# Electronic Supplementary Material (ESI) for RSC Advances # This journal is © The Royal Society of Chemistry 2012 data_l1+guest3 #TrackingRef '- complexes 1 and 2.cif' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Lu, Tong-Bu' _publ_contact_author_email lutongbu@mail.sysu.edu.cn _publ_section_title ; The recognition of 1,5-naphthalenedisulfonate anion by a protonated azamacrocyclic ligand via multiple supramolecular interactions ; loop_ _publ_author_name 'Gao-Yi Xie' 'Long Jiang' ; Tong-Bu Lu ; # Attachment '1.cif' data_1 #TrackingRef '- complexes 1 and 2.cif' _database_code_depnum_ccdc_archive 'CCDC 874373' #TrackingRef '1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H115 N8 O38 P S6' _chemical_formula_weight 1948.07 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.9514(4) _cell_length_b 14.2719(5) _cell_length_c 25.9721(9) _cell_angle_alpha 87.967(3) _cell_angle_beta 86.878(3) _cell_angle_gamma 67.322(3) _cell_volume 4422.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9661 _cell_measurement_theta_min 3.3538 _cell_measurement_theta_max 65.3311 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2060 _exptl_absorpt_coefficient_mu 2.413 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4688 _exptl_absorpt_correction_T_max 0.6844 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_measurement_method '\w scans' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_detector_area_resol_mean 10.5058 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30285 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0453 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 65.43 _reflns_number_total 14678 _reflns_number_gt 10932 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _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^)+(0.1146P)^2^+4.1304P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14678 _refine_ls_number_parameters 489 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0857 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.2017 _refine_ls_wR_factor_gt 0.1802 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.047 _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 O1W O 0.6649(8) 1.0635(7) 0.2099(4) 0.094(2) Uani 0.50 1 d PU A 1 O1A O 0.7168(9) 1.0518(8) 0.2512(4) 0.105(2) Uani 0.50 1 d PU B 2 O2W O 0.7306(14) 1.0603(15) 0.1479(6) 0.066(3) Uani 0.30 1 d PU C 1 O2A O 0.747(2) 1.065(2) 0.1338(10) 0.065(4) Uani 0.20 1 d PU D 2 O3W O 0.6522(9) 1.2568(9) 0.0137(4) 0.085(2) Uani 0.40 1 d PU E 1 O3A O 0.661(4) 1.338(4) 0.0079(17) 0.084(4) Uani 0.10 1 d PU F 2 O4W O 0.8235(7) 1.1772(7) 0.0762(3) 0.120(2) Uani 0.75 1 d PU G 1 O4A O 0.7137(18) 1.2153(17) 0.0630(8) 0.109(3) Uani 0.25 1 d PU H 2 O5W O 0.6971(3) 0.5029(3) 0.07265(16) 0.0830(12) Uani 1 1 d . . . O6W O 0.1676(7) 0.6405(6) 0.5260(3) 0.0757(17) Uani 0.50 1 d PU I 1 O6A O 0.1502(8) 0.6205(7) 0.5672(4) 0.095(2) Uani 0.50 1 d PU J 2 O7W O 0.0807(2) 0.1400(2) 0.46768(12) 0.0525(7) Uani 1 1 d . . . O8W O 0.3791(3) 0.5779(3) 0.55567(17) 0.0749(11) Uani 0.95 1 d PU K 1 O8A O 0.270(7) 0.598(6) 0.569(3) 0.081(2) Uani 0.05 1 d PU L 2 O9W O 0.4594(3) 0.7003(3) 0.49442(12) 0.0546(8) Uani 1 1 d . . . O10W O 0.9012(7) 0.5152(7) 0.4195(4) 0.087(2) Uani 0.50 1 d PU M 1 O10A O 0.9046(7) 0.5633(7) 0.3851(4) 0.089(2) Uani 0.50 1 d PU N 2 O11W O 0.9956(5) 0.5994(5) 0.4835(3) 0.157(3) Uani 1 1 d . . . O12W O 0.1211(13) 0.6157(12) 0.0725(5) 0.113(3) Uani 0.50 1 d PU O 1 O12A O 0.1406(14) 0.5900(13) 0.0558(6) 0.121(3) Uani 0.50 1 d PU P 2 O12B O 0.1219(11) 0.6666(11) 0.0265(5) 0.134(3) Uani 0.50 1 d PU Q 2 O13W O 1.0012(6) 0.9914(6) 0.0559(3) 0.147(3) Uani 0.90 1 d PU R 1 O13A O 0.907(6) 1.109(6) 0.057(3) 0.147(4) Uani 0.10 1 d PU S 2 O14W O 0.8466(9) 0.8631(8) 0.1514(4) 0.168(3) Uani 0.80 1 d PU T 1 O14A O 0.911(3) 0.889(3) 0.1185(16) 0.160(4) Uani 0.20 1 d PU U 2 O15W O 0.9628(6) 0.5401(5) 0.0475(3) 0.158(3) Uani 1 1 d . . . O16W O 0.8626(9) 0.8532(9) 0.2262(5) 0.184(4) Uani 0.80 1 d PU V 1 O16A O 0.958(4) 0.851(3) 0.2490(18) 0.178(5) Uani 0.20 1 d PU W 2 O17W O 1.032(2) 0.810(2) 0.1054(9) 0.149(4) Uani 0.35 1 d PU X 1 O17A O 1.058(4) 0.813(5) 0.081(2) 0.144(5) Uani 0.15 1 d PU Y 2 C1 C 0.3164(3) 0.4649(3) 0.43542(16) 0.0402(9) Uani 1 1 d . . . H1A H 0.2736 0.5386 0.4402 0.048 Uiso 1 1 calc R . . H1B H 0.3956 0.4501 0.4425 0.048 Uiso 1 1 calc R . . C2 C 0.2708(4) 0.4062(3) 0.47355(16) 0.0420(9) Uani 1 1 d . . . H2A H 0.2665 0.4336 0.5084 0.050 Uiso 1 1 calc R . . H2B H 0.1938 0.4167 0.4645 0.050 Uiso 1 1 calc R . . C3 C 0.2905(4) 0.2390(3) 0.51193(16) 0.0436(9) Uani 1 1 d . . . H3A H 0.2096 0.2613 0.5060 0.052 Uiso 1 1 calc R . . H3B H 0.2979 0.2574 0.5475 0.052 Uiso 1 1 calc R . . C4 C 0.3449(4) 0.1252(3) 0.50705(15) 0.0427(9) Uani 1 1 d . . . H4A H 0.4267 0.1054 0.5012 0.051 Uiso 1 1 calc R . . H4B H 0.3323 0.0933 0.5400 0.051 Uiso 1 1 calc R . . C5 C 0.3521(3) -0.0294(3) 0.46239(15) 0.0395(9) Uani 1 1 d . . . H5A H 0.3681 -0.0572 0.4979 0.047 Uiso 1 1 calc R . . H5B H 0.4242 -0.0510 0.4421 0.047 Uiso 1 1 calc R . . C6 C 0.2776(3) -0.0746(3) 0.43878(14) 0.0383(9) Uani 1 1 d . . . H6A H 0.2945 -0.1434 0.4538 0.046 Uiso 1 1 calc R . . H6B H 0.1986 -0.0326 0.4485 0.046 Uiso 1 1 calc R . . C7 C 0.3800(5) 0.3993(4) 0.04174(19) 0.0636(13) Uani 1 1 d . . . H7A H 0.4528 0.3426 0.0469 0.076 Uiso 1 1 calc R . . H7B H 0.3932 0.4484 0.0171 0.076 Uiso 1 1 calc R . . C8 C 0.3008(5) 0.3584(4) 0.01889(18) 0.0585(12) Uani 1 1 d . . . H8A H 0.2748 0.3201 0.0455 0.070 Uiso 1 1 calc R . . H8B H 0.2346 0.4151 0.0060 0.070 Uiso 1 1 calc R . . C9 C 0.2914(5) 0.2644(4) -0.05905(18) 0.0635(13) Uani 1 1 d . . . H9A H 0.3409 0.2167 -0.0851 0.076 Uiso 1 1 calc R . . H9B H 0.2444 0.3268 -0.0776 0.076 Uiso 1 1 calc R . . C10 C 0.2165(4) 0.2172(4) -0.03298(19) 0.0575(12) Uani 1 1 d . . . H10A H 0.1683 0.2637 -0.0062 0.069 Uiso 1 1 calc R . . H10B H 0.1671 0.2090 -0.0587 0.069 Uiso 1 1 calc R . . C11 C 0.2058(4) 0.0588(4) 0.00280(18) 0.0552(12) Uani 1 1 d . . . H11A H 0.1949 0.0303 -0.0297 0.066 Uiso 1 1 calc R . . H11B H 0.1316 0.1065 0.0159 0.066 Uiso 1 1 calc R . . C12 C 0.2522(4) -0.0265(4) 0.04179(16) 0.0516(11) Uani 1 1 d . . . H12A H 0.2134 -0.0738 0.0395 0.062 Uiso 1 1 calc R . . H12B H 0.3328 -0.0647 0.0332 0.062 Uiso 1 1 calc R . . C13 C 0.3236(3) 0.5162(3) 0.34289(15) 0.0365(8) Uani 1 1 d . . . H13A H 0.3951 0.5237 0.3483 0.044 Uiso 1 1 calc R . . H13B H 0.2618 0.5830 0.3487 0.044 Uiso 1 1 calc R . . C14 C 0.3231(3) 0.4834(3) 0.28823(15) 0.0349(8) Uani 1 1 d . . . C15 C 0.4248(3) 0.4235(3) 0.26297(16) 0.0379(9) Uani 1 1 d . . . C16 C 0.5301(3) 0.3912(3) 0.28769(18) 0.0458(10) Uani 1 1 d . . . H16 H 0.5318 0.4114 0.3220 0.055 Uiso 1 1 calc R . . C17 C 0.6263(4) 0.3325(4) 0.2627(2) 0.0580(12) Uani 1 1 d . . . H17 H 0.6945 0.3098 0.2801 0.070 Uiso 1 1 calc R . . C18 C 0.6272(4) 0.3045(4) 0.2112(2) 0.0622(13) Uani 1 1 d . . . H18 H 0.6963 0.2655 0.1939 0.075 Uiso 1 1 calc R . . C19 C 0.5304(4) 0.3326(4) 0.18604(19) 0.0525(11) Uani 1 1 d . . . H19 H 0.5325 0.3128 0.1513 0.063 Uiso 1 1 calc R . . C20 C 0.4252(3) 0.3917(3) 0.21109(17) 0.0418(9) Uani 1 1 d . . . C21 C 0.3234(3) 0.4187(3) 0.18665(16) 0.0396(9) Uani 1 1 d . . . C22 C 0.2215(3) 0.4797(3) 0.21160(16) 0.0394(9) Uani 1 1 d . . . C23 C 0.1171(4) 0.5111(3) 0.18701(18) 0.0497(11) Uani 1 1 d . . . H23 H 0.1162 0.4905 0.1527 0.060 Uiso 1 1 calc R . . C24 C 0.0201(4) 0.5694(4) 0.2113(2) 0.0585(12) Uani 1 1 d . . . H24 H -0.0480 0.5899 0.1939 0.070 Uiso 1 1 calc R . . C25 C 0.0188(4) 0.6004(4) 0.2627(2) 0.0558(12) Uani 1 1 d . . . H25 H -0.0502 0.6411 0.2796 0.067 Uiso 1 1 calc R . . C26 C 0.1157(3) 0.5721(3) 0.28796(18) 0.0442(10) Uani 1 1 d . . . H26 H 0.1135 0.5924 0.3226 0.053 Uiso 1 1 calc R . . C27 C 0.2211(3) 0.5121(3) 0.26308(15) 0.0363(8) Uani 1 1 d . . . C28 C 0.3219(4) 0.3790(3) 0.13369(16) 0.0469(10) Uani 1 1 d . . . H28A H 0.2500 0.3710 0.1300 0.056 Uiso 1 1 calc R . . H28B H 0.3832 0.3113 0.1297 0.056 Uiso 1 1 calc R . . C29 C 0.2645(3) 0.0154(3) 0.35110(15) 0.0369(8) Uani 1 1 d . . . H29A H 0.3242 0.0412 0.3556 0.044 Uiso 1 1 calc R . . H29B H 0.1927 0.0670 0.3642 0.044 Uiso 1 1 calc R . . C30 C 0.2573(3) -0.0017(3) 0.29459(14) 0.0335(8) Uani 1 1 d . . . C31 C 0.3571(3) -0.0412(3) 0.26349(14) 0.0355(8) Uani 1 1 d . . . C32 C 0.4644(3) -0.0622(3) 0.28290(16) 0.0424(9) Uani 1 1 d . . . H32 H 0.4701 -0.0520 0.3184 0.051 Uiso 1 1 calc R . . C33 C 0.5584(4) -0.0965(4) 0.25215(17) 0.0513(11) Uani 1 1 d . . . H33 H 0.6287 -0.1091 0.2663 0.062 Uiso 1 1 calc R . . C34 C 0.5540(4) -0.1136(4) 0.19959(17) 