# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 #TrackingRef 'CCDC833635.cif' #------------------ AUDIT DETAILS -------------------------------------------# _audit_creation_date 2012-01-13 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_update_record ? #------------------ AUTHOR DETAILS -------------------------------------------# # Name and address of author for correspondence _publ_contact_author_name 'Miguel Vazquez Lopez' _publ_contact_author_address ; Departamento de Quimica Inorganica, Facultade de Quimica, UniVersidade de Santiago de Compostela, 15782 Santiago de Compostela, Spain ; _publ_contact_author_email miguel.vazquez.lopez@usc.es _publ_requested_category FO loop_ _publ_author_name A.Aldrey A.Macias R.Bastida G.Zaragoza G.Rama M.V.Lopez #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_ba01yra2n _database_code_depnum_ccdc_archive 'CCDC 833635' #TrackingRef 'CCDC833635.cif' _audit_creation_date 2012-01-13T13:19:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C43 H45 N10 O8 S3, N O3, 4(C2 H3 N)' _chemical_formula_sum 'C51 H57 N15 O11 S3' _chemical_formula_weight 1152.3 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.535(4) _cell_length_b 14.086(5) _cell_length_c 16.533(6) _cell_angle_alpha 95.902(14) _cell_angle_beta 105.791(13) _cell_angle_gamma 91.983(13) _cell_volume 2788.1(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1935 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 26.06 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.75 _exptl_crystal_size_mid 0.29 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.206 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.541 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.1100 _diffrn_reflns_av_unetI/netI 0.1904 _diffrn_reflns_number 30269 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 18.86 _diffrn_reflns_theta_full 18.86 _diffrn_measured_fraction_theta_full 0.974 _diffrn_measured_fraction_theta_max 0.974 _reflns_number_total 4281 _reflns_number_gt 2364 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR-97 (Giacovazzo et all, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1773P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4281 _refine_ls_number_parameters 754 _refine_ls_number_restraints 553 _refine_ls_R_factor_all 0.1516 _refine_ls_R_factor_gt 0.1011 _refine_ls_wR_factor_ref 0.2891 _refine_ls_wR_factor_gt 0.2647 _refine_ls_goodness_of_fit_ref 0.997 _refine_ls_restrained_S_all 0.99 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.911 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.095 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.2307(9) 0.3665(10) 0.8389(7) 0.036(4) Uani 1 1 d U . . H1A H 0.1638 0.3287 0.8062 0.043 Uiso 1 1 calc R . . H1B H 0.2107 0.4317 0.8489 0.043 Uiso 1 1 calc R . . C2 C 0.2742(9) 0.3270(9) 0.9254(7) 0.028(3) Uani 1 1 d U . . H2A H 0.3546 0.3348 0.9431 0.033 Uiso 1 1 calc R . . H2B H 0.2469 0.3642 0.9673 0.033 Uiso 1 1 calc R . . C3 C 0.3072(9) 0.1587(10) 0.9053(7) 0.026(3) Uani 1 1 d U . . C4 C 0.3197(9) -0.0181(9) 0.8926(8) 0.024(3) Uani 1 1 d U . . C5 C 0.2813(9) -0.0430(9) 0.8063(8) 0.029(3) Uani 1 1 d U . . H5 H 0.2352 -0.0036 0.7725 0.035 Uiso 1 1 calc R . . C6 C 0.3123(9) -0.1277(9) 0.7702(8) 0.031(4) Uani 1 1 d U . . H6 H 0.2872 -0.1459 0.7122 0.038 Uiso 1 1 calc R . . C7 C 0.3775(10) -0.1809(10) 0.8200(8) 0.031(4) Uani 1 1 d U . . C8 C 0.4163(9) -0.1587(9) 0.9087(8) 0.032(4) Uani 1 1 d U . . H8 H 0.4598 -0.1999 0.9422 0.038 Uiso 1 1 calc R . . C9 C 0.3874(9) -0.0735(9) 0.9441(8) 0.030(3) Uani 1 1 d U . . H9 H 0.4139 -0.0545 1.002 0.036 Uiso 1 1 calc R . . C10 C 0.1370(8) 0.2042(9) 0.9463(7) 0.024(3) Uani 1 1 d U . . H10A H 0.1523 0.2142 1.0074 0.029 Uiso 1 1 calc R . . H10B H 0.1121 0.1376 0.9277 0.029 Uiso 1 1 calc R . . C11 C 0.0480(9) 0.2656(9) 0.9077(8) 0.031(4) Uani 1 1 d U . . C12 C 0.0203(9) 0.3464(9) 0.9583(8) 0.029(3) Uani 1 1 d U . . H12 H 0.0594 0.3617 1.0149 0.035 Uiso 1 1 calc R . . C13 C -0.0623(10) 0.3979(10) 0.9219(8) 0.039(4) Uani 1 1 d U . . H13 H -0.0811 0.4479 0.9557 0.047 Uiso 1 1 calc R . . C14 C -0.1215(10) 0.3831(10) 0.8391(8) 0.036(4) Uani 1 1 d U . . H14 H -0.1761 0.424 0.8173 0.044 Uiso 1 1 calc R . . C15 C -0.0996(9) 0.3054(9) 0.7865(8) 0.032(4) Uani 1 1 d U . . H15 H -0.1386 0.2924 0.7296 0.038 Uiso 1 1 calc R . . C16 C -0.0166(10) 0.2498(10) 0.8250(8) 0.030(3) Uani 1 1 d U . . C17 C -0.0576(10) 0.1393(9) 0.6965(8) 0.034(4) Uani 1 1 d U . . H17A H -0.0561 0.1882 0.6595 0.041 Uiso 1 1 calc R . . H17B H -0.1332 0.1301 0.7 0.041 Uiso 1 1 calc R . . C18 C -0.0238(9) 0.0493(9) 0.6604(8) 0.029(3) Uani 1 1 d U . . H18A H -0.0197 0.0012 0.6989 0.035 Uiso 1 1 calc R . . H18B H -0.0777 0.0259 0.6072 0.035 Uiso 1 1 calc R . . C19 C 0.1245(9) -0.0033(9) 0.6026(7) 0.028(3) Uani 1 1 d U . . C20 C 0.0660(10) -0.0929(9) 0.5718(7) 0.032(4) Uani 1 1 d U . . H20 H -0.0033 -0.107 0.5795 0.039 Uiso 1 1 calc R . . C21 C 0.1188(10) -0.1608(10) 0.5281(7) 0.038(4) Uani 1 1 d U . . H21 H 0.0843 -0.2214 0.5077 0.045 Uiso 1 1 calc R . . C22 C 0.2200(10) -0.1375(10) 0.5158(8) 0.040(4) Uani 1 1 d U . . H22 H 0.2516 -0.181 0.4844 0.048 Uiso 1 1 calc R . . C23 C 0.2743(10) -0.0511(9) 0.5493(7) 0.030(3) Uani 1 1 d U . . H23 H 0.3444 -0.0385 0.5424 0.036 Uiso 1 1 calc R . . C24 C 0.2304(9) 0.0182(9) 0.5929(7) 0.022(3) Uani 1 1 d U . . C25 C 0.2967(9) 0.1111(9) 0.6386(7) 0.031(4) Uani 1 1 d U . . H25A H 0.2997 0.1149 0.6981 0.037 Uiso 1 1 calc R . . H25B H 0.3722 0.1082 0.6344 0.037 Uiso 1 1 calc R . . C26 C 0.1965(9) 0.2603(9) 0.6574(8) 0.035(4) Uani 1 1 d U . . H26A H 0.1867 0.2269 0.7036 0.042 Uiso 1 1 calc R . . H26B H 0.1232 0.271 0.6224 0.042 Uiso 1 1 calc R . . C27 C 0.2580(10) 0.3579(9) 0.6947(7) 0.033(4) Uani 1 1 d U . . H27A H 0.3125 0.3707 0.6645 0.039 Uiso 1 1 calc R . . H27B H 0.205 0.407 0.685 0.039 Uiso 1 1 calc R . . C28 C 0.2507(9) 0.2201(9) 0.5288(8) 0.030(4) Uani 1 1 d U . . C29 C 0.3201(10) 0.1467(9) 0.4066(8) 0.029(4) Uani 1 1 d U . . C30 C 0.2341(12) 0.1442(10) 0.3454(9) 0.050(4) Uani 1 1 d U . . H30 H 0.1667 0.1614 0.354 0.06 Uiso 1 1 calc R . . C31 C 0.2427(13) 0.1136(11) 0.2612(10) 0.063(5) Uani 1 1 d U . . H31 H 0.1789 0.107 0.2159 0.075 Uiso 1 1 calc R . . C32 C 0.3345(11) 0.0957(10) 0.2482(8) 0.035(4) Uani 1 1 d U . . C33 C 0.4317(13) 0.0917(11) 0.3100(9) 0.064(5) Uani 1 1 d U . . H33 H 0.496 0.0707 0.2982 0.077 Uiso 1 1 calc R . . C34 C 0.4269(12) 0.1232(11) 0.3971(10) 0.066(5) Uani 1 1 d U . . H34 H 0.4897 0.1275 0.4432 0.079 Uiso 1 1 calc R . . C35 C 0.3940(9) 0.4526(9) 0.8173(8) 0.033(4) Uani 1 1 d U . . H35A H 0.4161 0.4599 0.8787 0.039 Uiso 1 1 calc R . . H35B H 0.3547 0.5083 0.7994 0.039 Uiso 1 1 calc R . . C36 C 0.5000(9) 0.4511(10) 0.7865(8) 0.038(4) Uani 1 1 d U . . H36A H 0.4794 0.4506 0.7254 0.045 Uiso 1 1 calc R . . H36B H 0.5472 0.5085 0.8114 0.045 Uiso 1 1 calc R . . C37 C 0.6273(10) 0.3618(10) 0.8839(8) 0.028(3) Uani 1 1 d U . . C38 C 0.7489(9) 0.2414(9) 0.9536(8) 0.026(3) Uani 1 1 d U . . C39 C 0.8021(9) 0.1584(9) 0.9335(8) 0.029(3) Uani 1 1 d U . . H39 H 0.7881 0.1332 0.8771 0.035 Uiso 1 1 calc R . . C40 C 0.8700(9) 0.1164(9) 0.9915(8) 0.030(3) Uani 1 1 d U . . H40 H 0.9031 0.062 0.976 0.035 Uiso 1 1 calc R . . C41 C 0.8931(10) 0.1528(10) 1.0767(8) 0.035(4) Uani 1 1 d U . . C42 C 0.8456(10) 0.2351(10) 1.0998(9) 0.040(4) Uani 1 1 d U . . H42 H 0.8616 0.2603 1.1563 0.048 Uiso 1 1 calc R . . C43 C 0.7757(10) 0.2782(11) 1.0393(8) 0.046(4) Uani 1 1 d U . . H43 H 0.7446 0.3337 1.0548 0.055 Uiso 1 1 calc R . . N1 N 0.3151(7) 0.3654(8) 0.7862(6) 0.026(3) Uani 1 1 d DU . . H1 H 0.373(6) 0.330(6) 0.809(6) 0.031 Uiso 1 1 d D . . N2 N 0.2399(7) 0.2257(7) 0.9225(6) 0.027(3) Uani 1 1 d U . . N3 N 0.2865(8) 0.0693(8) 0.9274(6) 0.032(3) Uani 1 1 d DU . . H3 H 0.283(8) 0.067(8) 0.979(2) 0.038 Uiso 1 1 d D . . N4 N 0.4123(9) -0.2732(9) 0.7845(8) 0.050(3) Uani 1 1 d U . . N5 N 0.5602(8) 0.3691(8) 0.8090(6) 0.030(3) Uani 1 1 d DU . . H5A H 0.545(8) 0.328(6) 0.765(4) 0.035 