data_global ############################################################################## ### CIF submission form for molecular structure report (Acta Cryst. C) ### ### Version: 7 October 1991 ### ############################################################################## # This is an electronic "form" for submitting a structural paper to Acta Cryst. # Section C as a Crystallographic Information File. Full details of the format # of such files are given in the paper "The Crystallographic Information File # (CIF): a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. An example of a # completed CIF form may be obtained by sending the one-line request # 'send example.cif' # to sendcif@iucr.ac.uk. Queries or requests for further information should be # directed to teched@iucr.ac.uk. # # Note that all fields should be numeric or character type EXCEPT those which # are flagged as 'text' - free-form text of any length may be included in # these latter fields provided the text block begins and ends with a semicolon # as the first character of a new line. . Note also that the query marks # '?' are significant as placeholders, and should not be deleted where a data # item is not given, UNLESS the accompanying data name is also deleted. # Lines should not exceed 80 characters in length. #============================================================================== #============================================================================== # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; ; _publ_contact_author_phone ' ' _publ_contact_author_fax ' ' _publ_contact_author_email ? _publ_requested_journal 'test' _publ_requested_coeditor_name ? #============================================================================== # 2. PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ? _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; write title here ; # The loop structure below should contain the names and addresses of all # authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name 'Luca Bernardi' 'Aase S. Gothelf' 'Rita G. Hazell' 'Karl Anker Jorgensen' _publ_author_address ; Department of Chemistry Aarhus University Langelandsgade 140 DK-8000 \%Arhus C Denmark ; #============================================================================== # 4. TEXT _publ_section_comment ; The asymmetric unit contains 4 molecules, all of the same chirality. They are pairvise related by approximate centres of symmetry, and the pairs are nearly parallel, though with some groups interchanged. The result is large correlations and probably also some disorder. Large residual density near the N1 nitrogens of molecules a and b was attempted modelled by inclusion of extra atoms, but they refined away. ; _publ_section_references ; Allen,F.H., Davies,J.E., Galloy,J.J., Johnson,O., Kennard,O., Macrae,C.F., Mitchell,E.M., Mitchell,G.F., Smith,J.M., Watson,D.G. (1991). J. Chem. Inf. Comp. Sci. 31, 187-204. Altomare,A., Cascarano,G., Giacovazzo,C., Guagliardi,A., Moliterni,.A,G,G., Burla,M.C., Polidori,G., Camalli,M. & Spagna,R. (1997). SIR97. University of Bari, Italy. Becker,P.J. & Coppens, P. (1974). Acta Cryst. A30, 129-153. Burnett,M.N. & Johnson,C.K. (1996). ORTEP-III. Report ORNL-6895. Oak Ridge National Laboratory, Tennessee, USA. Busing,W.R., Martin,K.O. & Levy,H.A. (1962). ORFLS. Report ORNL-TM-305. Oak Ridge National Laboratory, Tennessee, USA. Hazell,A. (1995). KRYSTAL, An integrated system of crystallographic programs. Aarhus University, Denmark. Rogers,D. (1981). Acta Cryst. A37, 734-741. Siemens (1995) SMART, SAINT and XPREP Area-Detector Control and Integration Software. Siemens Analytical X-ray Instruments Inc. Madison, Wisconsin, USA. ; #============================================================================== #=================================== data_cpd_4b #=================================== # 5. CHEMICAL DATA _chemical_name_systematic ; (2S,3R) Ethyl 2-( (diphenylmethylene)amino)-3-phenyl-3- (p-toluensulphonylamino) propanoate ; _chemical_formula_sum 'C31 H30 N2 O4 S' _chemical_formula_weight 526.64 #=================================== # 6. CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' _cell_length_a 11.099(1) _cell_length_b 15.508(2) _cell_length_c 16.210(2) _cell_angle_alpha 91.344(4) _cell_angle_beta 100.149(4) _cell_angle_gamma 92.319(4) _cell_volume 2743(1) _cell_formula_units_Z 4 _cell_measurement_temperature 120 _cell_measurement_reflns_used 8579 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 28.0 