#============================================================================ data_global #============================================================================ _audit_creation_date 7-12-10 _audit_creation_method 'SHELXL and local programs' _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _publ_contact_author_name 'Fanwick, Phillip E.' _publ_contact_author_address ; Department of Chemistry Purdue University 560 Oval Dr. W. Lafayette IN 47907-2084 USA ; _publ_contact_author_email 'pfanwick@purdue.edu' _publ_contact_author_fax '1(765)4940239' _publ_contact_author_phone '1(765)4944572' _publ_requested_journal ? _publ_requested_category ? _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_Cambridge ? _journal_name_full ? _journal_volume ? _journal_year ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? # 3. TITLE AND AUTHOR LIST _publ_section_title ; ? ; _publ_section_title_footnote ; ? ; # The loop structure below should contain the names and addresses and footnotes # of all authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address _publ_author_footnote 'Matson, Ellen' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; 'Bart, Suzanne C.' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; 'Fanwick, Phillip E.' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; ; ? ; # 4. TEXT _publ_section_abstract ; ? ; _publ_section_comment ; ? ; _database_code_CSD 'EMM14 ' _publ_section_experimental ; ? ; _publ_section_references ; P.T. Beurskens, G. Beurskens, R. deGelder,S. Garcia-Granda, R.O. Gould, J.M.M. Smits, (2008). The DIRDIF2008 Program System. Crystallography Laboratory, University. of Nijmegen, The Netherlands. Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. Fair, C.K. (1990). MolEN, An Interactive Intelligent System for Crystal Structure Analysis, User Manual, ,Enraf-Nonius, Delft, The Netherlands. Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Otwinowski Z. & Minor, W. (1997). Methods Enzymol., 276, 307-327. Prince, E. and Nicholson, W. L. (1983).Acta Cryst A39, 407-410. Sheldrick, G.M. (2008). Acta Cryst.,A64, 112-122. Spek A.L.(1997). J. Appl. Cryst, 36, 7-13. ; _publ_section_figure_captions ; ? ; _publ_section_acknowledgements ;? ; data_EMM14 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description needle _exptl_crystal_colour 'green' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _chemical_name_systematic ; ? ; _chemical_formula_sum 'C47.50 H61 B2 N12 S3 U1' _chemical_formula_moiety 'C37 H49 B2 N12 S3,U1,(C7 H8)' _chemical_formula_structural ? _chemical_formula_weight 1155.94 _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2943(5) _cell_length_b 14.3126(5) _cell_length_c 17.4998(8) _cell_angle_alpha 72.318(2) _cell_angle_beta 74.613(3) _cell_angle_gamma 69.986(3) _cell_volume 2490.96(18) _cell_measurement_reflns_used 8820 _cell_measurement_theta_min 2 _cell_measurement_theta_max 72 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' loop_ _atom_type_symbol _atom_type_radius_bond U 1.42 S 1.02 N 0.75 C 0.77 B 0.82 H 0.32 _diffrn_radiation_type CU-K\a _diffrn_radiation_wavelength 1.54184 _exptl_absorpt_coefficient_mu 11.384 _cell_measurement_temperature 150.0(2) _exptl_crystal_F_000 1166 # 6. DATA COLLECTION _diffrn_ambient_temperature 150.0(2) _diffrn_measurement_device_type Rigaku_Rapid_II _diffrn_radiation_monochromator 'confocal optics' _diffrn_measurement_method \w _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.3621 _exptl_absorpt_correction_T_max 0.5051 _diffrn_reflns_number 85018 _diffrn_measured_fraction_theta_max 0.8960 _diffrn_reflns_theta_full 72.1 _diffrn_measured_fraction_theta_full 0.8960 _reflns_number_total 8812 _reflns_number_gt 8593 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 72.14 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_max 21 _diffrn_special_details 'mosaicity from Denzo/Scalepack is 0.61' _diffrn_standards_number 0 _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_measurement_details ; Data were collected on a Rigaku Rapid which has a quarter chi circle and a 200 degree curved image plate at a fixed distance of 127.4mm. Strategy was optimized using the CrystalClear software. The completeness is the best that can be obtained with this geometry. The missing data are not cusp data but mostly high angle data. Also the use of HKL2000/SCALEPACK lowers the number of observed data as inconsistent equivalents are removed from the data set and not included in the collected total ; # 7. REFINEMENT DATA _refine_special_details ; Outlier data were removed using a local program based on the method of Prince and Nicholson. Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_all 0.039 _refine_ls_R_factor_gt 0.039 _refine_ls_wR_factor_ref 0.104 _refine_ls_wR_factor_gt 0.103 _refine_ls_hydrogen_treatment mixed _refine_ls_number_reflns 8812 _refine_ls_number_parameters 613 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+5.2742P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_shift/su_max 0.004 _refine_diff_density_max 1.90 _refine_diff_density_min -1.63 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection 'CrystalClear(Rigaku, 2001)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1996)' _computing_structure_solution ; PATTY (DIRDIF, Beurskins, 2008) ; _computing_structure_refinement 'SHELX97 (Sheldrick, 2008)' _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLATON (Spek, 2003) ; _computing_publication_material 'SHELX97(Sheldrick, 2008) and local programs' # 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_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 U1 0.214910(14) 0.180990(10) 0.203413(8) 0.02754(8) Uani 1 1 d . . . S41 0.02413(13) 0.21110(9) 0.10268(7) 0.0348(3) Uani 1 1 d . . . S42 0.08767(13) 0.02025(9) 0.23217(7) 0.0363(3) Uani 1 1 d . . . S43 -0.03865(15) 0.03638(10) 0.09506(9) 0.0434(3) Uani 1 1 d . . . N11 0.1750(4) 0.3611(3) 0.1109(2) 0.0305(9) Uani 1 1 d . . . N12 0.2565(4) 0.3792(3) 0.0377(2) 0.0323(9) Uani 1 1 d . . . N21 0.4443(4) 0.2015(3) 0.1490(2) 0.0315(9) Uani 1 1 d . . . N22 0.4712(4) 0.2530(3) 0.0683(2) 0.0304(9) Uani 1 1 d . . . N31 0.3361(4) 0.1109(3) 0.0668(3) 0.0321(9) Uani 1 1 d . . . N32 0.3275(4) 0.2017(3) 0.0078(3) 0.0325(9) Uani 1 1 d . . . N61 0.3107(4) 0.0413(3) 0.3218(2) 0.0343(9) Uani 1 1 d . . . N62 0.2872(4) 0.0539(3) 0.3990(2) 0.0337(9) Uani 1 1 d . . . N71 0.2601(4) 0.2830(3) 0.2930(3) 0.0340(9) Uani 1 1 d . . . N72 0.2457(4) 0.2453(3) 0.3767(3) 0.0337(9) Uani 1 1 d . . . N81 0.0233(4) 0.2060(3) 0.3332(3) 0.0336(9) Uani 1 1 d . . . N82 0.0583(5) 0.1707(3) 0.4096(3) 0.0370(10) Uani 1 1 d . . . C13 0.2186(5) 0.4796(4) -0.0006(3) 0.0353(11) Uani 1 1 d . . . C14 0.1101(6) 0.5269(4) 0.0479(3) 0.0400(12) Uani 1 1 d . . . C15 0.0870(5) 0.4510(4) 0.1168(3) 0.0339(11) Uani 1 1 d . . . C16 0.2876(7) 0.5261(4) -0.0805(3) 0.0464(14) Uani 1 1 d . . . C17 -0.0164(6) 0.4588(4) 0.1904(4) 0.0458(14) Uani 1 1 d . . . C23 0.5882(5) 0.2661(4) 0.0515(3) 0.0370(12) Uani 1 1 d . . . C24 0.6400(6) 0.2226(4) 0.1213(3) 0.0381(12) Uani 1 1 d . . . C25 0.5478(5) 0.1839(4) 0.1803(3) 0.0348(11) Uani 1 1 d . . . C26 0.6447(6) 0.3216(5) -0.0300(3) 0.0436(13) Uani 1 1 d . . . C27 0.5585(6) 0.1308(5) 0.2675(3) 0.0461(14) Uani 1 1 d . . . C33 0.3014(6) 0.1927(4) -0.0602(3) 0.0384(12) Uani 1 1 d . . . C34 0.2975(5) 0.0940(4) -0.0477(3) 0.0376(12) Uani 1 1 d . . . C35 0.3206(5) 0.0460(4) 0.0313(3) 0.0336(11) Uani 1 1 d . . . C36 0.2826(7) 0.2792(5) -0.1338(4) 0.0519(15) Uani 1 1 d . . . C37 0.3333(6) -0.0656(4) 0.0709(4) 0.0413(12) Uani 1 1 d . . . C40 0.0263(5) 0.0876(4) 0.1477(3) 0.0314(10) Uani 1 1 d . . . C41 -0.0472(6) -0.0848(4) 0.1600(3) 0.0398(12) Uani 1 1 d . . . C42 -0.1329(8) -0.0903(6) 0.2318(5) 0.066(2) Uani 1 1 d . . . C43 -0.1415(10) -0.1843(8) 0.2804(5) 0.083(3) Uani 1 1 d . . . C44 -0.0652(9) -0.2719(6) 0.2571(5) 0.072(2) Uani 1 1 d . . . C45 0.0203(8) -0.2668(5) 0.1831(5) 0.0652(19) Uani 1 1 d . . . C46 0.0301(6) -0.1729(4) 0.1345(4) 0.0491(14) Uani 1 1 d . . . C63 0.3590(6) -0.0296(4) 0.4459(3) 0.0393(12) Uani 1 1 d . . . C64 0.4279(6) -0.0961(4) 0.3981(3) 0.0413(12) Uani 1 1 d . . . C65 0.3978(5) -0.0506(4) 0.3213(3) 0.0389(12) Uani 1 1 d . . . C66 0.3561(6) -0.0394(5) 0.5343(3) 0.0445(13) Uani 1 1 d . . . C67 0.4512(7) -0.0882(5) 0.2443(4) 0.0514(16) Uani 1 1 d . . . C73 0.2910(6) 0.2971(4) 0.4103(3) 0.0381(12) Uani 1 1 d . . . C74 0.3367(6) 0.3689(4) 0.3481(3) 0.0414(12) Uani 1 1 d . . . C75 0.3144(6) 0.3589(4) 0.2766(3) 0.0365(12) Uani 1 1 d . . . C76 0.2828(7) 0.2801(5) 0.4996(3) 0.0484(14) Uani 1 1 d . . . C77 0.3469(6) 0.4243(4) 0.1927(3) 0.0425(13) Uani 1 1 d . . . C83 -0.0445(6) 0.1592(4) 0.4677(3) 0.0428(13) Uani 1 1 d . . . C84 -0.1488(6) 0.1912(4) 0.4312(3) 0.0410(12) Uani 1 1 d . . . C85 -0.1033(5) 0.2192(4) 0.3478(3) 0.0359(11) Uani 1 1 d . . . C86 -0.0375(7) 0.1162(6) 0.5572(4) 0.0597(18) Uani 1 1 d . . . C87 -0.1813(6) 0.2544(5) 0.2819(4) 0.0472(14) Uani 1 1 d . . . C911 0.6055(12) 0.3545(8) 0.6831(4) 0.230(14) Uani 1 1 d G . . C912 0.6172(10) 0.3327(6) 0.6088(5) 0.134(6) Uani 1 1 d G . . C913 0.5174(12) 0.3787(8) 0.5650(6) 0.153(6) Uani 1 1 d G . . C914 0.4061(10) 0.4465(9) 0.5956(9) 0.230(14) Uani 1 1 d G . . C915 0.3945(11) 0.4683(8) 0.6699(10) 0.188(10) Uani 1 1 d G . . C916 0.4942(15) 0.4222(9) 0.7136(6) 0.150(8) Uani 1 1 d G . . C917 0.6875(19) 0.3202(12) 0.7339(7) 0.157(8) Uani 1 1 d . . . C921 0.9883(14) 0.4815(11) 0.4686(9) 0.056(3) Uani 0.50 1 d P . . C922 1.0692(8) 0.5398(6) 0.4431(5) 0.067(2) Uani 1 1 d . . . C923 0.9044(17) 0.4119(12) 0.5107(12) 0.074(5) Uani 0.50 1 d P . . C925 1.0403(17) 0.4904(13) 0.3978(10) 0.074(5) Uani 0.50 1 d P . . C927 0.9554(9) 0.4315(7) 0.4206(7) 0.085(3) Uani 1 1 d . . . B1 0.3725(6) 0.2911(4) 0.0112(3) 0.0322(12) Uani 1 1 d . . . B2 0.1940(6) 0.1524(5) 0.4236(3) 0.0375(13) Uani 1 1 d . . . H1 0.414(6) 0.323(5) -0.052(4) 0.048(17) Uiso 1 1 d . . . H2 0.197(5) 0.142(4) 0.485(3) 0.029(13) Uiso 1 1 d . . . H14 0.0613 0.5967 0.0366 0.048 Uiso 1 1 calc R . . H24 0.7222 0.2196 0.1279 0.046 Uiso 1 1 calc R . . H34 0.2822 0.0649 -0.0849 0.045 Uiso 1 1 calc R . . H42 -0.1863 -0.0295 0.2480 0.080 Uiso 1 1 calc R . . H43 -0.2008 -0.1882 0.3304 0.099 Uiso 1 1 calc R . . H44 -0.0704 -0.3366 0.2914 0.087 Uiso 1 1 calc R . . H45 0.0717 -0.3277 0.1662 0.078 Uiso 1 1 calc R . . H46 0.0888 -0.1684 0.0843 0.059 Uiso 1 1 calc R . . H64 0.4858 -0.1615 0.4143 0.050 Uiso 1 1 calc R . . H74 0.3755 0.4158 0.3528 0.050 Uiso 1 1 calc R . . H84 -0.2348 0.1939 0.4573 0.049 Uiso 1 1 calc R . . H16A 0.3724 0.5238 -0.0743 0.070 Uiso 1 1 calc R . . H16B 0.2385 0.5974 -0.0990 0.070 Uiso 1 1 calc R . . H16C 0.2973 0.4878 -0.1207 0.070 Uiso 1 1 calc R . . H17A -0.0974 0.4635 0.1769 0.069 Uiso 1 1 calc R . . H17B -0.0257 0.5200 0.2082 0.069 Uiso 1 1 calc R . . H17C 0.0062 0.3979 0.2344 0.069 Uiso 1 1 calc R . . H26A 0.6518 0.2862 -0.0717 0.065 Uiso 1 1 calc R . . H26B 0.7299 0.3231 -0.0280 0.065 Uiso 1 1 calc R . . H26C 0.5893 0.3918 -0.0435 0.065 Uiso 1 1 calc R . . H27A 0.4858 0.1660 0.3035 0.069 Uiso 1 1 calc R . . H27B 0.6386 0.1321 0.2784 0.069 Uiso 1 1 calc R . . H27C 0.5581 0.0597 0.2775 0.069 Uiso 1 1 calc R . . H36A 0.2174 0.3391 -0.1178 0.078 Uiso 1 1 calc R . . H36B 0.2545 0.2590 -0.1733 0.078 Uiso 1 1 calc R . . H36C 0.3636 0.2961 -0.1587 0.078 Uiso 1 1 calc R . . H37A 0.4204 -0.1001 0.0820 0.062 Uiso 1 1 calc R . . H37B 0.3161 -0.0973 0.0342 0.062 Uiso 1 1 calc R . . H37C 0.2716 -0.0718 0.1221 0.062 Uiso 1 1 calc R . . H66A 0.3831 0.0162 0.5395 0.067 Uiso 1 1 calc R . . H66B 0.4144 -0.1053 0.5563 0.067 Uiso 1 1 calc R . . H66C 0.2688 -0.0354 0.5648 0.067 Uiso 1 1 calc R . . H67A 0.4051 -0.1343 0.2429 0.077 Uiso 1 1 calc R . . H67B 0.5423 -0.1250 0.2427 0.077 Uiso 1 1 calc R . . H67C 0.4410 -0.0298 0.1971 0.077 Uiso 1 1 calc R . . H76A 0.1932 0.2898 0.5270 0.073 Uiso 1 1 calc R . . H76B 0.3166 0.3291 0.5095 0.073 Uiso 1 1 calc R . . H76C 0.3333 0.2103 0.5211 0.073 Uiso 1 1 calc R . . H77A 0.3798 0.3818 0.1528 0.064 Uiso 1 1 calc R . . H77B 0.4121 0.4552 0.1926 0.064 Uiso 1 1 calc R . . H77C 0.2696 0.4784 0.1782 0.064 Uiso 1 1 calc R . . H86A 0.0271 0.0494 0.5645 0.090 Uiso 1 1 calc R . . H86B -0.1211 0.1083 0.5878 0.090 Uiso 1 1 calc R . . H86C -0.0138 0.1631 0.5773 0.090 Uiso 1 1 calc R . . H87A -0.1441 0.3003 0.2350 0.071 Uiso 1 1 calc R . . H87B -0.2694 0.2908 0.3024 0.071 Uiso 1 1 calc R . . H87C -0.1813 0.1950 0.2651 0.071 Uiso 1 1 calc R . . H912 0.6933 0.2864 0.5879 0.161 Uiso 1 1 calc R . . H913 0.5254 0.3639 0.5142 0.184 Uiso 1 1 calc R . . H914 0.3379 0.4780 0.5657 0.276 Uiso 1 1 calc R . . H915 0.3184 0.5146 0.6908 0.225 Uiso 1 1 calc R . . H916 0.4862 0.4371 0.7644 0.180 Uiso 1 1 calc R . . H91A 0.7673 0.2751 0.7107 0.235 Uiso 1 1 calc R . . H91B 0.6504 0.2819 0.7862 0.235 Uiso 1 1 calc R . . H91C 0.7056 0.3781 0.7426 0.235 Uiso 1 1 calc R . . 