Uiso 1 1 d D . . N6 N 0.6767(8) 0.2782(8) 0.8885(6) 0.036(3) Uani 1 1 d DU . . H6A H 0.654(6) 0.248(7) 0.837(3) 0.043 Uiso 1 1 d D . . N7 N 0.9617(9) 0.1058(9) 1.1409(8) 0.046(3) Uani 1 1 d U . . N8 N 0.2519(7) 0.1976(7) 0.6060(6) 0.022(3) Uani 1 1 d U . . N9 N 0.3194(9) 0.1641(9) 0.4930(7) 0.047(3) Uani 1 1 d DU . . H9A H 0.379(6) 0.147(9) 0.526(6) 0.057 Uiso 1 1 d D . . N10 N 0.3358(11) 0.0661(9) 0.1563(8) 0.055(4) Uani 1 1 d U . . N11 N 0.5849(10) 0.1748(9) 0.6623(8) 0.047(3) Uani 1 1 d U . . N12 N 1.1526(9) 0.5753(10) 0.7425(8) 0.079(4) Uani 1 1 d DU . . C44 C 1.0556(10) 0.5777(10) 0.7377(10) 0.074(5) Uani 1 1 d DU . . C45 C 0.9446(10) 0.5990(12) 0.7361(10) 0.077(5) Uani 1 1 d DU . . H45A H 0.8941 0.5468 0.7048 0.115 Uiso 1 1 calc R . . H45B H 0.9265 0.6561 0.7095 0.115 Uiso 1 1 calc R . . H45C H 0.9384 0.6086 0.793 0.115 Uiso 1 1 calc R . . N13 N 0.7564(13) 0.6586(12) 0.8535(11) 0.108(5) Uani 1 1 d U . . C46 C 0.7027(15) 0.6500(14) 0.7811(14) 0.097(6) Uani 1 1 d U . . C47 C 0.6387(13) 0.6352(13) 0.6922(10) 0.089(6) Uani 1 1 d U . . H47A H 0.5635 0.6511 0.6872 0.134 Uiso 1 1 calc R . . H47B H 0.6393 0.5695 0.6704 0.134 Uiso 1 1 calc R . . H47C H 0.6712 0.6754 0.6605 0.134 Uiso 1 1 calc R . . N14 N 0.703(2) 0.430(3) 0.6375(18) 0.177(12) Uani 0.575(10) 1 d PDU A 1 C48 C 0.6253(17) 0.399(2) 0.5791(16) 0.099(9) Uani 0.575(10) 1 d PDU A 1 C49 C 0.5490(14) 0.3468(16) 0.5064(12) 0.119(7) Uani 0.575(10) 1 d PDU A 1 H49A H 0.5565 0.2794 0.5088 0.178 Uiso 0.575(10) 1 calc PR A 1 H49B H 0.5647 0.3645 0.4561 0.178 Uiso 0.575(10) 1 calc PR A 1 H49C H 0.4745 0.3614 0.5056 0.178 Uiso 0.575(10) 1 calc PR A 1 N14B N 0.416(2) 0.460(3) 0.561(2) 0.177(12) Uani 0.425(10) 1 d PDU A 2 C48B C 0.483(3) 0.408(3) 0.5441(14) 0.099(9) Uani 0.425(10) 1 d PDU A 2 C49B C 0.5490(14) 0.3468(16) 0.5064(12) 0.119(7) Uani 0.425(10) 1 d PDU A 2 H49D H 0.5016 0.2986 0.4657 0.178 Uiso 0.425(10) 1 d P A 2 H49E H 0.5986 0.3165 0.5494 0.178 Uiso 0.425(10) 1 d P A 2 H49F H 0.5906 0.3843 0.4784 0.178 Uiso 0.425(10) 1 d P A 2 N15 N 0.9568(16) 0.4040(19) 0.5914(13) 0.092(7) Uani 0.575(10) 1 d PDU A 1 C50 C 0.8784(11) 0.4115(16) 0.5321(12) 0.109(7) Uani 0.575(10) 1 d PDU A 1 C51 C 0.803(2) 0.425(3) 0.4530(13) 0.097(10) Uani 0.575(10) 1 d PDU A 1 H51A H 0.8192 0.3846 0.4084 0.145 Uiso 0.575(10) 1 calc PR A 1 H51B H 0.8103 0.491 0.443 0.145 Uiso 0.575(10) 1 calc PR A 1 H51C H 0.7281 0.4103 0.4544 0.145 Uiso 0.575(10) 1 calc PR A 1 N15B N 0.866(2) 0.393(3) 0.5984(13) 0.092(7) Uani 0.425(10) 1 d PDU A 2 C50B C 0.8784(11) 0.4115(16) 0.5321(12) 0.109(7) Uani 0.425(10) 1 d PDU A 2 C51B C 0.868(3) 0.427(4) 0.4465(14) 0.097(10) Uani 0.425(10) 1 d PDU A 2 H51D H 0.8592 0.3668 0.4119 0.145 Uiso 0.425(10) 1 calc PR A 2 H51E H 0.9341 0.4621 0.4436 0.145 Uiso 0.425(10) 1 calc PR A 2 H51F H 0.8048 0.4634 0.4264 0.145 Uiso 0.425(10) 1 calc PR A 2 O1 O 0.4698(8) -0.3222(8) 0.8305(6) 0.066(3) Uani 1 1 d U . . O2 O 0.3848(8) -0.2884(7) 0.7066(7) 0.067(3) Uani 1 1 d U . . O3 O 0.9860(7) 0.1426(7) 1.2174(6) 0.057(3) Uani 1 1 d U . . O4 O 1.0024(7) 0.0267(7) 1.1243(6) 0.052(3) Uani 1 1 d U . . O5 O 0.4210(9) 0.0260(8) 0.1507(6) 0.074(3) Uani 1 1 d U . . O6 O 0.2634(8) 0.0800(7) 0.1013(6) 0.050(3) Uani 1 1 d U . . O7 O 0.0145(6) 0.1706(6) 0.7791(5) 0.028(2) Uani 1 1 d U . . O8 O 0.0829(6) 0.0673(6) 0.6469(4) 0.026(2) Uani 1 1 d U . . O9 O 0.5168(7) 0.2384(7) 0.6598(5) 0.044(3) Uani 1 1 d U . . O10 O 0.6622(7) 0.1656(6) 0.7241(6) 0.045(3) Uani 1 1 d DU . . O11 O 0.5682(7) 0.1150(7) 0.5931(6) 0.059(3) Uani 1 1 d U . . S1 S 0.4108(3) 0.1771(2) 0.8610(2) 0.0293(10) Uani 1 1 d U . . S2 S 0.6391(3) 0.4488(3) 0.9654(2) 0.0458(12) Uani 1 1 d U . . S3 S 0.1841(3) 0.3081(3) 0.4838(2) 0.0557(13) Uani 1 1 d U . . 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 C1 0.037(5) 0.036(6) 0.037(5) -0.005(4) 0.018(4) 0.002(4) C2 0.032(5) 0.023(5) 0.029(5) -0.009(4) 0.014(4) -0.002(4) C3 0.034(5) 0.024(5) 0.023(5) 0.004(4) 0.011(4) -0.002(4) C4 0.028(5) 0.023(5) 0.021(5) -0.008(4) 0.010(4) 0.001(4) C5 0.033(5) 0.031(6) 0.026(5) 0.001(4) 0.014(4) -0.001(4) C6 0.034(5) 0.031(6) 0.030(5) -0.006(4) 0.015(4) -0.003(4) C7 0.037(5) 0.029(6) 0.031(5) -0.003(4) 0.016(4) 0.001(4) C8 0.033(5) 0.031(6) 0.033(5) 0.006(4) 0.012(4) 0.001(4) C9 0.036(5) 0.029(6) 0.028(5) -0.002(4) 0.015(4) -0.002(4) C10 0.029(5) 0.026(5) 0.020(5) -0.002(4) 0.015(4) -0.006(4) C11 0.031(5) 0.034(6) 0.030(5) -0.001(4) 0.018(4) -0.009(4) C12 0.028(5) 0.030(5) 0.028(5) -0.005(4) 0.011(4) -0.003(4) C13 0.040(5) 0.036(6) 0.043(6) -0.005(4) 0.017(4) -0.005(4) C14 0.033(5) 0.038(6) 0.040(6) 0.002(4) 0.014(4) 0.002(4) C15 0.033(5) 0.033(6) 0.030(5) -0.005(4) 0.012(4) -0.004(4) C16 0.032(5) 0.031(6) 0.030(5) -0.002(4) 0.018(4) -0.005(4) C17 0.036(5) 0.033(6) 0.035(5) 0.004(4) 0.013(4) 0.000(4) C18 0.034(5) 0.028(6) 0.028(5) -0.003(4) 0.015(4) 0.000(4) C19 0.031(5) 0.025(6) 0.027(5) -0.004(4) 0.011(4) 0.003(4) C20 0.036(5) 0.032(6) 0.032(5) 0.000(4) 0.015(4) -0.001(4) C21 0.045(5) 0.033(6) 0.034(5) 0.000(4) 0.012(4) -0.003(4) C22 0.044(5) 0.039(6) 0.040(5) 0.000(4) 0.016(4) 0.002(4) C23 0.032(5) 0.031(6) 0.031(5) 0.001(4) 0.019(4) 0.004(4) C24 0.031(5) 0.020(5) 0.019(5) -0.006(4) 0.015(4) 0.000(4) C25 0.035(5) 0.037(6) 0.024(5) 0.000(4) 0.014(4) 0.000(4) C26 0.037(5) 0.033(6) 0.034(5) -0.003(4) 0.015(4) -0.001(4) C27 0.038(5) 0.029(6) 0.034(5) 0.003(4) 0.017(4) -0.008(4) C28 0.034(5) 0.027(6) 0.030(5) 0.001(4) 0.010(4) 0.003(4) C29 0.034(5) 0.034(6) 0.024(5) 0.008(4) 0.016(4) -0.005(4) C30 0.050(6) 0.054(6) 0.050(6) 0.006(5) 0.020(5) 0.006(4) C31 0.062(6) 0.061(7) 0.060(6) 0.002(5) 0.011(5) 0.001(5) C32 0.033(5) 0.041(6) 0.031(5) -0.011(4) 0.015(4) 0.001(4) C33 0.068(6) 0.066(7) 0.062(6) 0.004(5) 0.026(5) 0.006(5) C34 0.070(6) 0.065(7) 0.063(6) 0.008(5) 0.016(5) 0.003(5) C35 0.035(5) 0.030(6) 0.036(5) -0.002(4) 0.017(4) -0.003(4) C36 0.041(5) 0.038(6) 0.039(5) 0.004(4) 0.021(4) -0.005(4) C37 0.028(5) 0.027(6) 0.033(5) 0.003(4) 0.015(4) 0.004(4) C38 0.029(5) 0.022(5) 0.026(5) -0.009(4) 0.013(4) -0.005(4) C39 0.030(5) 0.028(6) 0.032(5) 0.001(4) 0.013(4) 0.000(4) C40 0.031(5) 0.029(6) 0.031(5) -0.006(4) 0.016(4) -0.004(4) C41 0.040(5) 0.033(6) 0.034(5) 0.007(5) 0.013(4) 0.002(4) C42 0.046(5) 0.040(6) 0.035(5) -0.005(4) 0.017(4) 0.003(4) C43 0.050(6) 0.046(6) 0.042(6) 0.006(5) 0.015(4) 0.002(4) N1 0.030(4) 0.025(5) 0.025(5) -0.003(4) 0.014(4) -0.004(4) N2 0.035(4) 0.023(5) 0.028(5) 0.001(4) 0.018(4) -0.005(4) N3 0.043(4) 0.030(5) 0.027(5) 0.003(4) 0.018(4) -0.004(4) N4 0.056(5) 0.048(6) 0.043(5) 0.003(4) 0.008(4) -0.002(4) N5 0.033(4) 0.031(5) 0.030(5) -0.001(4) 0.018(4) 0.001(4) N6 0.041(5) 0.034(5) 0.036(5) 0.001(4) 0.019(4) 0.001(4) N7 0.045(5) 0.046(5) 0.047(5) -0.001(4) 0.018(4) -0.003(4) N8 0.029(4) 0.021(5) 0.020(4) -0.003(4) 0.015(4) 0.002(4) N9 0.058(5) 0.048(5) 0.041(5) 0.004(4) 0.024(4) 0.001(4) N10 0.047(5) 0.059(6) 0.062(6) 0.009(4) 0.021(4) 0.003(4) N11 0.052(5) 0.044(5) 0.049(5) 0.004(4) 0.022(4) -0.005(4) N12 0.080(6) 0.075(6) 0.079(6) -0.006(4) 0.024(5) 0.007(4) C44 0.077(7) 0.071(7) 0.071(7) 0.003(5) 0.017(5) 0.007(5) C45 0.076(7) 0.080(7) 0.077(7) 0.003(5) 0.027(5) 0.006(5) N13 0.109(7) 0.111(7) 0.103(7) 0.008(5) 0.029(5) 0.003(5) C46 0.094(8) 0.099(8) 0.098(8) 0.009(5) 0.029(5) 0.007(5) C47 0.092(7) 0.090(8) 0.085(7) 0.012(5) 0.022(5) 0.006(5) N14 0.178(12) 0.178(12) 0.175(12) 0.022(4) 0.049(5) 0.007(4) C48 0.100(9) 0.100(10) 0.098(9) 0.014(4) 0.029(4) 0.004(4) C49 0.122(8) 0.119(8) 0.118(8) 0.015(4) 0.035(4) 0.006(4) N14B 0.178(12) 0.178(12) 0.175(12) 0.022(4) 0.049(5) 0.007(4) C48B 0.100(9) 0.100(10) 0.098(9) 0.014(4) 0.029(4) 0.004(4) C49B 0.122(8) 0.119(8) 0.118(8) 0.015(4) 0.035(4) 0.006(4) N15 0.093(8) 0.090(8) 0.092(8) 0.008(4) 0.026(4) 0.007(4) C50 0.111(8) 0.107(8) 0.108(8) 0.012(4) 0.030(4) 0.008(4) C51 0.098(10) 0.096(10) 0.096(10) 0.013(4) 0.027(4) 0.006(4) N15B 0.093(8) 0.090(8) 0.092(8) 0.008(4) 0.026(4) 0.007(4) C50B 0.111(8) 0.107(8) 0.108(8) 0.012(4) 0.030(4) 0.008(4) C51B 