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.27 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type 'integration' _exptl_absorpt_process_details 'XPREP 1995' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.98 #=================================== # 7. EXPERIMENTAL DATA _diffrn_ambient_temperature 120 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'x-ray tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation scans with narrow frames' _diffrn_standards_decay_% 0 _diffrn_reflns_number 21712 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.5 _diffrn_reflns_theta_max 28.0 _diffrn_reflns_reduction_process 21712 _reflns_number_total 18255 _reflns_number_gt 15695 _reflns_threshold_expression I>3\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution ; SIR97 (Altomare et al., 1997 ), KRYSTAL ; _computing_structure_refinement 'modified ORFLS(1962), KRYSTAL' _computing_molecular_graphics ; ORTEP-III (Burnett & Johnson, 1996), KRYSTAL ; _computing_publication_material KRYSTAL _atom_type_scat_source IntTabIV #=================================== # 8. REFINEMENT DATA _refine_special_details ; The asymmetric unit contains 4 molecules, all of the same chirality. They are pairvise related by approximate centres of symmetry, and the pairs are nearly parallel, though with some groups interchanged. The result is large correlations and probably also some disorder. The atomic displacement parameters reflect this as well as thermal motion. Large residual density and holes near the N1 nitrogens of molecules a and b were attempted modelled by inclusion of extra, partially occupied atoms, but they refined away. Hydrogen atoms were included at calculated positions except for those attached to nitrogen; these were found from difference maps. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w= 1/{[\s~cs~(F^2^)+1.03F^2^]^1/2^- |F|}^2^ ; _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method ; Type 1 Lorentzian isotropic ( Becker and Coppens, 1974) ; _refine_ls_extinction_coef 170(20) _refine_ls_abs_structure_details ; The absolute configuration was determined according to Rogers (1981) through least squares refinement using all 15695 significant reflections, including 7355 Bijvoet pairs. The Rogers' factor is 1 for the right chirality, -1 for the wrong hand. ; _refine_ls_abs_structure_Rogers 1.14(17) _refine_ls_number_reflns 15695 _refine_ls_number_parameters 1368 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_gt 0.071 _refine_ls_wR_factor_ref 0.107 _refine_ls_goodness_of_fit_ref 2.13 _refine_ls_shift/su_max 0.0084 _refine_ls_shift/su_mean 0.0017 _refine_diff_density_max 1.5(1) _refine_diff_density_min -0.8(1) #========================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type S1a -0.4396(2) -0.1029(1) 0.6186(1) 0.025(1) Uij S1b 0.2630(2) -0.0257(1) 0.7602(1) 0.025(1) Uij S1c 0.1266(2) 0.4514(1) 0.1211(2) 0.027(1) Uij S1d 0.8222(2) 0.4229(1) 0.2681(1) 0.021(1) Uij O1a -0.3806(4) -0.1690(3) 0.5775(3) 0.030(3) Uij O2a -0.5705(4) -0.0992(3) 0.5987(3) 0.031(3) Uij O3a -0.1250(6) -0.0252(4) 0.7527(4) 0.064(5) Uij O4a -0.2112(6) 0.0397(4) 0.8504(4) 0.067(5) Uij O1b 0.2011(4) 0.0357(3) 0.8044(3) 0.028(3) Uij O2b 0.3951(4) -0.0240(3) 0.7805(3) 0.031(3) Uij O3b 0.0385(6) 0.1622(3) 0.6390(4) 0.056(4) Uij O4b 0.1855(5) 0.1908(3) 0.5656(3) 0.042(3) Uij O1c -0.0019(4) 0.4704(3) 0.1025(3) 0.036(3) Uij O2c 0.2077(5) 0.4913(3) 0.0714(3) 0.039(3) Uij O3c 0.3213(5) 0.6586(3) 0.2219(3) 0.048(4) Uij O4c 0.3105(5) 0.6988(3) 0.3543(3) 0.041(3) Uij O1d 0.7527(4) 0.3699(3) 0.3171(3) 0.027(3) Uij O2d 0.9530(4) 0.4177(3) 0.2838(3) 0.025(3) Uij O3d 0.5458(4) 0.5130(3) 0.1681(3) 0.031(3) Uij O4d 0.5161(5) 0.5478(3) 0.0333(3) 0.042(3) Uij N1a -0.4005(5) -0.1138(4) 0.7181(4) 0.028(4) Uij N2a -0.3227(6) -0.1057(4) 0.8929(4) 0.032(4) Uij N1b 0.2299(5) -0.0113(3) 0.6630(3) 0.022(3) Uij N2b 0.1850(5) 0.0391(3) 0.4952(4) 0.022(3) Uij N1c 0.1707(5) 0.4809(3) 0.2177(3) 0.023(3) Uij N2c 0.2363(5) 0.5380(3) 0.3850(4) 0.022(3) Uij N1d 0.7722(5) 0.3981(3) 0.1707(3) 0.022(3) Uij N2d 0.6681(5) 0.4175(3) 0.0044(3) 0.019(3) Uij C1a -0.2977(6) -0.1622(4) 0.7570(4) 0.025(4) Uij C2a -0.2318(7) -0.1142(4) 0.8370(5) 0.035(5) Uij C3a -0.1783(7) -0.0280(6) 0.8089(6) 0.056(7) Uij C4a -0.3332(6) -0.2549(4) 0.7729(4) 0.026(4) Uij C5a -0.2448(7) -0.3172(5) 0.7764(5) 0.034(5) Uij C6a -0.2745(6) -0.4014(5) 0.7926(5) 0.039(4) Uij C7a -0.3920(7) -0.4277(5) 0.8006(5) 0.046(6) Uij C8a -0.4777(7) -0.3673(5) 0.7944(6) 0.054(6) Uij C9a -0.4501(7) -0.2791(5) 0.7820(5) 0.038(5) Uij C10a -0.1685(7) 