1 1 d . . . H13C H -0.4148 -0.4579 -0.0228 0.021 Uiso 1 1 calc R . . H13D H -0.5551 -0.5457 -0.1415 0.021 Uiso 1 1 calc R . . C14B C -0.6040(4) -0.4413(3) -0.0374(2) 0.0168(5) Uani 1 1 d . . . H14C H -0.5594 -0.3571 0.0087 0.020 Uiso 1 1 calc R . . H14D H -0.6083 -0.4888 0.0173 0.020 Uiso 1 1 calc R . . C15B C -0.7614(4) -0.4704(2) -0.1303(2) 0.0157(5) Uani 1 1 d . . . H15C H -0.8147 -0.4465 -0.0907 0.019 Uiso 1 1 calc R . . H15D H -0.7581 -0.4244 -0.1864 0.019 Uiso 1 1 calc R . . C16B C -0.8430(4) -0.6016(2) -0.1977(2) 0.0180(5) Uani 1 1 d . . . H16C H -0.7992 -0.6212 -0.2482 0.022 Uiso 1 1 calc R . . H16D H -0.8279 -0.6471 -0.1403 0.022 Uiso 1 1 calc R . . C17B C -1.0060(4) -0.6424(3) -0.2743(2) 0.0202(6) Uani 1 1 d . . . H17C H -1.0514 -0.7298 -0.3011 0.024 Uiso 1 1 calc R . . H17D H -1.0492 -0.6145 -0.2269 0.024 Uiso 1 1 calc R . . C18B C -1.1817(3) -0.6314(2) -0.4544(2) 0.0133(4) Uani 1 1 d . . . C19B C -1.3396(3) -0.63197(19) -0.65559(19) 0.0118(4) Uani 1 1 d . . . C20B C -1.4739(4) -0.6928(2) -0.6606(2) 0.0143(5) Uani 1 1 d . . . H20B H -1.4778 -0.7127 -0.5933 0.017 Uiso 1 1 calc R . . C21B C -1.6035(4) -0.7250(2) -0.7637(2) 0.0157(5) Uani 1 1 d . . . H21B H -1.6943 -0.7652 -0.7649 0.019 Uiso 1 1 calc R . . C22B C -1.6007(4) -0.6989(2) -0.8642(2) 0.0152(5) Uani 1 1 d . . . H22B H -1.6883 -0.7242 -0.9351 0.018 Uiso 1 1 calc R . . C23B C -1.4685(3) -0.6357(2) -0.8590(2) 0.0136(4) Uani 1 1 d . . . H23B H -1.4661 -0.6157 -0.9266 0.016 Uiso 1 1 calc R . . C24B C -1.3375(3) -0.6002(2) -0.7563(2) 0.0128(4) Uani 1 1 d . . . C25B C -1.1890(4) -0.3706(2) -0.7234(2) 0.0157(5) Uani 1 1 d . . . H25C H -1.2853 -0.3762 -0.7799 0.019 Uiso 1 1 calc R . . H25D H -1.1807 -0.3504 -0.6434 0.019 Uiso 1 1 calc R . . C26B C -1.0701(3) -0.27477(19) -0.73093(19) 0.0122(4) Uani 1 1 d . . . H26B H -1.0649 -0.3038 -0.8047 0.015 Uiso 1 1 calc R . . C27B C -1.0956(4) -0.1612(2) -0.7309(2) 0.0159(5) Uani 1 1 d . . . H27C H -1.1907 -0.1771 -0.7972 0.019 Uiso 1 1 calc R . . H27D H -1.0966 -0.1293 -0.6568 0.019 Uiso 1 1 calc R . . C28B C -0.9741(4) -0.0734(2) -0.7428(2) 0.0167(5) Uani 1 1 d . . . H28C H -0.9868 -0.0981 -0.8237 0.020 Uiso 1 1 calc R . . H28D H -0.9790 0.0050 -0.7291 0.020 Uiso 1 1 calc R . . N1SA N -0.2250(3) 0.0234(2) -0.56558(19) 0.0151(4) Uani 1 1 d . . . O1SA O -0.3266(3) -0.07806(18) -0.60837(19) 0.0205(5) Uani 1 1 d . . . O3SA O -0.2488(3) 0.10663(18) -0.60228(18) 0.0184(4) Uani 1 1 d . . . O2SA O -0.1030(3) 0.0419(2) -0.4872(2) 0.0281(6) Uani 1 1 d . . . N1SB N -0.7631(3) -0.40491(18) -0.42701(18) 0.0132(4) Uani 1 1 d . . . O2SB O -0.8840(3) -0.42451(18) -0.51114(18) 0.0196(4) Uani 1 1 d . . . O1SB O -0.6607(3) -0.30354(17) -0.38709(19) 0.0178(4) Uani 1 1 d . . . O3SB O -0.7444(3) -0.48492(18) -0.38291(19) 0.0202(4) 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 S1A 0.0120(4) 0.0154(2) 0.0121(2) 0.00278(16) 0.0051(2) 0.0066(2) N1A 0.0151(14) 0.0154(7) 0.0151(7) 0.0058(6) 0.0044(8) 0.0086(8) C1A 0.0131(14) 0.0111(7) 0.0127(8) 0.0017(6) 0.0046(9) 0.0049(8) O1A 0.0190(18) 0.0275(11) 0.0196(9) 0.0114(8) -0.0065(8) -0.0009(9) S2A 0.0129(4) 0.0160(2) 0.0150(2) 0.00612(18) 0.0066(2) 0.0050(2) N2A 0.0129(13) 0.0132(7) 0.0176(8) 0.0049(6) 0.0035(8) 0.0055(8) C2A 0.0209(17) 0.0161(9) 0.0178(9) 0.0076(7) 0.0106(10) 0.0086(9) O2A 0.0167(13) 0.0254(9) 0.0174(8) 0.0096(7) 0.0094(8) 0.0077(8) N3A 0.0146(14) 0.0147(7) 0.0129(7) 0.0054(6) 0.0018(8) 0.0037(8) C3A 0.0168(17) 0.0156(9) 0.0181(9) 0.0041(7) 0.0059(10) 0.0042(9) N4A 0.0149(15) 0.0187(8) 0.0125(7) 0.0069(6) 0.0019(8) 0.0024(8) C4A 0.0133(15) 0.0171(8) 0.0125(8) 0.0020(7) 0.0052(9) 0.0066(9) N5A 0.0117(14) 0.0190(8) 0.0146(8) 0.0067(7) 0.0058(8) 0.0044(8) C5A 0.0141(16) 0.0245(10) 0.0123(8) 0.0032(7) 0.0058(9) 0.0113(10) N6A 0.0095(13) 0.0204(8) 0.0113(7) 0.0059(6) 0.0032(8) 0.0023(8) C6A 0.0140(15) 0.0155(8) 0.0118(7) 0.0033(6) 0.0059(9) 0.0075(9) N7A 0.0134(14) 0.0148(8) 0.0191(8) 0.0060(7) 0.0037(9) 0.0046(8) C7A 0.0169(17) 0.0135(8) 0.0189(9) 0.0035(7) 0.0080(10) 0.0046(9) C8A 0.0142(17) 0.0188(9) 0.0225(10) 0.0037(8) 0.0078(11) 0.0032(10) C9A 0.0105(16) 0.0211(10) 0.0189(10) 0.0024(8) 0.0041(10) 0.0040(10) C10A 0.0141(16) 0.0217(10) 0.0146(8) 0.0050(7) 0.0058(9) 0.0079(10) C11A 0.0131(15) 0.0158(8) 0.0117(8) 0.0032(6) 0.0056(9) 0.0053(9) C12A 0.0159(16) 0.0154(8) 0.0119(8) 0.0042(7) 0.0025(9) 0.0055(9) C13A 0.0145(16) 0.0168(9) 0.0161(9) 0.0073(8) 0.0055(10) 0.0069(9) C14A 0.0171(17) 0.0214(10) 0.0108(8) 0.0053(8) 0.0049(10) 0.0093(10) C15A 0.0181(16) 0.0190(9) 0.0130(8) 0.0064(7) 0.0074(9) 0.0109(10) C16A 0.0150(15) 0.0180(9) 0.0159(8) 0.0082(7) 0.0069(9) 0.0082(9) C17A 0.0168(17) 0.0223(10) 0.0163(9) 0.0103(8) 0.0078(10) 