0.098(10) 0.096(10) 0.096(10) 0.013(4) 0.027(4) 0.006(4) O1 0.073(5) 0.060(5) 0.066(5) -0.001(4) 0.024(4) 0.012(4) O2 0.077(5) 0.062(5) 0.060(5) -0.006(4) 0.024(4) 0.002(4) O3 0.072(5) 0.054(5) 0.046(5) 0.005(4) 0.018(4) -0.003(4) O4 0.059(4) 0.045(5) 0.055(5) 0.002(4) 0.024(4) 0.004(4) O5 0.081(5) 0.073(5) 0.070(5) 0.001(4) 0.028(4) 0.002(4) O6 0.056(4) 0.061(5) 0.039(4) 0.016(4) 0.017(4) 0.001(4) O7 0.038(4) 0.025(4) 0.025(4) -0.008(3) 0.021(3) -0.005(3) O8 0.037(4) 0.024(4) 0.023(4) -0.006(3) 0.019(3) 0.000(3) O9 0.045(4) 0.045(5) 0.041(4) 0.001(4) 0.013(3) 0.014(4) O10 0.046(4) 0.044(5) 0.048(4) -0.005(4) 0.020(4) 0.004(4) O11 0.069(5) 0.060(5) 0.049(5) 0.002(4) 0.021(4) 0.009(4) S1 0.048(2) 0.019(2) 0.027(2) -0.0064(16) 0.0246(17) -0.0054(16) S2 0.060(2) 0.024(2) 0.056(2) -0.0209(19) 0.0306(19) -0.0027(18) S3 0.074(3) 0.044(3) 0.053(2) 0.007(2) 0.023(2) 0.004(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.542(14) . ? C1 C2 1.554(17) . ? C1 H1A 0.97 . ? C1 H1B 0.97 . ? C2 N2 1.468(15) . ? C2 H2A 0.97 . ? C2 H2B 0.97 . ? C3 N2 1.347(14) . ? C3 N3 1.380(15) . ? C3 S1 1.681(12) . ? C4 C9 1.358(16) . ? C4 C5 1.379(15) . ? C4 N3 1.429(15) . ? C5 C6 1.393(16) . ? C5 H5 0.93 . ? C6 C7 1.308(16) . ? C6 H6 0.93 . ? C7 C8 1.412(15) . ? C7 N4 1.498(17) . ? C8 C9 1.384(17) . ? C8 H8 0.93 . ? C9 H9 0.93 . ? C10 N2 1.478(13) . ? C10 C11 1.480(16) . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? C11 C16 1.378(15) . ? C11 C12 1.451(16) . ? C12 C13 1.328(16) . ? C12 H12 0.93 . ? C13 C14 1.359(16) . ? C13 H13 0.93 . ? C14 C15 1.410(16) . ? C14 H14 0.93 . ? C15 C16 1.378(17) . ? C15 H15 0.93 . ? C16 O7 1.410(14) . ? C17 O7 1.433(12) . ? C17 C18 1.470(16) . ? C17 H17A 0.97 . ? C17 H17B 0.97 . ? C18 O8 1.432(12) . ? C18 H18A 0.97 . ? C18 H18B 0.97 . ? C19 O8 1.375(13) . ? C19 C24 1.406(15) . ? C19 C20 1.412(16) . ? C20 C21 1.427(16) . ? C20 H20 0.93 . ? C21 C22 1.371(15) . ? C21 H21 0.93 . ? C22 C23 1.360(16) . ? C22 H22 0.93 . ? C23 C24 1.373(15) . ? C23 H23 0.93 . ? C24 C25 1.534(16) . ? C25 N8 1.452(15) . ? C25 H25A 0.97 . ? C25 H25B 0.97 . ? C26 N8 1.480(14) . ? C26 C27 1.536(16) . ? C26 H26A 0.97 . ? C26 H26B 0.97 . ? C27 N1 1.478(14) . ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? C28 N8 1.343(14) . ? C28 N9 1.395(16) . ? C28 S3 1.646(14) . ? C29 C30 1.259(15) . ? C29 N9 1.426(15) . ? C29 C34 1.436(17) . ? C30 C31 1.448(18) . ? C30 H30 0.93 . ? C31 C32 1.256(16) . ? C31 H31 0.93 . ? C32 C33 1.368(17) . ? C32 N10 1.537(16) . ? C33 C34 1.480(19) . ? C33 H33 0.93 . ? C34 H34 0.93 . ? C35 N1 1.504(15) . ? C35 C36 1.548(15) . ? C35 H35A 0.97 . ? C35 H35B 0.97 . ? C36 N5 1.427(15) . ? C36 H36A 0.97 . ? C36 H36B 0.97 . ? C37 N5 1.311(14) . ? C37 N6 1.348(15) . ? C37 S2 1.697(13) . ? C38 N6 1.365(15) . ? C38 C43 1.402(16) . ? C38 C39 1.420(16) . ? C39 C40 1.303(16) . ? C39 H39 0.93 . ? C40 C41 1.397(15) . ? C40 H40 0.93 . ? C41 C42 1.387(17) . ? C41 N7 1.411(16) . ? C42 C43 1.349(17) . ? C42 H42 0.93 . ? C43 H43 0.93 . ? N1 H1 0.91(2) . ? N3 H3 0.863(17) . ? N4 O1 1.191(13) . ? N4 O2 1.232(12) . ? N5 H5A 0.86(2) . ? N6 H6A 0.88(2) . ? N7 O3 1.266(12) . ? N7 O4 1.277(13) . ? N9 H9A 0.86(2) . ? N10 O6 1.135(12) . ? N10 O5 1.247(13) . ? N11 O10 1.224(12) . ? N11 O9 1.255(13) . ? N11 O11 1.312(13) . ? N12 C44 1.200(11) . ? C44 C45 1.428(13) . ? C45 H45A 0.96 . ? C45 H45B 0.96 . ? C45 H45C 0.96 . ? N13 C46 1.19(2) . ? C46 C47 1.46(2) . ? C47 H47A 0.96 . ? C47 H47B 0.96 . ? C47 H47C 0.96 . ? N14 C48 1.200(11) . ? C48 C49 1.428(13) . ? C48 H49E 1.21(2) . ? C49 H49A 0.96 . ? C49 H49B 0.96 . ? C49 H49C 0.96 . ? C49 H49D 0.963(19) . ? C49 H49E 0.96(2) . ? C49 H49F 0.96(2) . ? N14B C48B 1.200(11) . ? N15 C50 1.200(11) . ? C50 C51 1.428(13) . ? C51 H51A 0.96 . ? C51 H51B 0.96 . ? C51 H51C 0.96 . ? C51B H51D 0.96 . ? C51B H51E 0.96 . ? C51B H51F 0.96 . ? 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 113.9(9) . . ? N1 C1 H1A 108.8 . . ? C2 C1 H1A 108.8 . . ? N1 C1 H1B 108.8 . . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? N2 C2 C1 113.1(9) . . ? N2 C2 H2A 109 . . ? C1 C2 H2A 109 . . ? N2 C2 H2B 109 . . ? C1 C2 H2B 109 . . ? H2A C2 H2B 107.8 . . ? N2 C3 N3 115.1(10) . . ? N2 C3 S1 125.0(10) . . ? N3 C3 S1 119.9(10) . . ? C9 C4 C5 122.1(12) . . ? C9 C4 N3 120.0(11) . . ? C5 C4 N3 117.9(11) . . ? C4 C5 C6 119.4(12) . . ? C4 C5 H5 120.3 . . ? C6 C5 H5 120.3 . . ? C7 C6 C5 118.4(13) . . ? C7 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C6 C7 C8 123.7(13) . . ? C6 C7 N4 120.5(12) . . ? C8 C7 N4 115.8(12) . . ? C9 C8 C7 117.7(12) . . ? C9 C8 H8 121.1 . . ? C7 C8 H8 121.1 . . ? C4 C9 C8 118.6(12) . . ? C4 C9 H9 120.7 . . ? C8 C9 H9 120.7 . . ? N2 C10 C11 111.3(10) . . ? N2 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N2 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108 . . ? C16 C11 C12 115.2(12) . . ? C16 C11 C10 124.3(12) . . ? C12 C11 C10 120.4(11) . . ? C13 C12 C11 118.5(12) . . ? C13 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C12 C13 C14 125.0(13) . . ? C12 C13 H13 117.5 . . ? C14 C13 H13 117.5 . . ? C13 C14 C15 119.5(13) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 115.5(12) . . ? C16 C15 H15 122.3 . . ? C14 C15 H15 122.3 . . ? C15 C16 C11 126.2(12) . . ? C15 C16 O7 121.1(11) . . ? C11 C16 O7 112.6(11) . . ? O7 C17 C18 111.3(10) . . ? O7 C17 H17A 109.4 . . ? C18 C17 H17A 109.4 . . ? O7 C17 H17B 109.4 . . ? C18 C17 H17B 109.4 . . ? H17A C17 H17B 108 . . ? O8 C18 C17 108.3(10) . . ? O8 C18 H18A 110 . . ? C17 C18 H18A 110 . . ? O8 C18 H18B 110 . . ? C17 C18 H18B 110 . . ? H18A C18 H18B 108.4 . . ? O8 C19 C24 115.8(10) . . ? O8 C19 C20 121.8(10) . . ? C24 C19 C20 122.3(11) . . ? C19 C20 C21 116.5(11) . . ? C19 C20 H20 121.7 . . ? C21 C20 H20 121.7 . . ? C22 C21 C20 120.6(12) . . ? C22 C21 H21 119.7 . . ? C20 C21 H21 119.7 . . ? C23 C22 C21 120.3(13) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C24 123.0(12) . . ? C22 C23 H23 118.5 . . ? C24 C23 H23 118.5 . . ? C23 C24 C19 117.2(11) . . ? C23 C24 C25 122.7(10) . . ? C19 C24 C25 119.8(10) . . ? N8 C25 C24 114.6(9) . . ? N8 C25 H25A 108.6 . . ? C24 C25 H25A 108.6 . . ? N8 C25 H25B 108.6 . . ? C24 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? N8 C26 C27 115.4(9) . . ? N8 C26 H26A 108.4 . . ? C27 C26 H26A 108.4 . . ? N8 C26 H26B 108.4 . . ? C27 C26 H26B 108.4 . . ? H26A C26 H26B 107.5 . . ? N1 C27 C26 114.3(11) . . ? N1 C27 H27A 108.7 . . ? C26 C27 H27A 108.7 . . ? N1 C27 H27B 108.7 . . ? C26 C27 H27B 108.7 . . ? H27A C27 H27B 107.6 . . ? N8 C28 N9 111.8(12) . . ? N8 C28 S3 124.7(10) . . ? N9 C28 S3 123.3(10) . . ? C30 C29 N9 123.4(12) . . ? C30 C29 C34 123.4(13) . . ? N9 C29 C34 112.9(11) . . ? C29 C30 C31 118.3(14) . . ? C29 C30 H30 120.9 . . ? C31 C30 H30 120.9 . . ? C32 C31 C30 121.4(14) . . ? C32 C31 H31 119.3 . . ? C30 C31 H31 119.3 . . ? C31 C32 C33 125.0(14) . . ? C31 C32 N10 117.6(13) . . ? C33 C32 N10 117.1(12) . . ? C32 C33 C34 115.0(13) . . ? C32 C33 H33 122.5 . . ? C34 C33 H33 122.5 . . ? C29 C34 C33 116.4(13) . . ? C29 C34 H34 121.8 . . ? C33 C34 H34 121.8 . . ? N1 C35 C36 115.0(10) . . ? N1 C35 H35A 108.5 . . ? C36 C35 H35A 108.5 . . ? N1 C35 H35B 108.5 . . ? C36 C35 H35B 108.5 . . ? H35A C35 H35B 107.5 . . ? N5 C36 C35 111.3(10) . . ? N5 C36 H36A 109.4 . . ? C35 C36 H36A 109.4 . . ? N5 C36 H36B 109.4 . . ? C35 C36 H36B 109.4 . . ? H36A C36 H36B 108 . . ? N5 C37 N6 113.2(11) . . ? N5 C37 S2 120.6(11) . . ? N6 C37 S2 126.1(10) . . ? N6 C38 C43 125.8(12) . . ? N6 C38 C39 117.7(11) . . ? C43 C38 C39 116.5(12) . . ? C40 C39 C38 122.2(12) . . ? C40 C39 H39 118.9 . . ? C38 C39 H39 118.9 . . ? C39 C40 C41 120.3(13) . . ? C39 C40 H40 119.9 . . ? C41 C40 H40 119.9 . . ? C42 C41 C40 120.0(12) . . ? C42 C41 N7 118.7(12) . . ? C40 C41 N7 121.3(12) . . ? C43 C42 C41 119.3(13) . . ? C43 C42 H42 120.4 . . ? C41 C42 H42 120.4 . . ? C42 C43 C38 121.7(14) . . ? C42 C43 H43 119.1 . . ? C38 C43 H43 119.1 . . ? C27 N1 C35 113.3(10) . . ? C27 N1 C1 111.1(8) . . ? C35 N1 C1 