#============================================================================== # 1. SUBMISSION DETAILS #============================================================================== _publ_contact_author_name 'Richard H. Holm' _publ_contact_author_address ; Department of Chemistry and Chemical Biology Harvard University 12 Oxford Street Cambridge, MA 02138 USA ; _publ_contact_author_phone '617 495-0853' _publ_contact_author_fax '617 496-9289' _publ_contact_author_email holm@chemistry.harvard.edu _publ_requested_journal 'J. Am. Chem. Soc.' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as New Structures included in a paper submitted to J. Am. Chem. Soc. ; #============================================================================== # 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 ; Synthesis of Structural Analogues of the Oxidized Sites in the Xanthine Oxidoreductase Enzyme Family ; # 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 _publ_author_address 'Wang, Jun-Jieh' ; Department of Chemistry and Chemical Biology Harvard University 12 Oxford Street Cambridge, MA 02138 USA 'Groysman, Stanislav' ; Department of Chemistry and Chemical Biology Harvard University 12 Oxford Street Cambridge, MA 02138 USA ; 'Lee, Sonny C.' ; ?Department of Chemistry ?University of Waterloo ?Ontario, Canada N2L3G1 ; 'Holm, R.H.' ; Department of Chemistry and Chemical Biology Harvard University 12 Oxford Street Cambridge, MA 02138 USA ; #============================================================================== # 4. TEXT #============================================================================== _publ_section_abstract ; See Text ; _publ_section_comment ; See Text ; _publ_section_exptl_prep ; See text ; _publ_section_exptl_refinement ; The structure was solved by direct method with ShelxS-97. All non-H atoms were refined by full-matrix least-squares with anisotropic displacement parameters while hydrogen atoms were placed in idealized positions. ; _publ_section_references ; Bruker (2003). SAINT. Version 7.06A. Bruker AXS Inc., Madison, WI, USA. Bruker (2001a). SMART. Version 5.625. Bruker AXS Inc., Madison, WI, USA. Bruker (2001b). XPREP. Version 6.12. Bruker AXS Inc., Madison, WI, USA. Bruker (2000). SHELXTL. Version 6.10. Bruker AXS Inc., Madison, WI, USA. Farrugia, L. J. (1999). WINGX, J. App. Cryst. 32, 837-838. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Flack, H. D. and Schwarzenbach, D. (1988). Acta Cryst. A44, 499-506. Cooper, R. I., Gould, R. O., Parsons, S. & Watkin, D. J. (2002). J. Appl. Cryst. 35, 168-174. Sheldrick, G. M. (1997). SHELXS97 and SHELXL97. University of Gottingen, Germany. Sheldrick, G. M. (2002). SADABS. Version 2.05. Bruker AXS Inc., Madison, WI, USA. Spek, A. L. (1990). Acta Cryst. A46, C-34. Spek, A. L. (2005). PLATON, A Multipurpose Crystallographic Tool. University of Utrecht, Utrecht, The Netherlands. ; _publ_section_figure_captions ; See text ; _publ_section_table_legends ; See text ; _publ_section_acknowledgements ; See text ; data_jjw128 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H44 N2 O2 S3 W' _chemical_formula_weight 648.62 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' 0.0000 0.0000 '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 0.0060 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.430(2) _cell_length_b 15.430(3) _cell_length_c 24.460(5) _cell_angle_alpha 105.81(3) _cell_angle_beta 102.96(3) _cell_angle_gamma 90.01(3) _cell_volume 4036.3(14) _cell_formula_units_Z 6 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'blocks' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 4.546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3425 _exptl_absorpt_correction_T_max 0.5488 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23382 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14087 _reflns_number_gt 11605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material 'SHELXTL (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0092P)^2^+75.7960P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14087 _refine_ls_number_parameters 865 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1610 _refine_ls_wR_factor_gt 0.1548 _refine_ls_goodness_of_fit_ref 1.165 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max 0.020 _refine_ls_shift/su_mean 0.001 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 W1 W -0.12346(4) 0.09467(3) 0.82447(2) 0.02867(13) Uani 1 1 d . . . W2 W 0.44823(4) 0.59448(3) 0.82496(2) 0.03157(14) Uani 1 1 d . . . W3A W 0.83473(6) 0.22547(5) 0.51602(3) 0.03565(18) Uani 0.75 1 d PD A 1 W3B W 0.8156(2) 0.27317(19) 0.48557(11) 0.0580(7) Uani 0.25 1 d PD A 2 S2 S -0.0163(3) -0.0445(2) 0.83449(14) 0.0360(7) Uani 1 1 d . . . S1 S 0.0887(3) 0.1496(2) 0.84373(14) 0.0374(7) Uani 1 1 d . . . S3 S -0.2620(3) 0.0286(2) 0.85468(14) 0.0374(7) Uani 1 1 d . . . S4 S 0.3566(3) 0.4630(2) 0.84525(17) 0.0446(8) Uani 1 1 d . . . S5 S 0.2486(3) 0.6481(2) 0.83774(14) 0.0374(7) Uani 1 1 d . . . S6 S 0.6182(3) 0.5347(2) 0.86082(14) 0.0371(7) Uani 1 1 d . . . S7A S 0.6761(6) 0.3373(3) 0.5060(2) 0.0456(12) Uani 0.75 1 d PD A 1 S8A S 0.6444(5) 0.1273(3) 0.4873(3) 0.0420(11) Uani 0.75 1 d PD A 1 S9A S 0.9420(5) 0.3153(4) 0.4853(2) 0.0561(12) Uani 0.75 1 d P A 1 S7B S 0.6616(17) 0.3736(10) 0.5147(8) 0.0456(12) Uani 0.25 1 d PD A 2 S8B S 0.6657(19) 0.1583(12) 0.4892(10) 0.0420(11) Uani 0.25 1 d PD A 2 S9B S 0.9567(15) 0.1911(11) 0.5152(7) 0.0561(12) Uani 0.25 1 d P A 2 O1 O -0.1778(8) 0.0759(6) 0.7484(4) 0.044(2) Uani 1 1 d . . . O2 O -0.1365(9) 0.2107(6) 0.8567(5) 0.057(3) Uani 1 1 d . . . O3 O 0.4863(9) 0.7121(6) 0.8512(5) 0.060(3) Uani 1 1 d . . . O4 O 0.4329(8) 0.5698(7) 0.7491(4) 0.049(2) Uani 1 1 d . . . O5A O 0.8891(12) 0.1193(9) 0.4899(5) 0.051(3) Uani 0.75 1 d P A 1 O6A O 0.8837(10) 0.2535(8) 0.5921(5) 0.041(3) Uani 0.75 1 d P A 1 O5B O 0.888(3) 0.385(3) 0.5096(15) 0.051(3) Uani 0.25 1 d P A 2 O6B O 0.793(3) 0.246(3) 0.4110(17) 0.050(9) Uani 0.25 1 d P A 2 N1 N 0.0894(10) 0.0502(7) 0.6456(5) 0.044(3) Uani 1 1 d . . . N2 N 0.0590(9) 0.5415(7) 0.6437(4) 0.038(2) Uani 1 1 d . . . N3 N 0.6549(8) 0.3245(6) 0.9555(4) 0.030(2) Uani 1 1 d . . . N4 N 0.2172(9) 0.1638(7) 0.0411(4) 0.037(2) Uani 1 1 d . . . N5 N 0.6527(8) 0.3187(7) 0.6951(4) 0.033(2) Uani 1 1 d . . . N6 N 0.5501(9) 0.8145(7) 0.6921(4) 0.037(2) Uani 1 1 d . . . C2 C 0.1382(11) -0.0250(9) 0.8407(5) 0.037(3) Uani 1 1 d . . . C1 C 0.1860(10) 0.0603(8) 0.8449(5) 0.029(2) Uani 1 1 d . . . C6 C 0.3061(11) 0.0748(9) 0.8499(5) 0.041(3) Uani 1 1 d . . . H6 H 0.3366 0.1303 0.8493 0.049 Uiso 1 1 calc R . . C5 C 0.3849(12) 0.0048(13) 0.8563(6) 0.062(5) Uani 1 1 d . . . H5 H 0.4675 0.0157 0.8625 0.074 Uiso 1 1 calc R . . C4 C 0.3384(13) -0.0786(11) 0.8532(6) 0.055(4) Uani 1 1 d . . . H4 H 0.3894 -0.1250 0.8559 0.066 Uiso 1 1 calc R . . C3 C 0.2164(12) -0.0943(9) 0.8462(6) 0.043(3) Uani 1 1 d . . . H3 H 0.1857 -0.1507 0.8451 0.052 Uiso 1 1 calc R . . C7 C 0.2054(11) 0.4787(8) 0.8474(5) 0.036(3) Uani 1 1 d . . . C8 C 0.1574(10) 0.5613(8) 0.8449(5) 0.030(2) Uani 1 1 d . . . C9 C 0.0415(12) 0.5750(10) 0.8516(5) 0.046(3) Uani 1 1 d . . . H9 H 0.0098 0.6301 0.8503 0.055 Uiso 1 1 calc R . . C10 C -0.0284(11) 0.5099(10) 0.8602(6) 0.047(3) Uani 1 1 d . . . H10 H -0.1068 0.5202 0.8639 0.057 Uiso 1 1 calc R . . C11 C 0.0195(12) 0.4286(10) 0.8633(6) 0.049(3) Uani 1 1 d . . . H11 H -0.0263 0.3842 0.8698 0.059 Uiso 1 1 calc R . . C12 C 0.1352(12) 0.4129(9) 0.8567(6) 0.047(3) Uani 1 1 d . . . H12 H 0.1664 0.3578 0.8584 0.056 Uiso 1 1 calc R . . C13 C 0.5373(14) 0.2955(13) 0.5085(5) 0.067(5) Uani 1 1 d . . . C14 C 0.5305(15) 0.2016(9) 0.4985(6) 0.051(4) Uani 1 1 d . A . C15 C 0.4142(15) 0.1560(12) 0.4883(6) 