#data_PEACRYSO4 data_global _journal_name_full CrystEngComm #TrackingRef '- 09058.cif' _journal_coden_Cambridge 1350 _publ_contact_author 'Alamgir Hossain' _publ_contact_author_address ; Department of Chemistry Jackson State University 1325 Lynch Street Jackson, MS 39212, USA ; _publ_contact_author_email alamgir@chem.jsums.edu _publ_contact_author_fax 601-979-3748 _publ_contact_author_phone 601-979-3674 loop_ _publ_author_name _publ_author_address M.A.Saeed ; Department of Chemistry Jackson State University 1325 Lynch Street Jackson, MS 39212, USA ; G.Gryn'ova ; Department of Chemistry Jackson State University 1325 Lynch Street Jackson, MS 39212, USA ; D.R.Powell ; Department of Chemistry and Biochemistry University of Oklahoma 620 Parrington Oval, Room 208 Norman, OK 73019-3051 USA ; J.Leszczynskil ; Department of Chemistry Jackson State University 1325 Lynch Street Jackson, MS 39212, USA ; M.A.Hossain ; Department of Chemistry Jackson State University Jackson 1325 Lynch Street Jackson, MS 39212, USA ; _publ_section_title ; Trapped Methanol ; _publ_section_acknowledgements ; This work was supported by National Institutes of Health, Division of National Center for Research Resources, under Grant Number G12RR013459. ; _publ_contact_author_name 'Dr. Md. Alamgir Hossain' #============================================================ data_09058 _database_code_depnum_ccdc_archive 'CCDC 755129' #TrackingRef '- 09058.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H60 N8, 3(O4 S), (C H4 O), 12(H2 O)' _chemical_formula_sum 'C37 H88 N8 O25 S3' _chemical_formula_weight 1141.33 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' 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 15.303(2) _cell_length_b 16.583(2) _cell_length_c 23.124(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.234(8) _cell_angle_gamma 90.00 _cell_volume 5688.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2035 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 54.13 _exptl_crystal_description colorless _exptl_crystal_colour prism _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 1.918 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.483 _exptl_absorpt_correction_T_max 0.778 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Bruker APEX' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11543 _diffrn_reflns_av_R_equivalents 0.0811 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.76 _diffrn_reflns_theta_max 30.92 _reflns_number_total 1749 _reflns_number_gt 1394 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART, 1998' _computing_cell_refinement 'Bruker SAINT, 1998' _computing_data_reduction 'Bruker SAINT, 1998' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; The intensity data were truncated to 1.50 \%A resolution because data in higher resolution shells all had R(int) > 0.25. Restraints: sadi 0.005 n1 c2 n1 c2' n1 c30 n1 c30' n1 c31 n1 c31' sadi 0.005 c2 c3 c2' c3' c29 c30 c29' c30' c32 c31 c32' c31' sadi 0.005 n4 c3 n4 c3' n28 c29 n28 c29' n33 c32 n33 c32' sadi 0.009 n1 c3 n1 c29 n1 c32 n1 c3' n1 c29' n1 c32' sadi 0.009 n4 c2 n28 c30 n33 c31 n4 c2' n28 c30' n33 c31' delu 0.0010 n1 > c44 delu 0.009 s1a > o4a delu 0.009 s1b > o4b delu 0.009 s1c > o4c simu 0.009 n1 > n4 simu 0.009 n1 n28 > c30' simu 0.009 n1 c31 > n33 isor 0.010 c6 c8 c10 > n16 c18 C23 c25 C35 c36 c39 n42 o1b o3b isor 0.010 o3c o2t ; _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^)+(0.1200P)^2^+100.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1749 _refine_ls_number_parameters 698 _refine_ls_number_restraints 540 _refine_ls_R_factor_all 0.1026 _refine_ls_R_factor_gt 0.0829 _refine_ls_wR_factor_ref 0.2240 _refine_ls_wR_factor_gt 0.2064 _refine_ls_goodness_of_fit_ref 1.102 _refine_ls_restrained_S_all 0.921 _refine_ls_shift/su_max 0.002 _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 N1 N 0.3011(7) 0.8528(8) 0.5642(5) 0.043(3) Uani 1 1 d DU . . C2 C 0.3356(15) 0.9187(8) 0.5324(9) 0.043(3) Uani 0.598(11) 1 d PDU A 1 H2A H 0.3523 0.9654 0.5595 0.051 Uiso 0.598(11) 1 calc PR A 1 H2B H 0.2873 0.9361 0.4978 0.051 Uiso 0.598(11) 1 calc PR A 1 C3 C 0.4185(10) 0.8916(10) 0.5105(8) 0.043(4) Uani 0.598(11) 1 d PDU A 1 H3A H 0.4371 0.9362 0.4877 0.051 Uiso 0.598(11) 1 calc PR A 1 H3B H 0.4690 0.8804 0.5455 0.051 Uiso 0.598(11) 1 calc PR A 1 C2' C 0.3879(10) 0.8935(10) 0.5653(8) 0.042(3) Uani 0.402(11) 1 d PRDU A 2 H2C H 0.4369 0.8628 0.5923 0.051 Uiso 0.402(11) 1 d PR A 2 H2D H 0.3881 0.9488 0.5815 0.051 Uiso 0.402(11) 1 d PR A 2 C3' C 0.4079(17) 0.8975(9) 0.5033(9) 0.043(4) Uani 0.402(11) 1 d PDU A 2 H3C H 0.3653 0.9357 0.4782 0.051 Uiso 0.402(11) 1 calc PR A 2 H3D H 0.4695 0.9190 0.5078 0.051 Uiso 0.402(11) 1 calc PR A 2 N4 N 0.4009(9) 0.8193(8) 0.4726(6) 0.042(4) Uani 1 1 d DU . . H4A H 0.3430 0.8206 0.4517 0.051 Uiso 1 1 d R A . H4B H 0.4087 0.7751 0.4959 0.051 Uiso 1 1 d R . . C5 C 0.4584(13) 0.8131(12) 0.4303(8) 0.049(6) Uani 1 1 d U A . H5A H 0.5227 0.8145 0.4523 0.059 Uiso 1 1 calc R . . H5B H 0.4469 0.8595 0.4026 0.059 Uiso 1 1 calc R . . C6 C 0.4390(15) 0.7349(15) 0.3950(11) 0.044(5) Uani 1 1 d U . . C7 C 0.3845(13) 0.7321(13) 0.3362(9) 0.042(5) Uani 1 1 d U A . H7 H 0.3599 0.7801 0.3163 0.050 Uiso 1 1 calc R . . C8 C 0.3675(13) 0.6583(13) 0.3082(9) 0.043(5) Uani 1 1 d U . . H8 H 0.3319 0.6571 0.2683 0.051 Uiso 1 1 calc R A . C9 C 0.4728(13) 0.6637(14) 0.4222(10) 0.042(5) Uani 1 1 d U A . H9 H 0.5102 0.6647 0.4617 0.051 Uiso 1 1 calc R . . C10 C 0.4534(14) 0.5918(14) 0.3935(10) 0.050(5) Uani 1 1 d U . . H10 H 0.4772 0.5438 0.4137 0.060 Uiso 1 1 calc R A . C11 C 0.3996(13) 0.5860(14) 0.3350(10) 0.039(5) Uani 1 1 d U A . C12 C 0.3786(12) 0.5068(12) 0.3047(8) 0.042(5) Uani 1 1 d U . . H12A H 0.4203 0.4655 0.3270 0.050 Uiso 1 1 calc R A . H12B H 0.3887 0.5104 0.2641 0.050 Uiso 1 1 calc R . . N13 N 0.2840(9) 0.4810(9) 0.3002(7) 0.044(5) Uani 1 1 d U A . H13A H 0.2735 0.4798 0.3377 0.053 Uiso 1 1 calc R . . H13B H 0.2450 0.5176 0.2776 0.053 Uiso 1 1 calc R . . C14 C 0.2674(12) 0.4006(11) 0.2729(8) 0.033(5) Uani 1 1 d U . . H14A H 0.3070 0.3607 0.2986 0.039 Uiso 1 1 calc R A . H14B H 0.2824 0.4010 0.2336 0.039 Uiso 1 1 calc R . . C15 C 0.1692(11) 0.3755(11) 0.2647(8) 0.035(5) Uani 1 1 d U A . H15A H 0.1297 0.4163 0.2400 0.042 Uiso 1 1 calc R . . H15B H 0.1590 0.3234 0.2432 0.042 Uiso 1 1 calc R . . N16 N 0.1449(10) 0.3674(10) 0.3217(7) 0.036(4) Uani 1 1 d U . . C17 C 0.1765(12) 0.2889(11) 0.3492(8) 0.033(5) Uani 1 1 d U A . H17A H 0.2376 0.2786 0.3437 0.040 Uiso 1 1 calc R . . H17B H 0.1363 0.2461 0.3275 0.040 Uiso 1 1 calc R . . C18 C 0.1798(12) 0.2820(12) 0.4138(8) 0.035(5) Uani 1 1 d U . . H18A H 0.2056 0.2289 0.4286 0.042 Uiso 1 1 calc R A . H18B H 0.1176 0.2843 0.4192 0.042 Uiso 1 1 calc R . . N19 N 0.2348(9) 0.3471(9) 0.4502(6) 0.036(5) Uani 1 1 d U A . H19A H 0.2832 0.3580 0.4345 0.044 Uiso 1 1 calc R . . H19B H 0.2003 0.3931 0.4465 0.044 Uiso 1 1 calc R . . C20 C 0.2686(13) 0.3291(12) 0.5137(8) 0.038(6) Uani 1 1 d U . . H20A H 0.3186 0.2898 0.5189 0.046 Uiso 1 1 calc R A . H20B H 0.2198 0.3037 0.5287 0.046 Uiso 1 1 calc R . . C21 C 0.3006(13) 0.4014(15) 0.5494(11) 0.032(6) Uani 1 1 d U A . C22 C 0.3366(13) 0.4694(13) 0.5274(10) 0.036(6) Uani 1 1 d U . . H22 H 0.3453 0.4680 0.4881 0.043 Uiso 1 1 calc R A . C23 C 0.3598(13) 0.5389(13) 0.5615(9) 0.039(6) Uani 1 1 d U A . H23 H 0.3839 0.5840 0.5454 0.046 Uiso 1 1 calc R . . C24 C 0.2897(12) 0.4071(14) 0.6062(9) 0.039(6) Uani 1 1 d U . . H24 H 0.2626 0.3630 0.6213 0.046 Uiso 1 1 calc R A . C25 C 0.3160(12) 0.4741(12) 0.6436(10) 0.037(5) Uani 1 1 d U A . H25 H 0.3124 0.4735 0.6840 0.045 Uiso 1 1 calc R . . C26 C 0.3478(12) 0.5421(14) 0.6186(10) 0.032(5) Uani 1 1 d U . . C27 C 0.3680(13) 0.6170(11) 0.6568(9) 0.039(6) Uani 1 1 d U A . H27A H 0.3329 0.6159 0.6875 0.046 Uiso 1 1 calc R . . H27B H 0.4328 0.6182 0.6774 0.046 Uiso 1 1 calc R . . N28 N 0.3442(9) 0.6911(7) 0.6192(6) 0.042(4) Uani 1 1 d DU . . H28A H 0.2882 0.6859 0.5955 0.051 Uiso 1 1 d R A . H28B H 0.3829 0.6954 