0.1258(5) 0.8143(6) 0.048(6) Uij C11a -0.0381(8) 0.1443(5) 0.8558(6) 0.053(6) Uij C12a -0.3087(7) -0.1447(4) 0.9626(5) 0.030(5) Uij C13a -0.1991(9) -0.1931(6) 0.9993(5) 0.047(6) Uij C14a -0.0934(9) -0.1503(6) 1.0370(6) 0.056(6) Uij C15a 0.0079(9) -0.1975(8) 1.0720(6) 0.065(7) Uij C16a 0.0006(11) -0.2856(10) 1.0716(6) 0.083(9) Uij C17a -0.1066(10) -0.3274(6) 1.0328(6) 0.058(7) Uij C18a -0.2095(9) -0.2848(5) 0.9972(5) 0.054(6) Uij C19a -0.4082(7) -0.1369(4) 1.0139(5) 0.028(5) Uij C20a -0.3889(8) -0.1571(5) 1.0967(5) 0.045(6) Uij C21a -0.4822(9) -0.1484(5) 1.1455(5) 0.050(6) Uij C22a -0.5965(8) -0.1212(5) 1.1059(6) 0.047(6) Uij C23a -0.6131(7) -0.0994(4) 1.0236(5) 0.035(5) Uij C24a -0.5216(8) -0.1104(4) 0.9762(5) 0.037(5) Uij C25a -0.3774(6) -0.0014(4) 0.5931(4) 0.020(4) Uij C26a -0.2928(6) -0.0001(5) 0.5391(5) 0.031(4) Uij C27a -0.2522(6) 0.0784(4) 0.5158(4) 0.025(4) Uij C28a -0.2891(6) 0.1555(4) 0.5452(4) 0.020(4) Uij C29a -0.3750(7) 0.1534(4) 0.5979(5) 0.038(5) Uij C30a -0.4208(6) 0.0726(4) 0.6220(5) 0.031(4) Uij C31a -0.2409(7) 0.2411(5) 0.5202(5) 0.039(5) Uij C1b 0.1030(6) -0.0178(4) 0.6152(4) 0.020(4) Uij C2b 0.0901(6) 0.0494(4) 0.5471(4) 0.028(4) Uij C3b 0.0997(7) 0.1400(5) 0.5900(5) 0.033(5) Uij C4b 0.0592(6) -0.1088(4) 0.5781(5) 0.027(4) Uij C5b -0.0460(6) -0.1478(4) 0.5973(4) 0.027(4) Uij C6b -0.0820(6) -0.2309(5) 0.5716(5) 0.039(4) Uij C7b -0.0128(7) -0.2771(4) 0.5213(5) 0.033(5) Uij C8b 0.0947(7) -0.2400(5) 0.5067(5) 0.038(5) Uij C9b 0.1310(6) -0.1563(4) 0.5322(5) 0.030(4) Uij C10b 0.2085(8) 0.2772(5) 0.6042(5) 0.047(6) Uij C11b 0.3468(8) 0.2915(5) 0.6261(5) 0.049(6) Uij C12b 0.1614(6) 0.0491(4) 0.4162(5) 0.022(4) Uij C13b 0.0381(6) 0.0682(4) 0.3648(4) 0.020(4) Uij C14b -0.0308(7) 0.0070(5) 0.3132(5) 0.044(5) Uij C15b -0.1415(8) 0.0251(5) 0.2634(6) 0.051(6) Uij C16b -0.1860(7) 0.1070(6) 0.2665(5) 0.049(6) Uij C17b -0.1180(7) 0.1679(5) 0.3198(5) 0.031(5) Uij C18b -0.0078(7) 0.1505(4) 0.3693(4) 0.027(4) Uij C19b 0.2646(6) 0.0383(4) 0.3682(5) 0.024(4) Uij C20b 0.2571(7) 0.0698(4) 0.2883(5) 0.032(5) Uij C21b 0.3538(7) 0.0663(5) 0.2465(5) 0.035(5) Uij C22b 0.4617(7) 0.0312(5) 0.2834(5) 0.037(5) Uij C23b 0.4696(6) -0.0010(4) 0.3629(5) 0.030(5) Uij C24b 0.3726(6) 0.0033(4) 0.4061(5) 0.029(4) Uij C25b 0.2040(6) -0.1296(4) 0.7828(5) 0.028(4) Uij C26b 0.1295(6) -0.1378(4) 0.8391(4) 0.026(4) Uij C27b 0.0897(7) -0.2215(5) 0.8579(5) 0.037(5) Uij C28b 0.1208(6) -0.2929(4) 0.8187(5) 0.029(4) Uij C29b 0.1942(6) -0.2816(4) 0.7579(5) 0.032(5) Uij C30b 0.2364(6) -0.2006(4) 0.7411(4) 0.027(4) Uij C31b 0.0747(7) -0.3797(5) 0.8403(5) 0.047(6) Uij C1c 0.2996(6) 0.4789(4) 0.2606(4) 0.022(4) Uij C2c 0.3242(6) 0.5521(4) 0.3292(4) 0.021(4) Uij C3c 0.3160(7) 0.6402(4) 0.2924(5) 0.028(4) Uij C4c 0.3359(6) 0.3935(4) 0.3000(4) 0.015(3) Uij C5c 0.4541(7) 0.3705(4) 0.3046(5) 0.033(5) Uij C6c 0.4958(6) 0.2961(4) 0.3472(5) 0.029(4) Uij C7c 0.4161(7) 0.2477(4) 0.3879(5) 0.031(5) Uij C8c 0.2976(7) 0.2715(4) 0.3830(5) 0.032(5) Uij C9c 0.2557(6) 0.3442(4) 0.3396(4) 0.023(4) Uij C10c 0.3154(8) 0.7895(4) 0.3329(5) 0.049(6) Uij C11c 0.1921(9) 0.8133(5) 0.2911(6) 0.059(7) Uij C12c 0.2751(6) 0.5327(4) 0.4633(5) 0.023(4) Uij C13c 0.4062(6) 0.5396(4) 0.5063(5) 0.026(4) Uij C14c 0.4623(6) 0.6168(4) 0.5345(5) 0.029(4) Uij C15c 0.5856(6) 0.6230(4) 0.5730(5) 0.031(5) Uij C16c 0.6498(7) 0.5506(5) 0.5785(5) 0.038(5) Uij C17c 0.6001(7) 0.4732(5) 0.5475(5) 0.039(5) Uij C18c 0.4762(6) 0.4656(4) 0.5099(4) 0.027(4) Uij C19c 0.1784(6) 0.5125(4) 0.5156(4) 0.022(4) Uij C20c 0.2084(7) 0.5097(4) 0.6030(5) 0.032(5) Uij C21c 0.1167(7) 0.4922(5) 0.6507(5) 0.033(5) Uij C22c -0.0004(8) 0.4753(5) 0.6099(5) 0.040(5) Uij C23c -0.0312(7) 0.4725(5) 0.5259(6) 0.042(5) Uij C24c 0.0579(6) 0.4938(5) 0.4765(5) 0.030(4) Uij C25c 0.1370(6) 0.3379(4) 0.1096(4) 0.023(3) Uij C26c 0.0682(6) 0.2837(5) 0.1466(5) 0.033(5) Uij C27c 0.0643(7) 0.1945(5) 0.1324(5) 0.034(5) Uij C28c 0.1358(8) 0.1594(5) 0.0779(5) 0.042(5) Uij C29c 0.2100(8) 0.2161(6) 0.0400(5) 0.052(6) Uij C30c 0.2103(7) 0.3042(6) 0.0536(5) 0.046(6) Uij C31c 0.1300(9) 0.0626(5) 0.0583(6) 0.061(6) Uij C1d 0.6524(6) 0.3581(4) 0.1363(5) 0.023(4) Uij C2d 0.5882(6) 0.4099(4) 0.0659(4) 0.022(4) Uij C3d 0.5490(6) 0.4952(4) 0.0954(4) 0.019(4) Uij C4d 0.6561(6) 0.2644(4) 0.1088(4) 0.021(4) Uij C5d 0.5584(7) 0.2088(4) 0.1120(4) 0.028(4) Uij C6d 0.5525(7) 0.1228(4) 0.0770(5) 0.038(5) Uij C7d 0.6513(8) 0.0970(4) 0.0411(5) 0.042(5) Uij C8d 0.7491(7) 0.1515(5) 0.0396(5) 0.034(5) Uij C9d 0.7526(6) 0.2344(4) 0.0722(4) 0.028(4) Uij C10d 0.4663(10) 0.6297(5) 0.0582(6) 0.061(7) Uij