0.0080(10) C18A 0.0143(15) 0.0149(8) 0.0112(8) 0.0036(7) 0.0057(9) 0.0053(9) C19A 0.0128(14) 0.0129(8) 0.0123(8) 0.0034(6) 0.0062(9) 0.0053(8) C20A 0.0123(16) 0.0187(10) 0.0156(9) 0.0058(7) 0.0074(10) 0.0045(9) C21A 0.0150(17) 0.0181(9) 0.0214(10) 0.0070(8) 0.0081(11) 0.0071(10) C22A 0.0152(17) 0.0182(10) 0.0178(9) 0.0052(8) 0.0046(10) 0.0072(10) C23A 0.0124(15) 0.0144(8) 0.0126(8) 0.0035(6) 0.0034(8) 0.0054(8) C24A 0.0154(14) 0.0114(7) 0.0111(7) 0.0020(6) 0.0054(8) 0.0052(8) C25A 0.0153(16) 0.0154(8) 0.0124(8) 0.0045(7) 0.0030(9) 0.0028(9) C26A 0.0153(16) 0.0196(9) 0.0142(8) 0.0037(7) 0.0064(9) 0.0078(9) C27A 0.0164(18) 0.0199(10) 0.0276(12) 0.0046(9) 0.0067(11) 0.0121(11) C28A 0.0176(17) 0.0166(9) 0.0196(10) 0.0061(8) 0.0020(10) 0.0094(10) S1B 0.0119(4) 0.0161(2) 0.0133(2) 0.00357(17) 0.0044(2) 0.0058(2) N1B 0.0103(12) 0.0113(6) 0.0147(7) 0.0062(6) 0.0037(8) 0.0046(7) C1B 0.0140(14) 0.0116(7) 0.0119(7) 0.0050(6) 0.0065(8) 0.0067(8) O1B 0.0159(15) 0.0243(9) 0.0179(8) 0.0096(7) -0.0011(8) 0.0043(8) S2B 0.0117(4) 0.01291(19) 0.0141(2) 0.00423(16) 0.0070(2) 0.0045(2) N2B 0.0122(13) 0.0119(7) 0.0137(7) 0.0060(6) 0.0040(8) 0.0046(7) C2B 0.0151(16) 0.0154(8) 0.0187(9) 0.0101(7) 0.0076(10) 0.0063(9) O2B 0.0139(13) 0.0263(9) 0.0169(7) 0.0096(7) 0.0090(8) 0.0063(8) N3B 0.0153(13) 0.0145(7) 0.0126(7) 0.0039(6) 0.0036(8) 0.0046(8) C3B 0.0132(15) 0.0147(8) 0.0186(9) 0.0074(7) 0.0078(10) 0.0040(9) N4B 0.0152(14) 0.0163(8) 0.0141(7) 0.0047(6) 0.0026(8) 0.0044(8) C4B 0.0136(14) 0.0117(7) 0.0140(8) 0.0046(6) 0.0064(9) 0.0058(8) N5B 0.0116(14) 0.0202(8) 0.0139(8) 0.0075(7) 0.0054(8) 0.0052(8) C5B 0.0152(16) 0.0175(9) 0.0129(8) 0.0032(7) 0.0058(9) 0.0065(9) N6B 0.0112(13) 0.0169(8) 0.0107(7) 0.0048(6) 0.0045(7) 0.0030(8) C6B 0.0132(15) 0.0147(8) 0.0123(8) 0.0025(6) 0.0050(9) 0.0056(9) N7B 0.0123(13) 0.0120(7) 0.0153(7) 0.0062(6) 0.0048(8) 0.0043(7) C7B 0.0154(17) 0.0174(9) 0.0183(10) 0.0049(8) 0.0052(10) 0.0050(10) C8B 0.0140(18) 0.0207(10) 0.0217(11) 0.0052(9) 0.0066(11) 0.0033(10) C9B 0.0146(17) 0.0265(11) 0.0171(9) 0.0067(8) 0.0074(10) 0.0088(11) C10B 0.0165(16) 0.0227(10) 0.0141(8) 0.0059(8) 0.0074(10) 0.0099(10) C11B 0.0138(15) 0.0145(8) 0.0110(7) 0.0019(6) 0.0052(8) 0.0051(8) C12B 0.0178(16) 0.0158(8) 0.0126(8) 0.0041(7) 0.0050(9) 0.0074(9) C13B 0.0174(17) 0.0174(10) 0.0187(11) 0.0077(9) 0.0064(11) 0.0092(10) C14B 0.0166(17) 0.0208(10) 0.0129(9) 0.0053(8) 0.0048(10) 0.0096(10) C15B 0.0177(16) 0.0190(9) 0.0134(8) 0.0054(7) 0.0067(9) 0.0112(10) C16B 0.0200(17) 0.0184(9) 0.0178(9) 0.0081(8) 0.0080(10) 0.0098(10) C17B 0.0187(18) 0.0227(11) 0.0177(10) 0.0112(9) 0.0060(10) 0.0070(11) C18B 0.0135(15) 0.0157(8) 0.0122(8) 0.0037(7) 0.0069(9) 0.0065(9) C19B 0.0112(14) 0.0114(7) 0.0118(7) 0.0028(6) 0.0051(8) 0.0038(8) C20B 0.0145(16) 0.0125(8) 0.0175(9) 0.0053(7) 0.0091(10) 0.0045(9) C21B 0.0110(15) 0.0137(8) 0.0217(10) 0.0064(8) 0.0076(10) 0.0036(9) C22B 0.0114(15) 0.0157(9) 0.0167(9) 0.0061(7) 0.0045(9) 0.0048(9) C23B 0.0130(15) 0.0129(8) 0.0134(8) 0.0049(7) 0.0040(9) 0.0054(8) C24B 0.0143(15) 0.0125(8) 0.0129(8) 0.0039(6) 0.0073(9) 0.0052(8) C25B 0.0143(16) 0.0145(8) 0.0193(9) 0.0039(7) 0.0088(10) 0.0062(9) C26B 0.0093(14) 0.0123(7) 0.0121(7) 0.0027(6) 0.0031(8) 0.0036(8) C27B 0.0153(15) 0.0139(8) 0.0168(9) 0.0039(7) 0.0043(9) 0.0080(9) C28B 0.0147(15) 0.0150(8) 0.0159(9) 0.0067(7) 0.0020(9) 0.0058(9) N1SA 0.0127(13) 0.0178(8) 0.0125(7) 0.0054(6) 0.0052(8) 0.0037(8) O1SA 0.0138(13) 0.0171(8) 0.0214(8) 0.0069(7) 0.0014(8) 0.0028(7) O3SA 0.0191(13) 0.0188(8) 0.0208(8) 0.0101(7) 0.0091(8) 0.0100(8) O2SA 0.0148(16) 0.0261(10) 0.0312(11) 0.0163(9) -0.0002(10) 0.0036(9) N1SB 0.0136(13) 0.0151(7) 0.0110(6) 0.0048(6) 0.0053(8) 0.0060(8) O2SB 0.0140(13) 0.0185(8) 0.0175(8) 0.0072(6) -0.0005(8) 0.0047(7) O1SB 0.0143(13) 0.0152(7) 0.0196(8) 0.0057(6) 0.0060(8) 0.0027(7) O3SB 0.0244(14) 0.0163(7) 0.0193(8) 0.0094(6) 0.0064(8) 0.0101(8) _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 S1A C6A 1.771(3) . ? S1A C5A 1.830(2) . ? N1A C1A 1.328(3) . ? N1A C28A 1.472(4) . ? N1A C2A 1.473(4) . ? C1A N2A 1.344(4) . ? C1A N7A 1.348(4) . ? O1A C12A 1.224(4) . ? S2A C24A 1.779(3) . ? S2A C25A 1.825(3) . ? N2A C4A 1.464(4) . ? C2A C3A 1.514(4) . ? O2A C18A 1.234(4) . ? N3A C12A 1.397(3) . ? N3A C11A 1.407(4) . ? C3A C4A 1.519(4) . ? N4A C12A 1.355(4) . ? N4A C13A 1.457(4) . ? C4A C5A 1.526(4) . ? N5A C18A 1.355(4) . ? N5A C17A 1.458(3) . ? N6A C18A 1.394(3) . ? N6A C19A 1.398(4) . ? C6A C7A 1.409(4) . ? C6A C11A 1.414(3) . ? N7A C26A 1.456(4) . ? C7A C8A 1.373(5) . ? C8A C9A 1.398(4) . ? C9A C10A 1.398(4) . ? C10A C11A 1.392(5) . ? C13A C14A 1.538(5) . ? C14A C15A 1.526(5) . ? C15A C16A 1.538(4) . ? C16A C17A 