0.5957 0.051 Uiso 1 1 d R . . C29 C 0.347(2) 0.7646(7) 0.6552(6) 0.042(4) Uani 0.598(11) 1 d PDU A 1 H29A H 0.3952 0.7585 0.6925 0.051 Uiso 0.598(11) 1 calc PR A 1 H29B H 0.2892 0.7705 0.6663 0.051 Uiso 0.598(11) 1 calc PR A 1 C30 C 0.3656(13) 0.8420(9) 0.6232(7) 0.042(4) Uani 0.598(11) 1 d PDU A 1 H30A H 0.3615 0.8891 0.6487 0.050 Uiso 0.598(11) 1 calc PR A 1 H30B H 0.4276 0.8399 0.6177 0.050 Uiso 0.598(11) 1 calc PR A 1 C31 C 0.2130(10) 0.8699(15) 0.5777(7) 0.043(3) Uani 0.598(11) 1 d PDU A 1 H31A H 0.2187 0.9188 0.6029 0.051 Uiso 0.598(11) 1 calc PR A 1 H31B H 0.1969 0.8244 0.6007 0.051 Uiso 0.598(11) 1 calc PR A 1 C32 C 0.1367(12) 0.8827(8) 0.5211(6) 0.044(4) Uani 0.598(11) 1 d PDU A 1 H32A H 0.0806 0.8961 0.5331 0.053 Uiso 0.598(11) 1 calc PR A 1 H32B H 0.1521 0.9294 0.4989 0.053 Uiso 0.598(11) 1 calc PR A 1 C29' C 0.3500(12) 0.7650(8) 0.6550(6) 0.042(4) Uani 0.402(11) 1 d PRDU A 2 H29C H 0.4127 0.7854 0.6649 0.051 Uiso 0.402(11) 1 d PR A 2 H29D H 0.3344 0.7508 0.6928 0.051 Uiso 0.402(11) 1 d PR A 2 C30' C 0.2869(18) 0.8327(12) 0.6238(8) 0.043(3) Uani 0.402(11) 1 d PDU A 2 H30C H 0.2236 0.8157 0.6192 0.052 Uiso 0.402(11) 1 calc PR A 2 H30D H 0.2973 0.8815 0.6492 0.052 Uiso 0.402(11) 1 calc PR A 2 C31' C 0.2357(13) 0.9136(9) 0.5324(14) 0.044(4) Uani 0.402(11) 1 d PDU A 2 H31C H 0.2500 0.9273 0.4941 0.053 Uiso 0.402(11) 1 calc PR A 2 H31D H 0.2419 0.9634 0.5567 0.053 Uiso 0.402(11) 1 calc PR A 2 C32' C 0.1375(10) 0.8837(16) 0.5200(17) 0.044(4) Uani 0.402(11) 1 d PDU A 2 H32C H 0.1233 0.8705 0.5584 0.053 Uiso 0.402(11) 1 calc PR A 2 H32D H 0.0968 0.9278 0.5012 0.053 Uiso 0.402(11) 1 calc PR A 2 N33 N 0.1197(9) 0.8124(7) 0.4811(6) 0.045(4) Uani 1 1 d DU . . H33A H 0.1361 0.7671 0.5024 0.054 Uiso 1 1 d R A . H33B H 0.1532 0.8169 0.4542 0.054 Uiso 1 1 d R . . C34 C 0.0211(12) 0.8086(12) 0.4484(9) 0.053(6) Uani 1 1 d U A . H34A H -0.0151 0.8044 0.4784 0.064 Uiso 1 1 calc R . . H34B H 0.0047 0.8599 0.4267 0.064 Uiso 1 1 calc R . . C35 C -0.0047(14) 0.7412(15) 0.4054(11) 0.048(5) Uani 1 1 d U . . C36 C -0.0437(13) 0.6704(13) 0.4209(10) 0.043(5) Uani 1 1 d U A . H36 H -0.0488 0.6649 0.4609 0.052 Uiso 1 1 calc R . . C37 C -0.0750(13) 0.6082(14) 0.3816(9) 0.042(6) Uani 1 1 d U . . H37 H -0.0998 0.5614 0.3951 0.050 Uiso 1 1 calc R A . C38 C 0.0029(12) 0.7463(13) 0.3463(9) 0.043(6) Uani 1 1 d U A . H38 H 0.0288 0.7928 0.3332 0.052 Uiso 1 1 calc R . . C39 C -0.0276(13) 0.6827(13) 0.3064(10) 0.046(5) Uani 1 1 d U . . H39 H -0.0189 0.6863 0.2672 0.055 Uiso 1 1 calc R A . C40 C -0.0703(14) 0.6138(14) 0.3218(10) 0.035(6) Uani 1 1 d U A . C41 C -0.1120(13) 0.5553(12) 0.2746(9) 0.050(6) Uani 1 1 d U . . H41A H -0.0974 0.5711 0.2367 0.060 Uiso 1 1 calc R A . H41B H -0.1784 0.5572 0.2683 0.060 Uiso 1 1 calc R . . N42 N -0.0798(9) 0.4712(9) 0.2903(7) 0.039(5) Uani 1 1 d U A . H42A H -0.0981 0.4555 0.3236 0.046 Uiso 1 1 calc R . . H42B H -0.1071 0.4376 0.2595 0.046 Uiso 1 1 calc R . . C43 C 0.0194(12) 0.4604(12) 0.3022(9) 0.040(7) Uani 1 1 d U . . H43A H 0.0402 0.4813 0.2678 0.047 Uiso 1 1 calc R A . H43B H 0.0490 0.4926 0.3377 0.047 Uiso 1 1 calc R . . C44 C 0.0478(12) 0.3748(11) 0.3125(8) 0.037(6) Uani 1 1 d U A . H44A H 0.0297 0.3541 0.3481 0.044 Uiso 1 1 calc R . . H44B H 0.0172 0.3419 0.2777 0.044 Uiso 1 1 calc R . . S1A S 0.2024(6) 0.9011(5) 0.3632(4) 0.067(3) Uani 1 1 d U . . O1A O 0.2247(9) 0.8272(9) 0.4001(6) 0.054(4) Uani 1 1 d U . . O2A O 0.2818(11) 0.9525(10) 0.3745(6) 0.075(5) Uani 1 1 d U . . O3A O 0.1744(12) 0.8803(10) 0.3005(8) 0.103(6) Uani 1 1 d U . . O4A O 0.1283(11) 0.9440(10) 0.3813(8) 0.107(6) Uani 1 1 d U . . S1B S 0.5653(5) 0.7096(5) 0.5919(3) 0.048(2) Uani 1 1 d U . . O1B O 0.4694(9) 0.7040(7) 0.5555(5) 0.040(4) Uani 1 1 d U . . O2B O 0.6101(8) 0.6308(9) 0.5905(6) 0.046(4) Uani 1 1 d U . . O3B O 0.6106(9) 0.7701(9) 0.5636(6) 0.057(4) Uani 1 1 d U . . O4B O 0.5652(8) 0.7306(9) 0.6530(7) 0.061(5) Uani 1 1 d U . . S1C S 0.1082(5) 0.6495(5) 0.5813(4) 0.050(2) Uani 1 1 d U . . O1C O 0.1738(9) 0.6719(8) 0.5464(6) 0.044(4) Uani 1 1 d U . . O2C O 0.0364(9) 0.7088(9) 0.5729(6) 0.043(4) Uani 1 1 d U . . O3C O 0.0712(9) 0.5702(10) 0.5618(6) 0.061(4) Uani 1 1 d U . . O4C O 0.1584(9) 0.6435(9) 0.6452(7) 0.067(5) Uani 1 1 d U . . O1S O 0.2148(8) 0.5407(11) 0.3959(6) 0.051(5) Uani 1 1 d . . . H1S H 0.1808 0.5178 0.4182 0.061 Uiso 1 1 d R . . C2S C 0.2205(14) 0.6266(17) 0.4050(10) 0.074(9) Uani 1 1 d . . . H2SA H 0.2587 0.6500 0.3810 0.111 Uiso 1 1 d R . . H2SB H 0.2465 0.6383 0.4473 0.111 Uiso 1 1 d R . . H2SC H 0.1599 0.6500 0.3928 0.111 Uiso 1 1 d R . . O1T O 0.1567(8) 0.7420(8) 0.2305(6) 0.075(5) Uani 1 1 d . . . H1T1 H 0.1626 0.7863 0.2536 0.090 Uiso 1 1 d R . . H1T2 H 0.1575 0.7791 0.2023 0.090 Uiso 1 1 d R . . O2T O 0.1084(7) 0.4710(7) 0.4646(5) 0.046(4) Uani 1 1 d U . . H2T1 H 0.0969 0.5012 0.4942 0.055 Uiso 1 1 d R . . H2T2 H 0.0496 0.4575 0.4557 0.055 Uiso 1 1 d R . . O3T O 0.6657(9) 0.9180(8) 0.5386(6) 0.094(6) Uani 1 1 d . . . H3T1 H 0.6480 0.8684 0.5467 0.112 Uiso 1 1 d R . . H3T2 H 0.6826 0.9580 0.5653 0.112 Uiso 1 1 d R . . O4T O -0.0473(10) 0.9985(8) 0.3580(7) 0.114(7) Uani 1 1 d . . . H4T1 H 0.0104 0.9819 0.3656 0.137 Uiso 1 1 d R . . H4T2 H -0.0891 0.9678 0.3688 0.137 Uiso 1 1 d R . . O5T O 0.1702(8) 0.5807(8) 0.2251(6) 0.075(5) Uani 1 1 d . . . H5T1 H 0.1289 0.5589 0.1888 0.090 Uiso 1 1 d R . . H5T2 H 0.1571 0.6259 0.2365 0.090 Uiso 1 1 d R . . O6T O -0.0304(10) 0.8514(10) 0.6058(8) 0.140(8) Uani 1 1 d . . . H6T1 H -0.0082 0.8049 0.5952 0.168 Uiso 1 1 d R . . H6T2 H -0.0138 0.9033 0.6048 0.168 Uiso 1 1 d R . . O7T O -0.1673(11) 0.9096(11) 0.3925(10) 0.168(9) Uani 1 1 d . . . H7T1 H -0.1677 0.9062 0.4312 0.201 Uiso 1 1 d R . . H7T2 H -0.2045 0.8702 0.3743 0.201 Uiso 1 1 d R . . O8T O 0.8295(13) 0.8987(11) 0.4997(8) 0.084(7) Uiso 0.70 1 d P . . H8T1 H 0.7777 0.9048 0.5111 0.101 Uiso 0.70 1 d PR . . H8T2 H 0.8729 0.8840 0.5318 0.101 Uiso 0.70 1 d PR . . O9T O 0.3532(15) 1.0119(12) 0.2905(8) 0.081(8) Uiso 0.70 1 d P . . H9T1 H 0.3228 0.9936 0.3166 0.097 Uiso 0.70 1 d PR C . H9T2 H 0.3350 1.0634 0.2838 0.097 Uiso 0.70 1 d PR . . O10T O 0.6883(14) 0.8205(13) 0.7280(9) 0.107(9) Uiso 0.70 1 d P . . H10T H 0.6478 0.7911 0.7016 0.128 Uiso 0.70 1 d PR . . H10U H 0.6887 0.7883 0.7593 0.128 Uiso 0.70 1 d PR . . O11T O 0.672(3) 0.879(3) 0.420(2) 0.17(2) Uiso 0.40 1 d P . . H11T H 0.6711 0.8933 0.4575 0.203 Uiso 0.40 1 d PR . . H11U H 0.7246 0.8917 0.4110 0.203 Uiso 0.40 1 d PR . . O12T O 0.554(3) 0.935(2) 0.3234(17) 0.114(15) Uiso 0.40 1 d P B 1 H12T H 0.4997 0.9581 0.3150 0.137 Uiso 0.40 1 d PR B 1 H12U H 0.5940 0.9140 0.3554 0.137 Uiso 0.40 1 d PR B 1 O12U O 0.435(2) 1.0016(19) 0.3040(14) 0.142(12) Uiso 0.60 1 d P C 2 O13T O -0.2815(15) 0.7782(13) 0.3295(9) 0.038(8) Uiso 0.50 1 d P D 1 H13T H -0.2905 0.7473 0.2992 0.046 Uiso 0.50 1 d PR D 1 H13U H -0.2485 0.8158 0.3479 0.046 Uiso 0.50 1 d PR D 1 O14U O -0.376(2) 0.789(2) 0.3343(15) 0.121(13) Uiso 0.50 1 d P E 2 O14V O -0.442(2) 0.783(2) 0.2655(17) 0.143(14) Uiso 0.50 1 d P F 3 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 N1 0.023(5) 0.047(6) 0.059(7) -0.002(5) 0.008(5) 0.008(5) C2 0.025(7) 0.046(7) 0.056(8) -0.002(6) 0.010(6) 0.009(7) C3 0.026(7) 0.046(8) 0.056(8) 0.000(6) 0.010(6) 0.011(7) C2' 0.024(6) 0.046(8) 0.057(8) -0.002(6) 0.010(6) 0.008(6) C3' 0.026(7) 0.046(8) 0.056(8) 0.000(6) 0.009(6) 0.010(7) N4 0.025(7) 0.047(8) 0.055(8) 0.000(6) 0.010(6) 0.010(7) C5 0.043(16) 0.052(8) 0.057(13) -0.005(9) 0.019(9) -0.001(11) C6 0.035(10) 0.049(7) 0.051(8) -0.001(6) 0.017(6) -0.002(8) C7 0.047(17) 0.045(6) 0.041(11) 0.009(8) 0.025(10) -0.011(13) C8 0.040(10) 0.048(6) 0.043(8) 0.004(6) 0.017(7) -0.001(9) C9 0.028(16) 0.055(8) 0.047(11) -0.007(7) 0.016(10) 0.013(13) C10 0.047(10) 0.049(7) 0.051(8) 0.002(6) 0.006(7) 0.001(9) C11 0.029(9) 0.046(6) 0.045(8) 0.005(5) 0.016(6) -0.007(6) C12 0.035(7) 0.048(6) 0.046(9) 0.002(7) 0.020(8) -0.005(7) N13 0.036(7) 0.044(7) 0.055(9) 0.000(7) 0.016(7) -0.009(6) C14 0.028(7) 0.042(8) 0.031(9) 0.006(7) 0.013(7) 0.002(7) C15 0.027(7) 