108.4(9) . . ? C27 N1 H1 124(7) . . ? C35 N1 H1 88(7) . . ? C1 N1 H1 110(7) . . ? C3 N2 C2 119.0(10) . . ? C3 N2 C10 123.8(10) . . ? C2 N2 C10 117.0(9) . . ? C3 N3 C4 125.0(10) . . ? C3 N3 H3 117(7) . . ? C4 N3 H3 112(7) . . ? O1 N4 O2 124.6(13) . . ? O1 N4 C7 120.0(12) . . ? O2 N4 C7 115.2(12) . . ? C37 N5 C36 124.6(11) . . ? C37 N5 H5A 128(8) . . ? C36 N5 H5A 108(8) . . ? C37 N6 C38 132.1(11) . . ? C37 N6 H6A 105(6) . . ? C38 N6 H6A 122(7) . . ? O3 N7 O4 118.0(12) . . ? O3 N7 C41 120.1(12) . . ? O4 N7 C41 121.8(12) . . ? C28 N8 C25 123.3(10) . . ? C28 N8 C26 118.0(11) . . ? C25 N8 C26 118.6(9) . . ? C28 N9 C29 129.3(11) . . ? C28 N9 H9A 118(8) . . ? C29 N9 H9A 112(8) . . ? O6 N10 O5 125.9(13) . . ? O6 N10 C32 120.8(12) . . ? O5 N10 C32 113.3(12) . . ? O10 N11 O9 124.3(12) . . ? O10 N11 O11 120.0(13) . . ? O9 N11 O11 115.7(12) . . ? N12 C44 C45 169.4(13) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N13 C46 C47 177(2) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N14 C48 C49 167.7(13) . . ? N14 C48 H49E 129(2) . . ? C48 C49 H49D 166(2) . . ? H49A C49 H49D 56.9 . . ? H49B C49 H49D 81 . . ? H49C C49 H49D 74.5 . . ? C48 C49 H49E 56.9(15) . . ? H49A C49 H49E 52.5 . . ? H49B C49 H49E 125.2 . . ? H49C C49 H49E 125.3 . . ? H49D C49 H49E 109(2) . . ? C48 C49 H49F 80.9(18) . . ? H49A C49 H49F 122.4 . . ? H49C C49 H49F 120.1 . . ? H49D C49 H49F 109.4(19) . . ? H49E C49 H49F 110.0(17) . . ? N15 C50 C51 167.8(12) . . ? H51D C51B H51E 109.5 . . ? H51D C51B H51F 109.5 . . ? H51E C51B H51F 109.5 . . ? C16 O7 C17 116.9(9) . . ? C19 O8 C18 118.6(9) . . ? 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 -95.9(11) . . . . ? C9 C4 C5 C6 0.2(17) . . . . ? N3 C4 C5 C6 179.8(10) . . . . ? C4 C5 C6 C7 -0.2(17) . . . . ? C5 C6 C7 C8 1.6(19) . . . . ? C5 C6 C7 N4 179.4(10) . . . . ? C6 C7 C8 C9 -3.0(18) . . . . ? N4 C7 C8 C9 179.1(10) . . . . ? C5 C4 C9 C8 -1.7(18) . . . . ? N3 C4 C9 C8 178.8(10) . . . . ? C7 C8 C9 C4 2.9(17) . . . . ? N2 C10 C11 C16 79.4(14) . . . . ? N2 C10 C11 C12 -103.3(12) . . . . ? C16 C11 C12 C13 -0.5(17) . . . . ? C10 C11 C12 C13 -178.0(11) . . . . ? C11 C12 C13 C14 -2.5(19) . . . . ? C12 C13 C14 C15 3(2) . . . . ? C13 C14 C15 C16 -0.5(17) . . . . ? C14 C15 C16 C11 -2.5(18) . . . . ? C14 C15 C16 O7 -179.1(10) . . . . ? C12 C11 C16 C15 3.0(18) . . . . ? C10 C11 C16 C15 -179.6(12) . . . . ? C12 C11 C16 O7 179.9(9) . . . . ? C10 C11 C16 O7 -2.7(16) . . . . ? O7 C17 C18 O8 -65.5(13) . . . . ? O8 C19 C20 C21 -178.9(10) . . . . ? C24 C19 C20 C21 -1.4(18) . . . . ? C19 C20 C21 C22 -1.5(19) . . . . ? C20 C21 C22 C23 4(2) . . . . ? C21 C22 C23 C24 -3(2) . . . . ? C22 C23 C24 C19 0.2(19) . . . . ? C22 C23 C24 C25 173.4(12) . . . . ? O8 C19 C24 C23 179.7(11) . . . . ? C20 C19 C24 C23 2.0(18) . . . . ? O8 C19 C24 C25 6.4(16) . . . . ? C20 C19 C24 C25 -171.3(12) . . . . ? C23 C24 C25 N8 117.3(13) . . . . ? C19 C24 C25 N8 -69.8(14) . . . . ? N8 C26 C27 N1 -104.4(12) . . . . ? N9 C29 C30 C31 -172.0(13) . . . . ? C34 C29 C30 C31 2(2) . . . . ? C29 C30 C31 C32 -4(2) . . . . ? C30 C31 C32 C33 8(2) . . . . ? C30 C31 C32 N10 -178.5(12) . . . . ? C31 C32 C33 C34 -8(2) . . . . ? N10 C32 C33 C34 178.5(12) . . . . ? C30 C29 C34 C33 -2(2) . . . . ? N9 C29 C34 C33 172.2(12) . . . . ? C32 C33 C34 C29 5(2) . . . . ? N1 C35 C36 N5 -56.7(14) . . . . ? N6 C38 C39 C40 -178.1(11) . . . . ? C43 C38 C39 C40 2.0(18) . . . . ? C38 C39 C40 C41 -0.3(18) . . . . ? C39 C40 C41 C42 -1.3(18) . . . . ? C39 C40 C41 N7 176.7(11) . . . . ? C40 C41 C42 C43 1.1(19) . . . . ? N7 C41 C42 C43 -177.0(11) . . . . ? C41 C42 C43 C38 0.7(19) . . . . ? N6 C38 C43 C42 177.9(12) . . . . ? C39 C38 C43 C42 -2.2(18) . . . . ? C26 C27 N1 C35 167.7(10) . . . . ? C26 C27 N1 C1 -70.0(13) . . . . ? C36 C35 N1 C27 -70.0(14) . . . . ? C36 C35 N1 C1 166.2(10) . . . . ? C2 C1 N1 C27 152.7(11) . . . . ? C2 C1 N1 C35 -82.2(13) . . . . ? N3 C3 N2 C2 162.1(9) . . . . ? S1 C3 N2 C2 -17.6(15) . . . . ? N3 C3 N2 C10 -12.4(15) . . . . ? S1 C3 N2 C10 168.0(8) . . . . ? C1 C2 N2 C3 91.8(12) . . . . ? C1 C2 N2 C10 -93.4(11) . . . . ? C11 C10 N2 C3 -141.7(11) . . . . ? C11 C10 N2 C2 43.7(13) . . . . ? N2 C3 N3 C4 158.8(11) . . . . ? S1 C3 N3 C4 -21.5(15) . . . . ? C9 C4 N3 C3 120.7(13) . . . . ? C5 C4 N3 C3 -58.9(15) . . . . ? C6 C7 N4 O1 -178.4(12) . . . . ? C8 C7 N4 O1 -0.4(17) . . . . ? C6 C7 N4 O2 7.1(17) . . . . ? C8 C7 N4 O2 -174.9(10) . . . . ? N6 C37 N5 C36 -178.3(10) . . . . ? S2 C37 N5 C36 5.7(16) . . . . ? C35 C36 N5 C37 -80.4(14) . . . . ? N5 C37 N6 C38 -178.4(11) . . . . ? S2 C37 N6 C38 -2.5(19) . . . . ? C43 C38 N6 C37 12(2) . . . . ? C39 C38 N6 C37 -168.2(12) . . . . ? C42 C41 N7 O3 -5.4(18) . . . . ? C40 C41 N7 O3 176.5(10) . . . . ? C42 C41 N7 O4 175.6(11) . . . . ? C40 C41 N7 O4 -2.5(18) . . . . ? N9 C28 N8 C25 -14.1(15) . . . . ? S3 C28 N8 C25 170.1(8) . . . . ? N9 C28 N8 C26 171.0(9) . . . . ? S3 C28 N8 C26 -4.8(15) . . . . ? C24 C25 N8 C28 -67.5(14) . . . . ? C24 C25 N8 C26 107.4(11) . . . . ? C27 C26 N8 C28 -73.1(14) . . . . ? C27 C26 N8 C25 111.7(12) . . . . ? N8 C28 N9 C29 161.6(11) . . . . ? S3 C28 N9 C29 -22.5(18) . . . . ? C30 C29 N9 C28 -32(2) . . . . ? C34 C29 N9 C28 153.8(13) . . . . ? C31 C32 N10 O6 17(2) . . . . ? C33 C32 N10 O6 -169.1(14) . . . . ? C31 C32 N10 O5 -162.1(14) . . . . ? C33 C32 N10 O5 11.8(18) . . . . ? C15 C16 O7 C17 -12.1(16) . . . . ? C11 C16 O7 C17 170.9(9) . . . . ? C18 C17 O7 C16 -172.6(10) . . . . ? C24 C19 O8 C18 -178.8(10) . . . . ? C20 C19 O8 C18 -1.2(17) . . . . ? C17 C18 O8 C19 -171.0(10) . . . . ? 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 N3 H3 O6 0.863(17) 2.101(18) 2.957(12) 171(10) 1_556 N5 H5A O9 0.86(2) 1.98(3) 2.834(13) 176(11) . N6 H6A O10 0.88(2) 2.12(2) 2.960(13) 159(7) . N9 H9A O9 0.86(2) 2.59(10) 3.216(13) 131(11) . N9 H9A O11 0.86(2) 2.41(4) 3.243(14) 165(11) . N1 H1 S1 0.91(2) 2.41(7) 3.176(11) 142(9) . #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_mig12n _database_code_depnum_ccdc_archive 'CCDC 863706' #TrackingRef 'archive_CF3COO.cif' _audit_creation_date 2012-01-13T11:26:17-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C43 H45 N10 O8 S3, C2 F3 O2, 2(C2 H3 N)' _chemical_formula_sum 'C49 H51 F3 N12 O10 S3' _chemical_formula_weight 1121.2 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.6022(7) _cell_length_b 13.4737(10) _cell_length_c 18.5141(14) _cell_angle_alpha 79.826(4) _cell_angle_beta 84.575(4) _cell_angle_gamma 89.938(4) _cell_volume 2591.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1984 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 20.47 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.224 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_absorpt_correction_T_min 0.9230 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'BRUKER APPEX-II CCD' _diffrn_measurement_method 'omega and phi scans' _diffrn_reflns_av_R_equivalents 0.0660 _diffrn_reflns_av_unetI/netI 0.072 _diffrn_reflns_number 34955 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 23.26 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 7427 _reflns_number_gt 4666 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'APPEX2 (BRUKER AXS, 2005)' _computing_cell_refinement 'APPEX2 (BRUKER AXS, 2005)' _computing_data_reduction 'APPEX2 (BRUKER AXS, 2005)' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0471P)^2^+2.9862P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_number_reflns 7427 _refine_ls_number_parameters 776 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1072 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1416 _refine_ls_wR_factor_gt 0.1172 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.535 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.058 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 C1 C 0.6967(4) 0.7525(3) 0.7316(2) 0.0308(10) Uani 1 1 d . . . H1A H 0.7329 0.6935 0.7123 0.037 Uiso 1 1 calc R . . H1B H 0.6196 0.7725 0.7067 0.037 Uiso 1 1 calc R . . C2 C 0.6611(4) 0.7232(3) 0.8147(2) 0.0300(10) Uani 