0.064(4) Uani 1 1 d . . . H15 H 0.4047 0.0933 0.4781 0.077 Uiso 1 1 calc R A . C16 C 0.3154(16) 0.2093(13) 0.4943(7) 0.069(5) Uani 1 1 d . A . H16 H 0.2415 0.1812 0.4916 0.083 Uiso 1 1 calc R . . C17 C 0.3243(16) 0.3021(14) 0.5042(6) 0.070(5) Uani 1 1 d . . . H17 H 0.2574 0.3359 0.5070 0.084 Uiso 1 1 calc R A . C18 C 0.4346(15) 0.3427(11) 0.5097(7) 0.061(4) Uani 1 1 d . A . H18 H 0.4407 0.4045 0.5145 0.073 Uiso 1 1 calc R . . C19 C -0.0197(12) 0.0300(10) 0.5945(6) 0.051(3) Uani 1 1 d . . . H19A H -0.0154 0.0720 0.5717 0.061 Uiso 1 1 calc R . . H19B H -0.0155 -0.0303 0.5696 0.061 Uiso 1 1 calc R . . C20 C -0.1395(13) 0.0355(11) 0.6105(7) 0.059(4) Uani 1 1 d . . . H20A H -0.1381 0.0888 0.6421 0.089 Uiso 1 1 calc R . . H20B H -0.1554 -0.0168 0.6225 0.089 Uiso 1 1 calc R . . H20C H -0.2014 0.0379 0.5773 0.089 Uiso 1 1 calc R . . C21 C 0.0861(13) -0.0108(9) 0.6850(6) 0.046(3) Uani 1 1 d . . . H21A H 0.1603 0.0018 0.7152 0.055 Uiso 1 1 calc R . . H21B H 0.0208 0.0061 0.7044 0.055 Uiso 1 1 calc R . . C22 C 0.0712(18) -0.1099(10) 0.6571(8) 0.078(5) Uani 1 1 d . . . H22A H 0.1286 -0.1271 0.6335 0.118 Uiso 1 1 calc R . . H22B H -0.0088 -0.1256 0.6330 0.118 Uiso 1 1 calc R . . H22C H 0.0841 -0.1410 0.6868 0.118 Uiso 1 1 calc R . . C23 C 0.0918(14) 0.1469(9) 0.6813(6) 0.054(4) Uani 1 1 d . . . H23A H 0.0289 0.1519 0.7027 0.064 Uiso 1 1 calc R . . H23B H 0.0721 0.1841 0.6547 0.064 Uiso 1 1 calc R . . C24 C 0.2106(15) 0.1859(10) 0.7251(6) 0.064(4) Uani 1 1 d . . . H24A H 0.2652 0.2042 0.7050 0.095 Uiso 1 1 calc R . . H24B H 0.2453 0.1408 0.7430 0.095 Uiso 1 1 calc R . . H24C H 0.1958 0.2372 0.7546 0.095 Uiso 1 1 calc R . . C25 C 0.2004(13) 0.0328(13) 0.6215(7) 0.065(5) Uani 1 1 d . . . H25A H 0.1951 -0.0298 0.5985 0.078 Uiso 1 1 calc R . . H25B H 0.2703 0.0417 0.6538 0.078 Uiso 1 1 calc R . . C26 C 0.2192(18) 0.0930(15) 0.5832(9) 0.092(7) Uani 1 1 d . . . H26A H 0.2062 0.1543 0.6019 0.138 Uiso 1 1 calc R . . H26B H 0.1634 0.0729 0.5459 0.138 Uiso 1 1 calc R . . H26C H 0.3000 0.0896 0.5779 0.138 Uiso 1 1 calc R . . C27 C -0.0710(12) 0.5118(11) 0.6202(6) 0.054(4) Uani 1 1 d . . . H27A H -0.1091 0.5195 0.6527 0.065 Uiso 1 1 calc R . . H27B H -0.0778 0.4479 0.5998 0.065 Uiso 1 1 calc R . . C28 C -0.1398(14) 0.5624(13) 0.5784(7) 0.070(5) Uani 1 1 d . . . H28A H -0.1091 0.5495 0.5438 0.104 Uiso 1 1 calc R . . H28B H -0.1298 0.6261 0.5972 0.104 Uiso 1 1 calc R . . H28C H -0.2237 0.5432 0.5680 0.104 Uiso 1 1 calc R . . C29 C 0.0788(14) 0.6389(10) 0.6722(7) 0.055(4) Uani 1 1 d . . . H29A H 0.0625 0.6702 0.6421 0.066 Uiso 1 1 calc R . . H29B H 0.1630 0.6520 0.6920 0.066 Uiso 1 1 calc R . . C30 C 0.0024(15) 0.6775(10) 0.7166(7) 0.059(4) Uani 1 1 d . . . H30A H 0.0172 0.6469 0.7466 0.089 Uiso 1 1 calc R . . H30B H -0.0813 0.6687 0.6971 0.089 Uiso 1 1 calc R . . H30C H 0.0238 0.7408 0.7338 0.089 Uiso 1 1 calc R . . C31 C 0.1207(12) 0.5168(10) 0.5926(6) 0.049(3) Uani 1 1 d . . . H31A H 0.1037 0.4528 0.5732 0.058 Uiso 1 1 calc R . . H31B H 0.0852 0.5492 0.5648 0.058 Uiso 1 1 calc R . . C32 C 0.2545(12) 0.5366(10) 0.6084(6) 0.051(4) Uani 1 1 d . . . H32A H 0.2909 0.5071 0.6373 0.077 Uiso 1 1 calc R . . H32B H 0.2726 0.6006 0.6240 0.077 Uiso 1 1 calc R . . H32C H 0.2857 0.5149 0.5742 0.077 Uiso 1 1 calc R . . C33 C 0.1123(12) 0.4929(9) 0.6885(6) 0.045(3) Uani 1 1 d . . . H33A H 0.0696 0.5080 0.7196 0.055 Uiso 1 1 calc R . . H33B H 0.1955 0.5155 0.7055 0.055 Uiso 1 1 calc R . . C34 C 0.1087(15) 0.3914(10) 0.6657(8) 0.065(4) Uani 1 1 d . . . H34A H 0.1504 0.3753 0.6347 0.097 Uiso 1 1 calc R . . H34B H 0.0265 0.3676 0.6511 0.097 Uiso 1 1 calc R . . H34C H 0.1468 0.3667 0.6967 0.097 Uiso 1 1 calc R . . C35 C 0.5576(11) 0.3882(8) 0.9620(6) 0.042(3) Uani 1 1 d . . . H35A H 0.5379 0.4096 0.9274 0.051 Uiso 1 1 calc R . . H35B H 0.5892 0.4400 0.9951 0.051 Uiso 1 1 calc R . . C36 C 0.4415(13) 0.3513(10) 0.9706(7) 