0.0502(11) Uani 1 1 d . . . H34 H 0.6208 -0.1373 0.1784 0.060 Uiso 1 1 calc R . . C35 C 0.4542(4) -0.0964(3) 0.17911(16) 0.0430(9) Uani 1 1 d . . . H35 H 0.4520 -0.1084 0.1435 0.052 Uiso 1 1 calc R . . C36 C 0.3521(3) -0.0605(3) 0.20999(14) 0.0356(8) Uani 1 1 d . . . C37 C 0.2480(3) -0.0413(3) 0.18917(15) 0.0372(9) Uani 1 1 d . . . C38 C 0.1480(3) 0.0023(3) 0.21914(16) 0.0409(9) Uani 1 1 d . . . C39 C 0.0404(4) 0.0299(4) 0.19784(18) 0.0541(11) Uani 1 1 d . . . H39 H 0.0359 0.0173 0.1625 0.065 Uiso 1 1 calc R . . C40 C -0.0550(4) 0.0735(5) 0.2270(2) 0.0671(14) Uani 1 1 d . . . H40 H -0.1253 0.0922 0.2118 0.080 Uiso 1 1 calc R . . C41 C -0.0513(4) 0.0917(4) 0.2801(2) 0.0601(13) Uani 1 1 d . . . H41 H -0.1190 0.1212 0.3003 0.072 Uiso 1 1 calc R . . C42 C 0.0484(3) 0.0670(3) 0.30211(17) 0.0459(10) Uani 1 1 d . . . H42 H 0.0495 0.0792 0.3378 0.055 Uiso 1 1 calc R . . C43 C 0.1527(3) 0.0227(3) 0.27286(15) 0.0380(9) Uani 1 1 d . . . C44 C 0.2448(4) -0.0720(3) 0.13418(15) 0.0427(9) Uani 1 1 d . . . H44A H 0.3127 -0.1331 0.1260 0.051 Uiso 1 1 calc R . . H44B H 0.1788 -0.0900 0.1311 0.051 Uiso 1 1 calc R . . C45 C 0.1654(3) 0.2731(3) 0.29645(16) 0.0378(9) Uani 1 1 d . . . C46 C 0.2723(3) 0.2250(3) 0.27653(16) 0.0379(9) Uani 1 1 d . . . H46 H 0.3339 0.2066 0.2983 0.046 Uiso 1 1 calc R . . C47 C 0.2908(3) 0.2027(3) 0.22376(15) 0.0372(8) Uani 1 1 d . . . H47 H 0.3651 0.1684 0.2102 0.045 Uiso 1 1 calc R . . C48 C 0.2036(3) 0.2295(3) 0.19181(16) 0.0387(9) Uani 1 1 d . . . H48 H 0.2175 0.2135 0.1563 0.046 Uiso 1 1 calc R . . C49 C 0.0915(3) 0.2816(3) 0.21155(17) 0.0395(9) Uani 1 1 d . . . C50 C -0.0029(3) 0.3140(3) 0.17912(19) 0.0472(10) Uani 1 1 d . . . C51 C -0.1096(4) 0.3622(4) 0.2000(2) 0.0570(12) Uani 1 1 d . . . H51 H -0.1718 0.3822 0.1784 0.068 Uiso 1 1 calc R . . C52 C -0.1272(4) 0.3821(4) 0.2527(2) 0.0565(12) Uani 1 1 d . . . H52 H -0.2015 0.4149 0.2666 0.068 Uiso 1 1 calc R . . C53 C -0.0401(3) 0.3553(3) 0.28441(19) 0.0465(10) Uani 1 1 d . . . H53 H -0.0542 0.3712 0.3200 0.056 Uiso 1 1 calc R . . C54 C 0.0719(3) 0.3039(3) 0.26500(17) 0.0396(9) Uani 1 1 d . . . C55 C 0.4022(3) 0.6729(3) 0.18752(15) 0.0364(8) Uani 1 1 d . . . C56 C 0.2967(3) 0.7082(3) 0.20992(15) 0.0367(8) Uani 1 1 d . . . H56 H 0.2342 0.7191 0.1895 0.044 Uiso 1 1 calc R . . C57 C 0.2799(3) 0.7285(3) 0.26271(15) 0.0361(8) Uani 1 1 d . . . H57 H 0.2059 0.7550 0.2776 0.043 Uiso 1 1 calc R . . C58 C 0.3686(3) 0.7107(3) 0.29295(14) 0.0329(8) Uani 1 1 d . . . H58 H 0.3558 0.7231 0.3289 0.039 Uiso 1 1 calc R . . C59 C 0.4802(3) 0.6735(3) 0.27126(14) 0.0340(8) Uani 1 1 d . . . C60 C 0.5766(3) 0.6545(3) 0.30120(16) 0.0377(9) Uani 1 1 d . . . C61 C 0.6807(3) 0.6250(3) 0.27816(18) 0.0466(10) Uani 1 1 d . . . H61 H 0.7435 0.6134 0.2984 0.056 Uiso 1 1 calc R . . C62 C 0.6960(4) 0.6115(4) 0.22457(19) 0.0523(11) Uani 1 1 d . . . H62 H 0.7689 0.5934 0.2088 0.063 Uiso 1 1 calc R . . C63 C 0.6082(3) 0.6238(3) 0.19494(17) 0.0454(10) Uani 1 1 d . . . H63 H 0.6209 0.6109 0.1590 0.054 Uiso 1 1 calc R . . C64 C 0.4978(3) 0.6558(3) 0.21715(15) 0.0350(8) Uani 1 1 d . . . N1 N 0.3095(3) 0.4389(2) 0.38083(12) 0.0344(7) Uani 1 1 d . . . H1C H 0.2412 0.4349 0.3768 0.041 Uiso 1 1 calc R . . H1D H 0.3643 0.3761 0.3738 0.041 Uiso 1 1 calc R . . N2 N 0.3403(3) 0.2947(2) 0.47478(13) 0.0383(7) Uani 1 1 d . . . H2C H 0.4114 0.2844 0.4843 0.046 Uiso 1 1 calc R . . H2D H 0.3459 0.2691 0.4423 0.046 Uiso 1 1 calc R . . N3 N 0.3022(3) 0.0848(2) 0.46446(12) 0.0366(7) Uani 1 1 d . . . H3C H 0.3181 0.1109 0.4335 0.044 Uiso 1 1 calc R . . H3D H 0.2255 0.1064 0.4687 0.044 Uiso 1 1 calc R . . N4 N 0.2897(3) -0.0823(2) 0.38128(11) 0.0341(7) Uani 1 1 d . . . H4C H 0.2433 -0.1124 0.3708 0.041 Uiso 1 1 calc R . . H4D H 0.3621 -0.1250 0.3726 0.041 Uiso 1 1 calc R . . N5 N 0.3357(3) 0.4502(3) 0.09188(14) 0.0530(9) Uani 1 1 d . . . H5C H 0.2675 0.5021 0.0871 0.064 Uiso 1 1 calc R . . H5D H 0.3838 0.4784 0.1026 0.064 Uiso 1 1 calc R . . N6 N 0.3618(4) 0.2908(3) -0.02401(14) 0.0599(10) Uani 1 1 d . . . H6C H 0.4022 0.3215 -0.0432 0.072 Uiso 1 1 calc R . . H6D H 0.4122 0.2316 -0.0102 0.072 Uiso 1 1 calc R . . N7 N 0.2796(3) 0.1161(3) -0.00845(14) 0.0508(9) Uani 1 1 d . . . H7C H 0.3387 0.0789 -0.0302 0.061 Uiso 1 1 calc R . . H7D H 0.3082 0.1254 0.0217 0.061 Uiso 1 1 calc R . . N8 N 0.2388(3) 0.0108(3) 0.09609(12) 0.0397(7) Uani 1 1 d . . . H8C H 0.2944 0.0338 0.1019 0.048 Uiso 1 1 calc R . . H8D H 0.1709 0.0643 0.1005 0.048 Uiso 1 1 calc R . . O1 O 0.2546(2) 0.2420(2) 0.38591(11) 0.0424(6) Uani 1 1 d . . . O2 O 0.1089(2) 0.4062(2) 0.37048(11) 0.0429(6) Uani 1 1 d . . . O3 O 0.0624(2) 0.2574(2) 0.38310(12) 0.0514(7) Uani 1 1 d . . . O4 O 0.0871(4) 0.3447(3) 0.09240(14) 0.0792(11) Uani 1 1 d . . . O5 O -0.0980(3) 0.3450(3) 0.09187(16) 0.0810(12) Uani 1 1 d . . . O6 O 0.0566(3) 0.1885(3) 0.10283(15) 0.0704(10) Uani 1 1 d . . . O7 O 0.4762(3) 0.7088(2) 0.09663(11) 0.0542(8) Uani 1 1 d . . . O8 O 0.4841(3) 0.5390(2) 0.11489(11) 0.0494(7) Uani 1 1 d . . . O9 O 0.3058(3) 0.6770(3) 0.10207(12) 0.0611(9) Uani 1 1 d . . . O10 O 0.6778(2) 0.6300(2) 0.38743(12) 0.0522(8) Uani 1 1 d . . . O11 O 0.5076(2) 0.7776(2) 0.37922(11) 0.0433(6) Uani 1 1 d . . . O12 O 0.5000(3) 0.6117(2) 0.39086(12) 0.0521(8) Uani 1 1 d . . . O19 O 0.5165(3) 0.1331(3) 0.02487(14) 0.0714(10) Uani 1 1 d . . . O20 O 0.5281(3) 0.1440(3) 0.11633(16) 0.0750(11) Uani 1 1 d . . . H20 H 0.5864 0.1030 0.1296 0.113 Uiso 1 1 calc R . . O21 O 0.3748(3) 0.1175(3) 0.08336(12) 0.0585(8) Uani 1 1 d . . . O22 O 0.5583(3) -0.0168(3) 0.07764(14) 0.0693(10) Uani 1 1 d . . . P1 P 0.49576(9) 0.09336(9) 0.07617(4) 0.0462(3) Uani 1 1 d . . . S1 S 0.14594(8) 0.29608(7) 0.36381(4) 0.0395(2) Uani 1 1 d . . . S2 S 0.01323(9) 0.29700(9) 0.11157(5) 0.0532(3) Uani 1 1 d . . . S3 S 0.41744(10) 0.64845(8) 0.12011(4) 0.0453(3) Uani 1 1 d . . . S4 S 0.56480(8) 0.66902(8) 0.36956(4) 0.0402(2) Uani 1 1 d . . . O13 O 1.0823(2) -0.1687(2) 0.45904(10) 0.0445(7) Uani 1 1 d . . . O14 O 1.1325(2) -0.1630(2) 0.36889(11) 0.0456(7) Uani 1 1 d . . . O15 O 1.1080(2) -0.3116(2) 0.40534(13) 0.0549(8) Uani 1 1 d . . . O16 O 0.4943(2) 0.25528(19) 0.38639(11) 0.0401(6) Uani 1 1 d . . . O17 O 0.4902(2) 0.0909(2) 0.40881(13) 0.0517(8) Uani 1 1 d . . . O18 O 0.5313(2) 0.1283(2) 0.32042(11) 0.0470(7) Uani 1 1 d . . . S5 S 1.07461(7) -0.20218(7) 0.40765(4) 0.0367(2) Uani 1 1 d . . . S6 S 0.53825(7) 0.14733(7) 0.37386(4) 0.0363(2) Uani 1 1 d . . . C65 C 0.9306(3) -0.1488(3) 0.39218(14) 0.0317(8) Uani 1 1 d . . . C66 C 0.8862(3) -0.2138(3) 0.37431(16) 0.0387(9) Uani 1 1 d . . . H66 H 0.9310 -0.2843 0.3721 0.046 Uiso 1 1 calc R . . C67 C 0.7746(3) -0.1765(3) 0.35919(16) 0.0402(9) Uani 1 1 d . . . H67 H 0.7447 -0.2219 0.3463 0.048 Uiso 1 1 calc R . . C68 C 0.7093(3) -0.0760(3) 0.36291(15) 0.0349(8) Uani 1 1 d . . . H68 H 0.6341 -0.0523 0.3527 0.042 Uiso 1 1 calc R . . C69 C 0.7505(3) -0.0057(3) 0.38168(13) 0.0300(7) Uani 1 1 d . . . C70 C 0.6828(3) 0.0997(3) 0.38760(14) 0.0314(8) Uani 1 1 d . . . C71 C 0.7254(3) 0.1656(3) 0.40555(15) 0.0364(8) Uani 1 1 d . . . H71 H 0.6794 0.2357 0.4085 0.044 Uiso 1 1 calc R . . C72 C 0.8377(3) 0.1293(3) 0.41975(17) 0.0438(10) Uani 1 1 d . . . H72 H 0.8671 0.1755 0.4319 0.053 Uiso 1 1 calc R . . C73 C 0.9051(3) 0.0283(3) 0.41633(15) 0.0381(9) Uani 1 1 d . . . H73 H 0.9800 0.0052 0.4270 0.046 Uiso 1 1 calc R . . C74 C 0.8643(3) -0.0422(3) 0.39703(14) 0.0309(8) 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 O1W 0.094(4) 0.091(4) 0.106(4) 0.001(3) -0.006(3) -0.046(3) O1A 0.104(4) 0.103(4) 0.109(4) -0.001(3) 0.003(3) -0.042(3) O2W 0.060(4) 0.069(4) 0.068(5) 0.001(4) -0.011(4) -0.023(3) O2A 0.059(5) 0.068(5) 0.064(6) 0.000(4) -0.009(4) -0.021(4) O3W 0.086(4) 0.086(4) 0.088(4) -0.003(3) -0.006(3) -0.039(3) O3A 0.085(5) 0.085(5) 0.084(5) -0.003(4) -0.003(4) -0.037(4) O4W 0.119(3) 0.120(4) 0.129(4) -0.007(3) -0.020(3) -0.051(3) O4A 0.107(4) 0.108(4) 0.112(4) -0.007(3) -0.010(3) -0.041(3) O5W 0.076(2) 0.074(3) 0.079(3) 0.020(2) 0.010(2) -0.011(2) O6W 0.082(3) 0.069(3) 0.079(3) 0.001(3) -0.007(3) -0.032(2) O6A 0.093(3) 0.085(3) 0.101(3) -0.006(3) 0.003(3) -0.029(3) O7W 0.0437(16) 0.0540(19) 0.0599(19) -0.0013(15) 0.0031(13) -0.0195(14) O8W 0.075(2) 0.057(2) 0.092(2) 0.0098(18) 0.0027(18) -0.0262(17) O8A 0.083(3) 0.073(3) 0.088(3) 0.001(3) -0.002(3) -0.030(3) O9W 0.0535(18) 0.057(2) 0.0526(18) -0.0033(15) -0.0061(14) -0.0197(15) O10W 0.076(3) 0.088(4) 0.084(4) -0.005(3) 0.002(3) -0.018(3) O10A 0.080(3) 0.080(4) 0.102(4) -0.001(3) 0.006(3) -0.028(3) O11W 0.133(5) 0.087(4) 0.202(7) 