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 U1 0.03153(12) 0.02427(10) 0.02677(10) -0.01002(7) -0.00821(7) -0.00101(6) S41 0.0384(7) 0.0294(6) 0.0358(6) -0.0088(5) -0.0130(5) -0.0016(4) S42 0.0458(8) 0.0310(6) 0.0342(6) -0.0154(5) -0.0130(5) -0.0006(5) S43 0.0565(9) 0.0335(6) 0.0474(7) -0.0120(6) -0.0251(6) -0.0069(5) N11 0.032(2) 0.0254(19) 0.034(2) -0.0095(17) -0.0086(17) -0.0041(16) N12 0.043(3) 0.028(2) 0.0286(19) -0.0144(18) -0.0116(17) -0.0016(15) N21 0.037(2) 0.0273(19) 0.030(2) -0.0144(17) -0.0095(17) 0.0020(15) N22 0.031(2) 0.0301(19) 0.032(2) -0.0138(17) -0.0036(16) -0.0060(16) N31 0.035(2) 0.0273(19) 0.036(2) -0.0105(17) -0.0087(17) -0.0063(16) N32 0.033(2) 0.031(2) 0.032(2) -0.0119(18) -0.0073(17) -0.0016(16) N61 0.037(2) 0.032(2) 0.032(2) -0.0090(18) -0.0114(17) -0.0017(16) N62 0.036(2) 0.035(2) 0.030(2) -0.0118(18) -0.0126(17) 0.0008(16) N71 0.036(2) 0.039(2) 0.028(2) -0.0142(19) -0.0053(17) -0.0050(17) N72 0.036(2) 0.034(2) 0.031(2) -0.0109(18) -0.0069(17) -0.0055(17) N81 0.035(2) 0.038(2) 0.034(2) -0.0213(19) -0.0089(17) -0.0035(17) N82 0.040(3) 0.038(2) 0.030(2) -0.013(2) -0.0058(18) -0.0021(17) C13 0.049(3) 0.025(2) 0.033(2) -0.012(2) -0.015(2) 0.0008(18) C14 0.049(3) 0.026(2) 0.044(3) -0.009(2) -0.019(2) 0.000(2) C15 0.037(3) 0.022(2) 0.041(3) -0.007(2) -0.013(2) -0.0021(19) C16 0.063(4) 0.034(3) 0.038(3) -0.016(3) -0.008(3) -0.001(2) C17 0.041(3) 0.034(3) 0.056(3) -0.010(2) -0.001(3) -0.010(2) C23 0.038(3) 0.033(2) 0.042(3) -0.013(2) -0.004(2) -0.011(2) C24 0.032(3) 0.038(3) 0.046(3) -0.013(2) -0.009(2) -0.007(2) C25 0.035(3) 0.032(2) 0.040(3) -0.014(2) -0.010(2) -0.002(2) C26 0.041(3) 0.052(3) 0.039(3) -0.023(3) 0.000(2) -0.007(2) C27 0.040(3) 0.053(3) 0.041(3) -0.014(3) -0.017(2) 0.003(2) C33 0.046(3) 0.037(3) 0.034(3) -0.010(2) -0.012(2) -0.008(2) C34 0.036(3) 0.040(3) 0.043(3) -0.013(2) -0.006(2) -0.015(2) C35 0.032(3) 0.032(2) 0.038(3) -0.010(2) -0.005(2) -0.011(2) C36 0.075(5) 0.043(3) 0.042(3) -0.019(3) -0.027(3) 0.000(2) C37 0.047(3) 0.029(2) 0.048(3) -0.011(2) -0.007(2) -0.011(2) C40 0.027(3) 0.031(2) 0.037(2) -0.012(2) -0.0055(19) -0.0068(19) C41 0.042(3) 0.042(3) 0.044(3) -0.017(2) -0.015(2) -0.011(2) C42 0.075(5) 0.069(5) 0.065(4) -0.033(4) 0.004(4) -0.029(4) C43 0.116(8) 0.108(7) 0.051(4) -0.081(6) 0.003(4) -0.016(4) C44 0.104(7) 0.065(5) 0.066(5) -0.060(5) -0.035(4) 0.017(4) C45 0.076(5) 0.044(4) 0.081(5) -0.024(3) -0.029(4) -0.001(3) C46 0.055(4) 0.038(3) 0.058(4) -0.018(3) -0.014(3) -0.007(3) C63 0.041(3) 0.038(3) 0.040(3) -0.019(2) -0.018(2) 0.007(2) C64 0.042(3) 0.034(3) 0.045(3) -0.009(2) -0.019(2) 0.002(2) C65 0.039(3) 0.032(3) 0.044(3) -0.008(2) -0.015(2) -0.002(2) C66 0.051(4) 0.046(3) 0.035(3) -0.014(3) -0.019(2) 0.003(2) C67 0.059(4) 0.042(3) 0.046(3) -0.003(3) -0.016(3) -0.008(3) C73 0.047(3) 0.034(3) 0.037(3) -0.009(2) -0.015(2) -0.011(2) C74 0.054(4) 0.040(3) 0.040(3) -0.021(3) -0.013(2) -0.011(2) C75 0.040(3) 0.032(3) 0.038(3) -0.012(2) -0.009(2) -0.006(2) C76 0.062(4) 0.052(3) 0.038(3) -0.018(3) -0.019(3) -0.011(2) C77 0.058(4) 0.035(3) 0.038(3) -0.023(3) -0.010(3) 0.000(2) C83 0.045(3) 0.044(3) 0.036(3) -0.018(3) -0.003(2) -0.003(2) C84 0.035(3) 0.044(3) 0.042(3) -0.016(2) 0.001(2) -0.007(2) C85 0.033(3) 0.038(3) 0.041(3) -0.018(2) -0.007(2) -0.006(2) C86 0.048(4) 0.086(5) 0.032(3) -0.027(3) 0.001(2) 0.006(3) C87 0.041(3) 0.060(4) 0.045(3) -0.020(3) -0.011(2) -0.010(3) C911 0.51(4) 0.216(19) 0.072(7) -0.30(3) 0.027(15) -0.028(10) C912 0.278(19) 0.120(9) 0.057(5) -0.131(12) -0.024(8) -0.017(5) C913 0.148(14) 0.119(12) 0.185(17) -0.004(10) -0.024(12) -0.070(12) C914 0.20(2) 0.125(14) 0.42(4) -0.046(14) -0.19(3) -0.024(19) C915 0.21(2) 0.19(2) 0.21(2) -0.115(19) 0.012(19) -0.084(18) C916 0.165(15) 0.151(13) 0.159(14) -0.124(12) 0.093(12) -0.088(12) C917 0.28(2) 0.183(14) 0.080(7) -0.180(15) -0.077(10) 0.028(8) C921 0.048(8) 0.050(7) 0.063(8) 0.000(6) -0.016(6) -0.012(6) C922 0.062(5) 0.055(4) 0.071(5) 0.002(4) -0.018(4) -0.013(4) C923 0.065(10) 0.052(8) 0.102(13) 0.006(7) -0.033(9) -0.025(8) C925 0.068(10) 0.066(10) 0.068(10) 0.015(8) -0.024(8) -0.018(8) C927 0.070(6) 0.073(5) 0.117(8) -0.001(5) -0.030(5) -0.039(5) B1 0.036(3) 0.029(3) 0.030(3) -0.009(2) -0.008(2) -0.004(2) B2 0.040(3) 0.041(3) 0.028(3) -0.011(3) -0.006(2) -0.003(2) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag U1 N11 2.555(4) . . ? U1 N61 2.579(4) . . ? U1 N21 2.598(4) . . ? U1 N71 2.678(5) . . ? U1 N81 2.707(4) . . ? U1 N31 2.716(4) . . ? U1 S42 2.9643(13) . . ? U1 S41 2.9756(13) . . ? S41 C40 1.698(5) . . ? S42 C40 1.678(5) . . ? S43 C40 1.749(5) . . ? S43 C41 1.780(6) . . ? N11 C15 1.344(6) . . ? N11 N12 1.375(6) . . ? N12 C13 1.357(6) . . ? N12 B1 1.557(7) . . ? N21 C25 1.334(7) . . ? N21 N22 1.387(5) . . ? N22 C23 1.340(7) . . ? N22 B1 1.543(7) . . ? N31 C35 1.341(6) . . ? N31 N32 1.385(6) . . ? N32 C33 1.351(7) . . ? N32 B1 1.551(7) . . ? N61 C65 1.347(7) . . ? N61 N62 1.362(6) . . ? N62 C63 1.361(6) . . ? N62 B2 1.547(7) . . ? N71 C75 1.346(8) . . ? N71 N72 1.385(6) . . ? N72 C73 1.356(7) . . ? N72 B2 1.548(8) . . ? N81 C85 1.340(7) . . ? N81 N82 1.390(6) . . ? N82 C83 1.345(7) . . ? N82 B2 1.538(8) . . ? C13 C14 1.382(8) . . ? C13 C16 1.489(8) . . ? C14 C15 1.390(7) . . ? C14 H14 0.9500 . . ? C15 C17 1.495(8) . . ? C16 H16A 0.9800 . . ? C16 H16B 0.9800 . . ? C16 H16C 0.9800 . . ? C17 H17A 0.9800 . . ? C17 H17B 0.9800 . . ? C17 H17C 0.9800 . . ? C23 C24 1.375(8) . . ? C23 C26 1.499(8) . . ? C24 C25 1.392(8) . . ? C24 H24 0.9500 . . ? C25 C27 1.500(7) . . ? C26 H26A 0.9800 . . ? C26 H26B 0.9800 . . ? C26 H26C 0.9800 . . ? C27 H27A 0.9800 . . ? C27 H27B 0.9800 . . ? C27 H27C 0.9800 . . ? C33 C34 1.376(8) . . ? C33 C36 1.495(8) . . ? C34 C35 1.393(7) . . ? C34 H34 0.9500 . . ? C35 C37 1.509(7) . . ? C36 H36A 0.9800 . . ? C36 H36B 0.9800 . . ? C36 H36C 0.9800 . . ? C37 H37A 0.9800 . . ? C37 H37B 0.9800 . . ? C37 H37C 0.9800 . . ? C41 C42 1.367(9) . . ? C41 C46 1.389(8) . . ? C42 C43 1.376(12) . . ? C42 H42 0.9500 . . ? C43 C44 1.367(13) . . ? C43 H43 0.9500 . . ? C44 C45 1.394(12) . . ? C44 H44 0.9500 . . ? C45 