0.043(8) 0.033(8) -0.003(7) 0.005(7) 0.000(7) N16 0.022(7) 0.045(8) 0.045(7) 0.007(7) 0.013(7) 0.001(7) C17 0.020(11) 0.036(10) 0.047(8) 0.001(8) 0.015(11) -0.005(9) C18 0.026(10) 0.035(9) 0.043(7) 0.002(7) 0.005(7) 0.000(8) N19 0.016(13) 0.044(12) 0.048(8) 0.000(9) 0.005(10) -0.004(9) C20 0.026(16) 0.043(14) 0.045(8) -0.005(9) 0.009(11) -0.002(13) C21 0.014(17) 0.039(14) 0.049(10) -0.007(10) 0.018(12) 0.006(13) C22 0.026(17) 0.042(14) 0.038(12) -0.001(9) 0.002(13) -0.001(14) C23 0.036(10) 0.040(9) 0.038(9) -0.001(8) 0.008(8) -0.001(9) C24 0.017(15) 0.056(12) 0.049(12) -0.010(10) 0.018(14) -0.005(12) C25 0.031(10) 0.046(8) 0.034(9) 0.001(7) 0.006(8) 0.006(8) C26 0.013(14) 0.045(6) 0.037(11) 0.001(7) 0.002(13) 0.008(10) C27 0.028(15) 0.046(6) 0.045(12) -0.004(6) 0.016(13) 0.006(10) N28 0.019(7) 0.045(6) 0.062(9) 0.000(5) 0.009(7) 0.005(7) C29 0.020(7) 0.047(7) 0.061(8) 0.000(5) 0.011(7) 0.007(7) C30 0.021(6) 0.045(7) 0.059(7) -0.001(6) 0.009(6) 0.009(7) C31 0.022(6) 0.046(7) 0.059(8) -0.002(6) 0.007(5) 0.007(6) C32 0.024(6) 0.046(8) 0.061(8) -0.002(6) 0.004(6) 0.006(7) C29' 0.020(7) 0.047(7) 0.061(8) 0.000(5) 0.011(7) 0.007(7) C30' 0.021(7) 0.047(7) 0.060(7) -0.001(6) 0.009(6) 0.007(7) C31' 0.024(6) 0.046(7) 0.060(8) -0.002(6) 0.005(6) 0.006(6) C32' 0.024(6) 0.046(8) 0.060(9) -0.002(6) 0.005(6) 0.006(6) N33 0.026(6) 0.044(8) 0.061(8) -0.001(6) 0.004(6) 0.006(7) C34 0.031(9) 0.051(11) 0.067(12) -0.005(10) -0.006(10) 0.009(11) C35 0.038(9) 0.047(8) 0.054(7) 0.003(6) -0.002(7) 0.004(7) C36 0.035(10) 0.052(9) 0.040(8) 0.000(7) 0.005(8) 0.004(8) C37 0.015(15) 0.061(13) 0.051(12) -0.008(10) 0.015(16) -0.006(12) C38 0.018(15) 0.049(13) 0.058(11) 0.006(9) 0.000(13) -0.009(11) C39 0.038(10) 0.045(10) 0.053(8) 0.006(7) 0.006(8) 0.000(8) C40 0.014(15) 0.043(9) 0.038(11) 0.002(10) -0.009(14) 0.002(10) C41 0.037(12) 0.047(9) 0.052(14) -0.008(10) -0.017(15) 0.009(8) N42 0.022(7) 0.043(8) 0.049(9) 0.001(7) 0.003(8) -0.002(7) C43 0.027(8) 0.060(13) 0.038(15) 0.000(15) 0.019(14) 0.010(11) C44 0.019(7) 0.053(13) 0.034(15) -0.020(14) 0.000(10) 0.001(11) S1A 0.061(8) 0.065(9) 0.070(8) 0.019(7) 0.008(8) 0.006(6) O1A 0.047(11) 0.066(12) 0.048(12) 0.014(8) 0.007(9) 0.007(9) O2A 0.065(13) 0.089(14) 0.073(12) 0.019(10) 0.020(11) -0.010(9) O3A 0.153(17) 0.077(14) 0.058(10) 0.029(11) -0.015(12) -0.010(11) O4A 0.070(13) 0.092(15) 0.166(16) 0.037(12) 0.039(12) 0.032(10) S1B 0.022(6) 0.065(7) 0.056(6) 0.006(6) 0.007(5) -0.003(5) O1B 0.028(6) 0.050(8) 0.041(8) 0.002(7) 0.006(6) -0.001(7) O2B 0.022(10) 0.061(9) 0.061(11) 0.017(9) 0.022(8) 0.000(8) O3B 0.039(8) 0.056(8) 0.079(9) 0.010(7) 0.018(7) -0.002(6) O4B 0.035(10) 0.096(13) 0.044(8) 0.005(10) -0.006(8) 0.017(9) S1C 0.013(7) 0.060(7) 0.076(7) -0.009(6) 0.011(6) -0.004(5) O1C 0.017(11) 0.055(11) 0.061(10) -0.010(9) 0.010(8) 0.012(8) O2C 0.012(10) 0.058(10) 0.061(11) -0.009(9) 0.009(9) -0.007(7) O3C 0.038(8) 0.059(7) 0.086(9) -0.013(7) 0.017(7) 0.000(7) O4C 0.018(11) 0.112(13) 0.068(9) -0.001(10) 0.008(8) 0.005(9) O1S 0.015(10) 0.065(14) 0.075(12) 0.013(11) 0.015(9) -0.003(11) C2S 0.05(2) 0.09(3) 0.10(2) 0.02(2) 0.032(16) 0.00(2) O1T 0.070(12) 0.071(12) 0.078(12) 0.016(10) 0.010(9) 0.022(9) O2T 0.029(7) 0.055(8) 0.059(8) -0.014(7) 0.021(6) -0.005(6) O3T 0.096(13) 0.055(12) 0.135(15) 0.007(11) 0.037(11) -0.017(10) O4T 0.068(13) 0.072(13) 0.171(17) -0.001(12) -0.033(12) 0.003(10) O5T 0.041(11) 0.078(12) 0.096(13) 0.000(10) -0.004(9) 0.001(9) O6T 0.104(15) 0.109(15) 0.24(2) -0.096(15) 0.114(15) -0.060(13) O7T 0.109(16) 0.128(17) 0.27(2) 0.013(17) 0.047(16) 0.031(14) _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 N1 C31' 1.483(10) . ? N1 C30' 1.483(10) . ? N1 C31 1.484(10) . ? N1 C30 1.484(10) . ? N1 C2' 1.484(10) . ? N1 C2 1.485(10) . ? C2 C3 1.543(10) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N4 1.471(11) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C2' C3' 1.539(11) . ? C2' H2C 0.9898 . ? C2' H2D 0.9899 . ? C3' N4 1.469(11) . ? C3' H3C 0.9900 . ? C3' H3D 0.9900 . ? N4 C5 1.472(19) . ? N4 H4A 0.8999 . ? N4 H4B 0.8999 . ? C5 C6 1.52(2) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C9 1.38(2) . ? C6 C7 1.41(2) . ? C7 C8 1.38(2) . ? C7 H7 0.9500 . ? C8 C11 1.38(2) . ? C8 H8 0.9500 . ? C9 C10 1.36(2) . ? C9 H9 0.9500 . ? C10 C11 1.40(2) . ? C10 H10 0.9500 . ? C11 C12 1.49(2) . ? C12 N13 1.489(19) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? N13 C14 1.471(19) . ? N13 H13A 0.9200 . ? N13 H13B 0.9200 . ? C14 C15 1.53(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 N16 1.461(19) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? N16 C44 1.45(2) . ? N16 C17 1.477(19) . ? C17 C18 1.49(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 N19 1.494(19) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? N19 C20 1.464(19) . ? N19 H19A 0.9200 . ? N19 H19B 0.9200 . ? C20 C21 1.47(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C24 1.37(2) . ? C21 C22 1.40(2) . ? C22 C23 1.39(2) . ? C22 H22 0.9500 . ? C23 C26 1.38(2) . ? C23 H23 0.9500 . ? C24 C25 1.40(2) . ? C24 H24 0.9500 . ? C25 C26 1.41(2) . ? C25 H25 0.9500 . ? C26 C27 1.51(2) . ? C27 N28 1.498(19) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N28 C29' 1.468(11) . ? N28 C29 1.470(11) . ? N28 H28A 0.9001 . ? N28 H28B 0.9002 . ? C29 C30 1.539(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.538(10) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 N33 1.471(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C29' C30' 1.539(11) . ? C29' H29C 0.9901 . ? C29' H29D 0.9899 . ? C30' H30C 0.9900 . ? C30' H30D 0.9900 . ? C31' C32' 1.540(11) . ? C31' H31C 0.9900 . ? C31' H31D 0.9900 . ? C32' N33 1.470(11) . ? C32' H32C 0.9900 . ? C32' H32D 0.9900 . ? N33 C34 1.513(19) . ? N33 H33A 0.9001 . ? N33 H33B 0.9001 . ? C34 C35 1.48(2) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C38 1.40(2) . ? C35 C36 1.40(2) . ? C36 C37 1.38(2) . ? C36 H36 0.9500 . ? C37 C40 1.40(2) . ? C37 H37 0.9500 . ? C38 C39 1.40(2) . ? C38 H38 0.9500 . ? C39 C40 1.41(2) . ? C39 H39 0.9500 . ? C40 C41 1.48(2) . ? C41 N42 1.49(2) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? N42 C43 1.486(19) . ? N42 H42A 0.9200 . ? N42 H42B 0.9200 . ? C43 C44 1.49(2) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? S1A O3A 1.448(16) . ? S1A O2A 1.453(15) . ? S1A O1A 1.484(14) . ? S1A O4A 1.484(17) . ? S1B O4B 1.455(14) . ? S1B O3B 1.461(14) . ? S1B O2B 1.481(14) . ? S1B O1B 1.504(13) . ? S1C O2C 1.452(14) . ? S1C O3C 1.457(15) . ? S1C O1C 1.482(13) . ? S1C O4C 1.491(14) . ? O1S C2S 1.44(2) . ? O1S H1S 0.9000 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? O1T H1T1 0.9001 . ? O1T H1T2 0.9000 . ? O2T H2T1 0.9000 . ? O2T H2T2 0.9000 . ? O3T H3T1 0.9000 . ? O3T H3T2 0.9001 . ? O4T H4T1 0.9000 . ? O4T H4T2 0.8999 . ? O5T H5T1 0.9870 . ? O5T H5T2 0.8363 . ? O6T H6T1 0.8999 . ? O6T H6T2 0.8999 . ? O7T H7T1 0.8996 . ? O7T H7T2 0.9001 . ? O8T H8T1 0.8999 . ? O8T H8T2 0.9000 . ? O9T H9T1 0.9001 . ? O9T H9T2 0.9000 . ? O10T H10T 0.9000 . ? O10T H10U 0.9000 . ? O11T H11T 0.9002 . ? O11T H11U 0.8999 . ? O12T H12T 0.8999 . ? O12T H12U 0.8999 . ? O13T H13T 0.8502 . ? O13T H13U 0.8494 . ? 