0.056(4) Uani 1 1 d . . . H36A H 0.4596 0.3262 1.0032 0.084 Uiso 1 1 calc R . . H36B H 0.4030 0.3052 0.9360 0.084 Uiso 1 1 calc R . . H36C H 0.3887 0.3993 0.9781 0.084 Uiso 1 1 calc R . . C37 C 0.6955(12) 0.2971(10) 1.0116(6) 0.048(3) Uani 1 1 d . . . H37A H 0.7199 0.3515 1.0437 0.058 Uiso 1 1 calc R . . H37B H 0.6269 0.2680 1.0182 0.058 Uiso 1 1 calc R . . C38 C 0.7959(16) 0.2356(10) 1.0135(7) 0.064(4) Uani 1 1 d . . . H38A H 0.8676 0.2661 1.0116 0.096 Uiso 1 1 calc R . . H38B H 0.7751 0.1826 0.9808 0.096 Uiso 1 1 calc R . . H38C H 0.8099 0.2185 1.0492 0.096 Uiso 1 1 calc R . . C39 C 0.6074(12) 0.2380(8) 0.9062(6) 0.041(3) Uani 1 1 d . . . H39A H 0.6737 0.1995 0.9017 0.050 Uiso 1 1 calc R . . H39B H 0.5486 0.2061 0.9180 0.050 Uiso 1 1 calc R . . C40 C 0.5525(13) 0.2512(9) 0.8497(6) 0.049(3) Uani 1 1 d . . . H40A H 0.6139 0.2681 0.8328 0.074 Uiso 1 1 calc R . . H40B H 0.4974 0.2982 0.8547 0.074 Uiso 1 1 calc R . . H40C H 0.5098 0.1962 0.8244 0.074 Uiso 1 1 calc R . . C41 C 0.7566(11) 0.3670(8) 0.9404(5) 0.038(3) Uani 1 1 d . . . H41A H 0.8128 0.3215 0.9306 0.045 Uiso 1 1 calc R . . H41B H 0.7249 0.3867 0.9058 0.045 Uiso 1 1 calc R . . C42 C 0.8229(14) 0.4448(10) 0.9871(7) 0.058(4) Uani 1 1 d . . . H42A H 0.8592 0.4253 1.0207 0.086 Uiso 1 1 calc R . . H42B H 0.7681 0.4902 0.9974 0.086 Uiso 1 1 calc R . . H42C H 0.8843 0.4693 0.9734 0.086 Uiso 1 1 calc R . . C43 C 0.2341(13) 0.2496(9) 0.0243(6) 0.047(3) Uani 1 1 d . . . H43A H 0.2721 0.2358 -0.0085 0.056 Uiso 1 1 calc R . . H43B H 0.2883 0.2921 0.0568 0.056 Uiso 1 1 calc R . . C44 C 0.1185(14) 0.2944(9) 0.0079(6) 0.055(4) Uani 1 1 d . . . H44A H 0.0889 0.3198 0.0423 0.082 Uiso 1 1 calc R . . H44B H 0.0596 0.2504 -0.0200 0.082 Uiso 1 1 calc R . . H44C H 0.1339 0.3415 -0.0089 0.082 Uiso 1 1 calc R . . C45 C 0.1543(12) 0.1770(10) 0.0892(6) 0.048(3) Uani 1 1 d . . . H45A H 0.1491 0.1199 0.0983 0.057 Uiso 1 1 calc R . . H45B H 0.0727 0.1919 0.0751 0.057 Uiso 1 1 calc R . . C46 C 0.2093(12) 0.2485(9) 0.1455(6) 0.046(3) Uani 1 1 d . . . H46A H 0.1963 0.3073 0.1399 0.069 Uiso 1 1 calc R . . H46B H 0.2941 0.2418 0.1565 0.069 Uiso 1 1 calc R . . H46C H 0.1723 0.2419 0.1759 0.069 Uiso 1 1 calc R . . C47 C 0.3406(11) 0.1314(9) 0.0611(6) 0.043(3) Uani 1 1 d . . . H47A H 0.3849 0.1784 0.0945 0.051 Uiso 1 1 calc R . . H47B H 0.3298 0.0790 0.0745 0.051 Uiso 1 1 calc R . . C48 C 0.4178(15) 0.1067(12) 0.0171(7) 0.066(5) Uani 1 1 d . . . H48A H 0.4582 0.1604 0.0157 0.099 Uiso 1 1 calc R . . H48B H 0.3679 0.0777 -0.0208 0.099 Uiso 1 1 calc R . . H48C H 0.4763 0.0664 0.0283 0.099 Uiso 1 1 calc R . . C49 C 0.1490(14) 0.0915(9) -0.0127(6) 0.053(4) Uani 1 1 d . . . H49A H 0.0660 0.1067 -0.0224 0.064 Uiso 1 1 calc R . . H49B H 0.1839 0.0914 -0.0455 0.064 Uiso 1 1 calc R . . C50 C 0.1515(16) -0.0024(10) -0.0045(7) 0.068(5) Uani 1 1 d . . . H50A H 0.1125 -0.0038 0.0262 0.101 Uiso 1 1 calc R . . H50B H 0.2334 -0.0176 0.0058 0.101 Uiso 1 1 calc R . . H50C H 0.1101 -0.0451 -0.0401 0.101 Uiso 1 1 calc R . . C51 C 0.6891(12) 0.3996(9) 0.6756(6) 0.043(3) Uani 1 1 d . . . H51A H 0.7572 0.3843 0.6581 0.052 Uiso 1 1 calc R . . H51B H 0.6229 0.4088 0.6455 0.052 Uiso 1 1 calc R . . C52 C 0.7215(13) 0.4865(9) 0.7225(7) 0.053(4) Uani 1 1 d . . . H52A H 0.7939 0.4811 0.7499 0.079 Uiso 1 1 calc R . . H52B H 0.6574 0.5004 0.7424 0.079 Uiso 1 1 calc R . . H52C H 0.7341 0.5339 0.7055 0.079 Uiso 1 1 calc R . . C53 C 0.7523(11) 0.3023(9) 0.7445(5) 0.037(3) Uani 1 1 d . . . H53A H 0.7563 0.3515 0.7796 0.045 Uiso 1 1 calc R . . H53B H 0.7298 0.2472 0.7526 0.045 Uiso 1 1 calc R . . C54 C 0.8723(12) 0.2947(10) 0.7325(6) 0.050(3) Uani 1 1 d . . . H54A H 0.9147 0.3531 0.7466 0.075 Uiso 1 1 calc R . . H54B H 0.8650 0.2719 0.6912 0.075 Uiso 1 1 calc R . . H54C H 0.9159 0.2542 0.7520 0.075 Uiso 1 1 calc R . . C55 C 0.6312(13) 0.2380(9) 0.6417(5) 0.045(3) Uani 1 1 d . . . H55A H 