C11d 0.3723(10) 0.6553(6) -0.0096(7) 0.081(8) Uij C12d 0.6408(6) 0.3817(4) -0.0704(4) 0.022(4) Uij C13d 0.5187(6) 0.3357(5) -0.1047(4) 0.026(4) Uij C14d 0.5098(7) 0.2455(5) -0.1183(5) 0.038(5) Uij C15d 0.4004(9) 0.2064(5) -0.1490(5) 0.046(6) Uij C16d 0.2985(8) 0.2492(6) -0.1650(5) 0.051(6) Uij C17d 0.3017(7) 0.3390(6) -0.1520(5) 0.051(6) Uij C18d 0.4161(7) 0.3830(5) -0.1213(4) 0.033(5) Uij C19d 0.7385(6) 0.3786(4) -0.1216(4) 0.020(4) Uij C20d 0.7149(7) 0.3529(4) -0.2053(5) 0.031(5) Uij C21d 0.8101(7) 0.3481(5) -0.2508(5) 0.037(5) Uij C22d 0.9300(7) 0.3690(5) -0.2130(5) 0.037(5) Uij C23d 0.9530(6) 0.3953(5) -0.1282(5) 0.031(5) Uij C24d 0.8586(6) 0.3992(4) -0.0839(4) 0.024(4) Uij C25d 0.7946(6) 0.5325(4) 0.2892(4) 0.023(3) Uij C26d 0.8524(7) 0.5952(4) 0.2499(5) 0.034(5) Uij C27d 0.8355(7) 0.6820(4) 0.2676(5) 0.038(5) Uij C28d 0.7627(8) 0.7053(5) 0.3253(5) 0.039(5) Uij C29d 0.7047(7) 0.6404(5) 0.3638(5) 0.043(5) Uij C30d 0.7214(6) 0.5531(5) 0.3432(4) 0.031(4) Uij C31d 0.7487(9) 0.7994(5) 0.3505(5) 0.061(7) Uij H1na -0.452 -0.097 0.732 0.03 Uiso H1nb 0.291 -0.036 0.629 0.02 Uiso H1nc 0.097 0.460 0.240 0.04 Uiso H1nd 0.805 0.412 0.130 0.01 Uiso H1a -0.241 -0.164 0.719 0.03 Uiso H2a -0.167 -0.147 0.863 0.04 Uiso H5a -0.165 -0.301 0.767 0.04 Uiso H6a -0.212 -0.442 0.799 0.04 Uiso H7a -0.413 -0.486 0.810 0.05 Uiso H8a -0.559 -0.385 0.798 0.07 Uiso H9a -0.511 -0.238 0.780 0.05 Uiso H10aa -0.219 0.171 0.827 0.06 Uiso H10ab -0.175 0.119 0.755 0.06 Uiso H11aa -0.013 0.197 0.834 0.06 Uiso H11ab 0.011 0.099 0.843 0.06 Uiso H11ac -0.033 0.150 0.915 0.06 Uiso H14a -0.089 -0.089 1.039 0.07 Uiso H15a 0.083 -0.167 1.096 0.08 Uiso H16a 0.068 -0.317 1.098 0.10 Uiso H17a -0.110 -0.389 1.030 0.07 Uiso H18a -0.284 -0.316 0.972 0.06 Uiso H20a -0.312 -0.178 1.122 0.05 Uiso H21a -0.467 -0.160 1.204 0.06 Uiso H22a -0.662 -0.119 1.136 0.06 Uiso H23a -0.688 -0.076 0.998 0.04 Uiso H24a -0.537 -0.099 0.918 0.04 Uiso H26a -0.264 -0.052 0.519 0.04 Uiso H27a -0.196 0.080 0.478 0.03 Uiso H29a -0.402 0.206 0.618 0.05 Uiso H30a -0.480 0.070 0.658 0.04 Uiso H31aa -0.302 0.282 0.520 0.05 Uiso H31ab -0.221 0.235 0.466 0.05 Uiso H31ac -0.170 0.259 0.559 0.05 Uiso H1b 0.051 -0.003 0.653 0.02 Uiso H2b 0.012 0.041 0.513 0.03 Uiso H5b -0.095 -0.116 0.629 0.03 Uiso H6b -0.153 -0.258 0.587 0.05 Uiso H7b -0.041 -0.333 0.498 0.04 Uiso H8b 0.146 -0.273 0.478 0.05 Uiso H9b 0.204 -0.131 0.519 0.04 Uiso H10ba 0.173 0.281 0.653 0.06 Uiso H10bb 0.175 0.319 0.566 0.06 Uiso H11ba 0.361 0.348 0.651 0.06 Uiso H11bb 0.382 0.288 0.577 0.06 Uiso H11bc 0.380 0.250 0.664 0.06 Uiso H14b -0.002 -0.050 0.311 0.05 Uiso H15b -0.186 -0.018 0.227 0.06 Uiso H16b -0.262 0.120 0.233 0.06 Uiso H17b -0.149 0.224 0.323 0.04 Uiso H18b 0.036 0.194 0.406 0.03 Uiso H20b 0.183 0.094 0.262 0.04 Uiso H21b 0.347 0.089 0.192 0.04 Uiso H22b 0.529 0.029 0.255 0.04 Uiso H23b 0.543 -0.026 0.388 0.04 Uiso H24b 0.380 -0.018 0.461 0.04 Uiso H26b 0.104 -0.088 0.866 0.03 Uiso H27b 0.040 -0.228 0.900 0.04 Uiso H29b 0.215 -0.330 0.728 0.04 Uiso H30b 0.288 -0.194 0.700 0.03 Uiso H31ba 0.065 -0.379 0.897 0.06 Uiso H31bb 0.132 -0.422 0.832 0.06 Uiso H31bc -0.002 -0.395 0.805 0.06 Uiso H1c 0.350 0.491 0.221 0.03 Uiso H2c 0.404 0.547 0.361 0.02 Uiso H5c 0.509 0.405 0.279 0.04 Uiso H6c 0.577 0.279 0.348 0.03 Uiso H7c 0.444 0.199 0.419 0.04 Uiso H8c 0.243 0.238 0.409 0.04 Uiso H9c 0.174 0.360 0.337 0.03 Uiso H10ca 0.372 0.798 0.296 0.06 Uiso H10cb 0.340 0.824 0.383 0.06 Uiso H11ca 0.195 0.872 0.277 0.07 Uiso H11cb 0.135 0.804 0.328 0.07 Uiso H11cc 0.167 0.778 0.241 0.07 Uiso H14c 0.417 0.668 0.528 0.04 Uiso H15c 0.624 0.677 0.595 0.04 Uiso H16c 0.733 0.554 0.605 0.05 Uiso H17c 0.648 0.424 0.551 0.05 Uiso H18c 0.440 0.412 0.487 0.03 Uiso H20c 0.291 0.520 0.630 0.04 Uiso H21c 0.136 0.492 0.710 0.04 Uiso H22c -0.063 0.465 0.642 0.05 Uiso H23c -0.113 0.456 0.500 0.05 Uiso H24c 0.036 0.496 0.417 0.04 Uiso H26c 0.020 0.307 0.185 0.04 Uiso H27c 0.014 0.158 0.159 0.04 Uiso H29c 0.261 0.194 0.004 0.06 Uiso H30c 0.258 0.342 0.026 0.06 Uiso H31ca 0.145 0.053 0.003 0.07 Uiso H31cb 0.051 0.039 0.062 0.07 Uiso H31cc 0.190 0.036 0.097 0.07 Uiso H1d 0.605 0.360 0.179 0.03 Uiso H2d 0.516 0.377 0.040 0.03 Uiso H5d 0.493 0.228 0.138 0.03 Uiso H6d 0.483 0.085 0.078 0.05 Uiso H7d 0.650 0.040 0.018 0.05 Uiso H8d 0.815 0.132 0.015 0.04 Uiso H9d 0.822 0.272 0.070 0.03 Uiso H10da 0.531 0.673 0.069 0.07 Uiso H10db 0.432 0.622 0.107 0.07 Uiso H11da 0.341 0.708 0.006 0.10 Uiso H11db 0.309 0.612 -0.021 0.10 Uiso H11dc 0.407 0.664 -0.059 0.10 Uiso H14d 0.581 0.213 -0.106 0.04 