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 C31' N1 C30' 112.2(17) . . ? C31 N1 C30 105.3(13) . . ? C31' N1 C2' 101.0(13) . . ? C30' N1 C2' 114.9(14) . . ? C31 N1 C2 114.5(12) . . ? C30 N1 C2 107.9(13) . . ? N1 C2 C3 111.7(10) . . ? N1 C2 H2A 109.3 . . ? C3 C2 H2A 109.3 . . ? N1 C2 H2B 109.3 . . ? C3 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? N4 C3 C2 112.8(8) . . ? N4 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? N4 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? N1 C2' C3' 112.7(12) . . ? N1 C2' H2C 108.2 . . ? C3' C2' H2C 108.5 . . ? N1 C2' H2D 110.3 . . ? C3' C2' H2D 109.2 . . ? H2C C2' H2D 107.8 . . ? N4 C3' C2' 113.9(8) . . ? N4 C3' H3C 108.8 . . ? C2' C3' H3C 108.8 . . ? N4 C3' H3D 108.8 . . ? C2' C3' H3D 108.8 . . ? H3C C3' H3D 107.7 . . ? C3' N4 C5 113.5(14) . . ? C3 N4 C5 113.7(14) . . ? C3' N4 H4A 100.6 . . ? C3 N4 H4A 108.2 . . ? C5 N4 H4A 108.4 . . ? C3' N4 H4B 116.6 . . ? C3 N4 H4B 109.4 . . ? C5 N4 H4B 109.0 . . ? H4A N4 H4B 108.0 . . ? N4 C5 C6 110.3(17) . . ? N4 C5 H5A 109.6 . . ? C6 C5 H5A 109.6 . . ? N4 C5 H5B 109.6 . . ? C6 C5 H5B 109.6 . . ? H5A C5 H5B 108.1 . . ? C9 C6 C7 119(2) . . ? C9 C6 C5 119(2) . . ? C7 C6 C5 122(2) . . ? C8 C7 C6 119(2) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C7 C8 C11 124(2) . . ? C7 C8 H8 118.2 . . ? C11 C8 H8 118.2 . . ? C10 C9 C6 121(2) . . ? C10 C9 H9 119.5 . . ? C6 C9 H9 119.5 . . ? C9 C10 C11 122(2) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C8 C11 C10 116(2) . . ? C8 C11 C12 123(2) . . ? C10 C11 C12 122(2) . . ? C11 C12 N13 112.3(16) . . ? C11 C12 H12A 109.1 . . ? N13 C12 H12A 109.1 . . ? C11 C12 H12B 109.1 . . ? N13 C12 H12B 109.1 . . ? H12A C12 H12B 107.9 . . ? C14 N13 C12 110.7(15) . . ? C14 N13 H13A 109.5 . . ? C12 N13 H13A 109.5 . . ? C14 N13 H13B 109.5 . . ? C12 N13 H13B 109.5 . . ? H13A N13 H13B 108.1 . . ? N13 C14 C15 111.2(15) . . ? N13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? N13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? N16 C15 C14 112.0(15) . . ? N16 C15 H15A 109.2 . . ? C14 C15 H15A 109.2 . . ? N16 C15 H15B 109.2 . . ? C14 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? C44 N16 C15 109.8(15) . . ? C44 N16 C17 110.6(15) . . ? C15 N16 C17 109.9(15) . . ? N16 C17 C18 115.3(17) . . ? N16 C17 H17A 108.5 . . ? C18 C17 H17A 108.5 . . ? N16 C17 H17B 108.5 . . ? C18 C17 H17B 108.5 . . ? H17A C17 H17B 107.5 . . ? C17 C18 N19 112.7(16) . . ? C17 C18 H18A 109.1 . . ? N19 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? N19 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? C20 N19 C18 115.3(16) . . ? C20 N19 H19A 108.4 . . ? C18 N19 H19A 108.4 . . ? C20 N19 H19B 108.4 . . ? C18 N19 H19B 108.4 . . ? H19A N19 H19B 107.5 . . ? N19 C20 C21 112.6(19) . . ? N19 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? N19 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C24 C21 C22 116(3) . . ? C24 C21 C20 120(2) . . ? C22 C21 C20 124(2) . . ? C23 C22 C21 122(2) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C26 C23 C22 120(3) . . ? C26 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C21 C24 C25 124(3) . . ? C21 C24 H24 117.9 . . ? C25 C24 H24 117.9 . . ? C24 C25 C26 117(2) . . ? C24 C25 H25 121.4 . . ? C26 C25 H25 121.4 . . ? C23 C26 C25 120(2) . . ? C23 C26 C27 122(2) . . ? C25 C26 C27 117(2) . . ? N28 C27 C26 110.5(16) . . ? N28 C27 H27A 109.6 . . ? C26 C27 H27A 109.6 . . ? N28 C27 H27B 109.6 . . ? C26 C27 H27B 109.6 . . ? H27A C27 H27B 108.1 . . ? C29 N28 C27 112.5(12) . . ? C29' N28 H28A 109.8 . . ? C29 N28 H28A 108.5 . . ? C27 N28 H28A 109.5 . . ? C29' N28 H28B 108.5 . . ? C29 N28 H28B 110.0 . . ? C27 N28 H28B 108.2 . . ? H28A N28 H28B 108.1 . . ? N28 C29 C30 113.8(8) . . ? N28 C29 H29A 108.8 . . ? C30 C29 H29A 108.8 . . ? N28 C29 H29B 108.8 . . ? C30 C29 H29B 108.8 . . ? H29A C29 H29B 107.7 . . ? N1 C30 C29 112.6(11) . . ? N1 C30 H30A 109.1 . . ? C29 C30 H30A 109.1 . . ? H2C C30 H30A 105.2 . . ? N1 C30 H30B 109.1 . . ? C29 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? N1 C31 C32 112.8(11) . . ? N1 C31 H31A 109.0 . . ? C32 C31 H31A 109.0 . . ? N1 C31 H31B 109.0 . . ? C32 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? N33 C32 C31 113.9(8) . . ? N33 C32 H32A 108.8 . . ? C31 C32 H32A 108.8 . . ? N33 C32 H32B 108.8 . . ? C31 C32 H32B 108.8 . . ? H32A C32 H32B 107.7 . . ? N28 C29' C30' 113.6(8) . . ? N28 C29' H29C 109.7 . . ? C30' C29' H29C 108.6 . . ? N28 C29' H29D 107.9 . . ? C30' C29' H29D 109.1 . . ? H29C C29' H29D 107.8 . . ? N1 C30' C29' 112.4(11) . . ? N1 C30' H30C 109.1 . . ? C29' C30' H30C 109.1 . . ? N1 C30' H30D 109.1 . . ? C29' C30' H30D 109.1 . . ? H30C C30' H30D 107.9 . . ? N1 C31' C32' 112.4(11) . . ? N1 C31' H31C 109.1 . . ? C32' C31' H31C 109.1 . . ? N1 C31' H31D 109.1 . . ? C32' C31' H31D 109.1 . . ? H31C C31' H31D 107.8 . . ? N33 C32' C31' 113.6(8) . . ? N33 C32' H32C 108.9 . . ? C31' C32' H32C 108.9 . . ? N33 C32' H32D 108.9 . . ? C31' C32' H32D 108.9 . . ? H32C C32' H32D 107.7 . . ? C32' N33 C34 110.6(13) . . ? C32 N33 C34 110.4(13) . . ? C32' N33 H33A 110.6 . . ? C32 N33 H33A 109.6 . . ? C34 N33 H33A 110.3 . . ? C32' N33 H33B 107.7 . . ? C32 N33 H33B 109.0 . . ? C34 N33 H33B 109.0 . . ? H33A N33 H33B 108.6 . . ? C35 C34 N33 115.8(16) . . ? C35 C34 H34A 108.3 . . ? N33 C34 H34A 108.3 . . ? C35 C34 H34B 108.3 . . ? N33 C34 H34B 108.3 . . ? H34A C34 H34B 107.4 . . ? C38 C35 C36 116(2) . . ? C38 C35 C34 122(2) . . ? C36 C35 C34 121(2) . . ? C37 C36 C35 124(2) . . ? C37 C36 H36 118.1 . . ? C35 C36 H36 118.1 . . ? C36 C37 C40 120(3) . . ? C36 C37 H37 119.8 . . ? C40 C37 H37 119.8 . . ? C35 C38 C39 120(2) . . ? C35 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C38 C39 C40 123(2) . . ? C38 C39 H39 118.5 . . ? C40 C39 H39 118.5 . . ? C39 C40 C37 116(2) . . ? C39 C40 C41 119(2) . . ? C37 C40 C41 124(2) . . ? C40 C41 N42 112.0(17) . . ? C40 C41 H41A 109.2 . . ? N42 C41 H41A 109.2 . . ? C40 C41 H41B 109.2 . . ? N42 C41 H41B 109.2 . . ? H41A C41 H41B 107.9 . . ? C43 N42 C41 114.8(15) . . ? C43 N42 H42A 108.6 . . ? C41 N42 H42A 108.6 . . ? C43 N42 H42B 108.6 . . ? C41 N42 H42B 108.6 . . ? H42A N42 H42B 107.6 . . ? C44 C43 N42 113.0(17) . . ? C44 C43 H43A 109.0 . . ? N42 C43 H43A 109.0 . . ? C44 C43 H43B 109.0 . . ? N42 C43 H43B 109.0 . . ? H43A C43 H43B 107.8 . . ? N16 C44 C43 110.6(17) . . ? N16 C44 H44A 109.5 . . ? C43 C44 H44A 109.5 . . ? N16 C44 H44B 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? O3A S1A O2A 110.4(12) . . ? O3A S1A O1A 110.5(11) . . ? O2A S1A O1A 108.4(11) . . ? O3A S1A O4A 109.7(12) . . ? O2A S1A O4A 109.2(11) . . ? O1A S1A O4A 108.5(11) . . ? O4B S1B O3B 112.6(10) . . ? O4B S1B O2B 110.1(10) . . ? O3B S1B O2B 108.8(9) . . ? O4B S1B O1B 108.9(9) . . ? O3B S1B O1B 107.2(8) . . ? O2B S1B O1B 109.0(9) . . ? O2C S1C O3C 110.2(9) . . ? O2C S1C O1C 110.4(9) . . ? O3C S1C O1C 108.7(9) . . ? O2C S1C O4C 111.5(10) . . ? O3C S1C O4C 108.2(10) . . ? O1C S1C O4C 107.7(9) . . ? C2S O1S H1S 110.8 . . ? O1S C2S H2SA 109.4 . . ? O1S C2S H2SB 109.6 . . ? H2SA C2S H2SB 109.5 . . ? O1S C2S H2SC 109.4 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? H1T1 O1T H1T2 81.6 . . ? H2T1 O2T H2T2 86.5 . . ? H3T1 O3T H3T2 125.5 . . ? H4T1 O4T H4T2 120.2 . . ? H5T1 O5T H5T2 116.3 . . ? H6T1 O6T H6T2 133.3 . . ? H7T1 O7T H7T2 105.1 . . ? H8T1 O8T H8T2 108.2 . . ? O12U O9T H9T1 116.5 . . ? O12U O9T H9T2 115.4 . . ? H9T1 O9T H9T2 104.3 . . ? H10T O10T H10U 95.2 . . ? H11T O11T H11U 113.3 . . ? H12T O12T H12U 138.0 . . ? O9T O12U H12T 151.1 . . ? H13T O13T H13U 144.2 . . ? 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 C31 N1 C2 C3 -170.3(13) . . . . ? C30 N1 C2 C3 72.8(18) . . . . ? N1 C2 C3 N4 55.7(17) . . . . ? C31' N1 C2' C3' -70.6(19) . . . . ? C30' N1 C2' C3' 168.4(15) . . . . ? N1 C2' C3' N4 -52(2) . . . . ? C2' C3' N4 C5 -152.4(18) . . . . ? C2 C3 N4 C5 153.7(14) . . . . ? C3' N4 C5 C6 -173.1(18) . . . . ? C3 N4 C5 C6 177.4(17) . . . . ? N4 C5 C6 C9 -76(2) . . . . ? N4 C5 C6 C7 101(2) . . . . ? C9 C6 C7 C8 0(3) . . . . ? C5 C6 C7 C8 -177.6(18) . . . . ? C6 C7 C8 C11 1(3) . . . . ? C7 C6 C9 C10 -1(3) . . . . ? C5 C6 C9 C10 176.7(19) . . . . ? C6 C9 C10 C11 1(3) . . . . ? C7 C8 C11 C10 -1(3) . . . . ? C7 C8 C11 C12 178.3(18) . . . . ? C9 C10 C11 C8 0(3) . . . . ? C9 C10 C11 C12 -179.5(19) . . . . ? C8 C11 C12 N13 -74(2) . . . . ? C10 C11 C12 N13 106(2) . . . . ? C11 C12 N13 C14 -177.0(16) . . . . ? C12 N13 C14 C15 -176.6(15) . . . . ? N13 C14 C15 N16 -64(2) . . . . ? C14 C15 N16 C44 158.0(15) . . . . ? C14 C15 N16 C17 -80.1(19) . . . . ? C44 N16 C17 C18 -75(2) . . . . ? C15 N16 C17 C18 163.4(15) . . . . ? N16 C17 C18 N19 -55(2) . . . . ? C17 C18 N19 C20 -158.5(16) . . . . ? C18 N19 C20 C21 -164.8(16) . . . . ? N19 C20 C21 C24 145.8(18) . . . . ? N19 C20 C21 C22 -29(3) . . . . ? C24 C21 C22 C23 0(3) . . . . ? C20 C21 C22 C23 175.1(19) . . . . ? C21 C22 C23 C26 