0.024(4) 0.065(4) -0.001(4) O12W 0.116(4) 0.115(4) 0.108(4) 0.015(3) -0.017(3) -0.046(3) O12A 0.122(4) 0.118(4) 0.118(4) 0.018(3) -0.012(3) -0.040(3) O12B 0.132(4) 0.134(4) 0.124(4) 0.013(3) -0.012(3) -0.039(3) O13W 0.127(4) 0.157(4) 0.174(4) -0.026(3) -0.029(3) -0.068(3) O13A 0.136(5) 0.152(5) 0.161(5) -0.015(4) -0.017(4) -0.063(4) O14W 0.162(4) 0.170(5) 0.178(5) -0.004(4) -0.010(3) -0.070(3) O14A 0.159(5) 0.161(5) 0.163(5) -0.007(4) -0.014(4) -0.064(3) O15W 0.144(5) 0.096(4) 0.244(8) 0.067(5) -0.089(5) -0.054(4) O16W 0.173(5) 0.173(5) 0.208(5) 0.005(4) 0.008(4) -0.072(4) O16A 0.175(6) 0.173(6) 0.191(6) 0.002(4) -0.001(4) -0.072(4) O17W 0.149(5) 0.149(5) 0.154(5) -0.009(4) -0.018(4) -0.060(4) O17A 0.143(6) 0.146(6) 0.148(6) -0.005(4) -0.016(4) -0.060(4) C1 0.045(2) 0.028(2) 0.047(2) -0.0066(16) -0.0031(17) -0.0116(17) C2 0.049(2) 0.031(2) 0.041(2) -0.0087(16) 0.0069(17) -0.0099(18) C3 0.056(2) 0.045(2) 0.035(2) -0.0098(17) 0.0063(18) -0.027(2) C4 0.061(3) 0.044(2) 0.034(2) -0.0019(17) -0.0063(18) -0.030(2) C5 0.045(2) 0.037(2) 0.039(2) 0.0001(17) -0.0044(17) -0.0183(18) C6 0.050(2) 0.036(2) 0.035(2) -0.0040(16) 0.0006(17) -0.0236(18) C7 0.090(4) 0.073(3) 0.048(3) -0.006(2) 0.007(2) -0.054(3) C8 0.080(3) 0.064(3) 0.040(2) -0.005(2) 0.004(2) -0.038(3) C9 0.098(4) 0.067(3) 0.038(2) 0.002(2) -0.007(2) -0.045(3) C10 0.075(3) 0.055(3) 0.048(3) 0.003(2) -0.014(2) -0.030(3) C11 0.064(3) 0.072(3) 0.043(2) -0.001(2) -0.006(2) -0.040(3) C12 0.072(3) 0.051(3) 0.038(2) -0.0086(19) 0.002(2) -0.032(2) C13 0.040(2) 0.0283(19) 0.045(2) -0.0008(16) -0.0029(16) -0.0177(16) C14 0.039(2) 0.0269(19) 0.043(2) -0.0011(15) -0.0015(16) -0.0174(16) C15 0.037(2) 0.034(2) 0.047(2) -0.0012(17) 0.0024(17) -0.0198(17) C16 0.043(2) 0.046(2) 0.053(3) -0.0004(19) -0.0003(19) -0.021(2) C17 0.039(2) 0.059(3) 0.077(3) -0.003(3) -0.004(2) -0.019(2) C18 0.045(3) 0.056(3) 0.082(4) -0.014(3) 0.010(2) -0.016(2) C19 0.051(3) 0.049(3) 0.059(3) -0.013(2) 0.009(2) -0.021(2) C20 0.047(2) 0.031(2) 0.052(2) -0.0037(17) 0.0042(18) -0.0202(18) C21 0.048(2) 0.034(2) 0.045(2) -0.0031(17) -0.0010(17) -0.0238(18) C22 0.045(2) 0.033(2) 0.046(2) 0.0023(17) -0.0041(17) -0.0215(18) C23 0.054(3) 0.049(3) 0.054(3) -0.001(2) -0.011(2) -0.027(2) C24 0.041(2) 0.059(3) 0.076(3) -0.004(3) -0.014(2) -0.019(2) C25 0.039(2) 0.055(3) 0.070(3) -0.004(2) -0.004(2) -0.013(2) C26 0.042(2) 0.035(2) 0.054(3) -0.0035(18) -0.0027(18) -0.0139(18) C27 0.039(2) 0.0283(19) 0.045(2) 0.0001(16) -0.0008(16) -0.0160(16) C28 0.061(3) 0.042(2) 0.046(2) -0.0045(18) 0.0031(19) -0.029(2) C29 0.045(2) 0.030(2) 0.038(2) -0.0041(16) -0.0018(16) -0.0162(17) C30 0.043(2) 0.0266(19) 0.034(2) -0.0020(15) -0.0001(16) -0.0161(16) C31 0.047(2) 0.0301(19) 0.034(2) 0.0004(15) -0.0055(16) -0.0196(17) C32 0.048(2) 0.052(3) 0.036(2) -0.0026(18) -0.0034(17) -0.028(2) C33 0.049(2) 0.067(3) 0.045(2) -0.007(2) -0.0050(19) -0.029(2) C34 0.047(2) 0.058(3) 0.046(2) -0.007(2) 0.0052(19) -0.021(2) C35 0.056(2) 0.041(2) 0.034(2) -0.0060(17) -0.0013(18) -0.020(2) C36 0.048(2) 0.0267(19) 0.035(2) -0.0029(15) 0.0001(16) -0.0180(17) C37 0.050(2) 0.0292(19) 0.036(2) -0.0001(15) -0.0052(17) -0.0183(17) C38 0.046(2) 0.035(2) 0.043(2) -0.0010(17) -0.0066(18) -0.0170(18) C39 0.054(3) 0.062(3) 0.048(3) 0.000(2) -0.009(2) -0.023(2) C40 0.047(3) 0.090(4) 0.058(3) -0.003(3) -0.013(2) -0.018(3) C41 0.044(3) 0.067(3) 0.063(3) -0.006(2) 0.001(2) -0.015(2) C42 0.045(2) 0.043(2) 0.047(2) -0.0031(19) 0.0002(18) -0.0148(19) C43 0.045(2) 0.029(2) 0.039(2) -0.0005(16) -0.0031(17) -0.0132(17) C44 0.054(2) 0.042(2) 0.036(2) -0.0027(17) -0.0057(18) -0.023(2) C45 0.040(2) 0.030(2) 0.046(2) 0.0006(16) -0.0006(17) -0.0166(17) C46 0.0320(19) 0.033(2) 0.051(2) 0.0024(17) -0.0038(16) -0.0148(16) C47 0.035(2) 0.032(2) 0.045(2) -0.0009(16) -0.0003(16) -0.0136(16) C48 0.036(2) 0.033(2) 0.048(2) -0.0018(17) -0.0017(17) -0.0146(17) C49 0.036(2) 0.0267(19) 0.058(3) 0.0012(17) -0.0073(18) -0.0136(16) C50 0.037(2) 0.037(2) 0.069(3) -0.002(2) -0.013(2) -0.0142(18) C51 0.037(2) 0.048(3) 0.085(4) -0.006(2) -0.016(2) -0.013(2) C52 0.031(2) 0.048(3) 0.087(4) -0.012(2) -0.002(2) -0.0108(19) C53 0.035(2) 0.037(2) 0.065(3) -0.0056(19) 0.0006(19) -0.0120(18) C54 0.0316(19) 0.0277(19) 0.060(3) -0.0015(17) -0.0010(17) -0.0121(16) C55 0.047(2) 0.0258(19) 0.039(2) -0.0062(15) 0.0024(17) -0.0172(17) C56 0.042(2) 0.032(2) 0.042(2) -0.0008(16) -0.0039(17) -0.0203(17) C57 0.0348(19) 0.031(2) 0.046(2) -0.0030(16) 0.0036(16) -0.0165(16) C58 0.039(2) 0.0274(18) 0.036(2) -0.0046(15) 0.0026(15) -0.0170(16) C59 0.041(2) 0.0271(19) 0.038(2) -0.0024(15) -0.0015(16) -0.0173(16) C60 0.038(2) 0.030(2) 0.047(2) -0.0042(16) -0.0047(17) -0.0139(16) C61 0.039(2) 0.044(2) 0.060(3) -0.009(2) 0.0001(19) -0.0181(19) C62 0.038(2) 0.048(3) 0.071(3) -0.011(2) 0.014(2) -0.018(2) C63 0.048(2) 0.043(2) 0.047(2) -0.0091(18) 0.0094(19) -0.0195(19) C64 0.040(2) 0.0281(19) 0.040(2) -0.0062(15) 0.0051(16) -0.0170(16) N1 0.0333(16) 0.0262(16) 0.0436(18) -0.0045(13) 0.0009(13) -0.0113(13) N2 0.0434(18) 0.0333(17) 0.0391(18) -0.0071(13) 0.0032(14) -0.0157(14) N3 0.0427(18) 0.0385(18) 0.0345(17) -0.0039(13) 0.0007(13) -0.0220(15) N4 0.0387(17) 0.0316(17) 0.0332(16) -0.0051(13) -0.0017(13) -0.0145(14) N5 0.069(2) 0.051(2) 0.050(2) -0.0047(17) 0.0024(18) -0.035(2) N6 0.086(3) 0.069(3) 0.041(2) 0.0005(18) 0.0036(19) -0.048(2) N7 0.062(2) 0.054(2) 0.042(2) -0.0030(16) 0.0017(16) -0.0291(19) N8 0.0451(18) 0.0407(19) 0.0353(17) -0.0019(14) -0.0043(14) -0.0183(15) O1 0.0452(15) 0.0341(15) 0.0464(16) -0.0005(12) -0.0061(12) -0.0129(12) O2 0.0351(14) 0.0350(15) 0.0554(17) -0.0058(12) 0.0025(12) -0.0101(12) O3 0.0514(17) 0.0549(19) 0.0556(18) -0.0016(14) 0.0069(14) -0.0302(15) O4 0.099(3) 0.104(3) 0.060(2) 0.010(2) -0.020(2) -0.065(3) O5 0.061(2) 0.072(3) 0.089(3) -0.011(2) -0.039(2) 0.0028(19) O6 0.080(2) 0.0453(19) 0.076(2) -0.0137(17) -0.0213(19) -0.0091(17) O7 0.087(2) 0.0436(17) 0.0377(16) -0.0074(13) 0.0123(15) -0.0334(17) O8 0.0692(19) 0.0363(16) 0.0485(17) -0.0141(12) 0.0089(14) -0.0271(15) O9 0.074(2) 0.061(2) 0.0492(18) -0.0110(15) -0.0141(16) -0.0245(18) O10 0.0474(16) 0.0431(17) 0.064(2) -0.0059(14) -0.0190(14) -0.0128(14) O11 0.0451(15) 0.0367(15) 0.0452(16) -0.0092(12) -0.0034(12) -0.0115(12) O12 0.0661(19) 0.0562(19) 0.0470(17) 0.0044(14) -0.0121(14) -0.0371(16) O19 0.060(2) 0.081(3) 0.069(2) 0.0043(19) 0.0122(17) -0.0251(19) O20 0.063(2) 0.072(3) 0.091(3) -0.029(2) -0.0118(19) -0.0243(19) O21 0.0597(19) 0.072(2) 0.0523(19) -0.0116(16) 0.0101(14) -0.0354(17) O22 0.088(3) 0.053(2) 0.065(2) -0.0103(16) 0.0212(18) -0.0263(19) P1 0.0504(6) 0.0472(6) 0.0466(6) -0.0117(5) 0.0062(5) -0.0251(5) S1 0.0379(5) 0.0339(5) 0.0479(6) -0.0012(4) 0.0003(4) -0.0155(4) S2 0.0497(6) 0.0440(6) 0.0642(7) -0.0043(5) -0.0192(5) -0.0138(5) S3 0.0659(7) 0.0378(5) 0.0371(5) -0.0077(4) 0.0024(5) -0.0253(5) S4 0.0414(5) 0.0372(5) 0.0447(6) -0.0036(4) -0.0077(4) -0.0170(4) O13 0.0321(13) 0.0558(18) 0.0411(15) -0.0091(13) -0.0021(11) -0.0110(13) O14 0.0328(14) 0.0594(19) 0.0456(16) -0.0093(13) 0.0048(11) -0.0190(13) O15 0.0375(15) 0.0367(16) 0.082(2) -0.0084(15) -0.0087(14) -0.0034(13) O16 0.0317(13) 0.0282(14) 0.0541(17) -0.0042(12) 0.0035(11) -0.0049(11) O17 0.0305(14) 0.0408(17) 0.080(2) 0.0095(15) 0.0077(13) -0.0116(12) O18 0.0409(15) 0.0407(16) 0.0565(18) -0.0074(13) -0.0132(13) -0.0104(13) S5 0.0271(4) 0.0364(5) 0.0438(5) -0.0073(4) 0.0008(4) -0.0089(4) S6 0.0273(4) 0.0304(5) 0.0490(6) -0.0006(4) 0.0003(4) -0.0092(4) C65 0.0271(17) 0.0293(19) 0.0366(19) -0.0060(15) 0.0008(14) -0.0082(15) C66 0.0310(19) 0.033(2) 0.049(2) -0.0082(17) -0.0006(16) -0.0089(16) C67 0.040(2) 0.036(2) 0.047(2) -0.0098(17) -0.0031(17) -0.0167(18) C68 0.0299(18) 0.034(2) 0.042(2) -0.0037(16) -0.0052(15) -0.0128(16) C69 0.0294(18) 0.0326(19) 0.0296(18) -0.0046(14) 0.0027(14) -0.0137(15) C70 0.0277(17) 0.0316(19) 0.0322(19) -0.0061(15) 0.0034(14) -0.0086(15) C71 0.0352(19) 0.031(2) 0.043(2) -0.0099(16) 0.0043(16) -0.0123(16) C72 0.039(2) 0.036(2) 0.058(3) -0.0145(18) -0.0023(18) -0.0153(18) C73 0.0311(19) 0.040(2) 0.046(2) -0.0079(17) -0.0046(16) -0.0157(17) C74 0.0275(17) 0.0324(19) 0.0330(19) -0.0059(15) 0.0036(14) -0.0118(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.495(5) . ? C1 C2 1.514(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.495(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.501(5) . ? C3 C4 1.507(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N3 1.490(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 N3 1.506(5) . ? C5 C6 