1.511(5) . ? C19A C24A 1.416(3) . ? C19A C20A 1.418(4) . ? C20A C21A 1.385(5) . ? C21A C22A 1.392(4) . ? C22A C23A 1.381(5) . ? C23A C24A 1.400(4) . ? C25A C26A 1.525(3) . ? C26A C27A 1.533(4) . ? C27A C28A 1.512(5) . ? S1B C6B 1.774(3) . ? S1B C5B 1.822(2) . ? N1B C1B 1.341(3) . ? N1B C28B 1.469(4) . ? N1B C2B 1.471(4) . ? C1B N2B 1.342(4) . ? C1B N7B 1.345(4) . ? O1B C12B 1.234(4) . ? S2B C24B 1.765(3) . ? S2B C25B 1.822(2) . ? N2B C4B 1.463(4) . ? C2B C3B 1.516(4) . ? O2B C18B 1.231(4) . ? N3B C12B 1.396(3) . ? N3B C11B 1.407(4) . ? C3B C4B 1.524(3) . ? N4B C12B 1.347(4) . ? N4B C13B 1.456(4) . ? C4B C5B 1.523(4) . ? N5B C18B 1.366(4) . ? N5B C17B 1.469(3) . ? N6B C18B 1.385(3) . ? N6B C19B 1.407(4) . ? C6B C7B 1.400(4) . ? C6B C11B 1.412(3) . ? N7B C26B 1.471(4) . ? C7B C8B 1.379(5) . ? C8B C9B 1.400(4) . ? C9B C10B 1.381(5) . ? C10B C11B 1.403(5) . ? C13B C14B 1.518(5) . ? C14B C15B 1.549(5) . ? C15B C16B 1.525(4) . ? C16B C17B 1.522(5) . ? C19B C20B 1.391(4) . ? C19B C24B 1.420(3) . ? C20B C21B 1.402(4) . ? C21B C22B 1.393(4) . ? C22B C23B 1.377(4) . ? C23B C24B 1.401(4) . ? C25B C26B 1.511(4) . ? C26B C27B 1.524(3) . ? C27B C28B 1.509(4) . ? N1SA O2SA 1.241(4) . ? N1SA O3SA 1.256(3) . ? N1SA O1SA 1.262(3) . ? N1SB O3SB 1.248(3) . ? N1SB O2SB 1.260(3) . ? N1SB O1SB 1.267(3) . ? 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 C6A S1A C5A 96.85(13) . . ? C1A N1A C28A 119.8(3) . . ? C1A N1A C2A 122.0(3) . . ? C28A N1A C2A 117.5(2) . . ? N1A C1A N2A 121.3(3) . . ? N1A C1A N7A 121.5(3) . . ? N2A C1A N7A 117.2(2) . . ? C24A S2A C25A 102.43(13) . . ? C1A N2A C4A 121.9(2) . . ? N1A C2A C3A 110.9(2) . . ? C12A N3A C11A 124.6(2) . . ? C2A C3A C4A 109.5(2) . . ? C12A N4A C13A 121.4(2) . . ? N2A C4A C3A 107.8(2) . . ? N2A C4A C5A 110.3(2) . . ? C3A C4A C5A 115.0(2) . . ? C18A N5A C17A 119.2(2) . . ? C4A C5A S1A 113.29(19) . . ? C18A N6A C19A 127.2(3) . . ? C7A C6A C11A 118.5(3) . . ? C7A C6A S1A 119.37(19) . . ? C11A C6A S1A 122.1(2) . . ? C1A N7A C26A 125.0(2) . . ? C8A C7A C6A 121.5(2) . . ? C7A C8A C9A 119.6(3) . . ? C10A C9A C8A 120.1(3) . . ? C11A C10A C9A 120.4(3) . . ? C10A C11A N3A 122.6(2) . . ? C10A C11A C6A 119.8(3) . . ? N3A C11A C6A 117.6(3) . . ? O1A C12A N4A 123.6(2) . . ? O1A C12A N3A 124.2(3) . . ? N4A C12A N3A 112.1(2) . . ? N4A C13A C14A 112.4(2) . . ? C15A C14A C13A 114.6(2) . . ? C14A C15A C16A 112.1(2) . . ? C17A C16A C15A 115.9(2) . . ? N5A C17A C16A 112.0(2) . . ? O2A C18A N5A 121.7(2) . . ? O2A C18A N6A 123.5(3) . . ? N5A C18A N6A 114.7(3) . . ? N6A C19A C24A 119.2(3) . . ? N6A C19A C20A 123.1(2) . . ? C24A C19A C20A 117.7(3) . . ? C21A C20A C19A 120.9(2) . . ? C20A C21A C22A 120.9(3) . . ? C23A C22A C21A 118.9(3) . . ? C22A C23A C24A 121.6(2) . . ? C23A C24A C19A 119.9(3) . . ? C23A C24A S2A 118.49(18) . . ? C19A C24A S2A 121.5(2) . . ? C26A C25A S2A 114.53(18) . . ? N7A C26A C25A 112.1(2) . . ? N7A C26A C27A 109.0(3) . . ? C25A C26A C27A 111.1(2) . . ? C28A C27A C26A 111.1(2) . . ? N1A C28A C27A 109.8(2) . . ? C6B S1B C5B 99.09(13) . . ? C1B N1B C28B 122.3(2) . . ? C1B N1B C2B 123.0(2) . . ? C28B N1B C2B 114.60(19) . . ? N1B C1B N2B 120.0(2) . . ? N1B C1B N7B 120.4(2) . . ? N2B C1B N7B 119.6(2) . . ? C24B S2B C25B 97.33(13) . . ? C1B N2B C4B 118.90(19) . . ? N1B C2B C3B 112.10(18) . . ? C12B N3B C11B 123.8(2) . . ? C2B C3B C4B 108.6(2) . . ? C12B N4B C13B 120.8(2) . . ? N2B C4B C5B 111.38(19) . . ? N2B C4B C3B 107.20(19) . . ? C5B C4B C3B 111.6(2) . . ? C18B N5B C17B 117.7(3) . . ? C4B C5B S1B 108.91(19) . . ? C18B N6B C19B 126.9(2) . . ? C7B C6B C11B 119.9(3) . . ? C7B C6B S1B 119.7(2) . . ? C11B C6B S1B 120.3(2) . . ? C1B N7B C26B 120.92(19) . . ? C8B C7B C6B 121.0(3) . . ? C7B C8B C9B 119.2(3) . . ? C10B C9B C8B 120.6(3) . . ? C9B C10B C11B 120.9(3) . . ? C10B C11B N3B 122.7(2) . . ? C10B C11B C6B 118.3(2) . . ? N3B C11B C6B 119.0(3) . . ? O1B C12B N4B 124.2(2) . . ? O1B C12B N3B 122.4(3) . . ? N4B C12B N3B 113.3(2) . . ? N4B C13B C14B 112.3(2) . . ? C13B C14B C15B 114.7(3) . . ? C16B C15B C14B 112.0(2) . . ? C17B C16B C15B 115.6(2) . . ? N5B C17B C16B 112.2(3) . . ? O2B C18B N5B 121.7(2) . . ? O2B C18B N6B 123.4(3) . . ? N5B C18B N6B 114.9(2) . . ? C20B C19B N6B 124.0(2) . . ? C20B C19B C24B 118.3(3) . . ? N6B C19B C24B 117.6(3) . . ? C19B C20B C21B 120.8(2) . . ? C22B C21B C20B 120.7(3) . . ? C23B C22B C21B 118.8(3) . . ? C22B C23B C24B 121.7(2) . . ? C23B C24B C19B 119.6(3) . . ? C23B C24B S2B 118.04(18) . . ? C19B C24B S2B 122.3(2) . . ? C26B C25B S2B 110.4(2) . . ? N7B C26B C25B 110.3(2) . . ? N7B C26B C27B 107.1(2) . . ? C25B C26B C27B 112.5(2) . . ? C28B C27B C26B 108.2(2) . . ? N1B C28B C27B 111.5(2) . . ? O2SA N1SA O3SA 119.9(2) . . ? O2SA N1SA O1SA 120.8(2) . . ? O3SA N1SA O1SA 119.3(3) . . ? O3SB N1SB O2SB 120.1(2) . . ? O3SB N1SB O1SB 120.1(2) . . ? O2SB N1SB O1SB 119.8(2) . . ? 