1 1 d . . . H2A H 0.7076 0.7679 0.8405 0.036 Uiso 1 1 calc R . . H2B H 0.5693 0.7336 0.8256 0.036 Uiso 1 1 calc R . . C3 C 0.8107(4) 0.5933(3) 0.8512(2) 0.0301(10) Uani 1 1 d . . . C4 C 0.9521(4) 0.4527(3) 0.8928(2) 0.0285(10) Uani 1 1 d . . . C5 C 1.0411(4) 0.4519(3) 0.8328(2) 0.0331(11) Uani 1 1 d . . . H5 H 1.0216 0.4802 0.7845 0.04 Uiso 1 1 calc R . . C6 C 1.1588(4) 0.4096(3) 0.8437(3) 0.0390(12) Uani 1 1 d . . . H6 H 1.2212 0.4088 0.8034 0.047 Uiso 1 1 calc R . . C7 C 1.1823(4) 0.3685(3) 0.9152(3) 0.0358(11) Uani 1 1 d . . . C8 C 1.0937(4) 0.3650(3) 0.9739(2) 0.0344(11) Uani 1 1 d . . . H8 H 1.112 0.3339 1.0218 0.041 Uiso 1 1 calc R . . C9 C 0.9777(4) 0.4068(3) 0.9628(2) 0.0308(10) Uani 1 1 d . . . H9 H 0.9147 0.4042 1.0032 0.037 Uiso 1 1 calc R . . C10 C 0.5815(4) 0.5469(3) 0.8623(2) 0.0353(11) Uani 1 1 d . . . H10A H 0.5447 0.5493 0.9131 0.042 Uiso 1 1 calc R . . H10B H 0.6116 0.4776 0.8611 0.042 Uiso 1 1 calc R . . C11 C 0.4808(4) 0.5714(3) 0.8100(3) 0.0420(12) Uani 1 1 d . . . C12 C 0.3661(5) 0.6106(3) 0.8318(3) 0.0576(15) Uani 1 1 d . . . H12 H 0.3476 0.6209 0.8811 0.069 Uiso 1 1 calc R . . C13 C 0.2735(5) 0.6358(4) 0.7783(4) 0.0606(17) Uani 1 1 d . . . H13 H 0.1944 0.6646 0.7911 0.073 Uiso 1 1 calc R . . C14 C 0.3047(7) 0.6167(4) 0.7094(4) 0.0747(19) Uani 1 1 d . . . H14 H 0.2442 0.6321 0.6745 0.09 Uiso 1 1 calc R . . C15 C 0.4148(6) 0.5777(4) 0.6870(3) 0.0665(17) Uani 1 1 d . . . H15 H 0.4311 0.5657 0.638 0.08 Uiso 1 1 calc R . . C16 C 0.5046(5) 0.5550(4) 0.7373(3) 0.0483(13) Uani 1 1 d . . . C17 C 0.6463(7) 0.4806(4) 0.6525(3) 0.0743(19) Uani 1 1 d . . . H17A H 0.6327 0.5336 0.6097 0.089 Uiso 1 1 calc R . . H17B H 0.589 0.4227 0.6522 0.089 Uiso 1 1 calc R . . C18 C 0.7817(6) 0.4478(4) 0.6483(3) 0.0743(18) Uani 1 1 d . . . H18A H 0.8044 0.4163 0.6977 0.089 Uiso 1 1 calc R . . H18B H 0.795 0.3983 0.6148 0.089 Uiso 1 1 calc R . . C19 C 0.9826(6) 0.5218(4) 0.6002(3) 0.0542(15) Uani 1 1 d . . . C20 C 1.0484(7) 0.4322(3) 0.6246(3) 0.0628(17) Uani 1 1 d . . . H20 H 1.0054 0.3767 0.656 0.075 Uiso 1 1 calc R . . C21 C 1.1757(7) 0.4266(5) 0.6021(3) 0.0704(18) Uani 1 1 d . . . H21 H 1.22 0.3666 0.6181 0.084 Uiso 1 1 calc R . . C22 C 1.2379(6) 0.5049(4) 0.5578(3) 0.0654(16) Uani 1 1 d . . . H22 H 1.3254 0.5002 0.5423 0.079 Uiso 1 1 calc R . . C23 C 1.1733(6) 0.5919(4) 0.5351(3) 0.0565(15) Uani 1 1 d . . . H23 H 1.2182 0.6473 0.5048 0.068 Uiso 1 1 calc R . . C24 C 1.0442(6) 0.6015(3) 0.5551(2) 0.0447(13) Uani 1 1 d . . . C25 C 0.9801(5) 0.6987(3) 0.5269(2) 0.0467(13) Uani 1 1 d . . . H25A H 0.9985 0.7161 0.4727 0.056 Uiso 1 1 calc R . . H25B H 0.8872 0.6901 0.5383 0.056 Uiso 1 1 calc R . . C26 C 0.8614(4) 0.8469(3) 0.6396(2) 0.0348(11) Uani 1 1 d . . . H26A H 0.8924 0.9172 0.6229 0.042 Uiso 1 1 calc R . . H26B H 0.802 0.8318 0.6046 0.042 Uiso 1 1 calc R . . C27 C 1.1035(5) 0.8552(3) 0.5228(3) 0.0465(13) Uani 1 1 d . A . C28 C 0.9739(4) 0.7759(3) 0.6376(2) 0.0322(10) Uani 1 1 d . . . H28A H 1.0398 0.7962 0.6668 0.039 Uiso 1 1 calc R . . H28B H 0.946 0.706 0.6593 0.039 Uiso 1 1 calc R . . C35 C 0.7304(4) 0.9357(3) 0.7262(2) 0.0308(10) Uani 1 1 d . . . H35A H 0.6617 0.9221 0.7669 0.037 Uiso 1 1 calc R . . H35B H 0.6924 0.9666 0.6809 0.037 Uiso 1 1 calc R . . C36 C 0.8263(4) 1.0084(3) 0.7444(2) 0.0292(10) Uani 1 1 d . . . H36A H 0.8878 1.0297 0.7007 0.035 Uiso 1 1 calc R . . H36B H 0.7822 1.0692 0.7561 0.035 Uiso 1 1 calc R . . C37 C 0.8464(4) 0.9526(3) 0.8774(2) 0.0247(10) Uani 1 1 d . A . C44 C 0.8012(4) 0.0975(3) 0.2249(3) 0.0357(11) Uani 1 1 d . . . C45 C 0.6620(4) 0.0856(4) 0.2558(3) 0.0489(13) Uani 1 1 d . . . N1 N 0.7913(3) 0.8380(2) 0.71479(19) 0.0294(9) Uani 1 1 d . . . H1N H 0.848(4) 0.825(3) 0.749(2) 0.035 Uiso 1 1 d . . . N2 N 0.6904(3) 0.6187(2) 0.84274(18) 0.0295(8) Uani 1 1 d . . . N3 N 0.8318(3) 0.4964(3) 0.8842(2) 0.0321(9) Uani 1 1 d . . . H3N H 0.770(4) 0.469(3) 0.913(2) 0.039 Uiso 1 1 d . . . N4 N 1.3099(4) 0.3275(3) 0.9295(3) 0.0519(11) Uani 1 1 d . . . N5 N 0.8940(3) 0.9640(2) 0.80613(18) 0.0253(8) Uani 1 1 d . . . H5N H 0.969(4) 0.948(3) 0.792(2) 0.03 Uiso 1 1 d . . . N6 N 0.9339(3) 0.9135(2) 0.92398(19) 0.0279(9) Uani 1 1 d . . . H6N H 1.002(4) 0.904(3) 0.902(2) 0.033 Uiso 1 1 d . . . N8 N 1.0253(4) 0.7809(2) 0.56127(18) 0.0387(10) Uani 1 1 d . . . N9 N 1.1446(4) 0.9218(3) 0.5636(2) 0.0417(11) Uani 1 1 d . . . H9N H 1.122(4) 0.918(3) 0.609(3) 0.05 Uiso 1 1 d . . . O1 O 1.3332(3) 0.3043(3) 0.9943(2) 0.0689(11) Uani 1 1 d . . . O2 O 1.3823(3) 0.3191(3) 0.8763(2) 0.0699(11) Uani 1 1 d . . . O7 O 0.6203(3) 0.5193(2) 0.72025(17) 0.0523(9) Uani 1 1 d . . . O8 O 0.8567(4) 0.5359(2) 0.62092(18) 0.0624(11) Uani 1 1 d . . . O9 O 0.8793(3) 0.0889(2) 0.27177(16) 0.0388(8) Uani 1 1 d . . . O10 O 0.8211(3) 0.1102(2) 0.15698(18) 0.0389(8) Uani 1 1 d . . . S1 S 0.93303(10) 0.67681(8) 0.82491(6) 0.0317(3) Uani 1 1 d . . . S2 S 0.69779(10) 0.98456(8) 0.90082(6) 0.0351(3) Uani 1 1 d . . . S3 S 1.14277(17) 0.86483(10) 0.43207(7) 0.0713(5) Uani 1 1 d . . . F1 F 0.6379(3) 0.1182(3) 0.31899(18) 0.0782(10) Uani 1 1 d . . . F2 F 0.5830(2) 0.1347(2) 0.21118(18) 0.0677(9) Uani 1 1 d . . . F3 F 0.6261(3) -0.0108(2) 0.2677(2) 0.1021(14) Uani 1 1 d . . . N11 N 0.3333(4) 0.6577(4) 0.0222(3) 0.0898(19) Uani 1 1 d D . . C46 C 0.3686(4) 0.7378(4) 0.0017(3) 0.0446(13) Uani 1 1 d D . . C47 C 0.4111(4) 0.8383(3) -0.0267(3) 0.0518(14) Uani 1 1 d D . . H47A H 0.5025 0.8389 -0.0411 0.078 Uiso 1 1 calc R . . H47B H 0.3934 0.8801 0.0112 0.078 Uiso 1 1 calc R . . H47C H 0.3666 0.8653 -0.0698 0.078 Uiso 1 1 calc R . . N12 N 0.4232(10) 0.8333(8) 0.3536(6) 0.117(3) Uani 0.643(4) 1 d PD A 1 C48 C 0.4332(9) 0.8049(8) 0.2993(6) 0.075(3) Uani 0.643(4) 1 d PD A 1 C49 C 0.438(2) 0.7856(19) 0.2260(8) 0.123(6) Uani 0.643(4) 1 d PD A 1 H49A H 0.5093 0.7418 0.2171 0.185 Uiso 0.643(4) 1 calc PR A 1 H49B H 0.4487 0.8495 0.1912 0.185 Uiso 0.643(4) 1 calc PR A 1 H49C H 0.3587 0.7524 0.2193 0.185 Uiso 0.643(4) 1 calc PR A 1 N12B N 0.2954(17) 0.7115(14) 0.1831(10) 0.117(3) Uani 0.357(4) 1 d PD A 2 C48B C 0.3690(18) 0.7458(16) 0.2122(11) 0.075(3) Uani 0.357(4) 1 d PD A 2 C49B C 0.468(3) 0.776(4) 0.251(2) 0.123(6) Uani 0.357(4) 1 d PD A 2 H49D H 0.5494 0.7558 0.2293 0.185 Uiso 0.357(4) 1 calc PR A 2 H49E H 0.4544 0.7431 0.3029 0.185 Uiso 0.357(4) 1 calc PR A 2 H49F H 0.4669 0.8492 0.2478 0.185 Uiso 0.357(4) 1 calc PR A 2 C29 C 1.2158(17) 1.006(2) 0.5365(13) 0.025(3) Uani 0.643(4) 1 d P A 1 C30 C 1.3193(10) 1.0006(7) 0.4853(8) 0.034(3) Uani 0.643(4) 1 d P A 1 H30 H 1.3311 0.9427 0.4629 0.041 Uiso 0.643(4) 1 calc PR A 1 C31 C 1.4080(11) 1.0836(7) 0.4670(6) 0.033(2) Uani 0.643(4) 1 d P A 1 H31 H 1.4794 1.0822 0.4322 0.04 Uiso 0.643(4) 1 calc PR A 1 C32 C 1.3865(13) 1.1656(9) 0.5016(6) 0.028(2) Uani 0.643(4) 1 d P A 1 C33 C 1.2843(8) 1.1703(7) 0.5519(4) 0.035(2) Uani 0.643(4) 1 d P A 1 H33 H 1.2716 1.2282 0.5743 0.043 Uiso 0.643(4) 1 calc PR A 1 C34 C 1.1987(10) 1.0883(9) 0.5699(4) 0.032(2) Uani 0.643(4) 1 d P A 1 H34 H 1.1285 1.0901 0.6055 0.039 Uiso 0.643(4) 1 calc PR A 1 N10 N 1.4786(9) 1.2479(7) 0.4869(5) 0.043(2) Uani 0.643(4) 1 d P A 1 O5 O 1.4528(7) 1.3290(5) 0.5064(5) 0.074(2) Uani 0.643(4) 1 d P A 1 O6 O 1.5784(6) 1.2347(5) 0.4509(4) 0.0595(16) Uani 0.643(4) 1 d P A 1 C29B C 1.248(4) 1.006(4) 0.548(3) 0.025(3) Uani 0.357(4) 1 d P A 2 C30B C 1.223(2) 1.0792(17) 0.5942(9) 0.034(3) Uani 0.357(4) 1 d P A 2 H30B H 1.1548 1.068 0.632 0.041 Uiso 0.357(4) 1 calc PR A 2 C31B C 1.2938(15) 1.1636(13) 0.5854(9) 0.033(2) Uani 0.357(4) 1 d P A 2 H31B H 1.2785 1.2102 0.6181 0.04 Uiso 0.357(4) 1 calc PR A 2 C32B C 1.387(3) 1.182(2) 0.5295(11) 0.028(2) Uani 0.357(4) 1 d P A 2 C33B C 1.405(3) 1.1165(16) 0.4797(15) 0.035(2) Uani 0.357(4) 1 d P A 2 H33B H 1.4631 1.1353 0.4373 0.043 Uiso 0.357(4) 1 calc PR A 2 C34B C 1.343(2) 1.0272(17) 0.4890(16) 0.032(2) Uani 0.357(4) 1 d P A 2 H34B H 1.3621 0.9805 0.4569 0.039 Uiso 0.357(4) 1 calc PR A 2 N10B N 1.469(2) 1.2750(15) 0.5194(10) 0.043(2) Uani 0.357(4) 1 d P A 2 O5B O 1.5585(16) 1.2811(9) 