0.7053 0.2286 0.6284 0.054 Uiso 1 1 calc R . . H55B H 0.5713 0.2518 0.6108 0.054 Uiso 1 1 calc R . . C56 C 0.5894(13) 0.1501(10) 0.6510(7) 0.057(4) Uani 1 1 d . . . H56A H 0.5131 0.1571 0.6615 0.085 Uiso 1 1 calc R . . H56B H 0.6474 0.1360 0.6819 0.085 Uiso 1 1 calc R . . H56C H 0.5813 0.1020 0.6157 0.085 Uiso 1 1 calc R . . C57 C 0.5423(11) 0.3378(9) 0.7182(5) 0.038(3) Uani 1 1 d . . . H57A H 0.5599 0.3918 0.7511 0.046 Uiso 1 1 calc R . . H57B H 0.5243 0.2883 0.7330 0.046 Uiso 1 1 calc R . . C58 C 0.4313(13) 0.3511(10) 0.6754(7) 0.057(4) Uani 1 1 d . . . H58A H 0.4116 0.2979 0.6429 0.086 Uiso 1 1 calc R . . H58B H 0.4461 0.4019 0.6618 0.086 Uiso 1 1 calc R . . H58C H 0.3655 0.3619 0.6943 0.086 Uiso 1 1 calc R . . C59 C 0.4971(13) 0.8918(10) 0.6695(6) 0.055(4) Uani 1 1 d . . . H59A H 0.4130 0.8755 0.6504 0.066 Uiso 1 1 calc R . . H59B H 0.5381 0.9001 0.6405 0.066 Uiso 1 1 calc R . . C60 C 0.5067(14) 0.9811(10) 0.7171(7) 0.061(4) Uani 1 1 d . . . H60A H 0.5898 1.0014 0.7332 0.092 Uiso 1 1 calc R . . H60B H 0.4709 0.9727 0.7474 0.092 Uiso 1 1 calc R . . H60C H 0.4652 1.0254 0.7005 0.092 Uiso 1 1 calc R . . C61 C 0.4936(12) 0.7987(9) 0.7383(6) 0.047(3) Uani 1 1 d . . . H61A H 0.5175 0.8497 0.7729 0.056 Uiso 1 1 calc R . . H61B H 0.5259 0.7456 0.7486 0.056 Uiso 1 1 calc R . . C62 C 0.3590(13) 0.7859(13) 0.7227(7) 0.067(5) Uani 1 1 d . . . H62A H 0.3335 0.7367 0.6879 0.100 Uiso 1 1 calc R . . H62B H 0.3252 0.8401 0.7160 0.100 Uiso 1 1 calc R . . H62C H 0.3320 0.7726 0.7542 0.100 Uiso 1 1 calc R . . C63 C 0.5265(14) 0.7317(10) 0.6370(6) 0.053(4) Uani 1 1 d . . . H63A H 0.4407 0.7233 0.6197 0.063 Uiso 1 1 calc R . . H63B H 0.5658 0.7448 0.6086 0.063 Uiso 1 1 calc R . . C64 C 0.5695(16) 0.6455(10) 0.6486(7) 0.064(4) Uani 1 1 d . . . H64A H 0.5302 0.6313 0.6762 0.096 Uiso 1 1 calc R . . H64B H 0.6549 0.6522 0.6642 0.096 Uiso 1 1 calc R . . H64C H 0.5509 0.5976 0.6128 0.096 Uiso 1 1 calc R . . C65 C 0.6842(11) 0.8320(9) 0.7181(6) 0.043(3) Uani 1 1 d . . . H65A H 0.6966 0.8834 0.7525 0.052 Uiso 1 1 calc R . . H65B H 0.7135 0.7801 0.7309 0.052 Uiso 1 1 calc R . . C66 C 0.7584(14) 0.8496(11) 0.6794(7) 0.063(4) Uani 1 1 d . . . H66A H 0.7328 0.9022 0.6674 0.094 Uiso 1 1 calc R . . H66B H 0.7492 0.7986 0.6455 0.094 Uiso 1 1 calc R . . H66C H 0.8414 0.8595 0.7001 0.094 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0329(3) 0.0261(2) 0.0311(3) 0.01127(19) 0.0118(2) 0.00674(19) W2 0.0291(3) 0.0251(3) 0.0386(3) 0.0097(2) 0.0031(2) -0.00096(19) W3A 0.0427(4) 0.0387(4) 0.0262(3) 0.0095(3) 0.0086(3) -0.0026(3) W3B 0.0634(16) 0.0613(16) 0.0407(13) 0.0117(12) -0.0020(11) 0.0167(13) S2 0.0328(15) 0.0277(15) 0.0513(19) 0.0179(14) 0.0087(14) 0.0050(12) S1 0.0422(17) 0.0270(15) 0.0458(18) 0.0143(13) 0.0109(14) 0.0025(13) S3 0.0385(16) 0.0349(17) 0.0456(18) 0.0190(14) 0.0140(14) 0.0052(13) S4 0.0317(16) 0.0294(16) 0.082(3) 0.0290(16) 0.0152(16) 0.0048(13) S5 0.0484(18) 0.0283(15) 0.0381(17) 0.0124(13) 0.0115(14) 0.0105(13) S6 0.0339(16) 0.0347(16) 0.0415(18) 0.0136(13) 0.0028(13) 0.0025(13) S7A 0.074(3) 0.022(3) 0.034(3) 0.003(3) 0.004(2) -0.007(3) S8A 0.050(3) 0.029(3) 0.043(2) 0.012(3) 0.001(2) -0.012(2) S9A 0.072(3) 0.052(3) 0.054(3) 0.027(2) 0.019(2) -0.001(2) S7B 0.074(3) 0.022(3) 0.034(3) 0.003(3) 0.004(2) -0.007(3) S8B 0.050(3) 0.029(3) 0.043(2) 0.012(3) 0.001(2) -0.012(2) S9B 0.072(3) 0.052(3) 0.054(3) 0.027(2) 0.019(2) -0.001(2) O1 0.050(5) 0.053(6) 0.034(5) 0.019(4) 0.010(4) 0.016(4) O2 0.056(6) 0.032(5) 0.086(8) 0.003(5) 0.038(6) 0.016(4) O3 0.046(6) 0.029(5) 0.100(8) 0.014(5) 0.008(5) -0.007(4) O4 0.043(5) 0.071(7) 0.044(5) 0.031(5) 0.013(4) 0.017(5) O5A 0.060(8) 0.056(8) 0.031(6) 0.003(5) 0.010(6) 0.007(6) O6A 0.039(6) 0.056(8) 0.025(6) 0.005(5) 0.006(5) -0.006(5) O5B 0.060(8) 0.056(8) 0.031(6) 0.003(5) 0.010(6) 0.007(6) O6B 0.05(2) 0.06(2) 0.06(2) 0.032(19) 0.021(19) 0.026(19) N1 