1.515(5) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N4 1.497(5) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N5 1.489(6) . ? C7 C8 1.515(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N6 1.480(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N6 1.476(6) . ? C9 C10 1.501(7) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N7 1.496(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 N7 1.490(6) . ? C11 C12 1.511(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 N8 1.502(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N1 1.510(5) . ? C13 C14 1.512(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.404(6) . ? C14 C27 1.414(5) . ? C15 C20 1.436(6) . ? C15 C16 1.440(6) . ? C16 C17 1.350(7) . ? C16 H16 0.9500 . ? C17 C18 1.406(7) . ? C17 H17 0.9500 . ? C18 C19 1.358(7) . ? C18 H18 0.9500 . ? C19 C20 1.430(6) . ? C19 H19 0.9500 . ? C20 C21 1.404(6) . ? C21 C22 1.408(6) . ? C21 C28 1.510(6) . ? C22 C23 1.429(6) . ? C22 C27 1.429(6) . ? C23 C24 1.347(7) . ? C23 H23 0.9500 . ? C24 C25 1.419(7) . ? C24 H24 0.9500 . ? C25 C26 1.359(6) . ? C25 H25 0.9500 . ? C26 C27 1.435(6) . ? C26 H26 0.9500 . ? C28 N5 1.512(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 N4 1.504(5) . ? C29 C30 1.510(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C43 1.407(5) . ? C30 C31 1.413(6) . ? C31 C32 1.421(5) . ? C31 C36 1.436(5) . ? C32 C33 1.349(6) . ? C32 H32 0.9500 . ? C33 C34 1.404(6) . ? C33 H33 0.9500 . ? C34 C35 1.354(6) . ? C34 H34 0.9500 . ? C35 C36 1.430(6) . ? C35 H35 0.9500 . ? C36 C37 1.403(5) . ? C37 C38 1.405(6) . ? C37 C44 1.516(5) . ? C38 C39 1.432(6) . ? C38 C43 1.445(6) . ? C39 C40 1.351(7) . ? C39 H39 0.9500 . ? C40 C41 1.419(7) . ? C40 H40 0.9500 . ? C41 C42 1.354(6) . ? C41 H41 0.9500 . ? C42 C43 1.437(6) . ? C42 H42 0.9500 . ? C44 N8 1.496(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.368(6) . ? C45 C54 1.414(6) . ? C45 S1 1.778(4) . ? C46 C47 1.405(6) . ? C46 H46 0.9500 . ? C47 C48 1.363(5) . ? C47 H47 0.9500 . ? C48 C49 1.427(6) . ? C48 H48 0.9500 . ? C49 C54 1.422(6) . ? C49 C50 1.438(6) . ? C50 C51 1.375(7) . ? C50 S2 1.770(5) . ? C51 C52 1.396(7) . ? C51 H51 0.9500 . ? C52 C53 1.358(6) . ? C52 H52 0.9500 . ? C53 C54 1.422(6) . ? C53 H53 0.9500 . ? C55 C56 1.365(6) . ? C55 C64 1.429(5) . ? C55 S3 1.783(4) . ? C56 C57 1.399(6) . ? C56 H56 0.9500 . ? C57 C58 1.363(5) . ? C57 H57 0.9500 . ? C58 C59 1.425(5) . ? C58 H58 0.9500 . ? C59 C64 1.427(5) . ? C59 C60 1.437(5) . ? C60 C61 1.359(6) . ? C60 S4 1.786(4) . ? C61 C62 1.405(7) . ? C61 H61 0.9500 . ? C62 C63 1.360(6) . ? C62 H62 0.9500 . ? C63 C64 1.418(6) . ? C63 H63 0.9500 . ? N1 H1C 0.9200 . ? N1 H1D 0.9200 . ? N2 H2C 0.9200 . ? N2 H2D 0.9200 . ? N3 H3C 0.9200 . ? N3 H3D 0.9200 . ? N4 H4C 0.9200 . ? N4 H4D 0.9200 . ? N5 H5C 0.9200 . ? N5 H5D 0.9200 . ? N6 H6C 0.9200 . ? N6 H6D 0.9200 . ? N7 H7C 0.9200 . ? N7 H7D 0.9200 . ? N8 H8C 0.9200 . ? N8 H8D 0.9200 . ? O1 S1 1.458(3) . ? O2 S1 1.469(3) . ? O3 S1 1.452(3) . ? O4 S2 1.433(4) . ? O5 S2 1.449(3) . ? O6 S2 1.450(4) . ? O7 S3 1.453(3) . ? O8 S3 1.472(3) . ? O9 S3 1.443(3) . ? O10 S4 1.447(3) . ? O11 S4 1.461(3) . ? O12 S4 1.458(3) . ? O19 P1 1.481(4) . ? O20 P1 1.456(4) . ? O20 H20 0.8400 . ? O21 P1 1.470(3) . ? O22 P1 1.466(4) . ? O13 S5 1.455(3) . ? O14 S5 1.446(3) . ? O15 S5 1.453(3) . ? O16 S6 1.464(3) . ? O17 S6 1.460(3) . ? O18 S6 1.438(3) . ? S5 C65 1.785(3) . ? S6 C70 1.780(3) . ? C65 C66 1.370(5) . ? C65 C74 1.435(5) . ? C66 C67 1.408(5) . ? C66 H66 0.9500 . ? C67 C68 1.360(5) . ? C67 H67 0.9500 . ? C68 C69 1.416(5) . ? C68 H68 0.9500 . ? C69 C70 1.428(5) . ? C69 C74 1.435(5) . ? C70 C71 1.366(5) . ? C71 C72 1.408(5) . ? C71 H71 0.9500 . ? C72 C73 1.370(6) . ? C72 H72 0.9500 . ? C73 C74 1.421(5) . ? C73 H73 0.9500 . ? 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 N1 C1 C2 112.2(3) . . ? N1 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? N1 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? N2 C2 C1 113.3(3) . . ? N2 C2 H2A 108.9 . . ? C1 C2 H2A 108.9 . . ? N2 C2 H2B 108.9 . . ? C1 C2 H2B 108.9 . . ? H2A C2 H2B 107.7 . . ? N2 C3 C4 113.2(3) . . ? N2 C3 H3A 108.9 . . ? C4 C3 H3A 108.9 . . ? N2 C3 H3B 108.9 . . ? C4 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? N3 C4 C3 113.8(3) . . ? N3 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? N3 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N3 C5 C6 113.9(3) . . ? N3 C5 H5A 108.8 . . ? C6 C5 H5A 108.8 . . ? N3 C5 H5B 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.7 . . ? N4 C6 C5 114.6(3) . . ? N4 C6 H6A 108.6 . . ? C5 C6 H6A 108.6 . . ? N4 C6 H6B 108.6 . . ? C5 C6 H6B 108.6 . . ? H6A C6 H6B 107.6 . . ? N5 C7 C8 112.5(4) . . ? N5 C7 H7A 109.1 . . ? C8 C7 H7A 109.1 . . ? N5 C7 H7B 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.8 . . ? N6 C8 C7 108.2(4) . . ? N6 C8 H8A 110.1 . . ? C7 C8 H8A 110.1 . . ? N6 C8 H8B 110.1 . . ? C7 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? N6 C9 C10 114.7(4) . . ? N6 C9 H9A 108.6 . . ? C10 C9 H9A 108.6 . . ? N6 C9 H9B 108.6 . . ? C10 C9 H9B 108.6 . . ? H9A C9 H9B 107.6 . . ? N7 C10 C9 113.2(4) . . ? N7 C10 H10A 108.9 . . ? C9 C10 H10A 108.9 . . ? N7 C10 H10B 108.9 . . ? C9 C10 H10B 108.9 . . ? H10A C10 H10B 107.7 . . ? N7 C11 C12 113.3(4) . . ? N7 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? N7 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? N8 C12 C11 112.7(4) . . ? N8 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? N8 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? N1 C13 C14 110.3(3) . . ? N1 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N1 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? C15 C14 C27 120.5(4) . . ? C15 C14 C13 119.4(3) . . ? C27 C14 C13 120.2(3) . . ? C14 C15 C20 119.8(3) . . ? C14 C15 C16 122.1(4) . . ? C20 C15 C16 118.2(4) . . ? C17 C16 C15 120.7(4) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 121.1(4) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 120.7(4) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 120.8(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C21 C20 C19 122.1(4) . . ? C21 C20 C15 119.5(4) . . ? C19 C20 C15 118.4(4) . . ? C20 C21 C22 120.9(4) . . ? C20 C21 C28 120.0(4) . . ? C22 C21 C28 119.1(4) . . ? C21 C22 C23 122.1(4) . . ? C21 C22 C27 119.6(3) . . ? C23 C22 C27 118.3(4) . . ? C24 C23 C22 121.5(4) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 120.5(4) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 120.3(4) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 121.0(4) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C14 C27 C22 119.7(4) . . ? C14 C27 C26 121.9(4) . . ? C22 C27 C26 118.3(3) . . ? C21 C28 N5 111.2(3) . . ? C21 C28 H28A 109.4 . . ? N5 C28 H28A 109.4 . . ? C21 C28 H28B 109.4 . . ? N5 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? N4 C29 C30 110.2(3) . . ? N4 C29 H29A 109.6 . . ? C30 C29 H29A 109.6 . . ? N4 C29 H29B 109.6 . . ? C30 C29 H29B 109.6 . . ? H29A C29 H29B 108.1 . . ? C43 C30 C31 120.3(3) . . ? C43 C30 C29 120.6(3) . . ? C31 C30 C29 119.1(3) . . ? C30 C31 C32 122.5(3) . . ? C30 C31 C36 119.9(3) . . ? C32 C31 C36 117.6(4) . . ? C33 C32 C31 121.6(4) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C32 C33 C34 121.1(4) . . ? C32 C33 H33 119.4 . . ? C34 C33 H33 119.4 . . ? C35 C34 C33 119.9(4) . . ? C35 C34 H34 120.1 . . ? C33 C34 H34 120.1 . . ? C34 C35 C36 121.3(4) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C37 C36 C35 121.9(4) . . ? C37 C36 C31 119.6(4) . . ? C35 C36 C31 118.4(3) . . ? C36 C37 C38 120.9(4) . . ? C36 C37 C44 119.0(4) . . ? C38 C37 C44 120.0(3) . . ? C37 C38 C39 122.1(4) . . ? C37 C38 C43 119.6(3) . . ? C39 C38 C43 118.4(4) . . ? C40 C39 C38 121.3(4) . . ? C40 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C39 C40 C41 120.8(4) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 120.2(4) . . ? C42 C41 H41 119.9 . . ? C40 C41 H41 119.9 . . ? C41 C42 C43 121.6(4) . . ? C41 C42 H42 119.2 . . ? C43 C42 H42 119.2 . . ? C30 C43 C42 122.7(4) . . ? C30 C43 C38 119.6(4) . . ? C42 C43 C38 117.7(4) . . ? N8 C44 C37 112.2(3) . . ? N8 C44 H44A 109.2 . . ? C37 C44 H44A 109.2 . . ? N8 C44 H44B 109.2 . . ? C37 C44 H44B 109.2 . . ? H44A C44 H44B 107.9 . . ? C46 C45 C54 121.7(4) . . ? C46 C45 S1 118.2(3) . . ? C54 C45 S1 120.1(3) . . ? C45 C46 C47 119.8(4) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C48 C47 C46 120.9(4) . . ? C48 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? C47 C48 C49 120.2(4) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C54 