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 C28A N1A C1A N2A -173.2(2) . . . . ? C2A N1A C1A N2A -3.1(3) . . . . ? C28A N1A C1A N7A 8.6(4) . . . . ? C2A N1A C1A N7A 178.7(2) . . . . ? N1A C1A N2A C4A 10.7(3) . . . . ? N7A C1A N2A C4A -171.0(2) . . . . ? C1A N1A C2A C3A 24.4(3) . . . . ? C28A N1A C2A C3A -165.3(2) . . . . ? N1A C2A C3A C4A -50.8(3) . . . . ? C1A N2A C4A C3A -37.7(3) . . . . ? C1A N2A C4A C5A -164.0(2) . . . . ? C2A C3A C4A N2A 56.4(3) . . . . ? C2A C3A C4A C5A 179.8(2) . . . . ? N2A C4A C5A S1A 56.5(2) . . . . ? C3A C4A C5A S1A -65.6(3) . . . . ? C6A S1A C5A C4A 172.0(2) . . . . ? C5A S1A C6A C7A -92.9(2) . . . . ? C5A S1A C6A C11A 85.7(2) . . . . ? N1A C1A N7A C26A 1.3(4) . . . . ? N2A C1A N7A C26A -177.0(2) . . . . ? C11A C6A C7A C8A 0.3(4) . . . . ? S1A C6A C7A C8A 178.9(2) . . . . ? C6A C7A C8A C9A -3.0(4) . . . . ? C7A C8A C9A C10A 3.0(4) . . . . ? C8A C9A C10A C11A -0.3(4) . . . . ? C9A C10A C11A N3A 179.7(2) . . . . ? C9A C10A C11A C6A -2.4(4) . . . . ? C12A N3A C11A C10A -30.9(4) . . . . ? C12A N3A C11A C6A 151.2(3) . . . . ? C7A C6A C11A C10A 2.4(3) . . . . ? S1A C6A C11A C10A -176.17(18) . . . . ? C7A C6A C11A N3A -179.6(2) . . . . ? S1A C6A C11A N3A 1.9(3) . . . . ? C13A N4A C12A O1A -8.1(5) . . . . ? C13A N4A C12A N3A 171.8(3) . . . . ? C11A N3A C12A O1A 6.1(5) . . . . ? C11A N3A C12A N4A -173.8(3) . . . . ? C12A N4A C13A C14A -102.4(3) . . . . ? N4A C13A C14A C15A -72.2(3) . . . . ? C13A C14A C15A C16A -67.2(3) . . . . ? C14A C15A C16A C17A -171.4(2) . . . . ? C18A N5A C17A C16A 175.8(2) . . . . ? C15A C16A C17A N5A -68.4(3) . . . . ? C17A N5A C18A O2A -6.1(4) . . . . ? C17A N5A C18A N6A 176.6(2) . . . . ? C19A N6A C18A O2A 7.5(4) . . . . ? C19A N6A C18A N5A -175.3(2) . . . . ? C18A N6A C19A C24A 174.9(2) . . . . ? C18A N6A C19A C20A -5.0(4) . . . . ? N6A C19A C20A C21A 178.5(2) . . . . ? C24A C19A C20A C21A -1.5(3) . . . . ? C19A C20A C21A C22A -1.1(4) . . . . ? C20A C21A C22A C23A 2.2(4) . . . . ? C21A C22A C23A C24A -0.6(4) . . . . ? C22A C23A C24A C19A -2.0(4) . . . . ? C22A C23A C24A S2A -178.18(19) . . . . ? N6A C19A C24A C23A -177.0(2) . . . . ? C20A C19A C24A C23A 3.0(3) . . . . ? N6A C19A C24A S2A -0.9(3) . . . . ? C20A C19A C24A S2A 179.04(17) . . . . ? C25A S2A C24A C23A -60.5(2) . . . . ? C25A S2A C24A C19A 123.43(19) . . . . ? C24A S2A C25A C26A -96.4(2) . . . . ? C1A N7A C26A C25A -105.2(3) . . . . ? C1A N7A C26A C27A 18.2(3) . . . . ? S2A C25A C26A N7A -52.4(3) . . . . ? S2A C25A C26A C27A -174.6(2) . . . . ? N7A C26A C27A C28A -45.7(3) . . . . ? C25A C26A C27A C28A 78.2(3) . . . . ? C1A N1A C28A C27A -37.1(3) . . . . ? C2A N1A C28A C27A 152.4(2) . . . . ? C26A C27A C28A N1A 55.4(3) . . . . ? C28B N1B C1B N2B -167.1(2) . . . . ? C2B N1B C1B N2B 16.8(3) . . . . ? C28B N1B C1B N7B 11.4(3) . . . . ? C2B N1B C1B N7B -164.7(2) . . . . ? N1B C1B N2B C4B 8.8(3) . . . . ? N7B C1B N2B C4B -169.7(2) . . . . ? C1B N1B C2B C3B 1.0(3) . . . . ? C28B N1B C2B C3B -175.4(2) . . . . ? N1B C2B C3B C4B -39.6(3) . . . . ? C1B N2B C4B C5B -170.1(2) . . . . ? C1B N2B C4B C3B -47.8(3) . . . . ? C2B C3B C4B N2B 61.3(2) . . . . ? C2B C3B C4B C5B -176.51(18) . . . . ? N2B C4B C5B S1B -67.1(2) . . . . ? C3B C4B C5B S1B 173.20(15) . . . . ? C6B S1B C5B C4B -175.21(15) . . . . ? C5B S1B C6B C7B 68.4(2) . . . . ? C5B S1B C6B C11B -112.7(2) . . . . ? N1B C1B N7B C26B 2.9(3) . . . . ? N2B C1B N7B C26B -178.6(2) . . . . ? C11B C6B C7B C8B 0.8(4) . . . . ? S1B C6B C7B C8B 179.7(2) . . . . ? C6B C7B C8B C9B 0.8(4) . . . . ? C7B C8B C9B C10B -0.7(4) . . . . ? C8B C9B C10B C11B -1.2(4) . . . . ? C9B C10B C11B N3B -179.3(2) . . . . ? C9B C10B C11B C6B 2.7(3) . . . . ? C12B N3B C11B C10B 39.4(4) . . . . ? C12B N3B C11B C6B -142.7(3) . . . . ? C7B C6B C11B C10B -2.5(3) . . . . ? S1B C6B C11B C10B 178.57(18) . . . . ? C7B C6B C11B N3B 179.5(2) . . . . ? S1B C6B C11B N3B 0.6(3) . . . . ? C13B N4B C12B O1B 12.0(5) . . . . ? C13B N4B C12B N3B -170.0(3) . . . . ? C11B N3B C12B O1B -8.7(4) . . . . ? C11B N3B C12B N4B 173.2(3) . . . . ? C12B N4B C13B C14B 96.9(4) . . . . ? N4B C13B C14B C15B 69.4(3) . . . . ? C13B C14B C15B C16B 63.8(3) . . . . ? C14B C15B C16B C17B 169.0(2) . . . . ? C18B N5B C17B C16B 178.4(2) . . . . ? C15B C16B C17B N5B 70.1(3) . . . . ? C17B N5B C18B O2B 9.7(4) . . . . ? C17B N5B C18B N6B -172.6(2) . . . . ? C19B N6B C18B O2B -9.8(4) . . . . ? C19B N6B C18B N5B 172.6(2) . . . . ? C18B N6B C19B C20B 8.1(4) . . . . ? C18B N6B C19B C24B -172.5(2) . . . . ? N6B C19B C20B C21B -178.7(2) . . . . ? C24B