0(3) . . . . ? C22 C21 C24 C25 -3(3) . . . . ? C20 C21 C24 C25 -178.5(18) . . . . ? C21 C24 C25 C26 6(3) . . . . ? C22 C23 C26 C25 3(3) . . . . ? C22 C23 C26 C27 -177.3(17) . . . . ? C24 C25 C26 C23 -6(3) . . . . ? C24 C25 C26 C27 174.4(16) . . . . ? C23 C26 C27 N28 36(2) . . . . ? C25 C26 C27 N28 -144.3(17) . . . . ? C26 C27 N28 C29' 171.6(16) . . . . ? C26 C27 N28 C29 169.9(18) . . . . ? C27 N28 C29 C30 154.2(17) . . . . ? C31 N1 C30 C29 69(2) . . . . ? C2 N1 C30 C29 -168.6(15) . . . . ? N28 C29 C30 N1 54(2) . . . . ? C30 N1 C31 C32 -179.8(14) . . . . ? C2 N1 C31 C32 62(2) . . . . ? N1 C31 C32 N33 61(2) . . . . ? C2' N1 C30' C29' -70(2) . . . . ? N28 C29' C30' N1 -55(2) . . . . ? C30' N1 C31' C32' -62(2) . . . . ? C2' N1 C31' C32' 175.1(16) . . . . ? N1 C31' C32' N33 -62(2) . . . . ? C31' C32' N33 C34 -154.2(18) . . . . ? C31 C32 N33 C34 148.7(15) . . . . ? C32' N33 C34 C35 177(2) . . . . ? C32 N33 C34 C35 178.6(18) . . . . ? N33 C34 C35 C38 -85(2) . . . . ? N33 C34 C35 C36 99(2) . . . . ? C38 C35 C36 C37 -1(3) . . . . ? C34 C35 C36 C37 175.1(18) . . . . ? C35 C36 C37 C40 -1(3) . . . . ? C36 C35 C38 C39 0(3) . . . . ? C34 C35 C38 C39 -176.1(18) . . . . ? C35 C38 C39 C40 3(3) . . . . ? C38 C39 C40 C37 -5(3) . . . . ? C38 C39 C40 C41 171.2(19) . . . . ? C36 C37 C40 C39 4(3) . . . . ? C36 C37 C40 C41 -172.1(19) . . . . ? C39 C40 C41 N42 127.4(19) . . . . ? C37 C40 C41 N42 -57(3) . . . . ? C40 C41 N42 C43 -58(2) . . . . ? C41 N42 C43 C44 -175.1(17) . . . . ? C15 N16 C44 C43 -75(2) . . . . ? C17 N16 C44 C43 163.3(16) . . . . ? N42 C43 C44 N16 177.9(15) . . . . ? 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 N4 H4A O1A 0.90 1.91 2.806(19) 173.8 . N4 H4B O1B 0.90 1.88 2.727(18) 156.9 . N13 H13B O5T 0.92 1.79 2.702(19) 172.3 . N13 H13A O1S 0.92 2.06 2.86(2) 144.3 . N19 H19B O2T 0.92 2.03 2.896(18) 157.0 . N19 H19A O2B 0.92 1.87 2.784(18) 172.3 3_666 N28 H28A O1C 0.90 1.85 2.753(18) 178.2 . N28 H28A O4C 0.90 2.62 3.148(19) 118.0 . N28 H28B O1B 0.90 1.80 2.697(18) 174.2 . N33 H33A O1C 0.90 1.89 2.789(19) 178.2 . N33 H33A O2C 0.90 2.67 3.227(19) 120.8 . N33 H33B O1A 0.90 1.86 2.763(19) 178.6 . N42 H42A O4C 0.92 2.10 2.86(2) 139.6 3_566 N42 H42A O3C 0.92 2.61 3.46(2) 152.9 3_566 N42 H42B O3A 0.92 1.78 2.70(2) 171.8 2_545 O1S H1S O2T 0.90 1.89 2.790(18) 179.3 . O1T H1T1 O3A 0.90 1.88 2.78(2) 178.9 . O1T H1T2 O4C 0.90 1.84 2.74(2) 178.9 4_575 O2T H2T1 O3C 0.90 2.05 2.952(18) 179.7 . O2T H2T2 O3C 0.90 1.85 2.752(18) 179.5 3_566 O3T H3T1 O3B 0.90 1.80 2.70(2) 178.6 . O3T H3T2 O2A 0.90 2.02 2.92(2) 179.0 3_676 O4T H4T1 O4A 0.90 1.86 2.76(2) 178.1 . O4T H4T2 O7T 0.90 1.73 2.63(2) 177.8 . O5T H5T1 O4T 0.99 1.75 2.703(19) 160.8 2_545 O5T H5T2 O1T 0.84 1.93 2.688(19) 150.3 . O6T H6T1 O2C 0.90 1.86 2.76(2) 179.4 . O6T H6T2 O4T 0.90 1.97 2.80(2) 152.6 3_576 O7T H7T1 O8T 0.90 1.60 2.50(3) 178.6 1_455 O7T H7T2 O13T 0.90 2.05 2.95(3) 175.4 . O8T H8T1 O3T 0.90 1.98 2.88(2) 178.4 . O8T H8T2 O6T 0.90 2.04 2.94(3) 178.8 1_655 O9T H9T1 O2A 0.90 1.75 2.64(3) 170.3 . O9T H9T2 O10T 0.90 1.96 2.86(3) 172.7 3_676 O10T H10T O4B 0.90 1.78 2.68(3) 176.5 . O10T H10U O13T 0.90 1.92 2.81(3) 167.0 4_676 O11T H11T O3T 0.90 1.94 2.84(5) 176.9 . O11T H11U O7T 0.90 1.83 2.73(5) 176.0 1_655 O12T H12T O9T 0.90 2.35 3.25(4) 176.6 . O12T H12U O11T 0.90 1.77 2.67(6) 176.6 . O13T H13T O10T 0.85 1.96 2.81(3) 178.1 4_475 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 30.92 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.696 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.066 #===END # Attachment '- 09077.cif' #============================================================ data_09077 _database_code_depnum_ccdc_archive 'CCDC 755130' #TrackingRef '- 09077.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H56 N8 S3, H S O4, 3.5(S O4), C H4 O, 6(H2 O)' _chemical_formula_sum 'C31 H73 N8 O25 S7.50' _chemical_formula_weight 1198.42 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' _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 11.8698(14) _cell_length_b 14.1475(18) _cell_length_c 16.133(2) _cell_angle_alpha 97.812(7) _cell_angle_beta 96.193(7) _cell_angle_gamma 101.013(8) _cell_volume 2609.5(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1199 _cell_measurement_theta_min 34.5 _cell_measurement_theta_max 68.8 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1270 _exptl_absorpt_coefficient_mu 3.763 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.416 _exptl_absorpt_correction_T_max 0.507 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD Bruker APEX' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35658 _diffrn_reflns_av_R_equivalents 0.0794 _diffrn_reflns_av_sigmaI/netI 0.0750 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.91 _diffrn_reflns_theta_max 69.69 _reflns_number_total 9413 _reflns_number_gt 6712 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART, 1998' _computing_cell_refinement 'Bruker SAINT, 1998' _computing_data_reduction 'Bruker SAINT, 1998' _computing_structure_solution 'SHELXTL (Sheldrick, 2008)' _computing_structure_refinement 'SHELXTL (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _refine_special_details ; Restraints used in refinement: sadi 0.005 s1e o1e s1e o2e s1e o3e s1e o4e sadi 0.010 o1e o2e o1e o3e o1e o4e o2e o3e o2e o4e o3e o4e sadi 0.02 o1w h1w1 o1w h1w2 o2w h2w1 o2w h2w2 o3w h3w1 o3w h3w2 sadi 0.04 h1w1 h1w2 h2w1 h2w2 h3w1 h3w2 ; _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^)+(0.0800P)^2^+2.6000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9413 _refine_ls_number_parameters 712 _refine_ls_number_restraints 39 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1589 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.009 _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 0.37351(10) 0.57381(8) 0.15104(7) 0.0278(2) Uani 1 1 d . . . S2 S 0.86431(9) 0.61359(7) 0.07734(7) 0.0237(2) Uani 1 1 d . . . S3 S 0.87944(8) 0.57296(7) 0.48862(6) 0.0220(2) Uani 1 1 d . . . N1 N 0.7646(3) 0.9177(2) 0.3462(2) 0.0201(7) Uani 1 1 d . . . H1A H 0.7516 0.8501 0.3331 0.024 Uiso 1 1 calc R . . C2 C 0.6575(4) 0.9469(3) 0.3670(3) 0.0245(9) Uani 1 1 d . . . H2A H 0.6691 1.0187 0.3723 0.029 Uiso 1 1 calc R . . H2B H 0.6428 0.9291 0.4227 0.029 Uiso 1 1 calc R . . C3 C 0.5504(3) 0.9011(3) 0.3029(3) 0.0233(8) Uani 1 1 d . . . H3A H 0.4835 0.9277 0.3200 0.028 Uiso 1 1 calc R . . H3B H 0.5639 0.9188 0.2469 0.028 Uiso 1 1 calc R . . N4 N 0.5220(3) 0.7922(2) 0.2957(2) 0.0225(7) Uani 1 1 d . . . H4A H 0.5356 0.7751 0.3483 0.027 Uiso 1 1 calc R . . H4B H 0.5694 0.7657 0.2619 0.027 Uiso 1 1 calc R . . C5 C 0.3974(4) 0.7512(3) 0.2589(3) 0.0249(9) Uani 1 1 d . . . H5A H 0.3467 0.7768 0.2974 0.030 Uiso 1 1 calc R . . H5B H 0.3818 0.7738 0.2042 0.030 Uiso 1 1 calc R . . C6 C 0.3675(4) 0.6417(3) 0.2454(3) 0.0237(8) Uani 1 1 d . . . C7 C 0.3248(4) 0.5828(3) 0.3009(3) 0.0293(10) Uani 1 1 d . . . H7 H 0.3160 0.6068 0.3572 0.035 Uiso 1 1 calc R . . C8 C 0.2956(4) 0.4830(3) 0.2656(3) 0.0299(10) Uani 1 1 d . . . H8 H 0.2635 0.4328 0.2950 0.036 Uiso 1 1 calc R . . C9 C 0.3185(4) 0.4669(3) 0.1854(3) 0.0256(9) Uani 1 1 d . . . C10 C 0.2890(4) 0.3765(4) 0.1195(3) 0.0337(10) Uani 1 1 d . . . H10A H 0.2036 0.3576 0.1056 0.040 Uiso 1 1 calc R . . H10B H 0.3204 0.3929 0.0676 0.040 Uiso 1 1 calc R . . N11 N 0.3326(3) 0.2902(3) 0.1430(3) 0.0410(11) Uani 1 1 d . . . H11A H 0.3205 0.2438 0.0953 0.049 Uiso 1 1 calc R . . H11B H 0.2878 0.2644 0.1809 0.049 Uiso 1 1 calc R . . C12 C 0.4576(4) 0.3059(3) 0.1806(3) 0.0311(10) Uani 1 1 d . . . H12A H 0.4630 0.3054 0.2422 0.037 Uiso 1 1 calc R . . H12B H 0.5001 0.3702 0.1716 0.037 Uiso 1 1 calc R . . C13 C 0.5121(4) 0.2253(3) 0.1394(3) 0.0248(9) Uani 1 1 d . . . H13A H 0.4641 0.1609 0.1429 0.030 Uiso 1 1 calc R . . H13B H 0.5140 0.2304 0.0789 0.030 Uiso 1 1 calc R . . N14 N 0.6298(3) 0.2327(2) 0.1810(2) 0.0215(7) Uani 1 1 d . . . H14A H 0.6620 0.2983 0.2002 0.026 Uiso 1 1 calc R . . C15 C 0.7035(4) 0.1947(3) 0.1228(3) 0.0237(8) Uani 1 1 d . . . H15A H 0.6603 0.1316 