Uiso H15d 0.396 0.146 -0.159 0.05 Uiso H16d 0.223 0.219 -0.185 0.06 Uiso H17d 0.229 0.370 -0.164 0.06 Uiso H18d 0.422 0.444 -0.112 0.04 Uiso H20d 0.633 0.338 -0.232 0.04 Uiso H21d 0.793 0.330 -0.308 0.04 Uiso H22d 0.995 0.366 -0.244 0.04 Uiso H23d 1.035 0.410 -0.101 0.04 Uiso H24d 0.876 0.417 -0.026 0.03 Uiso H26d 0.903 0.580 0.211 0.04 Uiso H27d 0.875 0.726 0.241 0.05 Uiso H29d 0.655 0.655 0.404 0.05 Uiso H30d 0.679 0.509 0.368 0.04 Uiso H31da 0.670 0.805 0.366 0.07 Uiso H31db 0.754 0.835 0.304 0.07 Uiso H31dc 0.810 0.817 0.396 0.07 Uiso loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 S1a 0.026(1) 0.024(1) 0.025(1) 0.005(1) 0.005(1) 0.008(1) S1b 0.025(1) 0.023(1) 0.025(1) -0.002(1) 0.005(1) -0.004(1) S1c 0.026(1) 0.035(1) 0.021(1) 0.001(1) 0.005(1) 0.004(1) S1d 0.021(1) 0.023(1) 0.020(1) 0.001(1) 0.005(1) -0.001(1) O1a 0.034(3) 0.028(3) 0.030(3) 0.011(2) 0.013(2) -0.001(2) O2a 0.019(3) 0.022(2) 0.053(4) 0.005(2) 0.003(2) 0.004(2) O3a 0.074(5) 0.047(4) 0.076(5) -0.006(3) 0.031(4) -0.004(3) O4a 0.088(5) 0.047(4) 0.070(5) -0.009(3) 0.028(4) -0.001(3) O1b 0.028(3) 0.030(3) 0.029(3) -0.002(2) 0.012(2) -0.014(2) O2b 0.019(3) 0.021(2) 0.055(4) -0.006(2) 0.013(2) -0.005(2) O3b 0.070(4) 0.037(3) 0.076(5) 0.005(3) 0.056(4) -0.009(3) O4b 0.059(4) 0.033(3) 0.043(3) -0.001(3) 0.032(3) -0.010(2) O1c 0.025(3) 0.029(3) 0.050(4) 0.004(2) -0.003(3) 0.014(2) O2c 0.040(3) 0.056(3) 0.023(3) -0.001(3) 0.012(3) 0.003(2) O3c 0.089(5) 0.028(3) 0.039(4) 0.009(3) 0.042(3) 0.008(2) O4c 0.066(4) 0.018(2) 0.039(3) -0.003(2) 0.012(3) -0.001(2) O1d 0.032(3) 0.028(3) 0.022(3) 0.000(2) 0.009(2) 0.007(2) O2d 0.010(2) 0.032(3) 0.032(3) 0.003(2) 0.001(2) -0.002(2) O3d 0.037(3) 0.031(3) 0.026(3) -0.001(2) 0.009(2) -0.006(2) O4d 0.073(4) 0.027(3) 0.032(3) 0.023(3) 0.017(3) 0.000(2) N1a 0.029(4) 0.028(3) 0.032(4) 0.010(3) 0.015(3) 0.007(3) N2a 0.042(4) 0.032(3) 0.025(4) 0.011(3) 0.010(3) -0.002(3) N1b 0.018(3) 0.016(3) 0.029(4) -0.005(2) 0.001(3) -0.001(2) N2b 0.022(3) 0.018(3) 0.029(4) 0.002(2) 0.009(3) 0.002(2) N1c 0.029(3) 0.024(3) 0.017(3) -0.005(2) 0.006(3) 0.003(2) N2c 0.026(3) 0.017(3) 0.021(3) -0.005(2) 0.002(3) 0.000(2) N1d 0.021(3) 0.027(3) 0.019(3) -0.006(2) 0.008(3) 0.001(2) N2d 0.017(3) 0.021(3) 0.022(3) -0.004(2) 0.009(3) -0.002(2) C1a 0.017(4) 0.032(4) 0.027(4) 0.004(3) 0.004(3) 0.018(3) C2a 0.043(5) 0.027(4) 0.040(5) 0.009(3) 0.016(4) 0.010(3) C3a 0.021(5) 0.082(7) 0.062(7) 0.014(4) 0.006(5) -0.042(6) C4a 0.029(4) 0.025(4) 0.027(4) 0.008(3) 0.010(3) 0.011(3) C5a 0.038(5) 0.032(4) 0.033(5) 0.000(3) 0.013(4) 0.000(3) C6a 0.022(3) 0.033(3) 0.063(4) -0.007(2) 0.013(3) 0.012(3) C7a 0.037(5) 0.041(5) 0.063(6) 0.007(4) 0.017(5) 0.008(4) C8a 0.036(5) 0.040(5) 0.095(8) -0.005(4) 0.035(5) 0.023(5) C9a 0.030(4) 0.037(4) 0.053(5) 0.009(3) 0.021(4) 0.017(4) C10a 0.033(5) 0.048(5) 0.062(6) 0.001(4) 0.007(5) 0.006(4) C11a 0.046(6) 0.056(5) 0.057(6) 0.010(4) 0.009(5) 0.007(4) C12a 0.047(5) 0.008(3) 0.032(5) 0.002(3) 0.003(4) -0.004(3) C13a 0.075(7) 0.062(6) 0.007(4) 0.029(5) 0.011(4) 0.007(4) C14a 0.053(6) 0.072(6) 0.044(6) 0.017(5) 0.009(5) 0.008(5) C15a 0.050(6) 0.112(9) 0.032(6) 0.022(6) -0.002(5) 0.000(6) C16a 0.065(8) 0.158(12) 0.035(6) 0.076(8) 0.012(6) 0.027(7) C17a 0.096(8) 0.051(5) 0.035(6) 0.048(6) 0.025(6) 0.014(4) C18a 0.087(7) 0.051(5) 0.034(5) 0.028(5) 0.035(5) 0.011(4) C19a 0.045(5) 0.021(4) 0.018(4) 0.008(3) 0.005(4) 0.000(3) C20a 0.057(6) 0.038(5) 0.044(6) 0.019(4) 0.013(5) 0.002(4) C21a 0.067(7) 0.058(6) 0.029(5) 0.005(5) 0.016(5) 0.000(4) C22a 0.052(6) 0.044(5) 0.046(6) -0.002(4) 0.018(5) -0.010(4) C23a 0.046(5) 0.025(4) 0.036(5) 0.008(3) 0.014(4) 0.001(3) C24a 0.057(6) 0.029(4) 0.028(5) -0.001(4) 0.019(4) -0.001(3) C25a 0.021(4) 0.027(4) 0.015(4) 0.008(3) 0.006(3) 0.006(3) C26a 0.027(4) 0.036(4) 0.031(5) -0.002(3) 0.007(4) -0.001(3) C27a 0.014(4) 0.038(4) 0.024(4) 0.002(3) 0.006(3) 0.008(3) C28a 0.022(4) 0.020(3) 0.020(4) 0.000(3) 0.005(3) 0.003(3) C29a 0.051(5) 0.026(4) 0.036(5) -0.003(4) 0.006(4) 0.000(3) C30a 0.030(4) 0.028(4) 0.038(5) -0.006(3) 0.015(4) 0.013(3) C31a 0.034(5) 0.043(5) 0.039(5) -0.003(4) 0.003(4) 0.007(4) C1b 0.013(4) 0.012(3) 0.035(4) 0.000(2) 0.008(3) 0.003(3) C2b 0.027(4) 0.034(4) 0.023(4) 0.006(3) 0.005(3) 0.007(3) C3b 0.028(5) 0.030(4) 0.041(5) -0.003(3) 0.004(4) 0.017(4) C4b 0.020(4) 0.024(4) 0.034(5) -0.004(3) 0.000(3) 0.005(3) C5b 0.021(4) 0.029(4) 0.034(4) -0.004(3) 0.012(3) -0.007(3) C6b 0.022(3) 0.033(3) 0.063(4) -0.007(2) 0.013(3) 0.012(3) C7b 0.037(5) 0.012(3) 0.047(5) -0.010(3) 0.009(4) -0.005(3) C8b 0.026(4) 0.048(5) 0.042(5) 