C19B C20B C21B 2.0(3) . . . . ? C19B C20B C21B C22B 1.2(4) . . . . ? C20B C21B C22B C23B -3.1(4) . . . . ? C21B C22B C23B C24B 1.8(4) . . . . ? C22B C23B C24B C19B 1.4(3) . . . . ? C22B C23B C24B S2B -176.31(19) . . . . ? C20B C19B C24B C23B -3.3(3) . . . . ? N6B C19B C24B C23B 177.3(2) . . . . ? C20B C19B C24B S2B 174.38(17) . . . . ? N6B C19B C24B S2B -5.0(3) . . . . ? C25B S2B C24B C23B 82.6(2) . . . . ? C25B S2B C24B C19B -95.1(2) . . . . ? C24B S2B C25B C26B -173.43(18) . . . . ? C1B N7B C26B C25B -161.9(2) . . . . ? C1B N7B C26B C27B -39.2(3) . . . . ? S2B C25B C26B N7B -73.1(2) . . . . ? S2B C25B C26B C27B 167.48(17) . . . . ? N7B C26B C27B C28B 60.6(2) . . . . ? C25B C26B C27B C28B -178.1(2) . . . . ? C1B N1B C28B C27B 13.7(3) . . . . ? C2B N1B C28B C27B -169.9(2) . . . . ? C26B C27B C28B N1B -49.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.377 _diffrn_reflns_theta_full 39.44 _diffrn_measured_fraction_theta_full 0.377 _refine_diff_density_max 0.437 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.073 #===END data_pbl0106_0m _database_code_depnum_ccdc_archive 'CCDC 635653' _ccdc_compound_id 1 _ccdc_biological_activity ? _ccdc_polymorph ? _ccdc_chemdiag_type ? _ccdc_chemdiag_records ? _ccdc_disorder ? _ccdc_comments ? _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H40 N8 O5 S2' _chemical_formula_weight 644.81 _chemical_absolute_configuration rmad 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.8416(10) _cell_length_b 8.7033(7) _cell_length_c 13.7476(11) _cell_angle_alpha 90.00 _cell_angle_beta 96.649(2) _cell_angle_gamma 90.00 _cell_volume 1526.2(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6993 _cell_measurement_theta_min 2.78 _cell_measurement_theta_max 39.48 _exptl_crystal_description Plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.403 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 684 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.933502 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30934 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.78 _diffrn_reflns_theta_max 39.51 _reflns_number_total 14681 _reflns_number_gt 14085 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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^)+(0.0474P)^2^+0.0944P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(2) _refine_ls_number_reflns 14681 _refine_ls_number_parameters 467 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0346 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0897 _refine_ls_wR_factor_gt 0.0881 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _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 -0.123888(14) 0.61913(2) -0.089171(12) 0.01664(4) Uani 1 1 d . . . C1 C -0.00383(5) 0.45902(10) 0.21036(5) 0.01473(11) Uani 1 1 d . . . N1 N -0.06474(5) 0.38847(10) 0.26896(5) 0.01715(11) Uani 1 1 d . . . O1 O 0.03358(5) 0.33282(10) -0.37983(4) 0.02193(12) Uani 1 1 d . . . S2 S 0.319049(14) 0.65254(3) 0.301947(13) 0.01850(4) Uani 1 1 d . B . C2 C -0.16501(6) 0.31691(12) 0.23099(6) 0.01969(13) Uani 1 1 d . . . H2A H -0.2235 0.3827 0.2472 0.024 Uiso 1 1 calc R . . H2B H -0.1714 0.2161 0.2632 0.024 Uiso 1 1 calc R . . N2 N -0.03829(5) 0.48702(10) 0.11616(4) 0.01638(11) Uani 1 1 d . . . H2 H 0.0097(12) 0.497(2) 0.0784(11) 0.024(4) Uiso 1 1 d . . . O2 O 0.61713(5) 0.47640(14) 0.13077(7) 0.0361(2) Uani 1 1 d . . . C3 C -0.17354(6) 0.29429(11) 0.12084(6) 0.01933(13) Uani 1 1 d . . . H3A H -0.2460 0.2645 0.0955 0.023 Uiso 1 1 calc R . . H3B H -0.1256 0.2114 0.1048 0.023 Uiso 1 1 calc R . . N3 N -0.00670(5) 0.46858(10) -0.24480(4) 0.01858(12) Uani 1 1 d . . . H3 H 0.0099(11) 0.483(2) -0.1851(11) 0.022(3) Uiso 1 1 d . . . C4 C -0.14454(5) 0.44430(10) 0.07362(5) 0.01608(12) Uani 1 1 d . . . H4 H -0.1946 0.5263 0.0891 0.019 Uiso 1 1 calc R . . N4 N 0.14806(5) 0.33283(11) -0.24083(5) 0.02162(13) Uani 1 1 d . B . H4N H 0.1598(11) 0.358(2) -0.1832(10) 0.017(3) Uiso 1 1 d . . . C5 C -0.14799(6) 0.43019(11) -0.03744(5) 0.01718(12) Uani 1 1 d . . . H5A H -0.2175 0.3914 -0.0656 0.021 Uiso 1 1 calc R . . H5B H -0.0940 0.3564 -0.0538 0.021 Uiso 1 1 calc R . . N5 N 0.47693(7) 0.5062(2) 0.01485(7) 0.0498(4) Uani 1 1 d . . . H5 H 0.4117(15) 0.492(3) -0.0004(14) 0.043(5) Uiso 1 1 d . . . C6 C -0.16948(6) 0.59183(10) -0.21483(5) 0.01589(11) Uani 1 1 d . . . N6 N 0.44891(5) 0.46890(13) 0.17502(6) 0.02604(17) Uani 1 1 d . . . H6 H 0.3842(13) 0.494(3) 0.1564(12) 0.029(4) Uiso 1 1 d . . . C7 C -0.26907(6) 0.64803(11) -0.24879(6) 0.01869(12) Uani 1 1 d . . . H7A H -0.3107 0.6938 -0.2039 0.022 Uiso 1 1 calc R . . N7 N 0.09299(5) 0.50813(10) 0.24429(4) 0.01792(12) Uani 1 1 d . . . H7 H 0.1319(11) 0.538(2) 