C46 1.379(9) . . ? C45 H45 0.9500 . . ? C46 H46 0.9500 . . ? C63 C64 1.358(8) . . ? C63 C66 1.503(7) . . ? C64 C65 1.379(7) . . ? C64 H64 0.9500 . . ? C65 C67 1.502(8) . . ? C66 H66A 0.9800 . . ? C66 H66B 0.9800 . . ? C66 H66C 0.9800 . . ? C67 H67A 0.9800 . . ? C67 H67B 0.9800 . . ? C67 H67C 0.9800 . . ? C73 C74 1.377(8) . . ? C73 C76 1.489(7) . . ? C74 C75 1.397(7) . . ? C74 H74 0.9500 . . ? C75 C77 1.510(7) . . ? C76 H76A 0.9800 . . ? C76 H76B 0.9800 . . ? C76 H76C 0.9800 . . ? C77 H77A 0.9800 . . ? C77 H77B 0.9800 . . ? C77 H77C 0.9800 . . ? C83 C84 1.362(8) . . ? C83 C86 1.512(8) . . ? C84 C85 1.393(7) . . ? C84 H84 0.9500 . . ? C85 C87 1.498(8) . . ? C86 H86A 0.9800 . . ? C86 H86B 0.9800 . . ? C86 H86C 0.9800 . . ? C87 H87A 0.9800 . . ? C87 H87B 0.9800 . . ? C87 H87C 0.9800 . . ? C911 C917 1.323(16) . . ? C911 C912 1.3900 . . ? C911 C916 1.3900 . . ? C912 C913 1.3900 . . ? C912 H912 0.9500 . . ? C913 C914 1.3900 . . ? C913 H913 0.9500 . . ? C914 C915 1.3900 . . ? C914 H914 0.9500 . . ? C915 C916 1.3900 . . ? C915 H915 0.9500 . . ? C916 H916 0.9500 . . ? C917 H91A 0.9800 . . ? C917 H91B 0.9800 . . ? C917 H91C 0.9800 . . ? C921 C925 1.21(2) . . ? C921 C922 1.344(18) . . ? C921 C927 1.440(17) . . ? C921 C921 1.47(3) . 2_766 ? C921 C922 1.490(17) . 2_766 ? C921 C923 1.51(3) . . ? C922 C923 1.352(19) . 2_766 ? C922 C925 1.37(2) . . ? C922 C921 1.490(17) . 2_766 ? C923 C922 1.352(19) . 2_766 ? C923 C927 1.50(2) . . ? C925 C927 1.39(2) . . ? B1 H1 1.10(6) . . ? B2 H2 1.05(5) . . ? 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N11 U1 N61 152.43(14) . . . ? N11 U1 N21 77.09(13) . . . ? N61 U1 N21 85.78(13) . . . ? N11 U1 N71 78.88(13) . . . ? N61 U1 N71 75.15(13) . . . ? N21 U1 N71 70.92(13) . . . ? N11 U1 N81 102.40(13) . . . ? N61 U1 N81 76.99(13) . . . ? N21 U1 N81 139.61(13) . . . ? N71 U1 N81 69.45(13) . . . ? N11 U1 N31 87.10(12) . . . ? N61 U1 N31 105.63(13) . . . ? N21 U1 N31 66.06(13) . . . ? N71 U1 N31 136.72(13) . . . ? N81 U1 N31 153.80(13) . . . ? N11 U1 S42 130.59(10) . . . ? N61 U1 S42 76.22(10) . . . ? N21 U1 S42 137.15(9) . . . ? N71 U1 S42 137.19(10) . . . ? N81 U1 S42 73.56(9) . . . ? N31 U1 S42 81.69(9) . . . ? N11 U1 S41 70.68(10) . . . ? N61 U1 S41 136.41(10) . . . ? N21 U1 S41 126.19(9) . . . ? N71 U1 S41 138.27(10) . . . ? N81 U1 S41 89.65(9) . . . ? N31 U1 S41 70.31(9) . . . ? S42 U1 S41 60.19(3) . . . ? C40 S41 U1 86.50(18) . . . ? C40 S42 U1 87.22(19) . . . ? C40 S43 C41 104.7(2) . . . ? C15 N11 N12 106.6(4) . . . ? C15 N11 U1 134.0(3) . . . ? N12 N11 U1 119.5(3) . . . ? C13 N12 N11 109.4(4) . . . ? C13 N12 B1 130.0(4) . . . ? N11 N12 B1 120.5(4) . . . ? C25 N21 N22 105.7(4) . . . ? C25 N21 U1 136.8(3) . . . ? N22 N21 U1 117.1(3) . . . ? C23 N22 N21 110.2(4) . . . ? C23 N22 B1 127.9(4) . . . ? N21 N22 B1 121.9(4) . . . ? C35 N31 N32 105.1(4) . . . ? C35 N31 U1 134.4(3) . . . ? N32 N31 U1 101.2(3) . . . ? C33 N32 N31 110.2(4) . . . ? C33 N32 B1 123.9(4) . . . ? N31 N32 B1 124.5(4) . . . ? C65 N61 N62 106.3(4) . . . ? C65 N61 U1 130.0(3) . . . ? N62 N61 U1 123.4(3) . . . ? C63 N62 N61 109.7(4) . . . ? C63 N62 B2 128.3(4) . . . ? N61 N62 B2 122.0(4) . . . ? C75 N71 N72 105.5(4) . . . ? C75 N71 U1 135.0(3) . . . ? N72 N71 U1 118.6(3) . . . ? C73 N72 N71 110.3(4) . . . ? C73 N72 B2 125.3(4) . . . ? N71 N72 B2 124.2(4) . . . ? C85 N81 N82 105.2(4) . . . ? C85 N81 U1 135.3(3) . . . ? N82 N81 U1 116.7(3) . . . ? C83 N82 N81 109.8(5) . . . ? C83 N82 B2 126.4(5) . . . ? N81 N82 B2 123.8(4) . . . ? N12 C13 C14 108.0(5) . . . ? N12 C13 C16 123.7(5) . . . ? C14 C13 C16 128.3(5) . . . ? C13 C14 C15 105.7(4) . . . ? C13 C14 H14 127.10 . . . ? C15 C14 H14 127.10 . . . ? N11 C15 C14 110.2(5) . . . ? N11 C15 C17 120.6(4) . . . ? C14 C15 C17 129.2(5) . . . ? C13 C16 H16A 109.50 . . . ? C13 C16 H16B 109.50 . . . ? H16A C16 H16B 109.50 . . . ? C13 C16 H16C 109.50 . . . ? H16A C16 H16C 109.50 . . . ? H16B C16 H16C 109.50 . . . ? C15 C17 H17A 109.50 . . . ? C15 C17 H17B 109.50 . . . ? H17A C17 H17B 109.50 . . . ? C15 C17 H17C 109.50 . . . ? H17A C17 H17C 109.50 . . . ? H17B C17 H17C 109.50 . . . ? N22 C23 C24 107.7(5) . . . ? N22 C23 C26 123.6(5) . . . ? C24 C23 C26 128.7(5) . . . ? C23 C24 C25 106.1(5) . . . ? C23 C24 H24 127.00 . . . ? C25 C24 H24 127.00 . . . ? N21 C25 C24 110.3(5) . . . ? N21 C25 C27 123.4(5) . . . ? C24 C25 C27 126.3(5) . . . ? C23 C26 H26A 109.50 . . . ? C23 C26 H26B 109.50 . . . ? H26A C26 H26B 109.50 . . . ? C23 C26 H26C 109.50 . . . ? H26A C26 H26C 109.50 . . . ? H26B C26 H26C 109.50 . . . ? C25 C27 H27A 109.50 . . . ? C25 C27 H27B 109.50 . . . ? H27A C27 H27B 109.50 . . . ? C25 C27 H27C 109.50 . . . ? H27A C27 H27C 109.50 . . . ? H27B C27 H27C 109.50 . . . ? N32 C33 C34 108.1(5) . . . ? N32 C33 C36 122.7(5) . . . ? C34 C33 C36 129.1(5) . . . ? C33 C34 C35 105.3(5) . . . ? C33 C34 H34 127.40 . . . ? C35 C34 H34 127.40 . . . ? N31 C35 C34 111.2(5) . . . ? N31 C35 C37 123.9(5) . . . ? C34 C35 C37 124.8(5) . . . ? C33 C36 H36A 109.50 . . . ? C33 C36 H36B 109.50 . . . ? H36A C36 H36B 109.50 . . . ? C33 C36 H36C 109.50 . . . ? H36A C36 H36C 109.50 . . . ? H36B C36 H36C 109.50 . . . ? C35 C37 H37A 109.50 . . . ? C35 C37 H37B 109.50 . . . ? H37A C37 H37B 109.50 . . . ? C35 C37 H37C 109.50 . . . ? H37A C37 H37C 109.50 . . . ? H37B C37 H37C 109.50 . . . ? S42 C40 S41 123.9(3) . . . ? S42 C40 S43 123.3(3) . . . ? S41 C40 S43 112.8(3) . . . ? C42 C41 C46 121.0(6) . . . ? C42 C41 S43 120.1(5) . . . ? C46 C41 S43 118.8(5) . . . ? C41 C42 C43 119.8(7) . . . ? C41 C42 H42 120.10 . . . ? C43 C42 H42 120.10 . . . ? C44 C43 C42 120.3(8) . . . ? C44 C43 H43 119.90 . . . ? C42 C43 H43 119.90 . . . ? C43 C44 C45 120.3(7) . . . ? C43 C44 H44 119.90 . . . ? C45 C44 H44 119.90 . . . ? C46 C45 C44 119.6(7) . . . ? C46 C45 H45 120.20 . . . ? C44 C45 H45 120.20 . . . ? C45 C46 C41 119.1(7) . . . ? C45 C46 H46 120.50 . . . ? C41 C46 H46 120.50 . . . ? C64 C63 N62 107.5(5) . . . ? C64 C63 C66 129.6(5) . . . ? N62 C63 C66 122.9(5) . . . ? C63 C64 C65 106.9(5) . . . ? C63 C64 H64 126.60 . . . ? C65 C64 H64 126.60 . . . ? N61 C65 C64 109.6(5) . . . ? N61 C65 C67 121.1(5) . . . ? C64 C65 C67 129.2(5) . . . ? C63 C66 H66A 109.50 . . . ? C63 C66 H66B 109.50 . . . ? H66A C66 H66B 109.50 . . . ? C63 C66 H66C 109.50 . . . ? H66A C66 H66C 109.50 . . . ? H66B C66 H66C 109.50 . . . ? C65 C67 H67A 109.50 . . . ? C65 C67 H67B 109.50 . . . ? H67A C67 H67B 109.50 . . . ? C65 C67 H67C 109.50 . . . ? H67A C67 H67C 109.50 . . . ? H67B C67 H67C 109.50 . . . ? N72 C73 C74 107.7(5) . . . ? N72 C73 C76 124.1(5) . . . ? C74 C73 C76 128.1(5) . . . ? C73 C74 C75 106.0(5) . . . ? C73 C74 H74 127.00 . . . ? C75 C74 H74 127.00 . . . ? N71 C75 C74 110.5(5) . . . ? N71 C75 C77 124.9(5) . . . ? C74 C75 C77 124.5(5) . . . ? C73 C76 H76A 109.50 . . . ? C73 C76 H76B 109.50 . . . ? H76A C76 H76B 109.50 . . . ? C73 C76 H76C 109.50 . . . ? H76A C76 H76C 109.50 . . . ? H76B C76 H76C 109.50 . . . ? C75 C77 H77A 109.50 . . . ? C75 C77 H77B 109.50 . . . ? H77A C77 H77B 109.50 . . . ? C75 C77 H77C 109.50 . . . ? H77A C77 H77C 109.50 . . . ? H77B C77 H77C 109.50 . . . ? N82 C83 C84 108.5(5) . . . ? N82 C83 C86 123.1(5) . . . ? C84 C83 C86 128.4(5) . . . ? C83 C84 C85 105.8(5) . . . ? C83 C84 H84 127.10 . . . ? C85 C84 H84 127.10 . . . ? N81 C85 C84 110.7(5) . . . ? N81 C85 C87 123.5(5) . . . ? C84 C85 C87 125.8(5) . . . ? C83 C86 H86A 109.50 . . . ? C83 C86 H86B 109.50 . . . ? H86A C86 H86B 109.50 . . . ? C83 C86 H86C 109.50 . . . ? H86A C86 H86C 109.50 . . . ? H86B C86 H86C 109.50 . . . ? C85 C87 H87A 109.50 . . . ? C85 C87 H87B 109.50 . . . ? H87A C87 H87B 109.50 . . . ? C85 C87 H87C 109.50 . . . ? H87A C87 H87C 109.50 . . . ? H87B C87 H87C 109.50 . . . ? C917 C911 C912 130.0(12) . . . ? C917 C911 C916 110.0(12) . . . ? C912 C911 C916 120.00 . . . ? C913 C912 C911 120.00 . . . ? C913 C912 H912 120.00 . . . ? C911 C912 H912 120.00 . . . ? C912 C913 C914 120.00 . . . ? C912 C913 H913 120.00 . . . ? C914 C913 H913 120.00 . . . ? C915 C914 C913 120.00 . . . ? C915 C914 H914 120.00 . . . ? C913 C914 H914 120.00 . . . ? C914 C915 C916 120.00 . . . ? C914 C915 H915 120.00 . . . ? C916 C915 H915 120.00 . . . ? C915 C916 C911 120.00 . . . ? C915 C916 H916 120.00 . . . ? C911 C916 H916 120.00 . . . ? C911 C917 H91A 109.50 . . . ? C911 C917 H91B 109.50 . . . ? H91A C917 H91B 109.50 . . . ? C911 C917 H91C 109.50 . . . ? H91A C917 H91C 109.50 . . . ? H91B C917 H91C 109.50 . . . ? C925 C921 C922 64.5(14) . . . ? C925 C921 C927 62.6(13) . . . ? C922 C921 C927 127.1(13) . . . ? C925 C921 C921 128(2) . . 2_766 ? C922 C921 C921 63.8(12) . . 2_766 ? C927 C921 C921 169(2) . . 2_766 ? C925 C921 C922 174.6(14) . . 2_766 ? C922 C921 C922 117.9(11) . . 2_766 ? C927 C921 C922 115.0(13) . . 2_766 ? C921 C921 C922 54.1(10) 2_766 . 2_766 ? C925 C921 C923 123.6(17) . . . ? C922 C921 C923 170.5(14) . . . ? C927 C921 C923 61.3(10) . . . ? C921 C921 C923 107.6(17) 2_766 . . ? C922 C921 C923 53.7(10) 2_766 . . ? C921 C922 C923 125.7(13) . . 2_766 ? C921 C922 C925 53.0(11) . . . ? C923 C922 C925 178.7(15) 2_766 . . ? C921 C922 C921 62.2(11) . . 2_766 ? C923 C922 C921 63.8(11) 2_766 . 2_766 ? C925 C922 C921 115.0(13) . . 2_766 ? C922 C923 C927 119.7(15) 2_766 . . ? C922 C923 C921 62.6(10) 2_766 . . ? C927 C923 C921 57.2(10) . . . ? C921 C925 C922 62.5(12) . . . ? C921 C925 C927 66.8(14) . . . ? C922 C925 C927 129.3(15) . . . ? C925 C927 C921 50.6(10) . . . ? C925 C927 C923 111.7(12) . . . ? C921 C927 C923 61.5(10) . . . ? N22 B1 N32 110.9(4) . . . ? N22 B1 N12 111.1(4) . . . ? N32 B1 N12 111.0(4) . . . ? N22 B1 H1 112(3) . . . ? N32 B1 H1 106(3) . . . ? N12 B1 H1 106(3) . . . ? N82 B2 N62 111.3(5) . . . ? N82 B2 N72 111.2(4) . . . ? N62 B2 N72 110.2(4) . . . ? N82 B2 H2 112(3) . . . ? N62 B2 H2 105(3) . . . ? N72 B2 H2 106(3) . . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N11 U1 S41 C40 177.3(2) . . . . ? N61 U1 S41 C40 -8.8(2) . . . . ? N21 U1 S41 C40 120.7(2) . . . . ? N71 U1 S41 C40 -137.1(2) . . . . ? N81 U1 S41 C40 -79.37(19) . . . . ? N31 U1 S41 C40 83.4(2) . . . . ? S42 U1 S41 C40 -8.19(17) . . . . ? N11 U1 S42 C40 15.2(2) . . . . ? N61 U1 S42 C40 -172.2(2) . . . . ? N21 U1 S42 C40 -104.2(2) . . . . ? N71 U1 S42 C40 138.6(2) . . . . ? N81 U1 S42 C40 107.6(2) . . . . ? N31 U1 S42 C40 -63.73(19) . . . . ? S41 U1 S42 C40 8.28(17) . . . . ? N61 U1 N11 C15 -85.7(6) . . . . ? N21 U1 N11 C15 -138.6(5) . . . . ? N71 U1 N11 C15 -65.9(5) . . . . ? N81 U1 N11 C15 -0.1(5) . . . . ? N31 U1 N11 C15 155.3(5) . . . . ? S42 U1 N11 C15 78.8(5) . . . . ? S41 U1 N11 C15 85.1(5) . . . . ? N61 U1 N11 N12 93.4(4) . . . . ? N21 U1 N11 N12 40.4(3) . . . . ? N71 U1 N11 N12 113.2(3) . . . . ? N81 U1 N11 N12 179.0(3) . . . . ? N31 U1 N11 N12 -25.7(3) . . . . ? S42 U1 N11 N12 -102.2(3) . . . . ? S41 U1 N11 N12 -95.8(3) . . . . ? C15 N11 N12 C13 0.2(5) . . . . ? U1 N11 N12 C13 -179.1(3) . . . . ? C15 N11 N12 B1 179.1(4) . . . . ? U1 N11 N12 B1 -0.2(6) . . . . ? N11 U1 N21 C25 133.5(5) . . . . ? N61 U1 N21 C25 -24.8(5) . . . . ? N71 U1 N21 C25 51.0(5) . . . . ? N81 U1 N21 C25 39.4(6) . . . . ? N31 U1 N21 C25 -133.9(5) . . . . ? S42 U1 N21 C25 -89.2(5) . . . . ? S41 U1 N21 C25 -172.5(4) . . . . ? N11 U1 N21 N22 -38.3(3) . . . . ? N61 U1 N21 N22 163.5(3) . . . . ? N71 U1 N21 N22 -120.8(3) . . . . ? N81 U1 N21 N22 -132.3(3) . . . . ? N31 U1 N21 N22 54.3(3) . . . . ? S42 U1 N21 N22 99.0(3) . . . . ? S41 U1 N21 N22 15.7(4) . . . . ? C25 N21 N22 C23 -0.1(5) . . . . ? U1 N21 N22 C23 174.1(3) . . . . ? C25 N21 N22 B1 -177.7(4) . . . . ? U1 N21 N22 B1 -3.5(5) . . . . ? N11 U1 N31 C35 -122.7(5) . . . . ? N61 U1 N31 C35 82.1(5) . . . . ? N21 U1 N31 C35 160.1(5) . . . . ? N71 U1 N31 C35 166.9(4) . . . . ? N81 U1 N31 C35 -10.1(6) . . . . ? S42 U1 N31 C35 9.0(4) . . . . ? S41 U1 N31 C35 -52.2(4) . . . . ? N11 U1 N31 N32 1.9(3) . . . . ? N61 U1 N31 N32 -153.3(3) . . . . ? N21 U1 N31 N32 -75.3(3) . . . . ? N71 U1 N31 N32 -68.5(3) . . . . ? N81 U1 N31 N32 114.5(3) . . . . ? S42 U1 N31 N32 133.6(3) . . . . ? S41 U1 N31 N32 72.4(3) . . . . ? C35 N31 N32 C33 2.8(6) . . . . ? U1 N31 N32 C33 -139.7(4) . . . . ? C35 N31 N32 B1 -163.9(5) . . . . ? U1 N31 N32 B1 53.7(5) . . . . ? N11 U1 N61 C65 -117.9(5) . . . . ? N21 U1 N61 C65 -66.6(5) . . . . ? N71 U1 N61 C65 -138.0(5) . . . . ? N81 U1 N61 C65 150.2(5) . . . . ? N31 U1 N61 C65 -2.9(5) . . . . ? S42 U1 N61 C65 74.2(5) . . . . ? S41 U1 N61 C65 74.8(5) . . . . ? N11 U1 N61 N62 55.8(5) . . . . ? N21 U1 N61 N62 107.1(4) . . . . ? N71 U1 N61 N62 35.7(4) . . . . ? N81 U1 N61 N62 -36.1(4) . . . . ? N31 U1 N61 N62 170.8(4) . . . . ? S42 U1 N61 N62 -112.1(4) . . . . ? S41 U1 N61 N62 -111.6(4) . . . . ? C65 