0.050(7) 0.043(6) 0.043(6) 0.016(5) 0.015(5) 0.011(5) N2 0.035(5) 0.041(6) 0.036(6) 0.014(5) -0.001(5) -0.003(5) N3 0.037(5) 0.027(5) 0.026(5) 0.010(4) 0.007(4) 0.005(4) N4 0.039(6) 0.031(5) 0.035(6) 0.010(4) 0.000(5) -0.016(4) N5 0.034(5) 0.042(6) 0.028(5) 0.018(4) 0.010(4) 0.013(4) N6 0.040(6) 0.040(6) 0.028(5) 0.013(4) -0.002(4) -0.002(5) C2 0.038(7) 0.044(7) 0.033(7) 0.015(6) 0.012(5) 0.004(6) C1 0.031(6) 0.035(6) 0.020(6) 0.009(5) -0.001(5) 0.002(5) C6 0.042(7) 0.046(8) 0.039(7) 0.018(6) 0.011(6) -0.006(6) C5 0.025(7) 0.110(15) 0.037(8) 0.004(8) -0.001(6) -0.001(8) C4 0.040(8) 0.062(10) 0.058(10) 0.009(8) 0.013(7) 0.021(7) C3 0.043(7) 0.039(7) 0.044(8) 0.007(6) 0.010(6) 0.013(6) C7 0.035(6) 0.027(6) 0.037(7) 0.002(5) 0.000(5) -0.009(5) C8 0.028(6) 0.032(6) 0.021(6) 0.000(5) 0.000(5) 0.003(5) C9 0.044(7) 0.063(9) 0.029(7) 0.006(6) 0.011(6) 0.019(7) C10 0.028(7) 0.063(9) 0.045(8) 0.008(7) 0.005(6) -0.002(6) C11 0.042(8) 0.053(9) 0.052(9) 0.014(7) 0.011(7) -0.014(7) C12 0.051(8) 0.035(7) 0.050(8) 0.004(6) 0.012(7) -0.003(6) C13 0.058(9) 0.123(16) 0.001(6) -0.007(7) -0.004(6) -0.011(10) C14 0.085(11) 0.041(8) 0.053(9) 0.040(7) 0.034(8) 0.017(7) C15 0.074(11) 0.076(11) 0.039(8) 0.021(8) 0.003(8) -0.010(9) C16 0.060(10) 0.089(14) 0.067(11) 0.036(10) 0.012(9) 0.001(10) C17 0.067(11) 0.101(15) 0.033(8) 0.011(8) 0.004(7) 0.035(10) C18 0.065(10) 0.056(10) 0.078(12) 0.036(8) 0.027(9) 0.024(8) C19 0.052(8) 0.061(9) 0.046(8) 0.023(7) 0.016(7) 0.011(7) C20 0.052(9) 0.062(10) 0.063(10) 0.017(8) 0.012(8) -0.005(8) C21 0.055(8) 0.048(8) 0.038(7) 0.022(6) 0.003(6) 0.012(7) C22 0.100(14) 0.036(9) 0.093(14) 0.019(9) 0.007(11) 0.013(9) C23 0.076(10) 0.034(7) 0.057(9) 0.022(7) 0.016(8) 0.015(7) C24 0.089(12) 0.050(9) 0.043(9) 0.012(7) 0.000(8) -0.013(8) C25 0.043(8) 0.102(14) 0.046(9) 0.011(9) 0.016(7) 0.010(8) C26 0.091(14) 0.115(17) 0.077(13) 0.019(12) 0.043(12) -0.020(13) C27 0.039(8) 0.071(10) 0.047(8) 0.016(7) 0.002(6) -0.013(7) C28 0.047(9) 0.108(15) 0.050(10) 0.030(9) -0.005(7) 0.007(9) C29 0.057(9) 0.048(9) 0.067(10) 0.025(7) 0.016(8) 0.005(7) C30 0.071(10) 0.039(8) 0.066(10) 0.012(7) 0.017(8) 0.007(7) C31 0.053(8) 0.052(9) 0.042(8) 0.016(7) 0.009(6) 0.003(7) C32 0.045(8) 0.063(10) 0.050(9) 0.022(7) 0.013(7) 0.002(7) C33 0.049(8) 0.050(8) 0.036(7) 0.016(6) 0.001(6) -0.007(6) C34 0.068(10) 0.047(9) 0.087(12) 0.033(9) 0.018(9) 0.003(8) C35 0.038(7) 0.029(7) 0.059(9) 0.004(6) 0.021(6) 0.004(5) C36 0.055(9) 0.042(8) 0.077(11) 0.011(7) 0.035(8) 0.005(7) C37 0.047(8) 0.064(9) 0.032(7) 0.014(6) 0.005(6) -0.002(7) C38 0.092(12) 0.045(9) 0.054(10) 0.020(7) 0.009(9) 0.017(8) C39 0.040(7) 0.028(6) 0.053(8) 0.005(6) 0.014(6) 0.004(5) C40 0.065(9) 0.042(8) 0.039(8) 0.008(6) 0.009(7) -0.009(7) C41 0.048(7) 0.031(6) 0.032(7) 0.005(5) 0.009(6) 0.005(6) C42 0.056(9) 0.048(9) 0.066(10) 0.008(7) 0.017(8) -0.014(7) C43 0.060(9) 0.031(7) 0.057(9) 0.018(6) 0.023(7) 0.000(6) C44 0.086(11) 0.037(8) 0.047(8) 0.020(6) 0.017(8) 0.006(7) C45 0.047(8) 0.055(9) 0.046(8) 0.021(7) 0.011(6) -0.009(7) C46 0.047(8) 0.051(8) 0.038(7) 0.013(6) 0.006(6) 0.000(6) C47 0.042(7) 0.036(7) 0.047(8) 0.012(6) 0.002(6) -0.006(6) C48 0.068(10) 0.086(12) 0.055(10) 0.032(9) 0.019(8) 0.032(9) C49 0.065(9) 0.046(8) 0.042(8) 0.012(6) -0.003(7) -0.012(7) C50 0.095(13) 0.041(9) 0.057(10) 0.017(7) -0.006(9) -0.029(8) C51 0.050(8) 0.049(8) 0.042(8) 0.026(6) 0.016(6) 0.003(6) C52 0.059(9) 0.040(8) 0.071(10) 0.026(7) 0.025(8) 0.010(7) C53 0.043(7) 0.043(7) 0.025(6) 0.014(5) 0.001(5) 0.005(6) C54 0.044(8) 0.054(9) 0.045(8) 0.008(7) 0.004(6) 0.016(7) C55 0.055(8) 0.047(8) 0.031(7) 0.010(6) 0.007(6) 0.005(6) C56 0.052(9) 0.050(9) 0.062(10) 0.010(7) 0.007(7) 0.001(7) C57 0.041(7) 0.042(7) 0.032(7) 0.009(5) 0.009(5) -0.005(6) C58 0.046(8) 0.049(9) 0.073(11) 0.017(8) 0.008(8) 0.006(7) C59 0.052(9) 0.060(9) 0.050(9) 0.030(7) -0.014(7) 