0.005(4) 0.010(4) -0.014(4) C9b 0.020(4) 0.036(4) 0.040(5) 0.005(3) 0.021(4) -0.002(3) C10b 0.057(6) 0.024(4) 0.058(6) 0.001(4) 0.010(5) -0.011(4) C11b 0.057(6) 0.045(5) 0.042(5) -0.012(4) 0.008(4) -0.016(4) C12b 0.027(4) 0.013(3) 0.028(4) 0.003(3) 0.010(3) 0.006(3) C13b 0.011(4) 0.027(4) 0.024(4) -0.003(3) 0.007(3) 0.005(3) C14b 0.036(5) 0.038(5) 0.055(6) 0.008(4) -0.005(4) -0.006(4) C15b 0.041(5) 0.045(5) 0.061(6) -0.003(4) -0.007(5) -0.004(4) C16b 0.040(5) 0.059(6) 0.050(6) 0.001(4) 0.016(5) 0.031(5) C17b 0.023(4) 0.041(4) 0.032(5) 0.015(3) 0.009(4) 0.012(4) C18b 0.034(4) 0.027(4) 0.024(4) 0.006(3) 0.013(4) 0.004(3) C19b 0.023(4) 0.018(3) 0.034(5) -0.007(3) 0.012(3) -0.004(3) C20b 0.034(5) 0.031(4) 0.031(5) 0.003(3) 0.005(4) 0.005(3) C21b 0.023(4) 0.048(5) 0.033(5) 0.000(4) 0.002(4) 0.000(4) C22b 0.045(5) 0.040(4) 0.030(5) 0.008(4) 0.014(4) -0.006(4) C23b 0.018(4) 0.032(4) 0.040(5) 0.005(3) 0.002(4) -0.008(3) C24b 0.020(4) 0.033(4) 0.032(5) 0.008(3) -0.006(3) 0.005(3) C25b 0.023(4) 0.026(4) 0.031(5) -0.007(3) 0.000(4) 0.005(3) C26b 0.024(4) 0.033(4) 0.020(4) 0.003(3) 0.006(3) -0.004(3) C27b 0.026(4) 0.054(5) 0.032(5) -0.004(4) 0.009(4) 0.010(4) C28b 0.022(4) 0.023(4) 0.043(5) 0.005(3) 0.011(4) 0.001(3) C29b 0.026(4) 0.036(4) 0.037(5) -0.005(3) 0.015(4) -0.008(3) C30b 0.032(4) 0.028(4) 0.024(4) 0.002(3) 0.013(3) 0.001(3) C31b 0.040(5) 0.053(5) 0.055(6) -0.005(4) 0.024(4) 0.018(4) C1c 0.024(4) 0.024(3) 0.018(4) -0.004(3) 0.008(3) 0.001(3) C2c 0.018(4) 0.028(4) 0.021(4) 0.002(3) 0.012(3) 0.001(3) C3c 0.032(4) 0.029(4) 0.025(4) -0.001(3) 0.013(4) 0.009(3) C4c 0.010(3) 0.018(3) 0.013(3) -0.006(3) -0.002(3) -0.001(3) C5c 0.038(5) 0.030(4) 0.037(5) 0.001(3) 0.017(4) 0.008(3) C6c 0.023(4) 0.024(4) 0.040(5) 0.005(3) 0.010(4) -0.008(3) C7c 0.035(5) 0.011(3) 0.048(5) 0.000(3) 0.011(4) 0.000(3) C8c 0.027(4) 0.034(4) 0.035(5) -0.007(3) 0.006(4) -0.004(3) C9c 0.018(4) 0.023(4) 0.028(4) 0.002(3) 0.004(3) -0.004(3) C10c 0.085(7) 0.018(4) 0.039(5) -0.014(4) 0.001(5) 0.019(3) C11c 0.093(8) 0.044(5) 0.045(6) 0.019(5) 0.023(6) 0.005(4) C12c 0.030(4) 0.006(3) 0.031(4) -0.003(3) 0.005(3) -0.005(3) C13c 0.027(4) 0.012(3) 0.040(5) -0.008(3) 0.008(4) 0.004(3) C14c 0.025(4) 0.024(4) 0.038(5) -0.001(3) 0.004(4) -0.004(3) C15c 0.025(4) 0.028(4) 0.038(5) -0.008(3) -0.001(4) -0.005(3) C16c 0.033(5) 0.051(5) 0.027(5) 0.000(4) -0.005(4) -0.007(4) C17c 0.029(5) 0.038(5) 0.050(5) 0.014(4) 0.003(4) -0.016(4) C18c 0.029(4) 0.023(4) 0.030(4) 0.001(3) 0.008(3) -0.007(3) C19c 0.024(4) 0.021(3) 0.025(4) 0.008(3) 0.012(3) 0.000(3) C20c 0.028(4) 0.032(4) 0.033(5) 0.000(3) -0.004(4) -0.004(3) C21c 0.040(5) 0.040(4) 0.024(4) -0.002(4) 0.020(4) -0.001(3) C22c 0.043(5) 0.044(5) 0.042(6) -0.002(4) 0.030(4) 0.012(4) C23c 0.032(5) 0.049(5) 0.050(6) -0.002(4) 0.017(4) 0.012(4) C24c 0.023(4) 0.043(4) 0.028(4) 0.001(3) 0.013(4) -0.004(3) C25c 0.015(2) 0.032(3) 0.023(3) 0.002(2) 0.005(2) -0.009(2) C26c 0.020(4) 0.039(4) 0.037(5) 0.012(3) 0.000(4) -0.016(4) C27c 0.027(4) 0.031(4) 0.042(5) 0.001(3) 0.004(4) 0.000(3) C28c 0.044(5) 0.045(5) 0.036(5) 0.019(4) 0.003(4) -0.004(4) C29c 0.046(6) 0.079(7) 0.030(5) 0.038(5) -0.001(4) -0.015(5) C30c 0.038(5) 0.067(6) 0.035(5) 0.009(4) 0.008(4) -0.002(4) C31c 0.086(7) 0.039(5) 0.057(6) 0.019(5) 0.008(5) -0.012(4) C1d 0.006(3) 0.027(4) 0.037(5) 0.001(3) 0.003(3) -0.005(3) C2d 0.021(4) 0.019(3) 0.026(4) -0.004(3) 0.009(3) -0.005(3) C3d 0.008(4) 0.026(4) 0.022(4) -0.001(3) -0.002(3) -0.004(3) C4d 0.017(4) 0.014(3) 0.028(4) -0.007(3) -0.004(3) -0.002(3) C5d 0.035(4) 0.026(4) 0.023(4) -0.006(3) 0.006(3) 0.005(3) C6d 0.046(5) 0.019(4) 0.049(5) -0.016(3) 0.011(4) 0.000(3) C7d 0.060(6) 0.008(3) 0.059(6) -0.007(3) 0.015(5) -0.006(3) C8d 0.030(4) 0.037(4) 0.035(5) 0.008(3) 0.004(4) -0.003(3) C9d 0.027(4) 0.029(4) 0.031(4) 0.002(3) 0.012(3) 0.006(3) C10d 0.113(8) 0.027(4) 0.053(6) 0.027(5) 0.036(6) 0.002(4) C11d 0.093(8) 0.050(6) 0.100(9) 0.040(6) 0.011(7) -0.011(6) C12d 0.028(4) 0.016(3) 0.021(4) 0.004(3) 0.002(3) 0.007(3) C13d 0.018(4) 0.045(4) 0.017(4) -0.002(3) 0.005(3) 0.005(3) C14d 0.050(5) 0.038(4) 0.021(4) -0.002(4) -0.001(4) -0.007(3) C15d 0.064(6) 0.037(5) 0.033(5) -0.010(4) -0.004(5) -0.009(4) C16d 0.052(6) 0.063(6) 0.031(5) -0.039(5) 0.000(4) 0.013(4) C17d 0.031(5) 0.096(8) 0.029(5) 0.011(5) 0.012(4) 0.002(5) C18d 0.026(5) 0.051(5) 0.022(4) -0.001(4) 0.002(3) 0.002(3) C19d 0.026(4) 0.009(3) 0.028(4) -0.006(3) 0.011(3) 0.001(3) C20d 0.039(5) 0.035(4) 0.024(4) -0.003(3) 0.017(4) 0.000(3) C21d 0.033(5) 0.056(5) 0.022(5) -0.002(4) 0.005(4) -0.012(4) C22d 