N61 N62 C63 -0.2(6) . . . . ? U1 N61 N62 C63 -175.1(3) . . . . ? C65 N61 N62 B2 178.3(5) . . . . ? U1 N61 N62 B2 3.4(7) . . . . ? N11 U1 N71 C75 -37.0(5) . . . . ? N61 U1 N71 C75 133.7(6) . . . . ? N21 U1 N71 C75 43.1(5) . . . . ? N81 U1 N71 C75 -144.9(6) . . . . ? N31 U1 N71 C75 36.5(6) . . . . ? S42 U1 N71 C75 -176.8(5) . . . . ? S41 U1 N71 C75 -80.4(6) . . . . ? N11 U1 N71 N72 155.3(4) . . . . ? N61 U1 N71 N72 -34.0(3) . . . . ? N21 U1 N71 N72 -124.6(4) . . . . ? N81 U1 N71 N72 47.4(3) . . . . ? N31 U1 N71 N72 -131.2(3) . . . . ? S42 U1 N71 N72 15.5(4) . . . . ? S41 U1 N71 N72 111.9(3) . . . . ? C75 N71 N72 C73 -0.3(6) . . . . ? U1 N71 N72 C73 170.7(3) . . . . ? C75 N71 N72 B2 -176.3(5) . . . . ? U1 N71 N72 B2 -5.3(6) . . . . ? N11 U1 N81 C85 74.2(5) . . . . ? N61 U1 N81 C85 -134.0(5) . . . . ? N21 U1 N81 C85 158.8(4) . . . . ? N71 U1 N81 C85 147.2(5) . . . . ? N31 U1 N81 C85 -35.0(6) . . . . ? S42 U1 N81 C85 -54.8(5) . . . . ? S41 U1 N81 C85 4.1(5) . . . . ? N11 U1 N81 N82 -128.1(3) . . . . ? N61 U1 N81 N82 23.7(3) . . . . ? N21 U1 N81 N82 -43.5(4) . . . . ? N71 U1 N81 N82 -55.1(3) . . . . ? N31 U1 N81 N82 122.7(4) . . . . ? S42 U1 N81 N82 102.9(3) . . . . ? S41 U1 N81 N82 161.8(3) . . . . ? C85 N81 N82 C83 2.6(6) . . . . ? U1 N81 N82 C83 -161.4(4) . . . . ? C85 N81 N82 B2 -175.2(5) . . . . ? U1 N81 N82 B2 20.8(6) . . . . ? N11 N12 C13 C14 -0.8(6) . . . . ? B1 N12 C13 C14 -179.6(5) . . . . ? N11 N12 C13 C16 178.4(5) . . . . ? B1 N12 C13 C16 -0.5(9) . . . . ? N12 C13 C14 C15 1.0(6) . . . . ? C16 C13 C14 C15 -178.0(6) . . . . ? N12 N11 C15 C14 0.5(6) . . . . ? U1 N11 C15 C14 179.6(4) . . . . ? N12 N11 C15 C17 -179.2(5) . . . . ? U1 N11 C15 C17 -0.1(8) . . . . ? C13 C14 C15 N11 -1.0(6) . . . . ? C13 C14 C15 C17 178.7(6) . . . . ? N21 N22 C23 C24 0.3(6) . . . . ? B1 N22 C23 C24 177.8(5) . . . . ? N21 N22 C23 C26 -178.2(5) . . . . ? B1 N22 C23 C26 -0.8(8) . . . . ? N22 C23 C24 C25 -0.4(6) . . . . ? C26 C23 C24 C25 178.0(5) . . . . ? N22 N21 C25 C24 -0.2(6) . . . . ? U1 N21 C25 C24 -172.6(4) . . . . ? N22 N21 C25 C27 179.0(5) . . . . ? U1 N21 C25 C27 6.6(8) . . . . ? C23 C24 C25 N21 0.4(6) . . . . ? C23 C24 C25 C27 -178.8(5) . . . . ? N31 N32 C33 C34 -2.3(6) . . . . ? B1 N32 C33 C34 164.5(5) . . . . ? N31 N32 C33 C36 178.2(5) . . . . ? B1 N32 C33 C36 -15.1(9) . . . . ? N32 C33 C34 C35 0.9(6) . . . . ? C36 C33 C34 C35 -179.6(6) . . . . ? N32 N31 C35 C34 -2.3(6) . . . . ? U1 N31 C35 C34 121.0(5) . . . . ? N32 N31 C35 C37 174.9(5) . . . . ? U1 N31 C35 C37 -61.9(7) . . . . ? C33 C34 C35 N31 0.9(6) . . . . ? C33 C34 C35 C37 -176.2(5) . . . . ? U1 S42 C40 S41 -15.3(3) . . . . ? U1 S42 C40 S43 163.0(3) . . . . ? U1 S41 C40 S42 15.3(3) . . . . ? U1 S41 C40 S43 -163.2(3) . . . . ? C41 S43 C40 S42 9.6(4) . . . . ? C41 S43 C40 S41 -172.0(3) . . . . ? C40 S43 C41 C42 69.6(6) . . . . ? C40 S43 C41 C46 -113.4(5) . . . . ? C46 C41 C42 C43 1.1(11) . . . . ? S43 C41 C42 C43 178.1(6) . . . . ? C41 C42 C43 C44 -0.2(13) . . . . ? C42 C43 C44 C45 -1.2(13) . . . . ? C43 C44 C45 C46 1.8(12) . . . . ? C44 C45 C46 C41 -0.9(11) . . . . ? C42 C41 C46 C45 -0.6(10) . . . . ? S43 C41 C46 C45 -177.6(5) . . . . ? N61 N62 C63 C64 -0.4(6) . . . . ? B2 N62 C63 C64 -178.8(5) . . . . ? N61 N62 C63 C66 179.5(5) . . . . ? B2 N62 C63 C66 1.1(9) . . . . ? N62 C63 C64 C65 0.9(7) . . . . ? C66 C63 C64 C65 -179.1(6) . . . . ? N62 N61 C65 C64 0.7(6) . . . . ? U1 N61 C65 C64 175.2(4) . . . . ? N62 N61 C65 C67 -177.2(5) . . . . ? U1 N61 C65 C67 -2.7(8) . . . . ? C63 C64 C65 N61 -1.0(7) . . . . ? C63 C64 C65 C67 176.7(6) . . . . ? N71 N72 C73 C74 -0.5(6) . . . . ? B2 N72 C73 C74 175.4(5) . . . . ? N71 N72 C73 C76 176.2(5) . . . . ? B2 N72 C73 C76 -7.9(8) . . . . ? N72 C73 C74 C75 1.1(6) . . . . ? C76 C73 C74 C75 -175.4(6) . . . . ? N72 N71 C75 C74 1.0(6) . . . . ? U1 N71 C75 C74 -167.8(4) . . . . ? N72 N71 C75 C77 -178.9(5) . . . . ? U1 N71 C75 C77 12.2(9) . . . . ? C73 C74 C75 N71 -1.3(7) . . . . ? C73 C74 C75 C77 178.6(5) . . . . ? N81 N82 C83 C84 -2.9(6) . . . . ? B2 N82 C83 C84 174.8(5) . . . . ? N81 N82 C83 C86 176.4(6) . . . . ? B2 N82 C83 C86 -5.9(9) . . . . ? N82 C83 C84 C85 2.1(7) . . . . ? C86 C83 C84 C85 -177.2(6) . . . . ? N82 N81 C85 C84 -1.2(6) . . . . ? U1 N81 C85 C84 158.2(4) . . . . ? N82 N81 C85 C87 -178.4(5) . . . . ? U1 N81 C85 C87 -19.0(8) . . . . ? C83 C84 C85 N81 -0.5(6) . . . . ? C83 C84 C85 C87 176.7(5) . . . . ? C917 C911 C912 C913 -179.7(11) . . . . ? C916 C911 C912 C913 0.0 . . . . ? C911 C912 C913 C914 0.0 . . . . ? C912 C913 C914 C915 0.0 . . . . ? C913 C914 C915 C916 0.0 . . . . ? C914 C915 C916 C911 0.0 . . . . ? C917 C911 C916 C915 179.7(9) . . . . ? C912 C911 C916 C915 0.0 . . . . ? C925 C921 C922 C923 179.7(13) . . . 2_766 ? C927 C921 C922 C923 178.1(11) . . . 2_766 ? C921 C921 C922 C923 -5.7(15) 2_766 . . 2_766 ? C922 C921 C922 C923 -5.7(15) 2_766 . . 2_766 ? C923 C921 C922 C923 -32(8) . . . 2_766 ? C927 C921 C922 C925 -1.6(11) . . . . ? C921 C921 C922 C925 174.6(15) 2_766 . . . ? C922 C921 C922 C925 174.6(15) 2_766 . . . ? C923 C921 C922 C925 149(8) . . . . ? C925 C921 C922 C921 -174.6(15) . . . 2_766 ? C927 C921 C922 C921 -176.2(19) . . . 2_766 ? C922 C921 C922 C921 -0.001(2) 2_766 . . 2_766 ? C923 C921 C922 C921 -26(7) . . . 2_766 ? C925 C921 C923 C922 174.4(16) . . . 2_766 ? C922 C921 C923 C922 29(7) . . . 2_766 ? C927 C921 C923 C922 -178.1(10) . . . 2_766 ? C921 C921 C923 C922 4.4(11) 2_766 . . 