0.4630(10) 0.074(2) Uani 0.357(4) 1 d P A 2 O6B O 1.4568(10) 1.3244(9) 0.5585(7) 0.0595(16) Uani 0.357(4) 1 d P A 2 C38 C 0.9423(7) 0.8870(7) 0.9969(5) 0.0190(17) Uani 0.643(4) 1 d PU A 1 C39 C 1.0517(18) 0.8520(16) 1.0194(8) 0.026(3) Uani 0.643(4) 1 d P A 1 H39 H 1.1217 0.8477 0.9841 0.031 Uiso 0.643(4) 1 calc PR A 1 C40 C 1.0654(11) 0.8212(12) 1.0947(7) 0.030(3) Uani 0.643(4) 1 d P A 1 H40 H 1.1431 0.7945 1.1105 0.036 Uiso 0.643(4) 1 calc PR A 1 C41 C 0.9641(12) 0.8303(10) 1.1453(9) 0.029(3) Uani 0.643(4) 1 d P A 1 C42 C 0.8527(11) 0.8747(17) 1.1228(13) 0.036(4) Uani 0.643(4) 1 d P A 1 H42 H 0.7868 0.8859 1.1588 0.044 Uiso 0.643(4) 1 calc PR A 1 C43 C 0.837(4) 0.902(4) 1.051(3) 0.033(6) Uani 0.643(4) 1 d P A 1 H43 H 0.7594 0.9304 1.0357 0.04 Uiso 0.643(4) 1 calc PR A 1 N7 N 0.9795(9) 0.8008(7) 1.2222(6) 0.048(3) Uani 0.643(4) 1 d P A 1 O3 O 0.8875(8) 0.8115(6) 1.2695(4) 0.065(2) Uani 0.643(4) 1 d P A 1 O4 O 1.0798(7) 0.7644(4) 1.2422(4) 0.0523(16) Uani 0.643(4) 1 d P A 1 C38B C 0.9082(16) 0.8940(13) 1.0067(11) 0.0190(17) Uani 0.357(4) 1 d P A 2 C39B C 1.025(4) 0.848(3) 1.0408(17) 0.026(3) Uani 0.357(4) 1 d P A 2 H39B H 1.0979 0.8348 1.0104 0.031 Uiso 0.357(4) 1 calc PR A 2 C40B C 1.023(3) 0.827(3) 1.1159(17) 0.030(3) Uani 0.357(4) 1 d P A 2 H40B H 1.0949 0.7996 1.1389 0.036 Uiso 0.357(4) 1 calc PR A 2 C41B C 0.915(3) 0.845(2) 1.1567(19) 0.029(3) Uani 0.357(4) 1 d P A 2 C42B C 0.806(3) 0.872(4) 1.128(3) 0.036(4) Uani 0.357(4) 1 d P A 2 H42B H 0.7289 0.873 1.159 0.044 Uiso 0.357(4) 1 calc PR A 2 C43B C 0.810(9) 0.902(8) 1.046(7) 0.033(6) Uani 0.357(4) 1 d P A 2 H43B H 0.7358 0.9266 1.0244 0.04 Uiso 0.357(4) 1 calc PR A 2 N7B N 0.912(3) 0.8080(19) 1.2397(12) 0.048(3) Uani 0.357(4) 1 d P A 2 O4B O 0.8107(12) 0.8006(9) 1.2706(6) 0.0523(16) Uani 0.357(4) 1 d P A 2 O3B O 1.0115(18) 0.7925(10) 1.2647(7) 0.065(2) Uani 0.357(4) 1 d P A 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 C1 0.041(3) 0.017(2) 0.034(3) -0.0018(19) -0.011(2) 0.000(2) C2 0.035(2) 0.022(2) 0.033(3) -0.005(2) -0.008(2) 0.0012(19) C3 0.041(3) 0.021(2) 0.027(2) -0.0013(19) -0.004(2) -0.003(2) C4 0.033(3) 0.016(2) 0.037(3) -0.0019(19) -0.009(2) -0.0028(19) C5 0.039(3) 0.022(2) 0.037(3) -0.003(2) -0.004(2) -0.001(2) C6 0.043(3) 0.021(2) 0.050(3) -0.007(2) 0.009(2) -0.003(2) C7 0.033(3) 0.017(2) 0.058(3) -0.004(2) -0.015(3) 0.000(2) C8 0.044(3) 0.021(2) 0.041(3) -0.005(2) -0.016(2) -0.002(2) C9 0.042(3) 0.020(2) 0.031(3) -0.0036(19) -0.008(2) -0.001(2) C10 0.039(3) 0.029(3) 0.037(3) 0.000(2) -0.005(2) -0.003(2) C11 0.034(3) 0.023(3) 0.068(4) 0.002(2) -0.012(3) -0.003(2) C12 0.047(3) 0.033(3) 0.089(4) 0.003(3) -0.011(3) -0.012(3) C13 0.028(3) 0.028(3) 0.122(6) 0.000(3) -0.012(3) -0.003(2) C14 0.079(5) 0.045(4) 0.099(6) 0.004(4) -0.037(4) -0.016(3) C15 0.077(4) 0.048(4) 0.072(4) 0.010(3) -0.033(4) -0.011(3) C16 0.062(4) 0.034(3) 0.047(3) 0.011(2) -0.029(3) -0.014(3) C17 0.134(6) 0.055(4) 0.035(3) -0.002(3) -0.022(4) -0.035(4) C18 0.121(6) 0.044(4) 0.057(4) -0.014(3) 0.005(4) -0.010(4) C19 0.108(5) 0.027(3) 0.030(3) -0.010(2) -0.012(3) 0.004(3) C20 0.139(6) 0.020(3) 0.030(3) -0.001(2) -0.020(3) 0.000(3) C21 0.115(6) 0.049(4) 0.057(4) -0.027(3) -0.029(4) 0.025(4) C22 0.103(5) 0.043(4) 0.058(4) -0.017(3) -0.032(3) 0.017(3) C23 0.098(5) 0.028(3) 0.049(3) -0.012(2) -0.030(3) 0.004(3) C24 0.088(4) 0.026(3) 0.025(3) -0.007(2) -0.023(3) 0.006(3) C25 0.086(4) 0.027(3) 0.028(3) -0.003(2) -0.014(3) 0.002(3) C26 0.052(3) 0.021(2) 0.032(3) -0.0009(19) -0.014(2) 0.001(2) C27 0.078(4) 0.023(3) 0.035(3) 0.000(2) -0.002(3) 0.005(3) C28 0.048(3) 0.021(2) 0.025(3) 0.0038(19) -0.008(2) 0.000(2) C35 0.039(3) 0.020(2) 0.035(3) -0.0037(19) -0.012(2) 0.006(2) C36 0.038(3) 0.022(2) 0.028(2) -0.0031(19) -0.008(2) 0.000(2) C37 0.028(2) 0.016(2) 0.031(3) -0.0049(18) -0.006(2) -0.0008(18) C44 0.035(3) 0.025(3) 0.049(3) -0.014(2) -0.002(3) 0.002(2) C45 0.027(3) 0.040(3) 0.074(4) -0.001(3) 0.001(3) 0.004(2) N1 0.040(2) 0.0212(19) 0.028(2) -0.0002(16) -0.0141(17) 0.0013(17) N2 0.032(2) 0.0209(19) 0.034(2) -0.0001(16) -0.0080(17) 0.0031(16) N3 0.033(2) 0.027(2) 0.032(2) 0.0053(17) -0.0017(17) -0.0033(17) N4 0.045(3) 0.030(2) 0.079(4) -0.004(2) -0.011(3) -0.004(2) N5 0.0206(18) 0.025(2) 0.029(2) -0.0038(16) -0.0016(17) 0.0019(16) N6 0.030(2) 0.024(2) 0.030(2) -0.0039(16) -0.0059(17) 0.0013(17) N8 0.075(3) 0.0166(19) 0.024(2) 0.0001(16) -0.0084(19) 0.0040(19) N9 0.067(3) 0.027(2) 0.027(2) -0.0015(19) 0.009(2) -0.005(2) O1 0.061(2) 0.064(3) 0.084(3) -0.002(2) -0.037(2) 0.0097(19) O2 0.049(2) 0.055(3) 0.099(3) -0.006(2) 0.008(2) 0.0098(19) O7 0.071(3) 0.048(2) 0.040(2) -0.0062(17) -0.0146(18) -0.0066(19) O8 0.117(3) 0.0239(19) 0.043(2) -0.0004(16) 0.001(2) -0.011(2) O9 0.0313(17) 0.046(2) 0.0408(19) -0.0140(15) -0.0029(15) -0.0039(14) O10 0.0328(18) 0.0396(19) 0.046(2) -0.0094(16) -0.0088(15) 0.0016(14) S1 0.0364(6) 0.0226(6) 0.0343(7) 0.0026(5) -0.0082(5) -0.0022(5) S2 0.0287(6) 0.0383(7) 0.0389(7) -0.0102(5) -0.0005(5) 0.0003(5) S3 0.1507(15) 0.0349(8) 0.0229(7) 0.0043(6) 0.0014(8) -0.0005(8) F1 0.0511(19) 0.103(3) 0.070(2) -0.005(2) 0.0230(17) 0.0166(17) F2 0.0321(16) 0.068(2) 0.098(3) -0.0012(18) -0.0058(16) 0.0102(15) F3 0.0433(19) 0.0378(19) 0.212(4) 0.003(2) 0.006(2) -0.0124(15) N11 0.049(3) 0.080(4) 0.116(5) 0.062(3) -0.026(3) -0.018(3) C46 0.029(3) 0.059(4) 0.039(3) 0.011(3) -0.003(2) 0.000(3) C47 0.049(3) 0.037(3) 0.071(4) -0.014(3) -0.009(3) 0.003(2) N12 0.113(7) 0.122(8) 0.117(8) -0.027(6) -0.002(6) -0.015(6) C48 0.068(6) 0.075(7) 0.082(7) -0.025(6) 0.018(5) -0.005(5) C49 0.172(14) 0.097(9) 0.086(16) 0.004(12) 0.025(10) 0.037(10) N12B 0.113(7) 0.122(8) 0.117(8) -0.027(6) -0.002(6) -0.015(6) C48B 0.068(6) 0.075(7) 0.082(7) -0.025(6) 0.018(5) -0.005(5) C49B 0.172(14) 0.097(9) 0.086(16) 0.004(12) 0.025(10) 0.037(10) C29 0.022(10) 0.027(3) 0.023(8) 0.010(5) -0.011(5) 0.006(7) C30 0.034(5) 0.024(5) 0.038(5) 0.007(5) -0.004(4) -0.007(3) C31 0.034(4) 0.026(5) 0.034(6) 0.008(4) 0.000(4) 0.015(4) C32 0.038(3) 0.024(6) 0.021(8) -0.002(5) -0.003(7) 0.001(4) C33 0.046(5) 0.029(4) 0.025(5) 0.004(4) 0.006(4) -0.001(4) C34 0.038(5) 0.033(5) 0.025(4) -0.005(4) 0.000(4) 0.003(4) N10 0.038(3) 0.034(6) 0.050(7) 0.009(4) 0.006(5) 0.001(4) O5 0.083(5) 0.042(4) 0.085(5) 0.015(4) 0.004(4) -0.020(3) O6 0.047(3) 0.048(4) 0.075(4) 0.007(4) 0.003(3) -0.009(3) C29B 0.022(10) 0.027(3) 0.023(8) 0.010(5) -0.011(5) 0.006(7) C30B 0.034(5) 0.024(5) 0.038(5) 0.007(5) -0.004(4) -0.007(3) C31B 0.034(4) 0.026(5) 0.034(6) 0.008(4) 0.000(4) 0.015(4) C32B 0.038(3) 0.024(6) 0.021(8) -0.002(5) -0.003(7) 0.001(4) C33B 0.046(5) 0.029(4) 0.025(5) 0.004(4) 0.006(4) -0.001(4) C34B 0.038(5) 0.033(5) 0.025(4) -0.005(4) 0.000(4) 0.003(4) N10B 0.038(3) 0.034(6) 0.050(7) 0.009(4) 0.006(5) 0.001(4) O5B 0.083(5) 0.042(4) 0.085(5) 0.015(4) 0.004(4) -0.020(3) O6B 0.047(3) 0.048(4) 0.075(4) 0.007(4) 0.003(3) -0.009(3) C38 0.019(3) 0.017(2) 0.020(2) -0.0038(15) 0.0002(19) -0.0002(19) C39 0.036(8) 0.023(3) 0.017(9) 0.004(7) -0.002(5) -0.014(5) C40 0.038(8) 0.022(3) 0.027(8) 0.002(5) -0.008(5) -0.009(6) C41 0.051(12) 0.013(5) 0.026(7) -0.007(4) -0.004(7) 0.007(7) C42 0.052(12) 0.023(3) 0.032(5) -0.006(3) 0.009(10) -0.016(10) C43 0.053(19) 0.019(3) 0.029(8) -0.004(4) -0.014(12) -0.005(12) N7 0.092(11) 0.028(3) 0.022(6) -0.001(3) 0.006(5) -0.023(7) O3 0.097(7) 0.059(4) 0.037(4) 0.002(4) -0.022(5) -0.018(5) O4 0.083(5) 0.042(3) 0.032(3) 0.004(2) -0.021(3) -0.012(3) C38B 0.019(3) 0.017(2) 0.020(2) -0.0038(15) 0.0002(19) -0.0002(19) C39B 0.036(8) 0.023(3) 0.017(9) 0.004(7) -0.002(5) -0.014(5) C40B 0.038(8) 0.022(3) 0.027(8) 0.002(5) -0.008(5) -0.009(6) C41B 0.051(12) 0.013(5) 0.026(7) -0.007(4) -0.004(7) 0.007(7) C42B 0.052(12) 0.023(3) 0.032(5) -0.006(3) 0.009(10) -0.016(10) C43B 0.053(19) 0.019(3) 0.029(8) -0.004(4) -0.014(12) -0.005(12) N7B 0.092(11) 0.028(3) 0.022(6) -0.001(3) 0.006(5) -0.023(7) O4B 0.083(5) 0.042(3) 0.032(3) 0.004(2) -0.021(3) -0.012(3) O3B 0.097(7) 0.059(4) 0.037(4) 