0.1987(11) 0.021(3) Uiso 1 1 d . . . C8 C -0.30827(6) 0.63809(11) -0.34750(6) 0.02074(14) Uani 1 1 d . . . H8 H -0.3770 0.6729 -0.3697 0.025 Uiso 1 1 calc R . . C9 C -0.24474(7) 0.57624(11) -0.41267(6) 0.02038(13) Uani 1 1 d . . . H9 H -0.2701 0.5710 -0.4803 0.024 Uiso 1 1 calc R . . C10 C -0.14461(6) 0.52169(11) -0.38099(5) 0.01914(13) Uani 1 1 d . . . H10 H -0.1020 0.4821 -0.4272 0.023 Uiso 1 1 calc R . . C11 C -0.10600(5) 0.52483(10) -0.28091(5) 0.01563(11) Uani 1 1 d . . . C12 C 0.05720(6) 0.37473(11) -0.29436(5) 0.01662(12) Uani 1 1 d . . . C13 C 0.22458(7) 0.23705(13) -0.28289(6) 0.02359(16) Uani 1 1 d . . . H13A H 0.1882 0.1702 -0.3343 0.028 Uiso 1 1 calc R A 1 H13B H 0.2609 0.1703 -0.2314 0.028 Uiso 1 1 calc R A 1 C14 C 0.3086(2) 0.3419(4) -0.3292(2) 0.0225(4) Uani 0.567(3) 1 d P B 1 H14A H 0.3509 0.2749 -0.3676 0.027 Uiso 0.567(3) 1 calc PR B 1 H14B H 0.2702 0.4150 -0.3754 0.027 Uiso 0.567(3) 1 calc PR B 1 C14B C 0.2943(3) 0.3081(4) -0.3454(2) 0.0191(5) Uani 0.433(3) 1 d P B 2 H14C H 0.2530 0.3479 -0.4054 0.023 Uiso 0.433(3) 1 calc PR B 2 H14D H 0.3442 0.2305 -0.3651 0.023 Uiso 0.433(3) 1 calc PR B 2 C15 C 0.38421(14) 0.4343(2) -0.25595(14) 0.0196(3) Uani 0.567(3) 1 d P B 1 H15A H 0.4320 0.4949 -0.2926 0.023 Uiso 0.567(3) 1 calc PR B 1 H15B H 0.3432 0.5072 -0.2204 0.023 Uiso 0.567(3) 1 calc PR B 1 C15B C 0.35501(17) 0.4401(3) -0.29140(17) 0.0191(4) Uani 0.433(3) 1 d P B 2 H15D H 0.3948 0.4951 -0.3382 0.023 Uiso 0.433(3) 1 calc PR B 2 H15C H 0.3041 0.5136 -0.2687 0.023 Uiso 0.433(3) 1 calc PR B 2 C16 C 0.44931(12) 0.3320(2) -0.18189(13) 0.0194(3) Uani 0.567(3) 1 d P B 1 H16A H 0.4696 0.2383 -0.2159 0.023 Uiso 0.567(3) 1 calc PR B 1 H16B H 0.4048 0.2996 -0.1314 0.023 Uiso 0.567(3) 1 calc PR B 1 C16B C 0.43134(15) 0.3903(4) -0.20347(15) 0.0189(4) Uani 0.433(3) 1 d P B 2 H16C H 0.4840 0.3192 -0.2255 0.023 Uiso 0.433(3) 1 calc PR B 2 H16D H 0.3926 0.3350 -0.1560 0.023 Uiso 0.433(3) 1 calc PR B 2 C17 C 0.54941(11) 0.4079(2) -0.13046(11) 0.0226(3) Uani 0.567(3) 1 d P B 1 H17A H 0.5868 0.3315 -0.0858 0.027 Uiso 0.567(3) 1 calc PR B 1 H17B H 0.5958 0.4341 -0.1807 0.027 Uiso 0.567(3) 1 calc PR B 1 C17B C 0.48702(15) 0.5304(3) -0.15341(13) 0.0246(5) Uani 0.433(3) 1 d P B 2 H17C H 0.5335 0.5757 -0.1984 0.030 Uiso 0.433(3) 1 calc PR B 2 H17D H 0.4336 0.6085 -0.1423 0.030 Uiso 0.433(3) 1 calc PR B 2 C18 C 0.53199(18) 0.5524(3) -0.07177(16) 0.0232(3) Uani 0.567(3) 1 d P B 1 H18A H 0.6001 0.6014 -0.0491 0.028 Uiso 0.567(3) 1 calc PR B 1 H18B H 0.4886 0.6269 -0.1131 0.028 Uiso 0.567(3) 1 calc PR B 1 C18B C 0.55174(19) 0.4961(6) -0.05651(18) 0.0290(7) Uani 0.433(3) 1 d P B 2 H18C H 0.5829 0.3921 -0.0568 0.035 Uiso 0.433(3) 1 calc PR B 2 H18D H 0.6086 0.5724 -0.0424 0.035 Uiso 0.433(3) 1 calc PR B 2 C19 C 0.52140(7) 0.48231(17) 0.10728(7) 0.0313(2) Uani 1 1 d . B . C20 C 0.47658(6) 0.44733(12) 0.27560(6) 0.02117(14) Uani 1 1 d . B . C21 C 0.56165(7) 0.35329(14) 0.31016(9) 0.02915(19) Uani 1 1 d . . . H21 H 0.6021 0.3059 0.2649 0.035 Uiso 1 1 calc R B . C22 C 0.58722(7) 0.32894(15) 0.40936(10) 0.0329(2) Uani 1 1 d . B . H22 H 0.6465 0.2677 0.4316 0.039 Uiso 1 1 calc R . . C23 C 0.52775(8) 0.39242(14) 0.47677(8) 0.0303(2) Uani 1 1 d . . . H23 H 0.5442 0.3718 0.5447 0.036 Uiso 1 1 calc R B . C24 C 0.44351(7) 0.48685(13) 0.44404(6) 0.02399(16) Uani 1 1 d . B . H24 H 0.4031 0.5318 0.4902 0.029 Uiso 1 1 calc R . . C25 C 0.41734(6) 0.51677(11) 0.34398(5) 0.01842(12) Uani 1 1 d . . . C26 C 0.21380(6) 0.61624(12) 0.37654(5) 0.02002(13) Uani 1 1 d . . . H26A H 0.2454 0.5970 0.4446 0.024 Uiso 1 1 calc R B . H26B H 0.1709 0.7106 0.3772 0.024 Uiso 1 1 calc R . . C27 C 0.14098(6) 0.48231(11) 0.34462(5) 0.01683(12) Uani 1 1 d . B . H27 H 0.1812 0.3837 0.3487 0.020 Uiso 1 1 calc R . . C28 C 0.05402(6) 0.47607(12) 0.41145(5) 0.02016(14) Uani 1 1 d . . . H28A H 0.0841 0.4456 0.4782 0.024 Uiso 1 1 calc R B . H28B H 0.0224 0.5793 0.4154 0.024 Uiso 1 1 calc R . . C29 C -0.02994(7) 0.36198(12) 0.37294(5) 0.02056(14) Uani 1 1 d . B . H29A H -0.0019 0.2563 0.3818 0.025 Uiso 1 1 calc R . . H29B H -0.0906 0.3715 0.4109 0.025 Uiso 1 1 calc R . . N1S N 0.19593(5) 0.46801(10) 0.00138(5) 0.01835(12) Uani 1 1 d . . . O1S O 0.10023(4) 0.45815(10) -0.02970(4) 0.02039(12) Uani 1 1 d . . . O2S O 0.22493(5) 0.52620(11) 0.08256(4) 0.02574(15) Uani 1 1 d . . . O3S O 0.26219(5) 0.41945(14) -0.05164(5) 0.0327(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 S1 0.01698(7) 0.01818(9) 0.01445(6) -0.00105(5) 0.00048(5) 0.00036(6) C1 0.0141(2) 0.0181(3) 0.0122(2) 0.0011(2) 0.00277(17) 0.0009(2) N1 0.0164(2) 0.0219(3) 0.0137(2) 0.0031(2) 0.00431(17) -0.0003(2) O1 0.0239(3) 0.0279(4) 0.01360(19) -0.0021(2) 0.00029(17) 0.0028(2) S2 