2_766 ? C925 C921 C923 C927 -7.4(14) . . . . ? C922 C921 C923 C927 -153(7) . . . . ? C921 C921 C923 C927 -177.5(15) 2_766 . . . ? C922 C921 C923 C927 178.1(10) 2_766 . . . ? C927 C921 C925 C922 178.6(10) . . . . ? C921 C921 C925 C922 -6.2(17) 2_766 . . . ? C922 C921 C925 C922 -117(19) 2_766 . . . ? C923 C921 C925 C922 -174.1(15) . . . . ? C922 C921 C925 C927 -178.6(10) . . . . ? C921 C921 C925 C927 175(2) 2_766 . . . ? C922 C921 C925 C927 65(19) 2_766 . . . ? C923 C921 C925 C927 7.4(13) . . . . ? C923 C922 C925 C921 -10(49) 2_766 . . . ? C921 C922 C925 C921 5.3(14) 2_766 . . . ? C921 C922 C925 C927 1.7(12) . . . . ? C923 C922 C925 C927 -8(50) 2_766 . . . ? C921 C922 C925 C927 7.0(18) 2_766 . . . ? C922 C925 C927 C921 -1.6(12) . . . . ? C921 C925 C927 C923 -6.6(12) . . . . ? C922 C925 C927 C923 -8.2(19) . . . . ? C922 C921 C927 C925 1.6(12) . . . . ? C921 C921 C927 C925 -161(8) 2_766 . . . ? C922 C921 C927 C925 -174.7(14) 2_766 . . . ? C923 C921 C927 C925 -173.0(13) . . . . ? C925 C921 C927 C923 173.0(13) . . . . ? C922 C921 C927 C923 174.6(15) . . . . ? C921 C921 C927 C923 12(8) 2_766 . . . ? C922 C921 C927 C923 -1.6(9) 2_766 . . . ? C922 C923 C927 C925 7.7(16) 2_766 . . . ? C921 C923 C927 C925 5.8(11) . . . . ? C922 C923 C927 C921 1.9(11) 2_766 . . . ? C23 N22 B1 N32 126.8(5) . . . . ? N21 N22 B1 N32 -56.0(6) . . . . ? C23 N22 B1 N12 -109.2(5) . . . . ? N21 N22 B1 N12 68.0(6) . . . . ? C33 N32 B1 N22 -143.5(5) . . . . ? N31 N32 B1 N22 21.4(6) . . . . ? C33 N32 B1 N12 92.6(6) . . . . ? N31 N32 B1 N12 -102.6(5) . . . . ? C13 N12 B1 N22 112.9(6) . . . . ? N11 N12 B1 N22 -65.8(6) . . . . ? C13 N12 B1 N32 -123.3(5) . . . . ? N11 N12 B1 N32 58.0(6) . . . . ? C83 N82 B2 N62 107.7(6) . . . . ? N81 N82 B2 N62 -74.9(6) . . . . ? C83 N82 B2 N72 -128.9(5) . . . . ? N81 N82 B2 N72 48.5(7) . . . . ? C63 N62 B2 N82 -122.2(6) . . . . ? N61 N62 B2 N82 59.6(6) . . . . ? C63 N62 B2 N72 113.9(6) . . . . ? N61 N62 B2 N72 -64.3(6) . . . . ? C73 N72 B2 N82 125.5(5) . . . . ? N71 N72 B2 N82 -59.1(6) . . . . ? C73 N72 B2 N62 -110.5(6) . . . . ? N71 N72 B2 N62 64.9(6) . . . . ? _iucr_refine_instruction_details ; TITL xl in P-1 CELL 1.54178 11.2943 14.3126 17.4998 72.318 74.613 69.986 ZERR 2 0.0005 0.0005 0.0008 0.002 0.003 0.003 LATT 1 SFAC C H B N S U UNIT 74 98 4 24 6 2 OMIT 7 15 2 OMIT -5 6 15 OMIT -4 -3 16 OMIT -12 -2 3 OMIT 1 -1 6 OMIT 11 13 6 OMIT 11 9 7 OMIT -4 -9 13 L.S. 5 PLAN -20 SIZE 0.06 0.12 0.2 TEMP -123.3 BOND $H CONF FMAP 2 ACTA WGHT 0.072000 5.274200 FVAR 0.31529 U1 6 0.214910 0.180990 0.203413 11.00000 0.03153 0.02427 = 0.02677 -0.00101 -0.00821 -0.01002 S41 5 0.024130 0.211103 0.102682 11.00000 0.03836 0.02935 = 0.03576 -0.00159 -0.01304 -0.00882 S42 5 0.087674 0.020253 0.232174 11.00000 0.04575 0.03104 = 0.03417 -0.00056 -0.01304 -0.01541 S43 5 -0.038651 0.036376 0.095057 11.00000 0.05648 0.03354 = 0.04735 -0.00690 -0.02506 -0.01199 N11 4 0.175000 0.361094 0.110857 11.00000 0.03238 0.02540 = 0.03420 -0.00406 -0.00858 -0.00954 N12 4 0.256521 0.379229 0.037679 11.00000 0.04298 0.02818 = 0.02863 -0.00158 -0.01155 -0.01436 N21 4 0.444338 0.201549 0.149046 11.00000 0.03700 0.02733 = 0.03040 0.00203 -0.00952 -0.01439 N22 4 0.471202 0.253017 0.068305 11.00000 0.03098 0.03006 = 0.03199 -0.00595 -0.00364 -0.01377 N31 4 0.336148 0.110904 0.066810 11.00000 0.03457 0.02734 = 0.03632 -0.00628 -0.00874 -0.01047 N32 4 0.327546 0.201735 0.007790 11.00000 0.03339 0.03130 = 0.03172 -0.00158 -0.00732 -0.01187 N61 4 0.310688 0.041286 0.321797 11.00000 0.03735 0.03199 = 0.03197 -0.00168 -0.01144 -0.00899 N62 4 0.287207 0.053904 0.399014 11.00000 0.03594 0.03453 = 0.03025 0.00082 -0.01265 -0.01181 N71 4 0.260143 0.282952 0.293007 11.00000 0.03576 0.03855 = 0.02837 -0.00503 -0.00528 -0.01420 N72 4 0.245739 0.245345 0.376729 11.00000 0.03562 0.03413 = 0.03123 -0.00549 -0.00687 -0.01090 N81 4 0.023288 0.205981 0.333238 11.00000 0.03548 0.03809 = 0.03408 -0.00354 -0.00891 -0.02134 N82 4 0.058272 0.170692 0.409650 11.00000 0.03983 0.03781 = 0.03014 -0.00206 -0.00583 -0.01257 C13 1 0.218588 0.479595 -0.000615 11.00000 0.04883 0.02514 = 0.03260 0.00081 -0.01503 -0.01230 C14 1 0.110051 0.526863 0.047922 11.00000 0.04903 0.02609 = 0.04432 0.00000 -0.01948 -0.00887 AFIX 43 H14 2 0.061344 0.596714 0.036564 11.00000 -1.20000 AFIX 0 C15 1 0.086955 0.450973 0.116809 11.00000 0.03745 0.02249 = 0.04091 -0.00212 -0.01318 -0.00742 C16 1 0.287601 0.526125 -0.080472 11.00000 0.06327 0.03395 = 0.03760 -0.00071 -0.00824 -0.01581 AFIX 137 H16A 2 0.372368 0.523834 -0.074314 11.00000 -1.50000 H16B 2 0.238531 0.597399 -0.099006 11.00000 -1.50000 H16C 2 0.297338 0.487773 -0.120669 11.00000 -1.50000 AFIX 0 C17 1 -0.016389 0.458762 0.190405 11.00000 0.04118 0.03422 = 0.05552 -0.00978 -0.00090 -0.00951 AFIX 137 H17A 2 -0.097405 0.463479 0.176904 11.00000 -1.50000 H17B 2 -0.025721 0.519975 0.208182 11.00000 -1.50000 H17C 2 0.006199 0.397942 0.234385 11.00000 -1.50000 AFIX 0 C23 1 0.588163 0.266077 0.051478 11.00000 0.03795 0.03316 = 0.04160 -0.01059 -0.00433 -0.01269 C24 1 0.640011 0.222614 0.121290 11.00000 0.03225 0.03809 = 0.04601 -0.00694 -0.00949 -0.01341 AFIX 43 H24 2 0.722153 0.219630 0.127882 11.00000 -1.20000 AFIX 0 C25 1 0.547752 0.183892 0.180319 11.00000 0.03471 0.03156 = 0.03954 -0.00202 -0.00999 -0.01436 C26 1 0.644695 0.321597 -0.029972 11.00000 0.04142 0.05174 = 0.03890 -0.00747 0.00004 -0.02294 AFIX 137 H26A 2 0.651841 0.286234 -0.071673 11.00000 -1.50000 H26B 2 0.729926 0.323086 -0.027999 11.00000 -1.50000 H26C 2 0.589276 0.391770 -0.043493 11.00000 -1.50000 AFIX 0 C27 1 0.558511 0.130825 0.267499 11.00000 0.04048 0.05309 = 0.04091 0.00327 -0.01657 -0.01423 AFIX 137 H27A 2 0.485828 0.166013 0.303534 11.00000 -1.50000 H27B 2 0.638636 0.132054 0.278413 11.00000 -1.50000 H27C 2 0.558096 0.059741 0.277502 11.00000 -1.50000 AFIX 0 C33 1 0.301413 0.192688 -0.060190 11.00000 0.04576 0.03720 = 0.03389 -0.00830 -0.01239 -0.00980 C34 1 0.297464 0.094018 -0.047660 11.00000 0.03588 0.03965 = 0.04274 -0.01521 -0.00635 -0.01324 AFIX 43 H34 2 0.282228 0.064851 -0.084899 11.00000 -1.20000 AFIX 0 C35 1 0.320579 0.046042 0.031292 11.00000 0.03216 0.03175 = 0.03808 -0.01053 -0.00453 -0.00988 C36 1 0.282584 0.279151 -0.133839 11.00000 0.07529 0.04296 = 0.04213 -0.00049 -0.02682 -0.01868 AFIX 137 H36A 2 0.217361 0.339066 -0.117840 11.00000 -1.50000 H36B 2 0.254488 0.259021 -0.173303 11.00000 -1.50000 H36C 2 0.363557 0.296055 -0.158661 11.00000 -1.50000 AFIX 0 C37 1 0.333305 -0.065578 0.070863 11.00000 0.04743 0.02863 = 0.04821 -0.01082 -0.00669 -0.01125 AFIX 137 H37A 2 0.420408 -0.100078 0.082003 11.00000 -1.50000 H37B 2 0.316134 -0.097321 0.034155 11.00000 -1.50000 H37C 2 0.271642 -0.071840 0.122135 11.00000 -1.50000 AFIX 0 C40 1 0.026309 0.087568 0.147691 11.00000 0.02720 0.03098 = 0.03743 -0.00678 -0.00548 -0.01154 C41 1 -0.047249 -0.084813 0.159957 11.00000 0.04249 0.04206 = 0.04360 -0.01102 -0.01469 -0.01693 C42 1 -0.132913 -0.090313 0.231753 11.00000 0.07527 0.06854 = 0.06519 -0.02906 0.00381 -0.03321 AFIX 43 H42 2 -0.186304 -0.029484 0.248003 11.00000 -1.20000 AFIX 0 C43 1 -0.141547 -0.184277 0.280416 11.00000 0.11620 0.10788 = 0.05055 -0.01608 0.00263 -0.08067 AFIX 43 H43 2 -0.200824 -0.188243 