0.026(5) 0.037(4) 0.052(6) 0.003(3) 0.020(4) 0.005(4) C23d 0.029(5) 0.042(4) 0.025(4) 0.007(3) 0.012(4) 0.001(3) C24d 0.013(4) 0.029(4) 0.027(4) -0.003(3) -0.001(3) 0.007(3) C25d 0.015(2) 0.032(3) 0.023(3) 0.002(2) 0.005(2) -0.009(2) C26d 0.036(5) 0.024(4) 0.043(5) 0.001(3) 0.013(4) -0.003(3) C27d 0.050(5) 0.022(4) 0.044(5) 0.001(3) 0.009(4) 0.008(3) C28d 0.056(6) 0.022(4) 0.037(5) 0.006(4) 0.001(4) -0.008(3) C29d 0.048(5) 0.046(5) 0.036(5) 0.015(4) 0.009(4) -0.014(4) C30d 0.019(4) 0.049(5) 0.022(4) -0.006(3) -0.001(3) -0.003(3) C31d 0.125(9) 0.023(4) 0.039(6) 0.018(5) 0.022(6) 0.001(4) #================================= # 10. MOLECULAR GEOMETRY loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1a O2a 1.435(5) S1a O1a 1.449(5) S1a N1a 1.609(6) S1a C25a 1.780(7) S1b O1b 1.444(4) S1b O2b 1.444(5) S1b N1b 1.577(6) S1b C25b 1.785(7) S1c O2c 1.441(5) S1c O1c 1.448(5) S1c N1c 1.606(6) S1c C25c 1.776(7) S1d O2d 1.435(4) S1d O1d 1.449(4) S1d N1d 1.610(5) S1d C25d 1.776(7) O3a C3a 1.171(10) O4a C3a 1.332(9) O4a C10a 1.560(10) O3b C3b 1.185(9) O4b C3b 1.330(8) O4b C10b 1.460(8) O3c C3c 1.194(8) O4c C3c 1.349(8) O4c C10c 1.458(8) O3d C3d 1.211(7) O4d C3d 1.322(8) O4d C10d 1.481(9) N1a C1a 1.451(8) N2a C12a 1.282(9) N2a C2a 1.478(9) N1b C1b 1.481(7) N2b C12b 1.275(8) N2b C2b 1.471(8) N1c C1c 1.479(8) N2c C12c 1.272(8) N2c C2c 1.456(8) N1d C1d 1.456(8) N2d C12d 1.301(8) N2d C2d 1.449(8) C1a C2a 1.531(10) C1a C4a 1.514(9) C2a C3a 1.551(12) C4a C9a 1.370(9) C4a C5a 1.400(9) C5a C6a 1.376(9) C6a C7a 1.380(10) C7a C8a 1.354(10) C8a C9a 1.417(10) C10a C11a 1.498(11) C12a C13a 1.496(10) C12a C19a 1.502(10) C13a C14a 1.362(12) C13a C18a 1.421(11) C14a C15a 1.409(13) C15a C16a 1.364(15) C16a C17a 1.374(15) C17a C18a 1.386(12) C19a C20a 1.367(10) C19a C24a 1.382(10) C20a C21a 1.418(11) C21a C22a 1.403(11) C22a C23a 1.366(11) C23a C24a 1.391(10) C25a C30a 1.367(9) C25a C26a 1.392(9) C26a C27a 1.365(9) C27a C28a 1.382(9) C28a C29a 1.388(10) C28a C31a 1.501(9) C29a C30a 1.421(9) C1b C2b 1.530(9) C1b C4b 1.545(8) C2b C3b 1.544(10) C4b C5b 1.381(9) C4b C9b 1.402(9) C5b C6b 1.366(9) C6b C7b 1.417(10) C7b C8b 1.364(10) C8b C9b 1.375(9) C10b C11b 1.518(11) C12b C19b 1.506(9) C12b C13b 1.516(9) C13b C14b 1.365(9) C13b C18b 1.399(9) C14b C15b 1.388(10) C15b C16b 1.384(11) C16b C17b 1.372(11) C17b C18b 1.380(9) C19b C20b 1.385(9) C19b C24b 1.385(9) C20b C21b 1.368(10) C21b C22b 1.380(10) C22b C23b 1.382(10) C23b C24b 1.387(10) C25b C26b 1.339(9) C25b C30b 1.373(9) C26b C27b 1.411(10) C27b C28b 1.351(10) C28b C29b 1.395(9) C28b C31b 1.493(9) C29b C30b 1.372(9) C1c C2c 1.552(9) C1c C4c 1.521(8) C2c C3c 1.504(9) C4c C5c 1.363(9) C4c C9c 1.400(8) C5c C6c 1.411(10) C6c C7c 1.399(9) C7c C8c 1.369(9) C8c C9c 1.395(9) C10c C11c 1.482(12) C12c C13c 1.497(9) C12c C19c 1.508(9) C13c C14c 1.358(9) C13c C18c 1.409(9) C14c C15c 1.398(9) C15c C16c 1.351(10) C16c C17c 1.347(10) C17c C18c 1.402(9) C19c C24c 1.391(9) C19c C20c 1.399(9) C20c C21c 1.404(9) C21c C22c 1.363(10) C22c C23c 1.344(11) C23c C24c 1.412(10) C25c C26c 1.337(9) C25c C30c 1.425(10) C26c C27c 1.395(9) C27c C28c 1.402(10) C28c C29c 1.405(12) C28c C31c 1.523(11) C29c C30c 1.379(12) C1d C2d 1.503(9) C1d C4d 1.513(9) C2d C3d 1.503(9) C4d C5d 1.367(9) C4d C9d 1.404(9) C5d C6d 1.431(9) C6d C7d 1.397(10) C7d C8d 1.352(9) C8d C9d 1.374(9) C10d C11d 1.452(13) C12d C19d 1.480(9) C12d C13d 1.513(9) C13d C18d 1.370(9) C13d C14d 1.407(10) C14d C15d 1.343(10) C15d C16d 1.324(12) C16d C17d 1.401(12) C17d C18d 1.421(11) C19d C20d 1.381(9) C19d C24d 1.387(9) C20d C21d 1.394(10) C21d C22d 1.385(10) C22d C23d 1.402(10) C23d C24d 1.373(9) C25d C30d 1.337(9) C25d C26d 1.373(9) C26d C27d 1.396(10) C27d C28d 1.391(11) C28d C29d 1.391(11) C28d C31d 1.527(10) C29d C30d 1.414(10) N1a H1na 0.71 N1b H1nb 1.03 N1c H1nc 0.99 N1d H1nd 0.84 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle O1a S1a O2a 118.7(3) O2a S1a N1a 108.6(3) O2a S1a C25a 106.9(3) O1a S1a N1a 107.4(3) O1a S1a C25a 107.0(3) N1a S1a C25a 108.0(3) O1b S1b O2b 117.3(3) O1b S1b N1b 109.4(3) O1b S1b C25b 105.6(3) O2b S1b N1b 106.2(3) O2b S1b C25b 108.8(3) N1b S1b C25b 109.4(3) O1c S1c O2c 117.9(3) O2c S1c N1c 109.2(3) O2c S1c C25c 107.2(3) O1c S1c N1c 105.0(3) O1c S1c C25c 107.7(3) N1c S1c C25c 109.6(3) O1d S1d O2d 117.7(3) O2d S1d N1d 108.3(3) O2d S1d C25d 105.5(3) O1d S1d N1d 107.5(3) O1d S1d C25d 107.7(3) N1d S1d C25d 110.0(3) C3a O4a C10a 110.7(7) C3b O4b C10b 117.8(6) C3c O4c C10c 116.9(6) C3d O4d C10d 114.7(6) S1a N1a C1a 124.4(5) C2a N2a C12a 120.0(6) S1b N1b C1b 123.4(4) C2b N2b