0.0899 0.028 Uiso 1 1 calc R . . H15B H 0.7728 0.1824 0.1561 0.028 Uiso 1 1 calc R . . C16 C 0.7426(4) 0.2636(3) 0.0619(3) 0.0255(9) Uani 1 1 d . . . H16A H 0.7913 0.2338 0.0242 0.031 Uiso 1 1 calc R . . H16B H 0.6739 0.2737 0.0264 0.031 Uiso 1 1 calc R . . N17 N 0.8102(3) 0.3598(3) 0.1084(2) 0.0230(7) Uani 1 1 d . . . H17A H 0.8613 0.3499 0.1518 0.028 Uiso 1 1 calc R . . H17B H 0.7605 0.3953 0.1313 0.028 Uiso 1 1 calc R . . C18 C 0.8760(4) 0.4161(3) 0.0500(3) 0.0247(9) Uani 1 1 d . . . H18A H 0.8223 0.4184 -0.0007 0.030 Uiso 1 1 calc R . . H18B H 0.9364 0.3818 0.0314 0.030 Uiso 1 1 calc R . . C19 C 0.9321(4) 0.5183(3) 0.0913(3) 0.0224(8) Uani 1 1 d . . . C20 C 1.0369(4) 0.5508(3) 0.1406(3) 0.0246(9) Uani 1 1 d . . . H20 H 1.0876 0.5093 0.1551 0.029 Uiso 1 1 calc R . . C21 C 1.0619(4) 0.6531(3) 0.1678(3) 0.0247(9) Uani 1 1 d . . . H21 H 1.1309 0.6872 0.2032 0.030 Uiso 1 1 calc R . . C22 C 0.9779(4) 0.6976(3) 0.1384(3) 0.0230(8) Uani 1 1 d . . . C23 C 0.9759(4) 0.8037(3) 0.1542(3) 0.0244(9) Uani 1 1 d . . . H23A H 0.9529 0.8248 0.0999 0.029 Uiso 1 1 calc R . . H23B H 1.0549 0.8412 0.1772 0.029 Uiso 1 1 calc R . . N24 N 0.8933(3) 0.8266(2) 0.2151(2) 0.0209(7) Uani 1 1 d . . . H24A H 0.8185 0.7989 0.1908 0.025 Uiso 1 1 calc R . . H24B H 0.9083 0.8000 0.2630 0.025 Uiso 1 1 calc R . . C25 C 0.9054(4) 0.9347(3) 0.2385(3) 0.0233(8) Uani 1 1 d . . . H25A H 0.9182 0.9659 0.1879 0.028 Uiso 1 1 calc R . . H25B H 0.9743 0.9607 0.2815 0.028 Uiso 1 1 calc R . . C26 C 0.7998(4) 0.9616(3) 0.2728(3) 0.0262(9) Uani 1 1 d . . . H26A H 0.8148 1.0334 0.2886 0.031 Uiso 1 1 calc R . . H26B H 0.7337 0.9427 0.2267 0.031 Uiso 1 1 calc R . . C27 C 0.8574(4) 0.9522(3) 0.4186(3) 0.0252(9) Uani 1 1 d . . . H27A H 0.8669 1.0238 0.4339 0.030 Uiso 1 1 calc R . . H27B H 0.9310 0.9395 0.4005 0.030 Uiso 1 1 calc R . . C28 C 0.8375(4) 0.9061(3) 0.4967(3) 0.0223(8) Uani 1 1 d . . . H28A H 0.9093 0.9252 0.5378 0.027 Uiso 1 1 calc R . . H28B H 0.7757 0.9317 0.5233 0.027 Uiso 1 1 calc R . . N29 N 0.8037(3) 0.7971(2) 0.4776(2) 0.0212(7) Uani 1 1 d . . . H29A H 0.8456 0.7748 0.4372 0.025 Uiso 1 1 calc R . . H29B H 0.7265 0.7792 0.4556 0.025 Uiso 1 1 calc R . . C30 C 0.8238(4) 0.7491(3) 0.5544(3) 0.0228(8) Uani 1 1 d . . . H30A H 0.9070 0.7670 0.5780 0.027 Uiso 1 1 calc R . . H30B H 0.7788 0.7723 0.5982 0.027 Uiso 1 1 calc R . . C31 C 0.7876(4) 0.6408(3) 0.5308(3) 0.0216(8) Uani 1 1 d . . . C32 C 0.6815(4) 0.5842(3) 0.5322(3) 0.0246(9) Uani 1 1 d . . . H32 H 0.6186 0.6089 0.5521 0.030 Uiso 1 1 calc R . . C33 C 0.6750(4) 0.4846(3) 0.5010(3) 0.0240(9) Uani 1 1 d . . . H33 H 0.6076 0.4351 0.4983 0.029 Uiso 1 1 calc R . . C34 C 0.7759(4) 0.4674(3) 0.4751(3) 0.0216(8) Uani 1 1 d . . . C35 C 0.7999(4) 0.3715(3) 0.4374(3) 0.0221(8) Uani 1 1 d . . . H35A H 0.8789 0.3818 0.4211 0.027 Uiso 1 1 calc R . . H35B H 0.7964 0.3271 0.4799 0.027 Uiso 1 1 calc R . . N36 N 0.7132(3) 0.3260(2) 0.3614(2) 0.0205(7) Uani 1 1 d . . . H36A H 0.6399 0.3191 0.3766 0.025 Uiso 1 1 calc R . . H36B H 0.7183 0.3670 0.3216 0.025 Uiso 1 1 calc R . . C37 C 0.7307(4) 0.2287(3) 0.3230(3) 0.0235(8) Uani 1 1 d . . . H37A H 0.7353 0.1866 0.3670 0.028 Uiso 1 1 calc R . . H37B H 0.8044 0.2366 0.2986 0.028 Uiso 1 1 calc R . . C38 C 0.6303(4) 0.1815(3) 0.2544(3) 0.0217(8) Uani 1 1 d . . . H38A H 0.6350 0.1129 0.2359 0.026 Uiso 1 1 calc R . . H38B H 0.5565 0.1812 0.2779 0.026 Uiso 1 1 calc R . . S1A S 1.06422(8) 0.76997(7) 0.39826(6) 0.0207(2) Uani 1 1 d . . . O1A O 1.1151(3) 0.8590(2) 0.3560(2) 0.0305(7) Uani 1 1 d . . . H1AO H 1.183(5) 0.881(4) 0.378(4) 0.037 Uiso 1 1 d . . . O2A O 0.9428(2) 0.7430(2) 0.35628(18) 0.0216(6) Uani 1 1 d . . . O3A O 1.0708(3) 0.8035(2) 0.48812(19) 0.0270(6) Uani 1 1 d . . . O4A O 1.1285(3) 0.6947(2) 0.37790(19) 0.0265(6) Uani 1 1 d . . . S1B S 0.61160(9) 0.74162(8) 0.08344(6) 0.0229(2) Uani 1 1 d . . . O1B O 0.5765(3) 0.6410(2) 0.0382(2) 0.0302(7) Uani 1 1 d . . . O2B O 0.5100(3) 0.7876(2) 0.0829(2) 0.0330(7) Uani 1 1 d . . . O3B O 0.7027(3) 0.7960(3) 0.0407(2) 0.0384(8) Uani 1 1 d . . . O4B O 0.6612(3) 0.7420(2) 0.17185(18) 0.0275(6) Uani 1 1 d . . . S1C S 0.03457(11) 0.23783(9) 0.21094(8) 0.0344(3) Uani 1 1 d . . . O1C O 0.1568(3) 0.2490(3) 0.2424(3) 0.0484(10) Uani 1 1 d . . . O2C O -0.0375(3) 0.1584(3) 0.2389(3) 0.0437(9) Uani 1 1 d . . . O3C O -0.0075(4) 0.3287(3) 0.2234(3) 0.0551(11) Uani 1 1 d . . . O4C O 0.0240(4) 0.2130(3) 0.1119(2) 0.0537(11) Uani 1 1 d . . . S1D S 0.51484(9) 0.79587(8) 0.53801(7) 0.0244(2) Uani 1 1 d . . . O1D O 0.3990(3) 0.8136(3) 0.5162(3) 0.0429(9) Uani 1 1 d . . . O2D O 0.5958(3) 0.8863(2) 0.5814(2) 0.0379(8) Uani 1 1 d . . . O3D O 0.5609(3) 0.7598(2) 0.46024(18) 0.0267(6) Uani 1 1 d . . . O4D O 0.5091(2) 0.7227(2) 0.59516(18) 0.0234(6) Uani 1 1 d . . . S1E S 0.1441(3) 0.0053(2) 0.00906(19) 0.0570(8) Uani 0.50 1 d PD . . O1E O 0.2371(8) 0.0278(6) -0.0403(6) 0.095(4) Uani 0.50 1 d PD . . O2E O 0.1482(7) 0.0890(5) 0.0714(5) 0.065(3) Uani 0.50 1 d PD . . O3E O 0.1584(10) -0.0786(6) 0.0462(6) 0.100(5) Uani 0.50 1 d PD . . O4E O 0.0359(7) -0.0171(8) -0.0467(5) 0.104(5) Uani 0.50 1 d PD . . O1S O 0.7637(3) 0.4756(2) 0.26223(19) 0.0271(6) Uani 1 1 d . . . H1S H 0.834(5) 0.492(4) 0.283(4) 0.033 Uiso 1 1 d . . . C2S C 0.7022(4) 0.5529(3) 0.2763(3) 0.0334(10) Uani 1 1 d . . . H2SA H 0.6211 0.5297 0.2510 0.050 Uiso 1 1 calc R . . H2SB H 0.7376 0.6080 0.2504 0.050 Uiso 1 1 calc R . . H2SC H 0.7061 0.5740 0.3372 0.050 Uiso 1 1 calc R . . O1W O 0.9890(3) 0.5035(3) 0.3289(2) 0.0342(7) Uani 1 1 d D . . H1W1 H 1.026(4) 0.461(3) 0.307(3) 0.041 Uiso 1 1 d D . . H1W2 H 1.047(3) 0.552(3) 0.347(4) 0.041 Uiso 1 1 d D . . O2W O 0.3273(3) 0.9207(2) 0.4091(2) 0.0282(7) Uani 1 1 d D . . H2W1 H 0.362(4) 0.888(3) 0.440(3) 0.034 Uiso 1 1 d D . . H2W2 H 0.363(4) 0.980(2) 0.418(3) 0.034 Uiso 1 1 d D . . O3W O 0.6230(3) 0.4549(2) 0.0693(2) 0.0295(7) Uani 1 1 d D . . H3W1 H 0.615(4) 0.514(2) 0.076(3) 0.035 Uiso 1 1 d D . . H3W2 H 0.561(3) 0.423(3) 0.037(3) 0.035 Uiso 1 1 d D . . O4W O 0.4904(5) 0.9670(3) 0.0706(4) 0.0789(16) Uani 1 1 d . . . H4W1 H 0.4973 0.9055 0.0746 0.095 Uiso 1 1 d R . . H4W2 H 0.4257 0.9639 0.0955 0.095 Uiso 1 1 d R . . O5W O 0.3095(11) 0.9569(7) 0.1375(9) 0.156(7) Uani 0.760(15) 1 d P A 1 O5W' O 0.237(4) 1.045(4) 0.235(3) 0.18(3) Uani 0.240(15) 1 d P A 2 O6W O 0.3098(6) 0.1125(6) 0.2564(3) 0.050(2) Uani 0.81(2) 1 d P B 1 O6W' O 0.234(4) 0.059(2) 0.2621(14) 0.043(13) Uani 0.19(2) 1 d P B 2 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 0.0315(5) 0.0286(5) 0.0229(5) 0.0036(4) 0.0059(4) 0.0041(5) S2 0.0221(5) 0.0222(5) 0.0276(5) 0.0060(4) 0.0018(4) 0.0059(4) S3 0.0206(5) 0.0199(5) 0.0257(5) 0.0045(4) 0.0024(4) 0.0043(4) N1 0.0216(17) 0.0158(15) 0.0225(17) 0.0037(13) 0.0010(13) 0.0032(14) C2 0.025(2) 0.022(2) 0.027(2) 0.0060(17) 0.0058(17) 0.0052(18) C3 0.0202(19) 0.020(2) 0.031(2) 0.0079(17) 0.0056(16) 0.0046(17) N4 0.0219(17) 0.0216(17) 0.0235(17) 0.0038(14) 0.0018(14) 0.0038(15) C5 0.023(2) 0.021(2) 0.030(2) 0.0063(17) -0.0005(17) 0.0034(18) C6 0.0208(19) 0.026(2) 0.024(2) 0.0046(17) 0.0022(16) 0.0048(18) C7 0.034(2) 0.033(2) 0.020(2) 0.0083(18) 0.0056(17) -0.002(2) C8 0.032(2) 0.031(2) 0.028(2) 0.0072(19) 0.0062(18) 0.007(2) C9 0.0205(19) 0.025(2) 0.031(2) 0.0014(18) 0.0034(16) 0.0053(18) C10 0.033(2) 0.034(3) 0.034(3) 0.002(2) 0.008(2) 0.005(2) N11 0.025(2) 0.025(2) 0.069(3) -0.005(2) 0.005(2) 0.0067(18) C12 0.024(2) 0.022(2) 0.045(3) -0.0020(19) 0.0048(19) 0.0031(19) C13 0.024(2) 0.022(2) 0.027(2) 0.0020(17) 0.0025(17) 0.0046(18) N14 0.0218(17) 0.0168(16) 0.0254(18) 0.0027(14) 0.0036(14) 0.0030(14) C15 0.025(2) 0.0193(19) 0.027(2) 0.0035(16) 0.0067(17) 0.0044(17) C16 0.027(2) 0.022(2) 0.026(2) 0.0014(17) 0.0085(17) 0.0001(18) N17 0.0270(18) 0.0198(17) 0.0232(17) 0.0040(14) 0.0094(14) 0.0038(15) C18 0.026(2) 0.025(2) 0.026(2) 0.0080(17) 0.0111(17) 0.0052(18) C19 0.026(2) 0.022(2) 0.022(2) 0.0072(16) 0.0092(16) 0.0031(18) C20 0.023(2) 0.028(2) 0.026(2) 0.0079(17) 0.0086(16) 0.0085(18) C21 0.022(2) 0.028(2) 0.024(2) 0.0035(17) 0.0052(16) 0.0050(18) C22 