C49 C48 119.3(3) . . ? C54 C49 C50 118.4(4) . . ? C48 C49 C50 122.3(4) . . ? C51 C50 C49 120.3(4) . . ? C51 C50 S2 117.7(3) . . ? C49 C50 S2 122.0(3) . . ? C50 C51 C52 120.3(4) . . ? C50 C51 H51 119.9 . . ? C52 C51 H51 119.9 . . ? C53 C52 C51 121.3(4) . . ? C53 C52 H52 119.4 . . ? C51 C52 H52 119.4 . . ? C52 C53 C54 120.7(5) . . ? C52 C53 H53 119.6 . . ? C54 C53 H53 119.6 . . ? C45 C54 C53 123.1(4) . . ? C45 C54 C49 118.0(4) . . ? C53 C54 C49 118.9(4) . . ? C56 C55 C64 121.1(4) . . ? C56 C55 S3 118.0(3) . . ? C64 C55 S3 120.9(3) . . ? C55 C56 C57 120.4(4) . . ? C55 C56 H56 119.8 . . ? C57 C56 H56 119.8 . . ? C58 C57 C56 120.8(4) . . ? C58 C57 H57 119.6 . . ? C56 C57 H57 119.6 . . ? C57 C58 C59 120.7(4) . . ? C57 C58 H58 119.6 . . ? C59 C58 H58 119.6 . . ? C58 C59 C64 118.9(3) . . ? C58 C59 C60 123.1(3) . . ? C64 C59 C60 118.0(3) . . ? C61 C60 C59 120.8(4) . . ? C61 C60 S4 117.4(3) . . ? C59 C60 S4 121.8(3) . . ? C60 C61 C62 120.4(4) . . ? C60 C61 H61 119.8 . . ? C62 C61 H61 119.8 . . ? C63 C62 C61 121.0(4) . . ? C63 C62 H62 119.5 . . ? C61 C62 H62 119.5 . . ? C62 C63 C64 120.6(4) . . ? C62 C63 H63 119.7 . . ? C64 C63 H63 119.7 . . ? C63 C64 C59 119.1(4) . . ? C63 C64 C55 122.8(4) . . ? C59 C64 C55 118.1(3) . . ? C1 N1 C13 112.2(3) . . ? C1 N1 H1C 109.2 . . ? C13 N1 H1C 109.2 . . ? C1 N1 H1D 109.2 . . ? C13 N1 H1D 109.2 . . ? H1C N1 H1D 107.9 . . ? C2 N2 C3 111.6(3) . . ? C2 N2 H2C 109.3 . . ? C3 N2 H2C 109.3 . . ? C2 N2 H2D 109.3 . . ? C3 N2 H2D 109.3 . . ? H2C N2 H2D 108.0 . . ? C4 N3 C5 112.9(3) . . ? C4 N3 H3C 109.0 . . ? C5 N3 H3C 109.0 . . ? C4 N3 H3D 109.0 . . ? C5 N3 H3D 109.0 . . ? H3C N3 H3D 107.8 . . ? C6 N4 C29 116.8(3) . . ? C6 N4 H4C 108.1 . . ? C29 N4 H4C 108.1 . . ? C6 N4 H4D 108.1 . . ? C29 N4 H4D 108.1 . . ? H4C N4 H4D 107.3 . . ? C7 N5 C28 113.2(4) . . ? C7 N5 H5C 108.9 . . ? C28 N5 H5C 108.9 . . ? C7 N5 H5D 108.9 . . ? C28 N5 H5D 108.9 . . ? H5C N5 H5D 107.8 . . ? C9 N6 C8 115.6(4) . . ? C9 N6 H6C 108.4 . . ? C8 N6 H6C 108.4 . . ? C9 N6 H6D 108.4 . . ? C8 N6 H6D 108.4 . . ? H6C N6 H6D 107.4 . . ? C11 N7 C10 111.2(4) . . ? C11 N7 H7C 109.4 . . ? C10 N7 H7C 109.4 . . ? C11 N7 H7D 109.4 . . ? C10 N7 H7D 109.4 . . ? H7C N7 H7D 108.0 . . ? C44 N8 C12 111.0(3) . . ? C44 N8 H8C 109.4 . . ? C12 N8 H8C 109.4 . . ? C44 N8 H8D 109.4 . . ? C12 N8 H8D 109.4 . . ? H8C N8 H8D 108.0 . . ? P1 O20 H20 109.5 . . ? O20 P1 O22 111.9(2) . . ? O20 P1 O21 107.9(2) . . ? O22 P1 O21 110.4(2) . . ? O20 P1 O19 109.8(3) . . ? O22 P1 O19 108.6(2) . . ? O21 P1 O19 108.1(2) . . ? O3 S1 O1 112.41(18) . . ? O3 S1 O2 112.42(17) . . ? O1 S1 O2 111.00(16) . . ? O3 S1 C45 106.82(18) . . ? O1 S1 C45 106.47(17) . . ? O2 S1 C45 107.31(17) . . ? O4 S2 O5 112.5(3) . . ? O4 S2 O6 113.6(3) . . ? O5 S2 O6 110.1(2) . . ? O4 S2 C50 106.9(2) . . ? O5 S2 C50 106.2(2) . . ? O6 S2 C50 107.1(2) . . ? O9 S3 O7 113.0(2) . . ? O9 S3 O8 112.18(19) . . ? O7 S3 O8 111.49(19) . . ? O9 S3 C55 106.52(19) . . ? O7 S3 C55 106.95(18) . . ? O8 S3 C55 106.20(17) . . ? O10 S4 O12 112.19(18) . . ? O10 S4 O11 111.54(17) . . ? O12 S4 O11 111.64(18) . . ? O10 S4 C60 106.66(19) . . ? O12 S4 C60 107.64(18) . . ? O11 S4 C60 106.81(17) . . ? O14 S5 O15 112.92(19) . . ? O14 S5 O13 111.87(17) . . ? O15 S5 O13 112.45(19) . . ? O14 S5 C65 105.75(17) . . ? O15 S5 C65 105.78(17) . . ? O13 S5 C65 107.50(16) . . ? O18 S6 O17 112.96(19) . . ? O18 S6 O16 113.82(17) . . ? O17 S6 O16 111.46(17) . . ? O18 S6 C70 107.38(16) . . ? O17 S6 C70 104.79(17) . . ? O16 S6 C70 105.65(16) . . ? C66 C65 C74 121.2(3) . . ? C66 C65 S5 117.0(3) . . ? C74 C65 S5 121.8(3) . . ? C65 C66 C67 120.2(4) . . ? C65 C66 H66 119.9 . . ? C67 C66 H66 119.9 . . ? C68 C67 C66 120.4(4) . . ? C68 C67 H67 119.8 . . ? C66 C67 H67 119.8 . . ? C67 C68 C69 121.7(3) . . ? C67 C68 H68 119.2 . . ? C69 C68 H68 119.2 . . ? C68 C69 C70 122.9(3) . . ? C68 C69 C74 118.7(3) . . ? C70 C69 C74 118.3(3) . . ? C71 C70 C69 121.4(3) . . ? C71 C70 S6 118.3(3) . . ? C69 C70 S6 120.2(3) . . ? C70 C71 C72 119.8(3) . . ? C70 C71 H71 120.1 . . ? C72 C71 H71 120.1 . . ? C73 C72 C71 121.1(4) . . ? C73 C72 H72 119.5 . . ? C71 C72 H72 119.5 . . ? C72 C73 C74 120.8(3) . . ? C72 C73 H73 119.6 . . ? C74 C73 H73 119.6 . . ? C73 C74 C65 123.6(3) . . ? C73 C74 C69 118.6(3) . . ? C65 C74 C69 117.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 N2 67.2(4) . . . . ? N2 C3 C4 N3 -81.7(4) . . . . ? N3 C5 C6 N4 86.5(4) . . . . ? N5 C7 C8 N6 -167.8(4) . . . . ? N6 C9 C10 N7 -64.6(6) . . . . ? N7 C11 C12 N8 76.2(5) . . . . ? N1 C13 C14 C15 -90.3(4) . . . . ? N1 C13 C14 C27 89.1(4) . . . . ? C27 C14 C15 C20 0.4(6) . . . . ? C13 C14 C15 C20 179.9(3) . . . . ? C27 C14 C15 C16 -178.8(4) . . . . ? C13 C14 C15 C16 0.6(6) . . . . ? C14 C15 C16 C17 179.1(4) . . . . ? C20 C15 C16 C17 -0.1(6) . . . . ? C15 C16 C17 C18 2.5(7) . . . . ? C16 C17 C18 C19 -2.6(8) . . . . ? C17 C18 C19 C20 0.2(8) . . . . ? C18 C19 C20 C21 -177.6(4) . . . . ? C18 C19 C20 C15 2.0(7) . . . . ? C14 C15 C20 C21 -1.7(6) . . . . ? C16 C15 C20 C21 177.5(4) . . . . ? C14 C15 C20 C19 178.6(4) . . . . ? C16 C15 C20 C19 -2.1(6) . . . . ? C19 C20 C21 C22 -177.9(4) . . . . ? C15 C20 C21 C22 2.5(6) . . . . ? C19 C20 C21 C28 4.4(6) . . . . ? C15 C20 C21 C28 -175.3(4) . . . . ? C20 C21 C22 C23 177.8(4) . . . . ? C28 C21 C22 C23 -4.4(6) . . . . ? C20 C21 C22 C27 -1.9(6) . . . . ? C28 C21 C22 C27 175.8(3) . . . . ? C21 C22 C23 C24 179.9(4) . . . . ? C27 C22 C23 C24 -0.3(6) . . . . ? C22 C23 C24 C25 -0.8(7) . . . . ? C23 C24 C25 C26 0.4(8) . . . . ? C24 C25 C26 C27 1.0(7) . . . . ? C15 C14 C27 C22 0.1(5) . . . . ? C13 C14 C27 C22 -179.3(3) . . . . ? C15 C14 C27 C26 179.2(4) . . . . ? C13 C14 C27 C26 -0.2(5) . . . . ? C21 C22 C27 C14 0.6(5) . . . . ? C23 C22 C27 C14 -179.2(4) . . . . ? C21 C22 C27 C26 -178.5(4) . . . . ? C23 C22 C27 C26 1.7(5) . . . . ? C25 C26 C27 C14 178.8(4) . . . . ? C25 C26 C27 C22 -2.1(6) . . . . ? C20 C21 C28 N5 -90.1(5) . . . . ? C22 C21 C28 N5 92.1(5) . . . . ? N4 C29 C30 C43 98.6(4) . . . . ? N4 C29 C30 C31 -82.4(4) . . . . ? C43 C30 C31 C32 176.7(4) . . . . ? C29 C30 C31 C32 -2.3(5) . . . . ? C43 C30 C31 C36 -2.7(5) . . . . ? C29 C30 C31 C36 178.3(3) . . . . ? C30 C31 C32 C33 -177.6(4) . . . . ? C36 C31 C32 C33 1.8(6) . . . . ? C31 C32 C33 C34 -0.6(7) . . . . ? C32 C33 C34 C35 -0.4(7) . . . . ? C33 C34 C35 C36 0.2(7) . . . . ? C34 C35 C36 C37 179.3(4) . . . . ? C34 C35 C36 C31 1.1(6) . . . . ? C30 C31 C36 C37 -0.9(5) . . . . ? C32 C31 C36 C37 179.7(3) . . . . ? C30 C31 C36 C35 177.4(3) . . . . ? C32 C31 C36 C35 -2.0(5) . . . . ? C35 C36 C37 C38 -174.3(4) . . . . ? C31 C36 C37 C38 3.9(6) . . . . ? C35 C36 C37 C44 8.0(6) . . . . ? C31 C36 C37 C44 -173.8(3) . . . . ? C36 C37 C38 C39 175.1(4) . . . . ? C44 C37 C38 C39 -7.2(6) . . . . ? C36 C37 C38 C43 -3.3(6) . . . . ? C44 C37 C38 C43 174.4(4) . . . . ? C37 C38 C39 C40 -178.8(5) . . . . ? C43 C38 C39 C40 -0.3(7) . . . . ? C38 C39 C40 C41 -1.2(9) . . . . ? C39 C40 C41 C42 1.1(9) . . . . ? C40 C41 C42 C43 0.4(8) . . . . ? C31 C30 C43 C42 -177.4(4) . . . . ? C29 C30 C43 C42 1.7(6) . . . . ? C31 C30 C43 C38 3.2(6) . . . . ? C29 C30 C43 C38 -177.8(3) . . . . ? C41 C42 C43 C30 178.7(4) . . . . ? C41 C42 C43 C38 -1.9(6) . . . . ? C37 C38 C43 C30 -0.2(6) . . . . ? C39 C38 C43 C30 -178.7(4) . . . . ? C37 C38 C43 C42 -179.7(4) . . . . ? C39 C38 C43 C42 1.8(6) . . . . ? C36 C37 C44 N8 -89.9(4) . . . . ? C38 C37 C44 N8 92.3(4) . . . . ? C54 C45 C46 C47 -1.6(6) . . . . ? S1 C45 C46 C47 178.0(3) . . . . ? C45 C46 C47 C48 0.8(6) . . . . ? C46 C47 C48 C49 0.4(6) . . . . ? C47 C48 C49 C54 -0.8(6) . . . . ? C47 C48 C49 C50 178.2(4) . . . . ? C54 C49 C50 C51 -2.2(6) . . . . ? C48 C49 C50 C51 178.7(4) . . . . ? C54 C49 C50 S2 176.1(3) . . . . ? C48 C49 C50 S2 -3.0(6) . . . . ? C49 C50 C51 C52 1.3(7) . . . . ? S2 C50 C51 C52 -177.0(4) . . . . ? C50 C51 C52 C53 0.6(7) . . . . ? C51 C52 C53 C54 -1.6(7) . . . . ? C46 C45 C54 C53 -179.1(4) . . . . ? S1 C45 C54 C53 1.3(5) . . . . ? C46 C45 C54 C49 1.2(6) . . . . ? S1 C45 C54 C49 -178.5(3) . . . . ? C52 C53 C54 C45 -179.1(4) . . . . ? C52 C53 C54 C49 0.6(6) . . . . ? C48 C49 C54 C45 0.1(5) . . . . ? C50 C49 C54 C45 -179.0(3) . . . . ? C48 C49 C54 C53 -179.7(4) . . . . ? C50 C49 C54 C53 1.2(6) . . . . ? C64 C55 C56 C57 -0.1(6) . . . . ? S3 C55 C56 C57 179.9(3) . . . . ? C55 C56 C57 C58 -1.9(6) . . . . ? C56 C57 C58 C59 1.7(6) . . . . ? C57 C58 C59 C64 0.4(5) . . . . ? C57 C58 C59 C60 179.3(3) . . . . ? C58 C59 C60 C61 -176.0(4) . . . . ? C64 C59 C60 C61 2.9(6) . . . . ? C58 C59 C60 S4 3.8(5) . . . . ? C64 