0.330436 11.00000 -1.20000 AFIX 0 C44 1 -0.065175 -0.271946 0.257078 11.00000 0.10360 0.06511 = 0.06599 0.01734 -0.03550 -0.05980 AFIX 43 H44 2 -0.070416 -0.336627 0.291434 11.00000 -1.20000 AFIX 0 C45 1 0.020341 -0.266800 0.183083 11.00000 0.07558 0.04364 = 0.08087 -0.00098 -0.02856 -0.02365 AFIX 43 H45 2 0.071653 -0.327707 0.166226 11.00000 -1.20000 AFIX 0 C46 1 0.030074 -0.172852 0.134479 11.00000 0.05510 0.03798 = 0.05810 -0.00732 -0.01423 -0.01831 AFIX 43 H46 2 0.088842 -0.168365 0.084253 11.00000 -1.20000 AFIX 0 C63 1 0.358987 -0.029639 0.445892 11.00000 0.04090 0.03793 = 0.04007 0.00711 -0.01801 -0.01873 C64 1 0.427896 -0.096147 0.398051 11.00000 0.04191 0.03372 = 0.04545 0.00242 -0.01922 -0.00892 AFIX 43 H64 2 0.485778 -0.161542 0.414313 11.00000 -1.20000 AFIX 0 C65 1 0.397771 -0.050588 0.321339 11.00000 0.03917 0.03171 = 0.04361 -0.00198 -0.01511 -0.00764 C66 1 0.356053 -0.039379 0.534308 11.00000 0.05065 0.04584 = 0.03515 0.00350 -0.01946 -0.01410 AFIX 137 H66A 2 0.383112 0.016228 0.539511 11.00000 -1.50000 H66B 2 0.414359 -0.105305 0.556274 11.00000 -1.50000 H66C 2 0.268778 -0.035412 0.564783 11.00000 -1.50000 AFIX 0 C67 1 0.451174 -0.088179 0.244327 11.00000 0.05914 0.04182 = 0.04635 -0.00842 -0.01618 -0.00262 AFIX 137 H67A 2 0.405052 -0.134324 0.242916 11.00000 -1.50000 H67B 2 0.542320 -0.124959 0.242744 11.00000 -1.50000 H67C 2 0.440990 -0.029777 0.197079 11.00000 -1.50000 AFIX 0 C73 1 0.290958 0.297100 0.410344 11.00000 0.04732 0.03353 = 0.03746 -0.01053 -0.01480 -0.00916 C74 1 0.336703 0.368933 0.348068 11.00000 0.05411 0.04030 = 0.03982 -0.01095 -0.01314 -0.02080 AFIX 43 H74 2 0.375501 0.415796 0.352768 11.00000 -1.20000 AFIX 0 C75 1 0.314432 0.358852 0.276574 11.00000 0.04040 0.03191 = 0.03796 -0.00625 -0.00872 -0.01191 C76 1 0.282805 0.280127 0.499605 11.00000 0.06212 0.05179 = 0.03842 -0.01088 -0.01869 -0.01763 AFIX 137 H76A 2 0.193173 0.289772 0.526965 11.00000 -1.50000 H76B 2 0.316593 0.329131 0.509547 11.00000 -1.50000 H76C 2 0.333283 0.210305 0.521066 11.00000 -1.50000 AFIX 0 C77 1 0.346851 0.424316 0.192690 11.00000 0.05809 0.03471 = 0.03795 -0.00049 -0.01021 -0.02321 AFIX 137 H77A 2 0.379817 0.381803 0.152828 11.00000 -1.50000 H77B 2 0.412132 0.455173 0.192589 11.00000 -1.50000 H77C 2 0.269640 0.478450 0.178220 11.00000 -1.50000 AFIX 0 C83 1 -0.044545 0.159239 0.467681 11.00000 0.04546 0.04401 = 0.03561 -0.00284 -0.00259 -0.01804 C84 1 -0.148801 0.191192 0.431224 11.00000 0.03478 0.04403 = 0.04156 -0.00738 0.00085 -0.01621 AFIX 43 H84 2 -0.234777 0.193852 0.457272 11.00000 -1.20000 AFIX 0 C85 1 -0.103317 0.219171 0.347841 11.00000 0.03327 0.03789 = 0.04057 -0.00553 -0.00712 -0.01809 C86 1 -0.037457 0.116237 0.557212 11.00000 0.04811 0.08593 = 0.03207 0.00609 0.00057 -0.02651 AFIX 137 H86A 2 0.027133 0.049438 0.564503 11.00000 -1.50000 H86B 2 -0.121119 0.108337 0.587832 11.00000 -1.50000 H86C 2 -0.013791 0.163070 0.577320 11.00000 -1.50000 AFIX 0 C87 1 -0.181283 0.254370 0.281900 11.00000 0.04148 0.06018 = 0.04460 -0.00980 -0.01063 -0.02038 AFIX 137 H87A 2 -0.144114 0.300346 0.235034 11.00000 -1.50000 H87B 2 -0.269422 0.290788 0.302417 11.00000 -1.50000 H87C 2 -0.181328 0.195008 0.265101 11.00000 -1.50000 AFIX 66 C911 1 0.605548 0.354451 0.683072 11.00000 0.50571 0.21602 = 0.07243 -0.02838 0.02668 -0.29525 C912 1 0.617173 0.332701 0.608771 11.00000 0.27839 0.12009 = 0.05689 -0.01663 -0.02388 -0.13121 AFIX 43 H912 2 0.693279 0.286367 0.587889 11.00000 -1.20000 AFIX 65 C913 1 0.517446 0.378743 0.565024 11.00000 0.14760 0.11937 = 0.18506 -0.07027 -0.02389 -0.00404 AFIX 43 H913 2 0.525392 0.363878 0.514243 11.00000 -1.20000 AFIX 65 C914 1 0.406091 0.446537 0.595578 11.00000 0.19635 0.12471 = 0.42363 -0.02411 -0.19163 -0.04629 AFIX 43 H914 2 0.337932 0.478005 0.565678 11.00000 -1.20000 AFIX 65 C915 1 0.394464 0.468288 0.669878 11.00000 0.21213 0.18619 = 0.20907 -0.08419 0.01173 -0.11533 AFIX 43 H915 2 0.318358 0.514622 0.690759 11.00000 -1.20000 AFIX 65 C916 1 0.494191 0.422246 0.713626 11.00000 0.16529 0.15139 = 0.15950 -0.08798 0.09316 -0.12379 AFIX 43 H916 2 0.486244 0.437112 0.764407 11.00000 -1.20000 AFIX 0 C917 1 0.687546 0.320151 0.733926 11.00000 0.28376 0.18319 = 0.08035 0.02796 -0.07696 -0.17990 AFIX 137 H91A 2 0.767311 0.275069 0.710688 11.00000 -1.50000 H91B 2 0.650440 0.281914 0.786156 11.00000 -1.50000 H91C 2 0.705608 0.378072 0.742593 11.00000 -1.50000 AFIX 0 C921 1 0.988349 0.481547 0.468615 10.50000 0.04809 0.05005 = 0.06271 -0.01247 -0.01583 0.00009 C922 1 1.069220 0.539802 0.443082 11.00000 0.06247 0.05549 = 0.07092 -0.01256 -0.01819 0.00165 C923 1 0.904361 0.411886 0.510740 10.50000 0.06544 0.05207 = 0.10159 -0.02520 -0.03282 0.00613 C925 1 1.040253 0.490434 0.397834 10.50000 0.06821 0.06630 = 0.06829 -0.01764 -0.02432 0.01545 C927 1 0.955391 0.431467 0.420582 11.00000 0.06987 0.07280 = 0.11662 -0.03915 -0.03000 -0.00077 B1 3 0.372539 0.291130 0.011233 11.00000 0.03626 0.02913 = 0.02971 -0.00434 -0.00772 -0.00854 B2 3 0.194029 0.152421 0.423600 11.00000 0.03970 0.04058 = 0.02776 -0.00257 -0.00632 -0.01062 H2 2 0.196763 0.141916 0.485052 11.00000 0.02882 H1 2 0.413657 0.323231 -0.052086 11.00000 0.04825 HKLF 4 REM xl in P-1 REM R1 = 0.0387 for 8593 Fo > 4sig(Fo) and 0.0394 for all 8812 data REM 613 parameters refined using 0 restraints END WGHT 0.0721 5.2727 REM Highest difference peak 1.902, deepest hole -1.627, 1-sigma level 0.135 Q1 1 0.2962 0.1874 0.2025 11.00000 0.05 1.90 Q2 1 0.1396 0.1723 0.2023 11.00000 0.05 1.83 Q3 1 0.2229 0.2376 0.2127 11.00000 0.05 1.69 Q4 1 0.2811 0.1316 0.2145 11.00000 0.05 1.63 Q5 1 0.2098 0.1279 0.1960 11.00000 0.05 1.58 Q6 1 0.7374 0.2800 0.6777 11.00000 0.05 1.41 Q7 1 0.1491 0.2296 0.1886 11.00000 0.05 1.41 Q8 1 0.1605 0.1710 0.2548 11.00000 0.05 1.20 Q9 1 0.2714 0.1904 0.1535 11.00000 0.05 1.17 Q10 1 0.0338 0.0655 0.2008 11.00000 0.05 0.94 Q11 1 0.4790 0.4051 0.6598 11.00000 0.05 0.82 Q12 1 0.0601 0.2224 0.1426 11.00000 0.05 0.73 Q13 1 0.5758 0.3474 0.6127 11.00000 0.05 0.69 Q14 1 0.3990 0.1516 0.1550 11.00000 0.05 0.69 Q15 1 0.3629 0.4807 0.6499 11.00000 0.05 0.66 Q16 1 0.0378 0.2050 0.2618 11.00000 0.05 0.58 Q17 1 0.5447 0.4037 0.7296 11.00000 0.05 0.57 Q18 1 0.0464 0.1564 0.1102 11.00000 0.05 0.55 Q19 1 0.3811 0.2301 0.0060 11.00000 0.05 0.53 Q20 1 0.1247 0.0768 0.2239 11.00000 0.05 0.52 ;