0.023(2) 0.026(2) 0.022(2) 0.0041(16) 0.0100(16) 0.0066(18) C23 0.024(2) 0.026(2) 0.026(2) 0.0047(17) 0.0110(16) 0.0054(18) N24 0.0197(16) 0.0198(17) 0.0238(17) 0.0049(13) 0.0050(13) 0.0036(14) C25 0.028(2) 0.0179(19) 0.025(2) 0.0053(16) 0.0071(16) 0.0036(17) C26 0.028(2) 0.025(2) 0.029(2) 0.0094(18) 0.0078(17) 0.0084(19) C27 0.021(2) 0.0195(19) 0.033(2) 0.0016(17) 0.0009(17) 0.0007(17) C28 0.026(2) 0.0143(18) 0.025(2) -0.0003(15) 0.0030(16) 0.0038(17) N29 0.0202(16) 0.0173(16) 0.0252(18) 0.0045(14) 0.0032(13) 0.0011(14) C30 0.029(2) 0.0183(19) 0.020(2) 0.0026(16) 0.0005(16) 0.0046(17) C31 0.025(2) 0.021(2) 0.0198(19) 0.0043(16) 0.0033(16) 0.0067(18) C32 0.025(2) 0.024(2) 0.027(2) 0.0058(17) 0.0090(17) 0.0050(18) C33 0.024(2) 0.021(2) 0.027(2) 0.0036(17) 0.0059(16) 0.0043(18) C34 0.023(2) 0.022(2) 0.0209(19) 0.0089(16) 0.0006(15) 0.0045(17) C35 0.0217(19) 0.0200(19) 0.024(2) 0.0058(16) 0.0000(16) 0.0038(17) N36 0.0203(16) 0.0194(16) 0.0222(17) 0.0049(13) 0.0022(13) 0.0043(14) C37 0.028(2) 0.0173(19) 0.027(2) 0.0057(16) 0.0041(17) 0.0070(18) C38 0.027(2) 0.0154(18) 0.024(2) 0.0053(15) 0.0058(16) 0.0041(17) S1A 0.0200(5) 0.0210(5) 0.0222(5) 0.0056(4) 0.0029(4) 0.0056(4) O1A 0.0232(15) 0.0301(16) 0.0380(18) 0.0173(14) 0.0009(13) -0.0011(14) O2A 0.0188(13) 0.0208(14) 0.0252(15) 0.0051(11) 0.0038(11) 0.0028(12) O3A 0.0317(16) 0.0276(15) 0.0213(15) -0.0003(12) 0.0022(12) 0.0093(14) O4A 0.0273(15) 0.0291(16) 0.0254(15) 0.0040(12) 0.0025(12) 0.0127(14) S1B 0.0229(5) 0.0250(5) 0.0199(5) 0.0027(4) 0.0024(4) 0.0036(4) O1B 0.0295(16) 0.0278(16) 0.0292(16) -0.0023(13) 0.0012(13) 0.0023(14) O2B 0.0335(17) 0.0380(18) 0.0308(17) 0.0066(14) 0.0031(13) 0.0159(15) O3B 0.0365(19) 0.0365(19) 0.042(2) 0.0115(16) 0.0154(15) -0.0025(16) O4B 0.0269(15) 0.0366(17) 0.0181(14) 0.0010(12) -0.0010(11) 0.0090(14) S1C 0.0322(6) 0.0295(6) 0.0407(7) 0.0120(5) 0.0020(5) 0.0016(5) O1C 0.036(2) 0.061(3) 0.046(2) 0.026(2) -0.0002(16) -0.0022(19) O2C 0.0355(19) 0.0304(18) 0.068(3) 0.0185(18) 0.0171(18) 0.0017(16) O3C 0.073(3) 0.0260(18) 0.060(3) 0.0056(17) -0.016(2) 0.0102(19) O4C 0.052(2) 0.068(3) 0.034(2) 0.0062(19) -0.0031(17) 0.001(2) S1D 0.0234(5) 0.0221(5) 0.0301(5) 0.0097(4) 0.0087(4) 0.0043(4) O1D 0.0294(18) 0.053(2) 0.059(2) 0.0347(19) 0.0168(16) 0.0178(17) O2D 0.047(2) 0.0207(15) 0.042(2) 0.0036(14) 0.0125(16) -0.0043(15) O3D 0.0244(15) 0.0316(16) 0.0230(15) 0.0071(12) 0.0054(12) 0.0002(13) O4D 0.0245(14) 0.0228(14) 0.0255(15) 0.0097(12) 0.0088(11) 0.0039(12) S1E 0.089(2) 0.0325(13) 0.0477(17) 0.0033(12) 0.0166(16) 0.0058(15) O1E 0.135(11) 0.039(5) 0.115(10) -0.012(6) 0.052(9) 0.026(6) O2E 0.070(6) 0.077(6) 0.047(5) -0.010(5) 0.006(4) 0.028(5) O3E 0.188(15) 0.050(6) 0.092(9) 0.032(6) 0.083(10) 0.047(8) O4E 0.108(10) 0.119(11) 0.061(7) 0.013(7) -0.010(7) -0.025(9) O1S 0.0332(17) 0.0227(15) 0.0247(15) 0.0058(12) 0.0032(13) 0.0032(14) C2S 0.043(3) 0.027(2) 0.031(2) 0.0064(19) -0.001(2) 0.011(2) O1W 0.0373(18) 0.0328(18) 0.0318(17) 0.0042(14) 0.0088(14) 0.0042(15) O2W 0.0250(16) 0.0226(15) 0.0365(18) 0.0084(13) 0.0012(13) 0.0026(13) O3W 0.0264(16) 0.0283(16) 0.0309(17) 0.0011(13) -0.0014(13) 0.0042(14) O4W 0.102(4) 0.030(2) 0.094(4) -0.015(2) 0.021(3) 0.002(3) O5W 0.200(13) 0.066(6) 0.209(14) -0.016(7) 0.124(11) 0.019(7) O5W' 0.13(4) 0.22(6) 0.14(4) 0.10(4) -0.06(3) -0.10(3) O6W 0.057(4) 0.062(5) 0.038(3) 0.013(3) 0.012(2) 0.022(4) O6W' 0.11(3) 0.027(14) 0.010(9) 0.009(7) 0.005(10) 0.05(2) _geom_special_details ; ; 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 1.702(4) . ? S1 C9 1.718(5) . ? S2 C19 1.724(4) . ? S2 C22 1.727(4) . ? S3 C34 1.715(4) . ? S3 C31 1.718(4) . ? N1 C2 1.468(5) . ? N1 C26 1.473(5) . ? N1 C27 1.475(5) . ? N1 H1A 0.9300 . ? C2 C3 1.525(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 N4 1.498(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? N4 C5 1.505(5) . ? N4 H4A 0.9200 . ? N4 H4B 0.9200 . ? C5 C6 1.502(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.375(6) . ? C7 C8 1.411(7) . ? C7 H7 0.9500 . ? C8 C9 1.349(6) . ? C8 H8 0.9500 . ? C9 C10 1.505(6) . ? C10 N11 1.492(6) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? N11 C12 1.504(6) . ? N11 H11A 0.9200 . ? N11 H11B 0.9200 . ? C12 C13 1.526(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 N14 1.462(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? N14 C15 1.468(5) . ? N14 C38 1.469(5) . ? N14 H14A 0.9300 . ? C15 C16 1.522(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 N17 1.495(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? N17 C18 1.501(5) . ? N17 H17A 0.9200 . ? N17 H17B 0.9200 . ? C18 C19 1.502(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.364(6) . ? C20 C21 1.419(6) . ? C20 H20 0.9500 . ? C21 C22 1.354(6) . ? C21 H21 0.9500 . ? C22 C23 1.493(6) . ? C23 N24 1.508(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? N24 C25 1.501(5) . ? N24 H24A 0.9200 . ? N24 H24B 0.9200 . ? C25 C26 1.516(6) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.516(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 N29 1.497(5) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? N29 C30 1.510(5) . ? N29 H29A 0.9200 . ? N29 H29B 0.9200 . ? C30 C31 1.494(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.363(6) . ? C32 C33 1.414(6) . ? C32 H32 0.9500 . ? C33 C34 1.365(6) . ? C33 H33 0.9500 . ? C34 C35 1.501(6) . ? C35 N36 1.496(5) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? N36 C37 1.493(5) . ? N36 H36A 0.9200 . ? N36 H36B 0.9200 . ? C37 C38 1.518(6) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? S1A O4A 1.446(3) . ? S1A O3A 1.452(3) . ? S1A O2A 1.481(3) . ? S1A O1A 1.564(3) . ? O1A H1AO 0.83(6) . ? S1B O1B 1.468(3) . ? S1B O2B 1.476(3) . ? S1B O4B 1.482(3) . ? S1B O3B 1.491(3) . ? S1C O2C 1.432(4) . ? S1C O1C 1.456(4) . ? S1C O3C 1.463(4) . ? S1C O4C 1.575(4) . ? S1D O1D 1.459(3) . ? S1D O4D 1.474(3) . ? S1D O2D 1.481(3) . ? S1D O3D 1.488(3) . ? S1E O3E 1.430(6) . ? S1E O2E 1.436(6) . ? S1E O1E 1.441(6) . ? S1E O4E 1.441(6) . ? O1S C2S 1.433(6) . ? O1S H1S 0.84(6) . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? O1W H1W1 0.87(3) . ? O1W H1W2 0.86(3) . ? O2W H2W1 0.85(3) . ? O2W H2W2 0.85(3) . ? O3W H3W1 0.86(3) . ? O3W H3W2 0.86(3) . ? O4W H4W1 0.9001 . ? O4W H4W2 0.9000 . ? 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 C9 92.2(2) . . ? C19 S2 C22 92.0(2) . . ? C34 S3 C31 91.9(2) . . ? C2 N1 C26 108.7(3) . . ? C2 N1 C27 110.1(3) . . ? C26 N1 C27 109.4(3) . . ? C2 N1 H1A 109.5 . . ? C26 N1 H1A 109.5 . . ? C27 N1 H1A 109.5 . . ? N1 C2 C3 114.7(3) . . ? N1 C2 H2A 108.6 . . ? C3 C2 H2A 108.6 . . ? N1 C2 H2B 108.6 . . ? C3 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? N4 C3 C2 111.8(3) . . ? N4 C3 H3A 109.3 . . ? C2 C3 H3A 109.3 . . ? N4 C3 H3B 109.3 . . ? C2 C3 H3B 109.3 . . ? H3A C3 H3B 107.9 . . ? C3 N4 C5 111.1(3) . . ? C3 N4 H4A 109.4 . . ? C5 N4 H4A 109.4 . . ? C3 N4 H4B 109.4 . . ? C5 N4 H4B 109.4 . . ? H4A N4 H4B 108.0 . . ? C6 C5 N4 112.8(3) . . ? C6 C5 H5A 109.0 . . ? N4 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? N4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? C7 C6 C5 127.4(4) . . ? C7 C6 S1 110.7(3) . . ? C5 C6 S1 121.7(3) . . ? C6 C7 C8 113.1(4) . . ? C6 C7 H7 123.5 . . ? C8 C7 H7 123.5 . . ? C9 C8 C7 112.4(4) . . ? C9 C8 H8 123.8 . . ? C7 C8 H8 123.8 . . ? C8 C9 C10 131.6(4) . . ? C8 C9 S1 111.7(3) . . ? C10 C9 S1 116.1(3) . . ? N11 C10 C9 116.0(4) . . ? N11 C10 H10A 108.3 . . ? C9 C10 H10A 108.3 . . ? N11 C10 H10B 108.3 . . ? C9 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C10 N11 C12 117.8(4) . . ? C10 N11 H11A 107.9 . . ? C12 N11 H11A 107.9 . . ? C10 N11 H11B 107.9 . . ? C12 N11 H11B 107.9 . . ? H11A N11 H11B 107.2 . . ? N11 C12 C13 109.8(4) . . ? N11 C12 H12A 109.7 . . ? C13 C12 H12A 109.7 . . ? N11 C12 H12B 109.7 . . ? C13 C12 H12B 109.7 . . ? H12A C12 H12B 108.2 . . ? N14 C13 C12 110.9(4) . . ? N14 C13 H13A 109.5 . . ? C12 C13 H13A 109.5 . . ? N14 C13 H13B 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 108.0 . . ? C13 N14 