C59 C60 S4 -177.3(3) . . . . ? C59 C60 C61 C62 -0.7(6) . . . . ? S4 C60 C61 C62 179.6(3) . . . . ? C60 C61 C62 C63 -2.5(7) . . . . ? C61 C62 C63 C64 3.3(7) . . . . ? C62 C63 C64 C59 -0.9(6) . . . . ? C62 C63 C64 C55 178.1(4) . . . . ? C58 C59 C64 C63 176.8(3) . . . . ? C60 C59 C64 C63 -2.1(5) . . . . ? C58 C59 C64 C55 -2.2(5) . . . . ? C60 C59 C64 C55 178.8(3) . . . . ? C56 C55 C64 C63 -176.9(4) . . . . ? S3 C55 C64 C63 3.1(5) . . . . ? C56 C55 C64 C59 2.1(5) . . . . ? S3 C55 C64 C59 -177.9(3) . . . . ? C2 C1 N1 C13 163.9(3) . . . . ? C14 C13 N1 C1 176.5(3) . . . . ? C1 C2 N2 C3 -178.4(3) . . . . ? C4 C3 N2 C2 168.9(3) . . . . ? C3 C4 N3 C5 -176.3(3) . . . . ? C6 C5 N3 C4 153.1(3) . . . . ? C5 C6 N4 C29 -59.8(4) . . . . ? C30 C29 N4 C6 -168.4(3) . . . . ? C8 C7 N5 C28 63.6(6) . . . . ? C21 C28 N5 C7 156.8(4) . . . . ? C10 C9 N6 C8 -55.8(6) . . . . ? C7 C8 N6 C9 -165.2(4) . . . . ? C12 C11 N7 C10 -161.7(4) . . . . ? C9 C10 N7 C11 -163.0(4) . . . . ? C37 C44 N8 C12 171.9(3) . . . . ? C11 C12 N8 C44 158.9(4) . . . . ? C46 C45 S1 O3 -128.7(3) . . . . ? C54 C45 S1 O3 50.9(4) . . . . ? C46 C45 S1 O1 -8.4(4) . . . . ? C54 C45 S1 O1 171.3(3) . . . . ? C46 C45 S1 O2 110.5(3) . . . . ? C54 C45 S1 O2 -69.8(3) . . . . ? C51 C50 S2 O4 122.6(4) . . . . ? C49 C50 S2 O4 -55.7(4) . . . . ? C51 C50 S2 O5 2.3(4) . . . . ? C49 C50 S2 O5 -175.9(4) . . . . ? C51 C50 S2 O6 -115.2(4) . . . . ? C49 C50 S2 O6 66.5(4) . . . . ? C56 C55 S3 O9 2.2(4) . . . . ? C64 C55 S3 O9 -177.9(3) . . . . ? C56 C55 S3 O7 123.2(3) . . . . ? C64 C55 S3 O7 -56.8(3) . . . . ? C56 C55 S3 O8 -117.6(3) . . . . ? C64 C55 S3 O8 62.4(3) . . . . ? C61 C60 S4 O10 -8.3(4) . . . . ? C59 C60 S4 O10 171.9(3) . . . . ? C61 C60 S4 O12 -128.9(3) . . . . ? C59 C60 S4 O12 51.3(4) . . . . ? C61 C60 S4 O11 111.1(3) . . . . ? C59 C60 S4 O11 -68.7(3) . . . . ? O14 S5 C65 C66 110.5(3) . . . . ? O15 S5 C65 C66 -9.5(4) . . . . ? O13 S5 C65 C66 -129.9(3) . . . . ? O14 S5 C65 C74 -68.2(3) . . . . ? O15 S5 C65 C74 171.8(3) . . . . ? O13 S5 C65 C74 51.5(3) . . . . ? C74 C65 C66 C67 1.4(6) . . . . ? S5 C65 C66 C67 -177.2(3) . . . . ? C65 C66 C67 C68 -1.0(6) . . . . ? C66 C67 C68 C69 0.3(6) . . . . ? C67 C68 C69 C70 -177.9(4) . . . . ? C67 C68 C69 C74 0.1(6) . . . . ? C68 C69 C70 C71 -179.6(4) . . . . ? C74 C69 C70 C71 2.4(5) . . . . ? C68 C69 C70 S6 2.8(5) . . . . ? C74 C69 C70 S6 -175.2(3) . . . . ? O18 S6 C70 C71 121.4(3) . . . . ? O17 S6 C70 C71 -118.3(3) . . . . ? O16 S6 C70 C71 -0.4(3) . . . . ? O18 S6 C70 C69 -60.9(3) . . . . ? O17 S6 C70 C69 59.4(3) . . . . ? O16 S6 C70 C69 177.2(3) . . . . ? C69 C70 C71 C72 -1.4(6) . . . . ? S6 C70 C71 C72 176.2(3) . . . . ? C70 C71 C72 C73 -0.6(6) . . . . ? C71 C72 C73 C74 1.7(6) . . . . ? C72 C73 C74 C65 179.7(4) . . . . ? C72 C73 C74 C69 -0.6(6) . . . . ? C66 C65 C74 C73 178.6(4) . . . . ? S5 C65 C74 C73 -2.8(5) . . . . ? C66 C65 C74 C69 -1.1(5) . . . . ? S5 C65 C74 C69 177.5(3) . . . . ? C68 C69 C74 C73 -179.4(3) . . . . ? C70 C69 C74 C73 -1.4(5) . . . . ? C68 C69 C74 C65 0.3(5) . . . . ? C70 C69 C74 C65 178.4(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1C O2 0.92 1.93 2.840(4) 171.8 . N1 H1D O16 0.92 1.92 2.791(4) 156.6 . N2 H2C O9W 0.92 1.88 2.783(4) 165.2 2_666 N2 H2D O1 0.92 2.07 2.859(4) 143.4 . N2 H2D O16 0.92 2.29 2.880(4) 121.1 . N3 H3C O1 0.92 2.11 2.885(4) 140.7 . N3 H3C O17 0.92 2.20 2.793(4) 121.7 . N3 H3D O7W 0.92 1.75 2.662(4) 171.5 . N4 H4C O14 0.92 1.84 2.735(4) 163.4 1_455 N4 H4D O11 0.92 1.87 2.758(4) 160.3 1_545 N5 H5D O8 0.92 1.86 2.777(5) 172.3 . N6 H6C O7 0.92 1.97 2.746(5) 141.0 2_665 N6 H6C O5W 0.92 2.45 2.993(6) 117.8 2_665 N6 H6D O19 0.92 1.79 2.700(6) 168.4 . N7 H7C O22 0.92 1.75 2.668(5) 173.1 2_655 N7 H7D O21 0.92 1.84 2.748(5) 169.1 . N8 H8C O21 0.92 1.90 2.739(5) 150.7 . N8 H8D O6 0.92 1.82 2.721(5) 165.6 . _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 65.43 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.882 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.082 # start Validation Reply Form _vrf_PLAT306_1 ; PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) ....... O5W RESPONSE: The hydrogen atoms of disordered water molecules could not be located and were not included in the refinement. ; _vrf_PLAT430_1 ; PROBLEM: Short Inter D...A Contact O1W .. O2W .. 1.77 Ang. RESPONSE: The water molecules are disordered. ; # end Validation Reply Form # Attachment '2.cif' data_2 #TrackingRef '- complexes 1 and 2.cif' _database_code_depnum_ccdc_archive 'CCDC 874374' #TrackingRef '2.cif' _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C40 H52 N6), 3(C10 H6 O6 S2), 6(H2 O)' _chemical_formula_sum 'C70 H82 N6 O24 S6' _chemical_formula_weight 1583.78 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3839(7) _cell_length_b 22.0863(13) _cell_length_c 11.7496(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.793(4) _cell_angle_gamma 90.00 _cell_volume 3455.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4325 _cell_measurement_theta_max 65.4433 _cell_measurement_theta_min 3.3160 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1664 _exptl_absorpt_coefficient_mu 2.576 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4836 _exptl_absorpt_correction_T_max 0.5540 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type 'Cu K\a' _diffrn_source 'Enhance Ultra (Cu) X-ray Source' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'multiwire proportional' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 10.5058 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 13429 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0521 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 65.51 _reflns_number_total 5792 _reflns_number_gt 4619 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET) (compiled Oct 27 2011,15:02:11) ; _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1088P)^2^+2.1075P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5792 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0751 _refine_ls_R_factor_gt 0.0616 _refine_ls_wR_factor_ref 0.1810 _refine_ls_wR_factor_gt 0.1648 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 O1W O 0.6474(4) 0.2971(2) 0.3599(5) 0.1186(17) Uani 1 1 d . . . H1E H 0.6925 0.2857 0.3178 0.178 Uiso 1 1 d R . . H1F H 0.6884 0.3234 0.3902 0.178 Uiso 1 1 d R . . O2W O 0.4996(4) 0.3326(2) 0.4816(5) 0.131(2) Uani 1 1 d . . . H2E H 0.4876 0.3070 0.5328 0.197 Uiso 1 1 d R . . H2F H 0.5615 0.3422 0.4906 0.197 Uiso 1 1 d R . . O3W O 0.5265(3) 0.2532(2) 0.1479(4) 0.1011(15) Uani 1 1 d . . . H3E H 0.4878 0.2409 0.2001 0.152 Uiso 1 1 d R . . H3F H 0.5830 0.2584 0.1758 0.152 Uiso 1 1 d R . . C1 C 0.2000(2) 0.10964(15) 0.5312(3) 0.0307(7) Uani 1 1 d . . . H1A H 0.1886 0.0763 0.5847 0.037 Uiso 1 1 calc R . . H1B H 0.2081 0.0917 0.4554 0.037 Uiso 1 1 calc R . . C2 C 0.1109(2) 0.15224(15) 0.5215(3) 0.0302(7) Uani 1 1 d . . . H2A H 0.1080 0.1740 0.5948 0.036 Uiso 1 1 calc R . . H2B H 0.1186 0.1826 0.4610 0.036 Uiso 1 1 calc R . . C3 C -0.0677(2) 0.15681(16) 0.4423(3) 0.0309(7) Uani 1 1 d . . . H3A H -0.0652 0.1595 0.3585 0.037 Uiso 1 1 calc R . . H3B H -0.0597 0.1982 0.4744 0.037 Uiso 1 1 calc R . . C4 C -0.1683(2) 0.13128(15) 0.4672(3) 0.0275(7) Uani 1 1 d . . . H4A H -0.1740 0.0886 0.4420 0.033 Uiso 1 1 calc R . . H4B H -0.1741 0.1327 0.5505 0.033 Uiso 1 1 calc R . . C5 C -0.3558(2) 0.15144(15) 0.4294(3) 0.0302(7) Uani 1 1 d . . . H5A H -0.3693 0.1691 0.5038 0.036 Uiso 1 1 calc R . . H5B H -0.4047 0.1689 0.3695 0.036 Uiso 1 1 calc R . . C6 C 0.3913(2) 0.11251(15) 0.5580(3) 0.0292(7) Uani 1 1 d . . . H6A H 0.4425 0.1259 0.6196 0.035 Uiso 1 1 calc R . . H6B H 0.4139 0.1253 0.4841 0.035 Uiso 1 1 calc R . . C7 C 0.3842(2) 0.04425(14) 0.5603(3) 0.0257(7) Uani 1 1 d . . . C8 C 0.3894(2) 0.01411(15) 0.6668(3) 0.0271(7) Uani 1 1 d . . . C9 C 0.3993(2) 0.04650(16) 0.7728(3) 0.0314(7) Uani 1 1 d . . . H9 H 0.4003 0.0895 0.7719 0.038 Uiso 1 1 calc R . . C10 C 0.4074(3) 0.01687(18) 0.8748(3) 0.0358(8) Uani 1 1 d . . . H10 H 0.4127 0.0393 0.9441 0.043 Uiso 1 1 calc R . . C11 C 0.4080(2) -0.04721(17) 0.8784(3) 0.0330(7) Uani 1 1 d . . . H11 H 0.4170 -0.0676 0.9500 0.040 Uiso 1 1 calc R . . C12 C 0.3958(2) -0.07982(16) 0.7792(3) 0.0318(7) Uani 1 1 d . . . H12 H 0.3950 -0.1228 0.7830 0.038 Uiso 1 1 calc R . . C13 C 0.3840(2) -0.05099(15) 0.6699(3) 0.0268(7) Uani 1 1 d . . . C14 C 0.3702(2) -0.08361(14) 0.5670(3) 0.0263(7) Uani 1 1 d . . . C15 C 0.3651(2) -0.05376(15) 0.4605(3) 0.0262(7) Uani 1 1 d . . . C16 C 0.3530(2) -0.08564(16) 0.3532(3) 0.0306(7) Uani 1 1 