0.002(4) -0.022(5) -0.018(5) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N1 1.499(5) . ? C1 C2 1.530(5) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 N2 1.456(5) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 N2 1.337(5) . ? C3 N3 1.368(5) . ? C3 S1 1.695(4) . ? C4 C9 1.384(5) . ? C4 C5 1.391(6) . ? C4 N3 1.415(5) . ? C5 C6 1.388(6) . ? C5 H5 0.95 . ? C6 C7 1.388(6) . ? C6 H6 0.95 . ? C7 C8 1.361(6) . ? C7 N4 1.490(6) . ? C8 C9 1.370(6) . ? C8 H8 0.95 . ? C9 H9 0.95 . ? C10 N2 1.483(5) . ? C10 C11 1.506(6) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 C12 1.379(6) . ? C11 C16 1.401(7) . ? C12 C13 1.458(7) . ? C12 H12 0.95 . ? C13 C14 1.355(8) . ? C13 H13 0.95 . ? C14 C15 1.339(8) . ? C14 H14 0.95 . ? C15 C16 1.391(7) . ? C15 H15 0.95 . ? C16 O7 1.348(6) . ? C17 O7 1.444(6) . ? C17 C18 1.500(8) . ? C17 H17A 0.99 . ? C17 H17B 0.99 . ? C18 O8 1.418(6) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C24 1.364(7) . ? C19 O8 1.375(6) . ? C19 C20 1.419(7) . ? C20 C21 1.380(8) . ? C20 H20 0.95 . ? C21 C22 1.347(8) . ? C21 H21 0.95 . ? C22 C23 1.378(7) . ? C22 H22 0.95 . ? C23 C24 1.396(7) . ? C23 H23 0.95 . ? C24 C25 1.508(6) . ? C25 N8 1.473(5) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 N1 1.500(5) . ? C26 C28 1.530(6) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? C27 N8 1.354(6) . ? C27 N9 1.366(6) . ? C27 S3 1.675(5) . ? C28 N8 1.456(5) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C35 N1 1.505(5) . ? C35 C36 1.514(5) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 N5 1.447(5) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? C37 N5 1.350(5) . ? C37 N6 1.368(5) . ? C37 S2 1.670(4) . ? C44 O10 1.237(5) . ? C44 O9 1.246(5) . ? C44 C45 1.529(6) . ? C45 F1 1.323(6) . ? C45 F2 1.326(5) . ? C45 F3 1.329(5) . ? N1 H1N 0.90(4) . ? N3 H3N 0.84(4) . ? N4 O2 1.211(5) . ? N4 O1 1.234(5) . ? N5 H5N 0.85(4) . ? N6 C38 1.345(10) . ? N6 C38B 1.51(2) . ? N6 H6N 0.81(4) . ? N9 C29 1.36(3) . ? N9 C29B 1.55(5) . ? N9 H9N 0.84(4) . ? N11 C46 1.131(5) . ? C46 C47 1.421(6) . ? C47 H47A 0.98 . ? C47 H47B 0.98 . ? C47 H47C 0.98 . ? N12 C48 1.133(5) . ? C48 C49 1.421(7) . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? N12B C48B 1.132(5) . ? C48B C49B 1.421(7) . ? C49B H49D 0.98 . ? C49B H49E 0.98 . ? C49B H49F 0.98 . ? C29 C34 1.36(3) . ? C29 C30 1.39(3) . ? C30 C31 1.435(14) . ? C30 H30 0.95 . ? C31 C32 1.379(12) . ? C31 H31 0.95 . ? C32 C33 1.369(16) . ? C32 N10 1.451(17) . ? C33 C34 1.403(15) . ? C33 H33 0.95 . ? C34 H34 0.95 . ? N10 O6 1.226(11) . ? N10 O5 1.233(10) . ? C29B C34B 1.41(6) . ? C29B C30B 1.42(6) . ? C30B C31B 1.34(3) . ? C30B H30B 0.95 . ? C31B C32B 1.35(4) . ? C31B H31B 0.95 . ? C32B C33B 1.38(3) . ? C32B N10B 1.50(4) . ? C33B C34B 1.35(3) . ? C33B H33B 0.95 . ? C34B H34B 0.95 . ? N10B O6B 1.067(19) . ? N10B O5B 1.33(3) . ? C38 C39 1.33(2) . ? C38 C43 1.47(6) . ? C39 C40 1.41(2) . ? C39 H39 0.95 . ? C40 C41 1.376(15) . ? C40 H40 0.95 . ? C41 C42 1.39(3) . ? C41 N7 1.43(2) . ? C42 C43 1.34(6) . ? C42 H42 0.95 . ? C43 H43 0.95 . ? N7 O4 1.231(12) . ? N7 O3 1.273(11) . ? C38B C43B 1.23(12) . ? C38B C39B 1.52(5) . ? C39B C40B 1.37(5) . ? C39B H39B 0.95 . ? C40B C41B 1.35(3) . ? C40B H40B 0.95 . ? C41B C42B 1.34(5) . ? C41B N7B 1.53(4) . ? C42B C43B 1.50(12) . ? C42B H42B 0.95 . ? C43B H43B 0.95 . ? N7B O4B 1.16(3) . ? N7B O3B 1.20(4) . ? 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 111.0(3) . . ? N1 C1 H1A 109.4 . . ? C2 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? C2 C1 H1B 109.4 . . ? H1A C1 H1B 108 . . ? N2 C2 C1 112.3(3) . . ? N2 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? N2 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? N2 C3 N3 117.0(4) . . ? N2 C3 S1 122.4(3) . . ? N3 C3 S1 120.6(3) . . ? C9 C4 C5 120.3(4) . . ? C9 C4 N3 118.2(4) . . ? C5 C4 N3 121.5(4) . . ? C6 C5 C4 119.8(4) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C7 117.9(4) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? C8 C7 C6 122.7(4) . . ? C8 C7 N4 118.0(4) . . ? C6 C7 N4 119.3(4) . . ? C7 C8 C9 119.1(4) . . ? C7 C8 H8 120.4 . . ? C9 C8 H8 120.4 . . ? C8 C9 C4 120.1(4) . . ? C8 C9 H9 120 . . ? C4 C9 H9 120 . . ? N2 C10 C11 111.5(3) . . ? N2 C10 H10A 109.3 . . ? C11 C10 H10A 109.3 . . ? N2 C10 H10B 109.3 . . ? C11 C10 H10B 109.3 . . ? H10A C10 H10B 108 . . ? C12 C11 C16 119.2(5) . . ? C12 C11 C10 121.5(5) . . ? C16 C11 C10 119.3(4) . . ? C11 C12 C13 119.2(5) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? C14 C13 C12 117.3(5) . . ? C14 C13 H13 121.4 . . ? C12 C13 H13 121.4 . . ? C15 C14 C13 124.8(6) . . ? C15 C14 H14 117.6 . . ? C13 C14 H14 117.6 . . ? C14 C15 C16 118.4(6) . . ? C14 C15 H15 120.8 . . ? C16 C15 H15 120.8 . . ? O7 C16 C15 123.6(5) . . ? O7 C16 C11 115.2(4) . . ? C15 C16 C11 121.2(6) . . ? O7 C17 C18 107.6(5) . . ? O7 C17 H17A 110.2 . . ? C18 C17 H17A 110.2 . . ? O7 C17 H17B 110.2 . . ? C18 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? O8 C18 C17 106.6(5) . . ? O8 C18 H18A 110.4 . . ? C17 C18 H18A 110.4 . . ? O8 C18 H18B 110.4 . . ? C17 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? C24 C19 O8 115.8(5) . . ? C24 C19 C20 120.5(6) . . ? O8 C19 C20 123.7(5) . . ? C21 C20 C19 119.2(5) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? C22 C21 C20 120.9(6) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 119.3(6) . . ? C21 C22 H22 120.4 . . ? C23 C22 H22 120.4 . . ? C22 C23 C24 122.4(5) . . ? C22 C23 H23 118.8 . . ? C24 C23 H23 118.8 . . ? C19 C24 C23 117.6(5) . . ? C19 C24 C25 123.3(5) . . ? C23 C24 C25 119.1(5) . . ? N8 C25 C24 110.3(4) . . ? N8 C25 H25A 109.6 . . ? C24 C25 H25A 109.6 . . ? N8 C25 H25B 109.6 . . ? C24 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? N1 C26 C28 113.0(3) . . ? N1 C26 H26A 109 . . ? C28 C26 H26A 109 . . ? N1 C26 H26B 109 . . ? C28 C26 H26B 109 . . ? H26A C26 H26B 107.8 . . ? N8 C27 N9 114.7(4) . . ? N8 C27 S3 121.9(4) . . ? N9 C27 S3 123.3(4) . . ? N8 C28 C26 108.7(3) . . ? N8 C28 H28A 110 . . ? C26 C28 H28A 110 . . ? N8 C28 H28B 110 . . ? C26 C28 H28B 110 . . ? H28A C28 H28B 108.3 . . ? N1 C35 C36 111.0(3) . . ? N1 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? N1 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108 . . ? N5 C36 C35 112.1(3) . . ? N5 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? N5 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? N5 C37 N6 111.5(3) . . ? N5 C37 S2 121.4(3) . . ? N6 C37 S2 127.1(3) . . ? O10 C44 O9 128.8(4) . . ? O10 C44 C45 115.7(4) . . ? O9 C44 C45 115.5(4) . . ? F1 C45 F2 105.3(4) . . ? F1 C45 F3 107.0(4) . . ? F2 C45 F3 106.2(4) . . ? F1 C45 C44 113.6(4) . . ? F2 C45 C44 113.8(4) . . ? F3 C45 C44 110.4(4) . . ? C1 N1 C26 112.9(3) . . ? C1 N1 C35 111.1(3) . . ? C26 N1 C35 111.7(3) . . ? C1 N1 H1N 106(3) . . ? C26 N1 H1N 109(3) . . ? C35 N1 H1N 106(3) . . ? C3 N2 C2 119.3(3) . . ? C3 N2 C10 124.0(3) . . ? C2 N2 C10 116.7(3) . . ? C3 N3 C4 125.6(4) . . ? C3 N3 H3N 114(3) . . ? C4 N3 H3N 117(3) . . ? O2 N4 O1 125.3(5) . . ? O2 N4 C7 117.2(5) . . ? O1 N4 C7 117.6(5) . . ? C37 N5 C36 124.4(3) . . ? C37 N5 H5N 124(3) . . ? C36 N5 H5N 112(3) . . ? C38 N6 C37 138.6(5) . . ? C37 N6 C38B 123.5(7) . . ? C38 N6 H6N 109(3) . . ? C37 N6 H6N 112(3) . . ? C38B N6 H6N 124(3) . . ? C27 N8 C28 124.6(4) . . ? C27 N8 C25 121.6(4) . . ? C28 N8 C25 113.7(3) . . ? C29 N9 C27 125.6(10) . . ? C27 N9 C29B 133.6(19) . . ? C29 N9 H9N 111(3) . . ? C27 N9 H9N 123(3) . . ? C29B N9 H9N 103(4) . . ? C16 O7 C17 119.8(4) . . ? C19 O8 C18 116.7(4) . . ? N11 C46 C47 177.8(6) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N12 C48 C49 170.2(15) . . ? N12B C48B C49B 172(2) . . ? C48B C49B H49D 109.5 . . ? C48B C49B H49E 109.5 . . ? H49D C49B H49E 109.5 . . ? C48B C49B H49F 109.5 . . ? H49D C49B H49F 109.5 . . ? H49E C49B H49F 109.5 . . ? N9 C29 C34 119(2) . . ? N9 C29 C30 119(2) . . ? C34 C29 C30 121.1(18) . . ? C29 C30 C31 119.0(13) . . ? C29 C30 H30 120.5 . . ? C31 C30 H30 120.5 . . ? C32 C31 C30 118.0(12) . . ? C32 