C15 111.9(3) . . ? C13 N14 C38 111.6(3) . . ? C15 N14 C38 109.4(3) . . ? C13 N14 H14A 107.9 . . ? C15 N14 H14A 107.9 . . ? C38 N14 H14A 107.9 . . ? N14 C15 C16 113.3(3) . . ? N14 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? N14 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N17 C16 C15 111.2(3) . . ? N17 C16 H16A 109.4 . . ? C15 C16 H16A 109.4 . . ? N17 C16 H16B 109.4 . . ? C15 C16 H16B 109.4 . . ? H16A C16 H16B 108.0 . . ? C16 N17 C18 110.6(3) . . ? C16 N17 H17A 109.5 . . ? C18 N17 H17A 109.5 . . ? C16 N17 H17B 109.5 . . ? C18 N17 H17B 109.5 . . ? H17A N17 H17B 108.1 . . ? N17 C18 C19 112.2(3) . . ? N17 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? N17 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C20 C19 C18 128.5(4) . . ? C20 C19 S2 111.0(3) . . ? C18 C19 S2 120.4(3) . . ? C19 C20 C21 112.6(4) . . ? C19 C20 H20 123.7 . . ? C21 C20 H20 123.7 . . ? C22 C21 C20 113.5(4) . . ? C22 C21 H21 123.3 . . ? C20 C21 H21 123.3 . . ? C21 C22 C23 127.7(4) . . ? C21 C22 S2 110.8(3) . . ? C23 C22 S2 121.4(3) . . ? C22 C23 N24 112.4(3) . . ? C22 C23 H23A 109.1 . . ? N24 C23 H23A 109.1 . . ? C22 C23 H23B 109.1 . . ? N24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C25 N24 C23 110.9(3) . . ? C25 N24 H24A 109.5 . . ? C23 N24 H24A 109.5 . . ? C25 N24 H24B 109.5 . . ? C23 N24 H24B 109.5 . . ? H24A N24 H24B 108.1 . . ? N24 C25 C26 112.6(3) . . ? N24 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? N24 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? N1 C26 C25 116.5(3) . . ? N1 C26 H26A 108.2 . . ? C25 C26 H26A 108.2 . . ? N1 C26 H26B 108.2 . . ? C25 C26 H26B 108.2 . . ? H26A C26 H26B 107.3 . . ? N1 C27 C28 115.2(3) . . ? N1 C27 H27A 108.5 . . ? C28 C27 H27A 108.5 . . ? N1 C27 H27B 108.5 . . ? C28 C27 H27B 108.5 . . ? H27A C27 H27B 107.5 . . ? N29 C28 C27 112.7(3) . . ? N29 C28 H28A 109.1 . . ? C27 C28 H28A 109.1 . . ? N29 C28 H28B 109.1 . . ? C27 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? C28 N29 C30 112.9(3) . . ? C28 N29 H29A 109.0 . . ? C30 N29 H29A 109.0 . . ? C28 N29 H29B 109.0 . . ? C30 N29 H29B 109.0 . . ? H29A N29 H29B 107.8 . . ? C31 C30 N29 110.0(3) . . ? C31 C30 H30A 109.7 . . ? N29 C30 H30A 109.7 . . ? C31 C30 H30B 109.7 . . ? N29 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C32 C31 C30 127.4(4) . . ? C32 C31 S3 111.3(3) . . ? C30 C31 S3 121.0(3) . . ? C31 C32 C33 112.7(4) . . ? C31 C32 H32 123.7 . . ? C33 C32 H32 123.7 . . ? C34 C33 C32 112.7(4) . . ? C34 C33 H33 123.6 . . ? C32 C33 H33 123.6 . . ? C33 C34 C35 127.4(4) . . ? C33 C34 S3 111.4(3) . . ? C35 C34 S3 121.2(3) . . ? N36 C35 C34 110.5(3) . . ? N36 C35 H35A 109.6 . . ? C34 C35 H35A 109.6 . . ? N36 C35 H35B 109.6 . . ? C34 C35 H35B 109.6 . . ? H35A C35 H35B 108.1 . . ? C37 N36 C35 112.6(3) . . ? C37 N36 H36A 109.1 . . ? C35 N36 H36A 109.1 . . ? C37 N36 H36B 109.1 . . ? C35 N36 H36B 109.1 . . ? H36A N36 H36B 107.8 . . ? N36 C37 C38 109.3(3) . . ? N36 C37 H37A 109.8 . . ? C38 C37 H37A 109.8 . . ? N36 C37 H37B 109.8 . . ? C38 C37 H37B 109.8 . . ? H37A C37 H37B 108.3 . . ? N14 C38 C37 112.3(3) . . ? N14 C38 H38A 109.1 . . ? C37 C38 H38A 109.1 . . ? N14 C38 H38B 109.1 . . ? C37 C38 H38B 109.1 . . ? H38A C38 H38B 107.9 . . ? O4A S1A O3A 114.18(18) . . ? O4A S1A O2A 112.49(18) . . ? O3A S1A O2A 111.53(18) . . ? O4A S1A O1A 107.53(19) . . ? O3A S1A O1A 108.24(19) . . ? O2A S1A O1A 101.98(17) . . ? S1A O1A H1AO 109(4) . . ? O1B S1B O2B 109.5(2) . . ? O1B S1B O4B 110.05(19) . . ? O2B S1B O4B 109.52(19) . . ? O1B S1B O3B 108.4(2) . . ? O2B S1B O3B 110.8(2) . . ? O4B S1B O3B 108.5(2) . . ? O2C S1C O1C 112.8(2) . . ? O2C S1C O3C 113.3(3) . . ? O1C S1C O3C 113.7(3) . . ? O2C S1C O4C 107.2(2) . . ? O1C S1C O4C 106.0(2) . . ? O3C S1C O4C 102.7(3) . . ? O1D S1D O4D 109.19(19) . . ? O1D S1D O2D 111.2(2) . . ? O4D S1D O2D 108.46(19) . . ? O1D S1D O3D 110.0(2) . . ? O4D S1D O3D 109.71(18) . . ? O2D S1D O3D 108.25(19) . . ? O3E S1E O2E 112.2(4) . . ? O3E S1E O1E 108.1(4) . . ? O2E S1E O1E 108.4(4) . . ? O3E S1E O4E 109.3(4) . . ? O2E S1E O4E 110.2(4) . . ? O1E S1E O4E 108.4(4) . . ? C2S O1S H1S 113(4) . . ? O1S C2S H2SA 109.5 . . ? O1S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? O1S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? H1W1 O1W H1W2 99(4) . . ? H2W1 O2W H2W2 110(4) . . ? H3W1 O3W H3W2 105(4) . . ? H4W1 O4W H4W2 95.4 . . ? 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 C26 N1 C2 C3 69.9(4) . . . . ? C27 N1 C2 C3 -170.3(3) . . . . ? N1 C2 C3 N4 62.3(5) . . . . ? C2 C3 N4 C5 159.2(3) . . . . ? C3 N4 C5 C6 176.2(3) . . . . ? N4 C5 C6 C7 91.3(5) . . . . ? N4 C5 C6 S1 -93.8(4) . . . . ? C9 S1 C6 C7 0.3(4) . . . . ? C9 S1 C6 C5 -175.4(3) . . . . ? C5 C6 C7 C8 174.3(4) . . . . ? S1 C6 C7 C8 -1.0(5) . . . . ? C6 C7 C8 C9 1.4(6) . . . . ? C7 C8 C9 C10 -171.2(5) . . . . ? C7 C8 C9 S1 -1.2(5) . . . . ? C6 S1 C9 C8 0.6(4) . . . . ? C6 S1 C9 C10 172.2(4) . . . . ? C8 C9 C10 N11 -58.2(7) . . . . ? S1 C9 C10 N11 132.1(4) . . . . ? C9 C10 N11 C12 -48.1(6) . . . . ? C10 N11 C12 C13 -134.9(4) . . . . ? N11 C12 C13 N14 -173.8(4) . . . . ? C12 C13 N14 C15 -150.8(4) . . . . ? C12 C13 N14 C38 86.2(4) . . . . ? C13 N14 C15 C16 75.7(4) . . . . ? C38 N14 C15 C16 -160.1(3) . . . . ? N14 C15 C16 N17 59.5(5) . . . . ? C15 C16 N17 C18 164.0(3) . . . . ? C16 N17 C18 C19 172.3(3) . . . . ? N17 C18 C19 C20 85.4(5) . . . . ? N17 C18 C19 S2 -96.0(4) . . . . ? C22 S2 C19 C20 -0.1(3) . . . . ? C22 S2 C19 C18 -178.8(3) . . . . ? C18 C19 C20 C21 179.2(4) . . . . ? S2 C19 C20 C21 0.6(5) . . . . ? C19 C20 C21 C22 -1.0(5) . . . . ? C20 C21 C22 C23 -179.8(4) . . . . ? C20 C21 C22 S2 0.9(5) . . . . ? C19 S2 C22 C21 -0.5(3) . . . . ? C19 S2 C22 C23 -179.8(3) . . . . ? C21 C22 C23 N24 -106.0(5) . . . . ? S2 C22 C23 N24 73.3(4) . . . . ? C22 C23 N24 C25 172.3(3) . . . . ? C23 N24 C25 C26 159.6(3) . . . . ? C2 N1 C26 C25 -176.4(4) . . . . ? C27 N1 C26 C25 63.3(5) . . . . ? N24 C25 C26 N1 56.1(5) . . . . ? C2 N1 C27 C28 65.6(4) . . . . ? C26 N1 C27 C28 -175.0(3) . . . . ? N1 C27 C28 N29 49.3(5) . . . . ? C27 C28 N29 C30 160.0(3) . . . . ? C28 N29 C30 C31 179.7(3) . . . . ? N29 C30 C31 C32 -90.8(5) . . . . ? N29 C30 C31 S3 83.7(4) . . . . ? C34 S3 C31 C32 -1.4(3) . . . . ? C34 S3 C31 C30 -176.7(3) . . . . ? C30 C31 C32 C33 176.5(4) . . . . ? S3 C31 C32 C33 1.5(5) . . . . ? C31 C32 C33 C34 -0.9(6) . . . . ? C32 C33 C34 C35 -178.8(4) . . . . ? C32 C33 C34 S3 -0.1(5) . . . . ? C31 S3 C34 C33 0.8(3) . . . . ? C31 S3 C34 C35 179.6(3) . . . . ? C33 C34 C35 N36 55.3(5) . . . . ? S3 C34 C35 N36 -123.3(3) . . . . ? C34 C35 N36 C37 -178.1(3) . . . . ? C35 N36 C37 C38 172.2(3) . . . . ? C13 N14 C38 C37 -149.1(3) . . . . ? C15 N14 C38 C37 86.5(4) . . . . ? N36 C37 C38 N14 68.4(4) . . . . ? 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 N4 H4A O3D 0.92 1.85 2.760(5) 171.4 . N4 H4B O4B 0.92 1.94 2.828(5) 162.4 . N11 H11A O3B 0.92 2.16 3.001(6) 150.7 2_665 N11 H11B O1C 0.92 1.93 2.789(6) 155.3 . N14 H14A O1S 0.93 2.58 3.506(5) 175.1 . N17 H17A O3C 0.92 1.93 2.835(6) 166.6 1_655 N17 H17B O3W 0.92 2.19 2.866(5) 130.1 . N17 H17B O1S 0.92 2.25 2.947(5) 132.0 . N24 H24A O4B 0.92 1.86 2.759(5) 164.5 . N24 H24B O2A 0.92 1.84 2.764(4) 177.1 . N29 H29A O2A 0.92 1.90 2.813(4) 173.6 . N29 H29B O3D 0.92 1.94 2.805(5) 155.2 . N36 H36A O4D 0.92 1.88 2.786(4) 168.1 2_666 N36 H36B O1S 0.92 1.94 2.835(5) 163.7 . O1A H1AO O2W 0.83(6) 1.70(6) 2.516(4) 172(6) 1_655 O1S H1S O1W 0.84(6) 1.88(6) 2.707(5) 169(6) . O1W H1W1 O3C 0.87(3) 2.09(4) 2.815(5) 140(5) 1_655 O1W H1W2 O4A 0.86(3) 2.04(3) 2.848(5) 156(5) . O2W H2W1 O1D 0.85(3) 1.79(3) 2.624(5) 165(5) . O2W H2W2 O2D 0.85(3) 1.86(3) 2.686(4) 164(5) 2_676 O3W H3W1 O1B 0.86(3) 2.09(3) 2.888(5) 156(5) . O3W H3W2 O1B 0.86(3) 1.92(3) 2.777(4) 176(5) 2_665 O4W H4W1 O2B 0.90 1.72 2.625(6) 179.6 . O4W H4W2 O5W 0.90 1.59 2.493(12) 178.6 . _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 67.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.755 _refine_diff_density_min -0.745 _refine_diff_density_rms 0.087 #===END