d . . . H16 H 0.3470 -0.1285 0.3534 0.037 Uiso 1 1 calc R . . C17 C 0.3498(2) -0.05630(17) 0.2523(3) 0.0342(8) Uani 1 1 d . . . H17 H 0.3435 -0.0788 0.1830 0.041 Uiso 1 1 calc R . . C18 C 0.3559(3) 0.00712(17) 0.2486(3) 0.0346(8) Uani 1 1 d . . . H18 H 0.3520 0.0273 0.1769 0.041 Uiso 1 1 calc R . . C19 C 0.3674(2) 0.04003(16) 0.3474(3) 0.0316(7) Uani 1 1 d . . . H19 H 0.3720 0.0829 0.3433 0.038 Uiso 1 1 calc R . . C20 C 0.3727(2) 0.01137(14) 0.4568(3) 0.0258(7) Uani 1 1 d . . . C21 C 0.2056(3) 0.21529(16) 0.2468(3) 0.0385(8) Uani 1 1 d . . . C22 C 0.2142(3) 0.16610(17) 0.1791(3) 0.0417(9) Uani 1 1 d . . . H22 H 0.2782 0.1484 0.1734 0.050 Uiso 1 1 calc R . . C23 C 0.1281(3) 0.14151(18) 0.1175(3) 0.0418(9) Uani 1 1 d . . . H23 H 0.1341 0.1066 0.0713 0.050 Uiso 1 1 calc R . . C24 C 0.0361(3) 0.16719(16) 0.1233(3) 0.0381(8) Uani 1 1 d . . . H24 H -0.0213 0.1497 0.0818 0.046 Uiso 1 1 calc R . . C25 C 0.0249(3) 0.22007(16) 0.1908(3) 0.0355(8) Uani 1 1 d . . . C26 C -0.0685(3) 0.25030(16) 0.1980(3) 0.0373(8) Uani 1 1 d . . . C27 C -0.0753(3) 0.30094(18) 0.2632(3) 0.0434(9) Uani 1 1 d . . . H27 H -0.1382 0.3206 0.2654 0.052 Uiso 1 1 calc R . . C28 C 0.0107(3) 0.32392(18) 0.3272(3) 0.0445(9) Uani 1 1 d . . . H28 H 0.0054 0.3590 0.3730 0.053 Uiso 1 1 calc R . . C29 C 0.1007(3) 0.29695(17) 0.3244(3) 0.0427(9) Uani 1 1 d . . . H29 H 0.1576 0.3130 0.3692 0.051 Uiso 1 1 calc R . . C30 C 0.1121(3) 0.24471(16) 0.2556(3) 0.0363(8) Uani 1 1 d . . . N1 N 0.29295(19) 0.14345(12) 0.5735(2) 0.0281(6) Uani 1 1 d . . . H1C H 0.2909 0.1511 0.6502 0.034 Uiso 1 1 calc R . . H1D H 0.2920 0.1802 0.5366 0.034 Uiso 1 1 calc R . . N2 N 0.01623(18) 0.11757(12) 0.4933(2) 0.0254(6) Uani 1 1 d . . . H2C H -0.0023 0.0998 0.5588 0.030 Uiso 1 1 calc R . . H2D H 0.0275 0.0872 0.4425 0.030 Uiso 1 1 calc R . . N3 N -0.25055(18) 0.16825(12) 0.4047(2) 0.0278(6) Uani 1 1 d . . . H3C H -0.2464 0.1643 0.3273 0.033 Uiso 1 1 calc R . . H3D H -0.2398 0.2083 0.4232 0.033 Uiso 1 1 calc R . . O1 O 0.2950(2) 0.24410(12) 0.4465(2) 0.0474(7) Uani 1 1 d . . . O2 O 0.3965(2) 0.20158(14) 0.3071(2) 0.0518(7) Uani 1 1 d . . . O3 O 0.3332(2) 0.30460(13) 0.2871(2) 0.0529(8) Uani 1 1 d . . . O4 O -0.19930(18) 0.16352(11) 0.1804(2) 0.0377(6) Uani 1 1 d . . . O5 O -0.2584(2) 0.26578(14) 0.1432(3) 0.0601(8) Uani 1 1 d . . . O6 O -0.1675(2) 0.21496(14) 0.0052(2) 0.0518(7) Uani 1 1 d . . . S1 S 0.31709(7) 0.24324(4) 0.32755(8) 0.0434(3) Uani 1 1 d . . . S2 S -0.18284(7) 0.22110(4) 0.12520(8) 0.0403(3) Uani 1 1 d . . . C31 C -0.0455(2) 0.00542(14) 0.1457(3) 0.0261(7) Uani 1 1 d . . . C32 C -0.1417(2) 0.02605(16) 0.1189(3) 0.0324(7) Uani 1 1 d . . . H32 H -0.1841 0.0328 0.1778 0.039 Uiso 1 1 calc R . . C33 C -0.1773(3) 0.03719(18) 0.0041(3) 0.0377(8) Uani 1 1 d . . . H33 H -0.2436 0.0521 -0.0135 0.045 Uiso 1 1 calc R . . C34 C -0.1189(2) 0.02706(17) -0.0823(3) 0.0323(7) Uani 1 1 d . . . H34 H -0.1453 0.0343 -0.1592 0.039 Uiso 1 1 calc R . . C35 C 0.0190(2) -0.00568(14) 0.0585(3) 0.0252(6) Uani 1 1 d . . . S3 S -0.00333(6) -0.00235(3) 0.29404(6) 0.0274(2) Uani 1 1 d . . . O7 O -0.08973(18) 0.00708(11) 0.35650(19) 0.0349(6) Uani 1 1 d . . . O8 O 0.03798(18) -0.06330(11) 0.31099(18) 0.0349(5) Uani 1 1 d . . . O9 O 0.07268(18) 0.04438(11) 0.31897(18) 0.0343(5) 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 O1W 0.130(4) 0.098(4) 0.122(4) 0.032(3) -0.016(3) -0.017(3) O2W 0.150(5) 0.085(4) 0.147(5) -0.017(3) -0.044(4) -0.031(3) O3W 0.069(2) 0.110(4) 0.124(4) 0.030(3) 0.007(2) -0.009(2) C1 0.0283(16) 0.0227(17) 0.0400(18) -0.0011(14) -0.0022(13) 0.0000(13) C2 0.0298(16) 0.0254(17) 0.0342(17) -0.0002(14) -0.0024(13) 0.0001(13) C3 0.0303(17) 0.0271(17) 0.0345(17) 0.0043(14) -0.0006(13) 0.0025(14) C4 0.0271(15) 0.0229(16) 0.0322(16) 0.0032(13) 0.0014(12) 0.0002(13) C5 0.0313(16) 0.0199(16) 0.0387(18) -0.0006(14) 0.0000(13) 0.0012(13) C6 0.0285(16) 0.0218(17) 0.0365(17) 0.0002(13) -0.0007(13) -0.0001(13) C7 0.0215(14) 0.0211(16) 0.0333(17) 0.0003(13) -0.0039(12) -0.0003(12) C8 0.0240(15) 0.0239(17) 0.0324(17) -0.0022(13) -0.0020(12) 0.0001(12) C9 0.0316(16) 0.0260(17) 0.0349(18) -0.0035(14) -0.0048(13) -0.0011(14) C10 0.0367(18) 0.039(2) 0.0304(17) -0.0051(15) -0.0023(13) -0.0003(15) C11 0.0348(17) 0.036(2) 0.0273(16) 0.0039(14) 0.0000(13) 0.0020(15) C12 0.0285(16) 0.0293(18) 0.0366(18) 0.0046(14) -0.0012(13) -0.0016(14) C13 0.0223(14) 0.0239(16) 0.0331(17) 0.0018(13) -0.0022(12) 0.0001(12) C14 0.0227(14) 0.0223(17) 0.0330(17) 0.0011(13) -0.0022(12) 0.0013(12) C15 0.0228(15) 0.0234(16) 0.0315(16) -0.0024(13) -0.0019(12) -0.0001(12) C16 0.0295(16) 0.0263(18) 0.0347(17) -0.0044(14) -0.0025(13) -0.0014(13) C17 0.0330(17) 0.038(2) 0.0302(17) -0.0047(15) -0.0025(13) 0.0001(15) C18 0.0333(17) 0.040(2) 0.0293(17) 0.0022(15) -0.0029(13) 0.0002(15) C19 0.0287(16) 0.0298(18) 0.0353(18) 0.0048(14) -0.0015(13) 0.0003(14) C20 0.0214(15) 0.0228(16) 0.0324(17) 0.0016(13) -0.0014(12) 0.0011(12) C21 0.051(2) 0.0269(18) 0.0361(18) 0.0101(15) -0.0046(15) -0.0087(16) C22 0.050(2) 0.030(2) 0.044(2) 0.0067(16) -0.0005(16) 0.0004(16) C23 0.053(2) 0.0285(19) 0.043(2) 0.0007(16) 0.0011(16) -0.0051(17) C24 0.049(2) 0.0281(19) 0.0360(18) 0.0046(15) -0.0025(15) -0.0096(16) C25 0.051(2) 0.0243(18) 0.0303(17) 0.0095(14) -0.0008(15) -0.0044(15) C26 0.050(2) 0.0266(18) 0.0347(19) 0.0096(14) 0.0020(15) -0.0016(16) C27 0.057(2) 0.034(2) 0.039(2) 0.0073(16) -0.0013(16) 0.0030(17) C28 0.069(3) 0.028(2) 0.0350(19) 0.0032(15) -0.0029(17) 0.0032(18) C29 0.063(2) 0.030(2) 0.0328(18) 0.0041(15) -0.0080(16) -0.0045(18) C30 0.051(2) 0.0251(18) 0.0310(18) 0.0094(14) -0.0050(15) -0.0051(15) N1 0.0312(14) 0.0194(13) 0.0323(14) -0.0025(11) -0.0040(10) 0.0010(11) N2 0.0297(13) 0.0215(14) 0.0244(13) 0.0012(10) 0.0006(10) 0.0006(11) N3 0.0294(14) 0.0185(13) 0.0351(14) 0.0021(11) 0.0006(11) -0.0015(11) O1 0.0642(17) 0.0347(15) 0.0391(14) 0.0086(11) -0.0144(12) -0.0083(13) O2 0.0495(15) 0.0464(17) 0.0578(17) 0.0085(14) -0.0036(12) -0.0018(13) O3 0.0640(17) 0.0380(16) 0.0521(16) 0.0188(13) -0.0169(13) -0.0197(13) O4 0.0474(14) 0.0315(14) 0.0343(12) 0.0080(10) 0.0040(10) -0.0041(11) O5 0.0568(17) 0.0418(17) 0.078(2) 0.0059(15) -0.0097(15) 0.0098(14) O6 0.0606(17) 0.0564(19) 0.0354(14) 0.0123(13) -0.0096(12) -0.0190(14) S1 0.0507(6) 0.0322(5) 0.0441(5) 0.0118(4) -0.0104(4) -0.0098(4) S2 0.0461(5) 0.0336(5) 0.0397(5) 0.0104(4) -0.0035(4) -0.0022(4) C31 0.0371(17) 0.0176(15) 0.0228(15) 0.0020(12) -0.0005(12) -0.0021(13) C32 0.0372(18) 0.0326(19) 0.0276(16) -0.0013(14) 0.0037(13) 0.0003(15) C33 0.0373(18) 0.045(2) 0.0296(17) 0.0004(16) -0.0009(14) 0.0078(16) C34 0.0357(17) 0.037(2) 0.0225(15) 0.0009(14) -0.0040(12) 0.0011(15) C35 0.0343(16) 0.0181(15) 0.0224(15) 0.0011(11) -0.0010(12) -0.0033(12) S3 0.0404(5) 0.0219(4) 0.0195(4) 0.0004(3) 0.0005(3) 0.0002(3) O7 0.0480(14) 0.0331(14) 0.0242(11) 0.0001(9) 0.0062(10) -0.0001(11) O8 0.0543(14) 0.0229(12) 0.0275(11) 0.0052(9) 0.0044(10) 0.0042(11) O9 0.0465(13) 0.0321(13) 0.0233(11) -0.0027(10) -0.0017(9) -0.0056(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 O1W H1E 0.8560 . ? O1W H1F 0.8521 . ? O2W H2E 0.8530 . ? O2W H2F 0.8512 . ? O3W H3E 0.8852 . ? O3W H3F 0.8018 . ? C1 N1 1.492(4) . ? C1 C2 1.515(5) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 N2 1.489(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N2 1.495(4) . ? C3 C4 1.515(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 N3 1.502(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C14 1.512(4) 3_556 ? C5 N3 1.512(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 N1 1.510(4) . ? C6 C7 1.511(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C20 1.411(4) . ? C7 C8 1.413(4) . ? C8 C9 1.431(5) . ? C8 C13 1.440(5) . ? C9 C10 1.360(5) . ? C9 H9 0.9500 . ? C10 C11 1.416(5) . ? C10 H10 0.9500 . ? C11 C12 1.366(5) . ? C11 H11 0.9500 . ? C12 C13 1.428(5) . ? C12 H12 0.9500 . ? C13 C14 1.403(4) . ? C14 C15 1.409(4) . ? C14 C5 1.512(4) 3_556 ? C15 C16 1.440(4) . ? C15 C20 1.443(4) . ? C16 C17 1.348(5) . ? C16 H16 0.9500 . ? C17 C18 1.404(5) . ? C17 H17 0.9500 . ? C18 C19 1.365(5) . ? C18 H18 0.9500 . ? C19 C20 1.428(5) . ? C19 H19 0.9500 . ? C21 C22 1.358(5) . ? C21 C30 1.424(6) . ? C21 S1 1.795(4) . ? C22 C23 1.406(5) . ? C22 H22 0.9500 . ? C23 C24 1.364(6) . ? C23 H23 0.9500 . ? C24 C25 1.428(5) . ? C24 H24 0.9500 . ? C25 C26 1.428(5) . ? C25 C30 1.434(5) . ? C26 C27 1.364(6) . ? C26 S2 1.796(4) . ? C27 C28 1.405(6) . ? C27 H27 0.9500 . ? C28 C29 1.346(6) . ? C28 H28 0.9500 . ? C29 C30 1.426(5) . ? C29 H29 0.9500 . ? N1 H1C 0.9200 . ? N1 H1D 0.9200 . ? N2 H2C 0.9200 . ? N2 H2D 0.9200 . ? N3 H3C 0.9200 . ? N3 H3D 0.9200 . ? O1 S1 1.458(3) . ? O2 S1 1.444(3) . ? O3 S1 1.459(3) . ? O4 S2 1.454(2) . ? O5 S2 1.444(3) . ? O6 S2 1.451(3) . ? C31 C32 1.372(5) . ? C31 C35 1.425(5) . ? C31 S3 1.786(3) . ? C32 C33 1.406(5) . ? C32 H32 0.9500 . ? C33 C34 1.361(5) . ? C33 H33 0.9500 . ? C34 C35 1.420(5) 3 ? C34 H34 0.9500 . ? C35 C34 1.420(5) 3 ? C35 C35 1.439(6) 3 ? S3 O7 1.446(2) . ? S3 O9 1.458(2) . ? S3 O8 1.461(2) . ? 