C31 H31 121 . . ? C30 C31 H31 121 . . ? C33 C32 C31 122.5(12) . . ? C33 C32 N10 118.5(9) . . ? C31 C32 N10 118.9(12) . . ? C32 C33 C34 119.0(9) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C29 C34 C33 120.4(13) . . ? C29 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? O6 N10 O5 122.5(10) . . ? O6 N10 C32 117.0(8) . . ? O5 N10 C32 120.4(9) . . ? C34B C29B C30B 119(4) . . ? C34B C29B N9 129(4) . . ? C30B C29B N9 112(3) . . ? C31B C30B C29B 121(3) . . ? C31B C30B H30B 119.3 . . ? C29B C30B H30B 119.3 . . ? C30B C31B C32B 119.3(19) . . ? C30B C31B H31B 120.3 . . ? C32B C31B H31B 120.3 . . ? C31B C32B C33B 120(3) . . ? C31B C32B N10B 120.2(17) . . ? C33B C32B N10B 120(3) . . ? C34B C33B C32B 123(3) . . ? C34B C33B H33B 118.6 . . ? C32B C33B H33B 118.6 . . ? C33B C34B C29B 117(3) . . ? C33B C34B H34B 121.4 . . ? C29B C34B H34B 121.4 . . ? O6B N10B O5B 127(2) . . ? O6B N10B C32B 119.4(19) . . ? O5B N10B C32B 113.0(17) . . ? N6 C38 C39 118.3(7) . . ? N6 C38 C43 121(2) . . ? C39 C38 C43 120(2) . . ? C38 C39 C40 120.8(10) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C41 C40 C39 118.9(16) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C40 C41 C42 120.8(16) . . ? C40 C41 N7 118.6(13) . . ? C42 C41 N7 120.5(12) . . ? C43 C42 C41 121(3) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C42 C43 C38 118(3) . . ? C42 C43 H43 121 . . ? C38 C43 H43 121 . . ? O4 N7 O3 120.5(10) . . ? O4 N7 C41 120.4(9) . . ? O3 N7 C41 119.1(10) . . ? C43B C38B C39B 120(5) . . ? C43B C38B N6 130(5) . . ? C39B C38B N6 109.3(15) . . ? C40B C39B C38B 119(3) . . ? C40B C39B H39B 120.5 . . ? C38B C39B H39B 120.5 . . ? C41B C40B C39B 118(4) . . ? C41B C40B H40B 120.9 . . ? C39B C40B H40B 120.9 . . ? C42B C41B C40B 124(4) . . ? C42B C41B N7B 118(3) . . ? C40B C41B N7B 116(3) . . ? C41B C42B C43B 117(5) . . ? C41B C42B H42B 121.3 . . ? C43B C42B H42B 121.3 . . ? C38B C43B C42B 121(7) . . ? C38B C43B H43B 119.7 . . ? C42B C43B H43B 119.7 . . ? O4B N7B O3B 129(2) . . ? O4B N7B C41B 114(3) . . ? O3B N7B C41B 117(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 N1 C1 C2 N2 -120.4(4) . . . . ? C9 C4 C5 C6 -3.4(6) . . . . ? N3 C4 C5 C6 179.1(4) . . . . ? C4 C5 C6 C7 0.5(6) . . . . ? C5 C6 C7 C8 2.5(6) . . . . ? C5 C6 C7 N4 -176.7(4) . . . . ? C6 C7 C8 C9 -2.5(6) . . . . ? N4 C7 C8 C9 176.7(4) . . . . ? C7 C8 C9 C4 -0.6(6) . . . . ? C5 C4 C9 C8 3.5(6) . . . . ? N3 C4 C9 C8 -178.9(4) . . . . ? N2 C10 C11 C12 -109.0(5) . . . . ? N2 C10 C11 C16 70.4(5) . . . . ? C16 C11 C12 C13 -1.2(6) . . . . ? C10 C11 C12 C13 178.1(4) . . . . ? C11 C12 C13 C14 1.6(7) . . . . ? C12 C13 C14 C15 -0.9(8) . . . . ? C13 C14 C15 C16 -0.2(8) . . . . ? C14 C15 C16 O7 -177.3(5) . . . . ? C14 C15 C16 C11 0.7(7) . . . . ? C12 C11 C16 O7 178.2(4) . . . . ? C10 C11 C16 O7 -1.2(6) . . . . ? C12 C11 C16 C15 0.1(7) . . . . ? C10 C11 C16 C15 -179.3(4) . . . . ? O7 C17 C18 O8 -81.8(5) . . . . ? C24 C19 C20 C21 0.0(7) . . . . ? O8 C19 C20 C21 -178.3(5) . . . . ? C19 C20 C21 C22 0.3(8) . . . . ? C20 C21 C22 C23 0.4(8) . . . . ? C21 C22 C23 C24 -1.4(8) . . . . ? O8 C19 C24 C23 177.5(4) . . . . ? C20 C19 C24 C23 -0.9(7) . . . . ? O8 C19 C24 C25 -1.8(7) . . . . ? C20 C19 C24 C25 179.7(4) . . . . ? C22 C23 C24 C19 1.6(7) . . . . ? C22 C23 C24 C25 -178.9(4) . . . . ? C19 C24 C25 N8 110.4(5) . . . . ? C23 C24 C25 N8 -69.0(5) . . . . ? N1 C26 C28 N8 172.9(3) . . . . ? N1 C35 C36 N5 -53.7(5) . . . . ? O10 C44 C45 F1 -150.3(4) . . . . ? O9 C44 C45 F1 32.5(6) . . . . ? O10 C44 C45 F2 -29.8(6) . . . . ? O9 C44 C45 F2 152.9(4) . . . . ? O10 C44 C45 F3 89.5(5) . . . . ? O9 C44 C45 F3 -87.8(5) . . . . ? C2 C1 N1 C26 160.7(3) . . . . ? C2 C1 N1 C35 -73.0(4) . . . . ? C28 C26 N1 C1 -83.0(4) . . . . ? C28 C26 N1 C35 150.9(3) . . . . ? C36 C35 N1 C1 153.6(3) . . . . ? C36 C35 N1 C26 -79.4(4) . . . . ? N3 C3 N2 C2 174.0(3) . . . . ? S1 C3 N2 C2 -4.4(5) . . . . ? N3 C3 N2 C10 -4.2(6) . . . . ? S1 C3 N2 C10 177.5(3) . . . . ? C1 C2 N2 C3 75.6(5) . . . . ? C1 C2 N2 C10 -106.1(4) . . . . ? C11 C10 N2 C3 -145.4(4) . . . . ? C11 C10 N2 C2 36.4(5) . . . . ? N2 C3 N3 C4 174.7(4) . . . . ? S1 C3 N3 C4 -6.9(6) . . . . ? C9 C4 N3 C3 126.9(4) . . . . ? C5 C4 N3 C3 -55.5(6) . . . . ? C8 C7 N4 O2 170.7(4) . . . . ? C6 C7 N4 O2 -10.1(6) . . . . ? C8 C7 N4 O1 -8.9(6) . . . . ? C6 C7 N4 O1 170.4(4) . . . . ? N6 C37 N5 C36 -176.6(3) . . . . ? S2 C37 N5 C36 3.3(5) . . . . ? C35 C36 N5 C37 -78.0(5) . . . . ? N5 C37 N6 C38 179.8(7) . . . . ? S2 C37 N6 C38 -0.1(9) . . . . ? N5 C37 N6 C38B 179.1(9) . . . . ? S2 C37 N6 C38B -0.8(10) . . . . ? N9 C27 N8 C28 7.3(6) . . . . ? S3 C27 N8 C28 -171.4(3) . . . . ? N9 C27 N8 C25 -175.4(4) . . . . ? S3 C27 N8 C25 5.9(6) . . . . ? C26 C28 N8 C27 79.7(5) . . . . ? C26 C28 N8 C25 -97.8(4) . . . . ? C24 C25 N8 C27 107.7(5) . . . . ? C24 C25 N8 C28 -74.7(5) . . . . ? N8 C27 N9 C29 -174.9(10) . . . . ? S3 C27 N9 C29 3.7(12) . . . . ? N8 C27 N9 C29B 169(2) . . . . ? S3 C27 N9 C29B -12(2) . . . . ? C15 C16 O7 C17 -14.5(7) . . . . ? C11 C16 O7 C17 167.5(4) . . . . ? C18 C17 O7 C16 179.3(4) . . . . ? C24 C19 O8 C18 161.6(4) . . . . ? C20 C19 O8 C18 -20.0(7) . . . . ? C17 C18 O8 C19 -168.9(4) . . . . ? C27 N9 C29 C34 147.2(8) . . . . ? C29B N9 C29 C34 -85(12) . . . . ? C27 N9 C29 C30 -44.9(15) . . . . ? C29B N9 C29 C30 83(12) . . . . ? N9 C29 C30 C31 -168.5(11) . . . . ? C34 C29 C30 C31 -1(2) . . . . ? C29 C30 C31 C32 0.3(19) . . . . ? C30 C31 C32 C33 -0.3(17) . . . . ? C30 C31 C32 N10 176.7(11) . . . . ? C31 C32 C33 C34 0.8(15) . . . . ? N10 C32 C33 C34 -176.2(8) . . . . ? N9 C29 C34 C33 169.1(8) . . . . ? C30 C29 C34 C33 1.5(19) . . . . ? C32 C33 C34 C29 -1.4(14) . . . . ? C33 C32 N10 O6 168.7(9) . . . . ? C31 C32 N10 O6 -8.4(14) . . . . ? C33 C32 N10 O5 -15.3(15) . . . . ? C31 C32 N10 O5 167.6(11) . . . . ? C29 N9 C29B C34B -73(11) . . . . ? C27 N9 C29B C34B -11(5) . . . . ? C29 N9 C29B C30B 94(12) . . . . ? C27 N9 C29B C30B 156.8(14) . . . . ? C34B C29B C30B C31B -5(4) . . . . ? N9 C29B C30B C31B -173.8(17) . . . . ? C29B C30B C31B C32B 3(3) . . . . ? C30B C31B C32B C33B 3(3) . . . . ? C30B C31B C32B N10B -178.9(17) . . . . ? C31B C32B C33B C34B -8(4) . . . . ? N10B C32B C33B C34B 174(2) . . . . ? C32B C33B C34B C29B 6(5) . . . . ? C30B C29B C34B C33B 0(4) . . . . ? N9 C29B C34B C33B 167(3) . . . . ? C31B C32B N10B O6B 4(3) . . . . ? C33B C32B N10B O6B -179(2) . . . . ? C31B C32B N10B O5B 179(2) . . . . ? C33B C32B N10B O5B -4(3) . . . . ? C37 N6 C38 C39 -178.8(11) . . . . ? C38B N6 C38 C39 -177(5) . . . . ? C37 N6 C38 C43 -3(3) . . . . ? C38B N6 C38 C43 -1(4) . . . . ? N6 C38 C39 C40 -178.7(14) . . . . ? C43 C38 C39 C40 5(3) . . . . ? C38 C39 C40 C41 -2(3) . . . . ? C39 C40 C41 C42 -4(3) . . . . ? C39 C40 C41 N7 -178.7(13) . . . . ? C40 C41 C42 C43 6(4) . . . . ? N7 C41 C42 C43 -180(3) . . . . ? C41 C42 C43 C38 -2(5) . . . . ? N6 C38 C43 C42 -179(3) . . . . ? C39 C38 C43 C42 -3(5) . . . . ? C40 C41 N7 O4 -3(2) . . . . ? C42 C41 N7 O4 -177.6(13) . . . . ? C40 C41 N7 O3 178.1(13) . . . . ? C42 C41 N7 O3 3.2(19) . . . . ? C38 N6 C38B C43B -173(9) . . . . ? C37 N6 C38B C43B 5(7) . . . . ? C38 N6 C38B C39B 0(3) . . . . ? C37 N6 C38B C39B 178.6(17) . . . . ? C43B C38B C39B C40B -7(7) . . . . ? N6 C38B C39B C40B 179(3) . . . . ? C38B C39B C40B C41B 2(6) . . . . ? C39B C40B C41B C42B 7(7) . . . . ? C39B C40B C41B N7B 173(3) . . . . ? C40B C41B C42B C43B -11(8) . . . . ? N7B C41B C42B C43B -176(5) . . . . ? C39B C38B C43B C42B 4(11) . . . . ? N6 C38B C43B C42B 177(4) . . . . ? C41B C42B C43B C38B 5(11) . . . . ? C42B C41B N7B O4B 5(4) . . . . ? C40B C41B N7B O4B -161(3) . . . . ? C42B C41B N7B O3B -173(3) . . . . ? C40B C41B N7B O3B 20(5) . . . . ? 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 H1N S1 0.90(4) 2.46(4) 3.184(3) 138(3) . N6 H6N O10 0.81(4) 2.11(4) 2.921(5) 176(4) 2_766 N5 H5N O9 0.85(4) 2.02(4) 2.840(4) 161(4) 2_766 N9 H9N O9 0.84(4) 2.19(5) 3.013(5) 164(4) 2_766 N3 H3N N11 0.84(4) 2.14(4) 2.923(6) 154(4) 2_666 # END of CIF