0.005(7) C60 0.066(10) 0.048(9) 0.068(11) 0.028(8) 0.000(8) -0.001(8) C61 0.051(8) 0.043(8) 0.049(8) 0.011(6) 0.018(7) 0.002(6) C62 0.043(8) 0.097(13) 0.062(10) 0.032(9) 0.004(8) -0.010(8) C63 0.055(9) 0.057(9) 0.036(8) 0.002(7) 0.004(7) -0.008(7) C64 0.083(12) 0.040(9) 0.059(10) -0.002(7) 0.017(9) 0.008(8) C65 0.044(7) 0.043(8) 0.040(7) 0.015(6) 0.000(6) -0.001(6) C66 0.052(9) 0.062(10) 0.081(12) 0.026(9) 0.023(8) -0.003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.766(8) . ? W1 O2 1.769(9) . ? W1 S3 2.242(3) . ? W1 S1 2.468(3) . ? W1 S2 2.515(3) . ? W2 O4 1.756(9) . ? W2 O3 1.771(9) . ? W2 S6 2.252(3) . ? W2 S5 2.484(3) . ? W2 S4 2.498(3) . ? W3A O6A 1.750(10) . ? W3A O5A 1.757(13) . ? W3A S9A 2.229(5) . ? W3A S8A 2.501(5) . ? W3A S7A 2.521(6) . ? W3B O6B 1.72(4) . ? W3B O5B 1.80(4) . ? W3B S9B 2.169(17) . ? W3B S7B 2.443(15) . ? W3B S8B 2.498(13) . ? S2 C2 1.757(12) . ? S1 C1 1.774(12) . ? S4 C7 1.755(13) . ? S5 C8 1.767(12) . ? S7A C13 1.733(17) . ? S8A C14 1.753(16) . ? S7B C13 1.82(3) . ? S8B C14 1.72(3) . ? N1 C23 1.507(17) . ? N1 C25 1.510(17) . ? N1 C19 1.517(17) . ? N1 C21 1.526(16) . ? N2 C29 1.468(17) . ? N2 C27 1.491(16) . ? N2 C33 1.510(16) . ? N2 C31 1.530(17) . ? N3 C35 1.491(15) . ? N3 C41 1.497(15) . ? N3 C37 1.519(15) . ? N3 C39 1.536(15) . ? N4 C45 1.482(16) . ? N4 C43 1.514(15) . ? N4 C47 1.517(16) . ? N4 C49 1.524(16) . ? N5 C57 1.494(15) . ? N5 C55 1.513(16) . ? N5 C53 1.540(14) . ? N5 C51 1.540(15) . ? N6 C61 1.494(16) . ? N6 C65 1.515(16) . ? N6 C59 1.517(16) . ? N6 C63 1.556(16) . ? C2 C1 1.394(17) . ? C2 C3 1.409(17) . ? C1 C6 1.363(16) . ? C6 C5 1.43(2) . ? C5 C4 1.37(2) . ? C4 C3 1.379(19) . ? C7 C12 1.391(17) . ? C7 C8 1.399(17) . ? C8 C9 1.381(17) . ? C9 C10 1.37(2) . ? C10 C11 1.38(2) . ? C11 C12 1.381(19) . ? C13 C18 1.38(2) . ? C13 C14 1.40(2) . ? C14 C15 1.44(2) . ? C15 C16 1.41(2) . ? C16 C17 1.39(2) . ? C17 C18 1.37(2) . ? C19 C20 1.503(19) . ? C21 C22 1.49(2) . ? C23 C24 1.53(2) . ? C25 C26 1.53(2) . ? C27 C28 1.53(2) . ? C29 C30 1.54(2) . ? C31 C32 1.501(19) . ? C33 C34 1.510(19) . ? C35 C36 1.523(17) . ? C37 C38 1.49(2) . ? C39 C40 1.452(18) . ? C41 C42 1.477(18) . ? C43 C44 1.52(2) . ? C45 C46 1.514(18) . ? C47 C48 1.512(19) . ? C49 C50 1.516(19) . ? C51 C52 1.490(19) . ? C53 C54 1.463(18) . ? C55 C56 1.530(19) . ? C57 C58 1.506(18) . ? C59 C60 1.53(2) . ? C61 C62 1.499(19) . ? C63 C64 1.50(2) . ? C65 C66 1.480(19) . ? 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 O1 W1 O2 106.2(5) . . ? O1 W1 S3 106.3(3) . . ? O2 W1 S3 102.3(3) . . ? O1 W1 S1 104.4(3) . . ? O2 W1 S1 80.7(3) . . ? S3 W1 S1 146.80(11) . . ? O1 W1 S2 104.6(3) . . ? O2 W1 S2 146.3(4) . . ? S3 W1 S2 81.70(11) . . ? S1 W1 S2 78.65(10) . . ? O4 W2 O3 104.3(5) . . ? O4 W2 S6 106.9(3) . . ? O3 W2 S6 103.1(3) . . ? O4 W2 S5 103.0(3) . . ? O3 W2 S5 80.7(3) . . ? S6 W2 S5 147.73(11) . . ? O4 W2 S4 108.0(3) . . ? O3 W2 S4 144.6(4) . . ? S6 W2 S4 81.10(11) . . ? S5 W2 S4 78.34(10) . . ? O6A W3A O5A 105.6(6) . . ? O6A W3A S9A 107.1(4) . . ? O5A W3A S9A 102.4(5) . . ? O6A W3A S8A 107.7(4) . . ? O5A W3A S8A 79.7(5) . . ? S9A W3A S8A 143.1(2) . . ? O6A W3A S7A 100.2(4) . . ? O5A W3A S7A 149.9(4) . . ? S9A W3A S7A 84.27(19) . . ? S8A W3A S7A 77.86(18) . . ? O6B W3B O5B 103.1(17) . . ? O6B W3B S9B 106.5(12) . . ? O5B W3B S9B 103.5(13) . . ? O6B W3B S7B 108.4(12) . . ? O5B W3B S7B 74.8(13) . . ? S9B W3B S7B 144.5(6) . . ? O6B W3B S8B 97.5(14) . . ? O5B W3B S8B 152.1(13) . . ? S9B W3B S8B 88.2(7) . . ? S7B W3B S8B 81.1(7) . . ? C2 S2 W1 109.7(4) . . ? C1 S1 W1 111.2(4) . . ? C7 S4 W2 110.6(4) . . ? C8 S5 W2 110.8(4) . . ? C13 S7A W3A 111.7(7) . . ? C14 S8A W3A 105.4(5) . . ? C13 S7B W3B 102.9(9) . . ? C14 S8B W3B 113.2(10) . . ? C23 N1 C25 111.2(12) . . ? C23 N1 C19 109.3(10) . . ? C25 N1 C19 108.0(10) . . ? C23 N1 C21 108.5(10) . . ? C25 N1 C21 108.3(11) . . ? C19 N1 C21 