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 H1E O1W H1F 88.9 . . ? H2E O2W H2F 109.2 . . ? H3E O3W H3F 110.8 . . ? N1 C1 C2 109.7(3) . . ? N1 C1 H1A 109.7 . . ? C2 C1 H1A 109.7 . . ? N1 C1 H1B 109.7 . . ? C2 C1 H1B 109.7 . . ? H1A C1 H1B 108.2 . . ? N2 C2 C1 110.1(3) . . ? N2 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 . . ? N2 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 . . ? H2A C2 H2B 108.2 . . ? N2 C3 C4 110.7(3) . . ? N2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? N3 C4 C3 109.0(2) . . ? N3 C4 H4A 109.9 . . ? C3 C4 H4A 109.9 . . ? N3 C4 H4B 109.9 . . ? C3 C4 H4B 109.9 . . ? H4A C4 H4B 108.3 . . ? C14 C5 N3 111.9(3) 3_556 . ? C14 C5 H5A 109.2 3_556 . ? N3 C5 H5A 109.2 . . ? C14 C5 H5B 109.2 3_556 . ? N3 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? N1 C6 C7 113.1(3) . . ? N1 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? N1 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? C20 C7 C8 120.8(3) . . ? C20 C7 C6 120.0(3) . . ? C8 C7 C6 119.2(3) . . ? C7 C8 C9 121.8(3) . . ? C7 C8 C13 119.6(3) . . ? C9 C8 C13 118.5(3) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 120.5(3) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120.1(3) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121.7(3) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C14 C13 C12 122.6(3) . . ? C14 C13 C8 119.6(3) . . ? C12 C13 C8 117.8(3) . . ? C13 C14 C15 121.0(3) . . ? C13 C14 C5 119.4(3) . 3_556 ? C15 C14 C5 119.6(3) . 3_556 ? C14 C15 C16 122.7(3) . . ? C14 C15 C20 119.7(3) . . ? C16 C15 C20 117.6(3) . . ? C17 C16 C15 121.8(3) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C18 120.6(3) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 120.5(3) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 121.3(3) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C7 C20 C19 122.6(3) . . ? C7 C20 C15 119.2(3) . . ? C19 C20 C15 118.2(3) . . ? C22 C21 C30 122.3(3) . . ? C22 C21 S1 118.0(3) . . ? C30 C21 S1 119.6(3) . . ? C21 C22 C23 119.8(4) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? C24 C23 C22 120.7(4) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C25 120.9(3) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 123.9(3) . . ? C26 C25 C30 117.5(3) . . ? C24 C25 C30 118.7(3) . . ? C27 C26 C25 121.7(3) . . ? C27 C26 S2 117.4(3) . . ? C25 C26 S2 120.9(3) . . ? C26 C27 C28 119.9(4) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 120.9(4) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C28 C29 C30 121.3(4) . . ? C28 C29 H29 119.4 . . ? C30 C29 H29 119.4 . . ? C21 C30 C29 123.8(3) . . ? C21 C30 C25 117.5(3) . . ? C29 C30 C25 118.7(4) . . ? C1 N1 C6 116.1(2) . . ? C1 N1 H1C 108.3 . . ? C6 N1 H1C 108.3 . . ? C1 N1 H1D 108.3 . . ? C6 N1 H1D 108.3 . . ? H1C N1 H1D 107.4 . . ? C2 N2 C3 112.3(2) . . ? C2 N2 H2C 109.1 . . ? C3 N2 H2C 109.1 . . ? C2 N2 H2D 109.1 . . ? C3 N2 H2D 109.1 . . ? H2C N2 H2D 107.9 . . ? C4 N3 C5 115.1(2) . . ? C4 N3 H3C 108.5 . . ? C5 N3 H3C 108.5 . . ? C4 N3 H3D 108.5 . . ? C5 N3 H3D 108.5 . . ? H3C N3 H3D 107.5 . . ? O2 S1 O1 113.09(16) . . ? O2 S1 O3 113.69(18) . . ? O1 S1 O3 110.56(17) . . ? O2 S1 C21 106.22(18) . . ? O1 S1 C21 105.86(17) . . ? O3 S1 C21 106.81(16) . . ? O5 S2 O6 112.07(19) . . ? O5 S2 O4 113.12(17) . . ? O6 S2 O4 113.22(17) . . ? O5 S2 C26 105.11(18) . . ? O6 S2 C26 107.39(17) . . ? O4 S2 C26 105.17(15) . . ? C32 C31 C35 121.0(3) . . ? C32 C31 S3 116.9(2) . . ? C35 C31 S3 122.0(2) . . ? C31 C32 C33 119.8(3) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C34 C33 C32 121.5(3) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C33 C34 C35 120.5(3) . 3 ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 3 . ? C34 C35 C31 122.8(3) 3 . ? C34 C35 C35 118.7(4) 3 3 ? C31 C35 C35 118.4(4) . 3 ? O7 S3 O9 111.94(14) . . ? O7 S3 O8 111.99(14) . . ? O9 S3 O8 112.21(14) . . ? O7 S3 C31 106.95(14) . . ? O9 S3 C31 105.88(14) . . ? O8 S3 C31 107.43(14) . . ? 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 N1 C1 C2 N2 -173.0(2) . . . . ? N2 C3 C4 N3 -174.2(2) . . . . ? N1 C6 C7 C20 98.6(3) . . . . ? N1 C6 C7 C8 -81.5(3) . . . . ? C20 C7 C8 C9 -178.9(3) . . . . ? C6 C7 C8 C9 1.2(4) . . . . ? C20 C7 C8 C13 0.7(4) . . . . ? C6 C7 C8 C13 -179.2(3) . . . . ? C7 C8 C9 C10 -177.9(3) . . . . ? C13 C8 C9 C10 2.5(5) . . . . ? C8 C9 C10 C11 1.2(5) . . . . ? C9 C10 C11 C12 -3.1(5) . . . . ? C10 C11 C12 C13 1.2(5) . . . . ? C11 C12 C13 C14 -179.3(3) . . . . ? C11 C12 C13 C8 2.4(4) . . . . ? C7 C8 C13 C14 -2.2(4) . . . . ? C9 C8 C13 C14 177.4(3) . . . . ? C7 C8 C13 C12 176.2(3) . . . . ? C9 C8 C13 C12 -4.2(4) . . . . ? C12 C13 C14 C15 -176.0(3) . . . . ? C8 C13 C14 C15 2.3(4) . . . . ? C12 C13 C14 C5 6.9(4) . . . 3_556 ? C8 C13 C14 C5 -174.8(3) . . . 3_556 ? C13 C14 C15 C16 178.8(3) . . . . ? C5 C14 C15 C16 -4.1(4) 3_556 . . . ? C13 C14 C15 C20 -1.0(4) . . . . ? C5 C14 C15 C20 176.2(3) 3_556 . . . ? C14 C15 C16 C17 -179.0(3) . . . . ? C20 C15 C16 C17 0.8(4) . . . . ? C15 C16 C17 C18 -1.6(5) . . . . ? C16 C17 C18 C19 1.5(5) . . . . ? C17 C18 C19 C20 -0.6(5) . . . . ? C8 C7 C20 C19 -179.8(3) . . . . ? C6 C7 C20 C19 0.1(4) . . . . ? C8 C7 C20 C15 0.6(4) . . . . ? C6 C7 C20 C15 -179.5(3) . . . . ? C18 C19 C20 C7 -179.8(3) . . . . ? C18 C19 C20 C15 -0.2(4) . . . . ? C14 C15 C20 C7 -0.5(4) . . . . ? C16 C15 C20 C7 179.7(3) . . . . ? C14 C15 C20 C19 179.9(3) . . . . ? C16 C15 C20 C19 0.1(4) . . . . ? C30 C21 C22 C23 -2.0(5) . . . . ? S1 C21 C22 C23 177.8(3) . . . . ? C21 C22 C23 C24 1.2(6) . . . . ? C22 C23 C24 C25 0.8(5) . . . . ? C23 C24 C25 C26 178.1(3) . . . . ? C23 C24 C25 C30 -2.0(5) . . . . ? C24 C25 C26 C27 -179.6(3) . . . . ? C30 C25 C26 C27 0.4(5) . . . . ? C24 C25 C26 S2 2.7(5) . . . . ? C30 C25 C26 S2 -177.2(2) . . . . ? C25 C26 C27 C28 -1.2(5) . . . . ? S2 C26 C27 C28 176.5(3) . . . . ? C26 C27 C28 C29 0.6(6) . . . . ? C27 C28 C29 C30 0.8(6) . . . . ? C22 C21 C30 C29 -179.0(3) . . . . ? S1 C21 C30 C29 1.2(5) . . . . ? C22 C21 C30 C25 0.7(5) . . . . ? S1 C21 C30 C25 -179.0(2) . . . . ? C28 C29 C30 C21 178.2(3) . . . . ? C28 C29 C30 C25 -1.6(5) . . . . ? C26 C25 C30 C21 -178.8(3) . . . . ? C24 C25 C30 C21 1.2(5) . . . . ? C26 C25 C30 C29 0.9(5) . . . . ? C24 C25 C30 C29 -179.0(3) . . . . ? C2 C1 N1 C6 -164.1(3) . . . . ? C7 C6 N1 C1 -29.6(4) . . . . ? C1 C2 N2 C3 -159.5(3) . . . . ? C4 C3 N2 C2 -152.4(3) . . . . ? C3 C4 N3 C5 -175.0(3) . . . . ? C14 C5 N3 C4 -42.4(4) 3_556 . . . ? C22 C21 S1 O2 -4.0(3) . . . . ? C30 C21 S1 O2 175.8(3) . . . . ? C22 C21 S1 O1 -124.5(3) . . . . ? C30 C21 S1 O1 55.3(3) . . . . ? C22 C21 S1 O3 117.7(3) . . . . ? C30 C21 S1 O3 -62.6(3) . . . . ? C27 C26 S2 O5 7.4(3) . . . . ? C25 C26 S2 O5 -174.8(3) . . . . ? C27 C26 S2 O6 126.9(3) . . . . ? C25 C26 S2 O6 -55.4(3) . . . . ? C27 C26 S2 O4 -112.2(3) . . . . ? C25 C26 S2 O4 65.5(3) . . . . ? C35 C31 C32 C33 -0.8(5) . . . . ? S3 C31 C32 C33 175.6(3) . . . . ? C31 C32 C33 C34 1.1(6) . . . . ? C32 C33 C34 C35 -1.0(6) . . . 3 ? C32 C31 C35 C34 -180.0(3) . . . 3 ? S3 C31 C35 C34 3.8(4) . . . 3 ? C32 C31 C35 C35 0.4(5) . . . 3 ? S3 C31 C35 C35 -175.7(3) . . . 3 ? C32 C31 S3 O7 8.6(3) . . . . ? C35 C31 S3 O7 -175.1(3) . . . . ? C32 C31 S3 O9 -111.0(3) . . . . ? C35 C31 S3 O9 65.4(3) . . . . ? C32 C31 S3 O8 129.0(3) . . . . ? C35 C31 S3 O8 -54.7(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H1F O6 0.85 2.39 2.876(5) 116.3 4_666 O1W H1E O5 0.86 2.26 3.034(7) 150.3 1_655 O2W H2E O3W 0.85 1.93 2.719(8) 153.4 4_566 O2W H2F O1W 0.85 2.24 2.672(9) 111.3 . O3W H3E O2 0.89 2.03 2.912(5) 171.9 . O3W H3F O5 0.80 2.20 2.898(5) 145.6 1_655 O3W H3F O1W 0.80 2.40 2.992(7) 131.1 . N1 H1C O3 0.92 1.92 2.763(4) 151.7 4_566 N1 H1D O1 0.92 1.77 2.679(4) 170.9 . N2 H2C O8 0.92 1.84 2.755(3) 179.1 3_556 N2 H2D O9 0.92 1.88 2.773(3) 162.3 . N3 H3C O4 0.92 1.90 2.791(4) 163.5 . N3 H3D O6 0.92 2.13 3.003(4) 157.7 4_566 _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 65.51 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.559 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.089