C12b 121.0(6) S1c N1c C1c 122.9(4) C2c N2c C12c 119.2(6) S1d N1d C1d 125.8(4) C2d N2d C12d 122.8(5) N1a C1a C4a 113.1(5) N1a C1a C2a 109.8(6) C2a C1a C4a 112.2(5) N2a C2a C1a 106.8(6) N2a C2a C3a 115.5(6) C1a C2a C3a 106.5(6) O3a C3a O4a 125.9(10) O3a C3a C2a 122.0(8) O4a C3a C2a 111.8(8) C5a C4a C9a 119.6(6) C1a C4a C9a 121.5(6) C1a C4a C5a 118.9(6) C4a C5a C6a 119.8(7) C5a C6a C7a 121.7(7) C6a C7a C8a 117.9(7) C7a C8a C9a 122.5(7) C4a C9a C8a 118.5(7) O4a C10a C11a 106.6(6) N2a C12a C13a 125.7(7) N2a C12a C19a 117.0(6) C13a C12a C19a 117.3(7) C14a C13a C18a 120.8(8) C12a C13a C14a 120.7(8) C12a C13a C18a 118.4(8) C13a C14a C15a 119.5(9) C14a C15a C16a 121.1(10) C15a C16a C17a 118.3(9) C16a C17a C18a 123.4(9) C13a C18a C17a 116.8(9) C20a C19a C24a 119.7(7) C12a C19a C20a 121.1(7) C12a C19a C24a 119.3(7) C19a C20a C21a 121.1(8) C20a C21a C22a 118.2(8) C21a C22a C23a 119.8(8) C22a C23a C24a 121.1(8) C19a C24a C23a 119.9(7) C26a C25a C30a 122.1(6) S1a C25a C30a 119.0(5) S1a C25a C26a 118.7(5) C25a C26a C27a 117.9(6) C26a C27a C28a 122.8(6) C27a C28a C29a 118.7(6) C29a C28a C31a 119.4(6) C27a C28a C31a 121.8(6) C28a C29a C30a 119.7(7) C25a C30a C29a 118.7(6) N1b C1b C2b 108.8(5) N1b C1b C4b 115.0(5) C2b C1b C4b 111.3(6) N2b C2b C1b 109.9(5) N2b C2b C3b 111.8(6) C1b C2b C3b 108.3(6) O3b C3b O4b 123.6(7) O3b C3b C2b 124.5(6) O4b C3b C2b 111.9(6) C5b C4b C9b 118.8(6) C1b C4b C5b 119.8(6) C1b C4b C9b 121.1(6) C4b C5b C6b 121.5(6) C5b C6b C7b 119.4(6) C6b C7b C8b 118.6(6) C7b C8b C9b 121.8(7) C4b C9b C8b 119.5(6) O4b C10b C11b 106.4(6) N2b C12b C19b 117.3(6) N2b C12b C13b 126.4(6) C13b C12b C19b 116.2(6) C14b C13b C18b 118.2(6) C12b C13b C14b 121.9(6) C12b C13b C18b 119.9(6) C13b C14b C15b 122.1(7) C14b C15b C16b 119.8(7) C15b C16b C17b 118.0(8) C16b C17b C18b 122.5(7) C13b C18b C17b 119.3(6) C20b C19b C24b 118.9(6) C12b C19b C20b 120.6(6) C12b C19b C24b 120.3(7) C19b C20b C21b 121.2(7) C20b C21b C22b 120.5(7) C21b C22b C23b 118.7(7) C22b C23b C24b 121.1(7) C19b C24b C23b 119.6(7) C26b C25b C30b 120.9(6) S1b C25b C26b 120.7(5) S1b C25b C30b 118.5(5) C25b C26b C27b 118.7(6) C26b C27b C28b 121.9(6) C27b C28b C29b 117.7(6) C27b C28b C31b 119.7(7) C29b C28b C31b 122.6(6) C28b C29b C30b 120.7(6) C25b C30b C29b 120.0(6) N1c C1c C4c 115.0(5) N1c C1c C2c 108.6(5) C2c C1c C4c 109.3(5) N2c C2c C1c 107.2(5) N2c C2c C3c 111.9(5) C1c C2c C3c 112.1(6) O3c C3c O4c 123.8(6) O3c C3c C2c 127.5(7) O4c C3c C2c 108.5(6) C5c C4c C9c 119.8(6) C1c C4c C5c 118.2(5) C1c C4c C9c 121.6(6) C4c C5c C6c 120.7(6) C5c C6c C7c 119.4(6) C6c C7c C8c 119.4(6) C7c C8c C9c 121.2(6) C4c C9c C8c 119.5(6) O4c C10c C11c 109.1(6) N2c C12c C13c 126.2(6) N2c C12c C19c 115.6(6) C13c C12c C19c 118.1(6) C14c C13c C18c 119.0(6) C12c C13c C14c 121.7(6) C12c C13c C18c 118.9(5) C13c C14c C15c 121.3(7) C14c C15c C16c 118.4(6) C15c C16c C17c 122.6(7) C16c C17c C18c 119.7(7) C13c C18c C17c 118.7(6) C20c C19c C24c 119.1(6) C12c C19c C24c 119.7(6) C12c C19c C20c 121.1(6) C19c C20c C21c 120.3(7) C20c C21c C22c 118.6(7) C21c C22c C23c 122.7(7) C22c C23c C24c 119.8(7) C19c C24c C23c 119.3(7) C26c C25c C30c 119.4(7) S1c C25c C26c 120.8(5) S1c C25c C30c 119.6(6) C25c C26c C27c 122.5(7) C26c C27c C28c 119.4(7) C27c C28c C29c 118.2(7) C27c C28c C31c 120.8(8) C29c C28c C31c 120.9(8) C28c C29c C30c 121.4(7) C25c C30c C29c 119.1(8) N1d C1d C2d 110.6(5) N1d C1d C4d 113.9(5) C2d C1d C4d 110.8(6) N2d C2d C3d 113.7(5) N2d C2d C1d 107.3(5) C1d C2d C3d 112.9(6) O3d C3d O4d 123.7(6) O3d C3d C2d 123.6(6) O4d C3d C2d 112.7(6) C5d C4d C9d 118.3(6) C1d C4d C5d 119.9(6) C1d C4d C9d 121.5(5) C4d C5d C6d 121.3(7) C5d C6d C7d 117.6(6) C6d C7d C8d 121.1(6) C7d C8d C9d 120.6(7) C4d C9d C8d 121.1(6) O4d C10d C11d 108.9(7) N2d C12d C19d 118.0(6) N2d C12d C13d 123.8(6) C13d C12d C19d 118.0(6) C14d C13d C18d 120.2(6) C12d C13d C18d 119.0(6) C12d C13d C14d 120.8(6) C13d C14d C15d 119.6(7) C14d C15d C16d 122.4(8) C15d C16d C17d 120.5(7) C16d C17d C18d 118.7(8) C13d C18d C17d 118.5(7) C20d C19d C24d 118.7(6) C12d C19d C20d 122.3(6) C12d C19d C24d 119.0(6) C19d C20d C21d 120.5(7) C20d C21d C22d 120.7(7) C21d C22d C23d 118.4(7) C22d C23d C24d 120.4(7) C19d C24d C23d 121.3(7) C26d C25d C30d 121.2(7) S1d C25d C30d 120.6(6) S1d C25d C26d 118.2(5) C25d C26d C27d 119.3(7) C26d C27d C28d 120.7(7) C27d C28d C29d 118.7(7) C29d C28d C31d 119.0(7) C27d C28d C31d 122.2(7) C28d C29d C30d 119.3(7) C25d C30d C29d 120.8(7) C1a N1a H1na 135 S1a N1a H1na 100 C1b N1b H1nb 111 S1b N1b H1nb 115 C1c N1c H1nc 126 S1c N1c H1nc 99 C1d N1d H1nd 107 S1d N1d H1nd 127 #===END