0.01684(7) 0.02269(10) 0.01535(6) 0.00002(6) -0.00075(5) 0.00111(6) C2 0.0178(3) 0.0230(4) 0.0190(3) 0.0033(3) 0.0056(2) -0.0030(3) N2 0.0134(2) 0.0236(3) 0.01217(19) 0.00193(19) 0.00143(15) -0.0022(2) O2 0.0138(2) 0.0551(6) 0.0404(4) -0.0162(4) 0.0074(2) -0.0049(3) C3 0.0182(3) 0.0204(4) 0.0196(3) 0.0006(2) 0.0030(2) -0.0026(2) N3 0.0158(2) 0.0261(4) 0.0132(2) -0.0018(2) -0.00096(16) 0.0036(2) C4 0.0131(2) 0.0203(3) 0.0149(2) 0.0001(2) 0.00180(18) -0.0001(2) N4 0.0174(2) 0.0313(4) 0.0158(2) -0.0020(2) 0.00032(18) 0.0054(3) C5 0.0166(3) 0.0196(3) 0.0150(2) -0.0006(2) 0.00022(19) -0.0012(2) N5 0.0208(3) 0.1071(13) 0.0229(3) -0.0223(5) 0.0087(3) -0.0259(5) C6 0.0150(2) 0.0178(3) 0.0144(2) 0.0011(2) -0.00013(18) 0.0001(2) N6 0.0122(2) 0.0433(5) 0.0228(3) -0.0061(3) 0.00309(19) -0.0004(3) C7 0.0159(2) 0.0193(3) 0.0203(3) 0.0025(2) -0.0004(2) 0.0010(2) N7 0.0147(2) 0.0279(4) 0.01111(18) 0.0019(2) 0.00142(15) -0.0020(2) C8 0.0172(3) 0.0209(4) 0.0225(3) 0.0035(3) -0.0045(2) 0.0004(2) C9 0.0215(3) 0.0203(4) 0.0175(3) 0.0021(2) -0.0055(2) -0.0011(3) C10 0.0209(3) 0.0217(4) 0.0140(2) 0.0006(2) -0.0019(2) 0.0001(3) C11 0.0152(2) 0.0173(3) 0.0138(2) 0.0008(2) -0.00068(18) -0.0005(2) C12 0.0157(2) 0.0202(3) 0.0139(2) 0.0013(2) 0.00173(18) -0.0001(2) C13 0.0194(3) 0.0299(5) 0.0216(3) -0.0007(3) 0.0026(2) 0.0059(3) C14 0.0232(9) 0.0252(13) 0.0198(9) -0.0016(7) 0.0052(7) -0.0013(8) C14B 0.0202(10) 0.0204(14) 0.0167(10) -0.0024(8) 0.0029(7) -0.0013(8) C15 0.0210(6) 0.0177(6) 0.0202(7) 0.0016(5) 0.0035(5) -0.0016(5) C15B 0.0179(7) 0.0227(9) 0.0167(7) 0.0010(6) 0.0020(6) -0.0025(6) C16 0.0172(5) 0.0188(7) 0.0227(6) 0.0004(5) 0.0043(4) -0.0008(5) C16B 0.0145(6) 0.0261(12) 0.0165(6) 0.0002(7) 0.0035(5) 0.0008(7) C17 0.0149(5) 0.0286(8) 0.0247(6) -0.0018(5) 0.0043(4) -0.0008(5) C17B 0.0185(7) 0.0379(13) 0.0175(7) 0.0000(7) 0.0014(5) -0.0086(7) C18 0.0212(8) 0.0272(10) 0.0218(7) -0.0030(6) 0.0049(6) -0.0037(6) C18B 0.0129(8) 0.058(2) 0.0169(8) -0.0039(11) 0.0025(6) -0.0074(10) C19 0.0145(3) 0.0518(7) 0.0287(4) -0.0179(4) 0.0066(3) -0.0070(4) C20 0.0120(2) 0.0249(4) 0.0259(3) -0.0035(3) -0.0008(2) -0.0011(2) C21 0.0136(3) 0.0262(5) 0.0470(5) 0.0005(4) 0.0009(3) 0.0002(3) C22 0.0172(3) 0.0271(5) 0.0512(6) 0.0079(4) -0.0093(3) -0.0013(3) C23 0.0263(4) 0.0274(5) 0.0331(4) 0.0061(4) -0.0145(3) -0.0037(3) C24 0.0257(3) 0.0241(4) 0.0198(3) -0.0005(3) -0.0078(2) -0.0013(3) C25 0.0153(2) 0.0208(4) 0.0179(2) -0.0016(2) -0.00369(19) -0.0014(2) C26 0.0186(3) 0.0262(4) 0.0151(2) -0.0037(3) 0.00105(19) 0.0011(3) C27 0.0170(2) 0.0216(4) 0.0117(2) 0.0006(2) 0.00076(18) 0.0040(2) C28 0.0214(3) 0.0276(4) 0.0119(2) 0.0015(2) 0.00362(19) 0.0026(3) C29 0.0221(3) 0.0262(4) 0.0142(2) 0.0051(2) 0.0055(2) 0.0012(3) N1S 0.0116(2) 0.0289(4) 0.0143(2) 0.0039(2) 0.00059(16) -0.0012(2) O1S 0.01157(18) 0.0329(4) 0.0162(2) 0.0032(2) -0.00064(15) -0.0004(2) O2S 0.0186(2) 0.0445(5) 0.0139(2) -0.0057(2) 0.00082(17) -0.0030(3) O3S 0.0140(2) 0.0629(6) 0.0219(3) -0.0140(3) 0.00438(19) 0.0000(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 C6 1.7747(7) . ? S1 C5 1.8321(9) . ? C1 N1 1.3356(10) . ? C1 N2 1.3414(9) . ? C1 N7 1.3461(10) . ? N1 C29 1.4658(10) . ? N1 C2 1.4706(11) . ? O1 C12 1.2341(9) . ? S2 C25 1.7761(9) . ? S2 C26 1.8163(8) . ? C2 C3 1.5184(11) . ? N2 C4 1.4688(9) . ? O2 C19 1.2354(11) . ? C3 C4 1.5233(13) . ? N3 C12 1.3907(11) . ? N3 C11 1.4021(10) . ? C4 C5 1.5273(10) . ? N4 C12 1.3554(10) . ? N4 C13 1.4582(12) . ? N5 C19 1.3475(15) . ? N5 C18B 1.453(3) . ? N5 C18 1.508(2) . ? C6 C7 1.3980(10) . ? C6 C11 1.4147(11) . ? N6 C19 1.3958(12) . ? N6 C20 1.4000(12) . ? C7 C8 1.3944(11) . ? N7 C27 1.4614(9) . ? C8 C9 1.3883(13) . ? C9 C10 1.3924(11) . ? C10 C11 1.4076(10) . ? C13 C14B 1.449(4) . ? C13 C14 1.600(3) . ? C14 C15 1.541(3) . ? C14B C15B 1.531(4) . ? C15 C16 1.526(3) . ? C15B C16B 1.528(3) . ? C16 C17 1.542(2) . ? C16B C17B 1.535(3) . ? C17 C18 1.525(3) . ? C17B C18B 1.516(3) . ? C20 C21 1.4032(13) . ? C20 C25 1.4118(12) . ? C21 C22 1.3816(17) . ? C22 C23 1.3825(19) . ? C23 C24 1.3913(14) . ? C24 C25 1.4021(11) . ? C26 C27 1.5267(13) . ? C27 C28 1.5270(10) . ? C28 C29 1.5154(14) . ? N1S O2S 1.2427(9) . ? N1S O3S 1.2559(10) . ? N1S O1S 1.2565(8) . ? 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 S1 C5 101.90(4) . . ? N1 C1 N2 121.00(6) . . ? N1 C1 N7 121.26(6) . . ? N2 C1 N7 117.71(6) . . ? C1 N1 C29 121.79(7) . . ? C1 N1 C2 122.04(6) . . ? C29 N1 C2 115.79(6) . . ? C25 S2 C26 104.35(4) . . ? N1 C2 C3 111.59(6) . . ? C1 N2 C4 121.72(6) . . ? C2 C3 C4 108.72(7) . . ? C12 N3 C11 126.56(6) . . ? N2 C4 C3 108.00(6) . . ? N2 C4 C5 109.66(6) . . ? C3 C4 C5 112.14(7) . . ? C12 N4 C13 121.05(7) . . ? C4 C5 S1 109.22(6) . . ? C19 N5 C18B 112.72(14) . . ? C19 N5 C18 126.83(11) . . ? C18B N5 C18 22.49(15) . . ? C7 C6 C11 120.17(6) . . ? C7 C6 S1 117.66(6) . . ? C11 C6 S1 122.04(5) . . ? C19 N6 C20 123.89(7) . . ? C8 C7 C6 121.10(8) . . ? C1 N7 C27 123.36(6) . . ? C9 C8 C7 118.63(7) . . ? C8 C9 C10 121.38(7) . . ? C9 C10 C11 120.47(7) . . ? N3 C11 C10 122.84(7) . . ? N3 C11 C6 118.99(6) . . ? C10 C11 C6 118.15(7) . . ? O1 C12 N4 122.59(8) . . ? O1 C12 N3 123.10(7) . . ? N4 C12 N3 114.31(6) . . ? C14B C13 N4 118.80(17) . . ? C14B C13 C14 13.98(11) . . ? N4 C13 C14 110.38(14) . . ? C15 C14 C13 116.15(18) . . ? C13 C14B C15B 110.4(2) . . ? C16 C15 C14 112.72(17) . . ? C16B C15B C14B 114.5(2) . . ? C15 C16 C17 114.80(17) . . ? C15B C16B C17B 110.6(2) . . ? C18 C17 C16 115.48(14) . . ? C18B C17B C16B 114.7(3) . . ? N5 C18 C17 107.97(17) . . ? N5 C18B C17B 104.1(2) . . ? O2 C19 N5 123.58(9) . . ? O2 C19 N6 122.85(10) . . ? N5 C19 N6 113.54(8) . . ? N6 C20 C21 120.75(9) . . ? N6 C20 C25 120.37(8) . . ? C21 C20 C25 118.86(9) . . ? C22 C21 C20 120.69(10) . . ? C21 C22 C23 120.92(9) . . ? C22 C23 C24 119.24(9) . . ? C23 C24 C25 121.07(9) . . ? C24 C25 C20 119.17(8) . . ? C24 C25 S2 121.55(7) . . ? C20 C25 S2 119.05(6) . . ? C27 C26 S2 116.21(5) . . ? N7 C27 C26 109.34(7) . . ? N7 C27 C28 108.39(6) . . ? C26 C27 C28 108.70(7) . . ? C29 C28 C27 110.69(7) . . ? N1 C29 C28 111.22(7) . . ? O2S N1S O3S 120.37(6) . . ? O2S N1S O1S 120.85(7) . . ? O3S N1S O1S 118.78(7) . . ? 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 N2 C1 N1 C29 -177.69(8) . . . . ? N7 C1 N1 C29 0.48(13) . . . . ? N2 C1 N1 C2 9.66(13) . . . . ? N7 C1 N1 C2 -172.17(8) . . . . ? C1 N1 C2 C3 16.04(12) . . . . ? C29 N1 C2 C3 -157.02(8) . . . . ? N1 C1 N2 C4 1.11(13) . . . . ? N7 C1 N2 C4 -177.13(8) . . . . ? N1 C2 C3 C4 -49.07(9) . . . . ? C1 N2 C4 C3 -35.34(10) . . . . ? C1 N2 C4 C5 -157.81(8) . . . . ? C2 C3 C4 N2 57.39(8) . . . . ? C2 C3 C4 C5 178.33(6) . . . . ? N2 C4 C5 S1 -65.10(8) . . . . ? C3 C4 C5 S1 174.93(5) . . . . ? C6 S1 C5 C4 -163.12(5) . . . . ? C5 S1 C6 C7 100.56(7) . . . . ? C5 S1 C6 C11 -83.48(7) . . . . ? C11 C6 C7 C8 0.65(14) . . . . ? S1 C6 C7 C8 176.70(7) . . . . ? N1 C1 N7 C27 3.16(13) . . . . ? N2 C1 N7 C27 -178.61(8) . . . . ? C6 C7 C8 C9 -2.43(14) . . . . ? C7 C8 C9 C10 1.38(14) . . . . ? C8 C9 C10 C11 1.45(14) . . . . ? C12 N3 C11 C10 -14.89(14) . . . . ? C12 N3 C11 C6 166.98(8) . . . . ? C9 C10 C11 N3 178.67(9) . . . . ? C9 C10 C11 C6 -3.18(13) . . . . ? C7 C6 C11 N3 -179.64(8) . . . . ? S1 C6 C11 N3 4.50(11) . . . . ? C7 C6 C11 C10 2.14(12) . . . . ? S1 C6 C11 C10 -173.72(7) . . . . ? C13 N4 C12 O1 1.22(15) . . . . ? C13 N4 C12 N3 -178.76(9) . . . . ? C11 N3 C12 O1 2.20(15) . . . . ? C11 N3 C12 N4 -177.82(9) . . . . ? C12 N4 C13 C14B 79.78(18) . . . . ? C12 N4 C13 C14 92.08(14) . . . . ? C14B C13 C14 C15 -162.1(12) . . . . ? N4 C13 C14 C15 68.5(2) . . . . ? N4 C13 C14B C15B 55.9(3) . . . . ? C14 C13 C14B C15B 0.2(8) . . . . ? C13 C14 C15 C16 59.1(2) . . . . ? C13 C14B C15B C16B 65.7(3) . . . . ? C14 C15 C16 C17 160.50(16) . . . . ? C14B C15B C16B C17B -179.1(2) . . . . ? C15 C16 C17 C18 59.90(19) . . . . ? C15B C16B C17B C18B 171.02(17) . . . . ? C19 N5 C18 C17 98.6(2) . . . . ? C18B N5 C18 C17 41.8(4) . . . . ? C16 C17 C18 N5 67.6(2) . . . . ? C19 N5 C18B C17B -178.5(2) . . . . ? C18 N5 C18B C17B -45.1(3) . . . . ? C16B C17B C18B N5 -86.0(3) . . . . ? C18B N5 C19 O2 10.6(3) . . . . ? C18 N5 C19 O2 -9.7(3) . . . . ? C18B N5 C19 N6 -171.0(2) . . . . ? C18 N5 C19 N6 168.67(18) . . . . ? C20 N6 C19 O2 -0.1(2) . . . . ? C20 N6 C19 N5 -178.46(13) . . . . ? C19 N6 C20 C21 -37.81(17) . . . . ? C19 N6 C20 C25 143.94(12) . . . . ? N6 C20 C21 C22 -178.32(10) . . . . ? C25 C20 C21 C22 -0.04(15) . . . . ? C20 C21 C22 C23 2.10(17) . . . . ? C21 C22 C23 C24 -2.49(17) . . . . ? C22 C23 C24 C25 0.85(16) . . . . ? C23 C24 C25 C20 1.16(14) . . . . ? C23 C24 C25 S2 -173.29(8) . . . . ? N6 C20 C25 C24 176.73(9) . . . . ? C21 C20 C25 C24 -1.56(13) . . . . ? N6 C20 C25 S2 -8.67(12) . . . . ? C21 C20 C25 S2 173.04(7) . . . . ? C26 S2 C25 C24 -42.73(8) . . . . ? C26 S2 C25 C20 142.81(7) . . . . ? C25 S2 C26 C27 -81.04(6) . . . . ? C1 N7 C27 C26 -148.29(8) . . . . ? C1 N7 C27 C28 -29.95(12) . . . . ? S2 C26 C27 N7 -58.22(8) . . . . ? S2 C26 C27 C28 -176.37(6) . . . . ? N7 C27 C28 C29 52.07(10) . . . . ? C26 C27 C28 C29 170.82(7) . . . . ? C1 N1 C29 C28 24.00(12) . . . . ? C2 N1 C29 C28 -162.91(8) . . . . ? C27 C28 C29 N1 -50.16(10) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 39.51 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.558 _refine_diff_density_min -0.499 _refine_diff_density_rms 0.060 #===END