111.4(11) . . ? C29 N2 C27 112.6(11) . . ? C29 N2 C33 107.9(10) . . ? C27 N2 C33 109.0(10) . . ? C29 N2 C31 109.4(10) . . ? C27 N2 C31 107.7(10) . . ? C33 N2 C31 110.2(10) . . ? C35 N3 C41 110.2(9) . . ? C35 N3 C37 109.0(10) . . ? C41 N3 C37 112.0(9) . . ? C35 N3 C39 110.4(9) . . ? C41 N3 C39 108.0(9) . . ? C37 N3 C39 107.2(9) . . ? C45 N4 C43 112.9(10) . . ? C45 N4 C47 108.1(10) . . ? C43 N4 C47 108.1(9) . . ? C45 N4 C49 110.6(10) . . ? C43 N4 C49 109.0(10) . . ? C47 N4 C49 108.0(10) . . ? C57 N5 C55 111.8(10) . . ? C57 N5 C53 107.4(9) . . ? C55 N5 C53 110.7(9) . . ? C57 N5 C51 109.5(9) . . ? C55 N5 C51 106.3(9) . . ? C53 N5 C51 111.1(9) . . ? C61 N6 C65 107.3(10) . . ? C61 N6 C59 112.1(11) . . ? C65 N6 C59 111.6(10) . . ? C61 N6 C63 111.8(10) . . ? C65 N6 C63 109.6(10) . . ? C59 N6 C63 104.4(10) . . ? C1 C2 C3 119.3(11) . . ? C1 C2 S2 120.8(9) . . ? C3 C2 S2 119.7(10) . . ? C6 C1 C2 120.4(11) . . ? C6 C1 S1 120.5(9) . . ? C2 C1 S1 119.1(9) . . ? C1 C6 C5 119.8(12) . . ? C4 C5 C6 119.7(12) . . ? C5 C4 C3 120.5(14) . . ? C4 C3 C2 120.1(13) . . ? C12 C7 C8 119.1(12) . . ? C12 C7 S4 120.8(10) . . ? C8 C7 S4 119.9(9) . . ? C9 C8 C7 119.0(12) . . ? C9 C8 S5 121.3(10) . . ? C7 C8 S5 119.6(9) . . ? C10 C9 C8 122.0(13) . . ? C9 C10 C11 119.0(12) . . ? C12 C11 C10 120.3(13) . . ? C11 C12 C7 120.7(13) . . ? C18 C13 C14 120.3(15) . . ? C18 C13 S7A 126.1(16) . . ? C14 C13 S7A 112.7(13) . . ? C18 C13 S7B 108.4(15) . . ? C14 C13 S7B 131.1(14) . . ? S7A C13 S7B 18.6(5) . . ? C13 C14 C15 118.4(15) . . ? C13 C14 S8B 110.7(12) . . ? C15 C14 S8B 130.1(13) . . ? C13 C14 S8A 127.9(12) . . ? C15 C14 S8A 113.2(12) . . ? S8B C14 S8A 17.3(4) . . ? C16 C15 C14 117.9(16) . . ? C17 C16 C15 122.4(17) . . ? C18 C17 C16 118.0(16) . . ? C17 C18 C13 122.7(16) . . ? C20 C19 N1 115.4(11) . . ? C22 C21 N1 117.4(12) . . ? N1 C23 C24 116.2(12) . . ? N1 C25 C26 114.3(14) . . ? N2 C27 C28 114.7(12) . . ? N2 C29 C30 115.6(12) . . ? C32 C31 N2 115.6(11) . . ? N2 C33 C34 115.3(11) . . ? N3 C35 C36 116.7(11) . . ? C38 C37 N3 116.2(11) . . ? C40 C39 N3 115.5(11) . . ? C42 C41 N3 114.8(10) . . ? N4 C43 C44 114.2(11) . . ? N4 C45 C46 117.1(11) . . ? C48 C47 N4 117.4(11) . . ? C50 C49 N4 113.3(11) . . ? C52 C51 N5 115.7(10) . . ? C54 C53 N5 115.2(10) . . ? N5 C55 C56 114.9(11) . . ? N5 C57 C58 116.0(10) . . ? N6 C59 C60 113.9(11) . . ? N6 C61 C62 116.0(12) . . ? C64 C63 N6 114.3(12) . . ? C66 C65 N6 116.5(11) . . ? 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 O1 W1 S2 C2 95.7(5) . . . . ? O2 W1 S2 C2 -59.8(7) . . . . ? S3 W1 S2 C2 -159.5(5) . . . . ? S1 W1 S2 C2 -6.4(4) . . . . ? O1 W1 S1 C1 -95.9(5) . . . . ? O2 W1 S1 C1 159.6(5) . . . . ? S3 W1 S1 C1 61.3(5) . . . . ? S2 W1 S1 C1 6.5(4) . . . . ? O4 W2 S4 C7 -93.0(5) . . . . ? O3 W2 S4 C7 61.9(7) . . . . ? S6 W2 S4 C7 162.1(5) . . . . ? S5 W2 S4 C7 7.1(4) . . . . ? O4 W2 S5 C8 99.5(5) . . . . ? O3 W2 S5 C8 -157.8(6) . . . . ? S6 W2 S5 C8 -58.0(5) . . . . ? S4 W2 S5 C8 -6.5(4) . . . . ? O6A W3A S7A C13 -87.5(6) . . . . ? O5A W3A S7A C13 61.2(10) . . . . ? S9A W3A S7A C13 166.1(5) . . . . ? S8A W3A S7A C13 18.6(5) . . . . ? O6A W3A S8A C14 81.4(7) . . . . ? O5A W3A S8A C14 -175.4(6) . . . . ? S9A W3A S8A C14 -78.4(6) . . . . ? S7A W3A S8A C14 -15.6(5) . . . . ? O6B W3B S7B C13 87.0(17) . . . . ? O5B W3B S7B C13 -174.0(16) . . . . ? S9B W3B S7B C13 -82.0(14) . . . . ? S8B W3B S7B C13 -8.0(10) . . . . ? O6B W3B S8B C14 -98.7(16) . . . . ? O5B W3B S8B C14 39(3) . . . . ? S9B W3B S8B C14 154.9(12) . . . . ? S7B W3B S8B C14 8.9(12) . . . . ? W1 S2 C2 C1 5.7(11) . . . . ? W1 S2 C2 C3 -179.4(9) . . . . ? C3 C2 C1 C6 4.8(18) . . . . ? S2 C2 C1 C6 179.7(9) . . . . ? C3 C2 C1 S1 -175.0(9) . . . . ? S2 C2 C1 S1 -0.1(14) . . . . ? W1 S1 C1 C6 174.5(8) . . . . ? W1 S1 C1 C2 -5.8(10) . . . . ? C2 C1 C6 C5 -5.6(18) . . . . ? S1 C1 C6 C5 174.1(10) . . . . ? C1 C6 C5 C4 4(2) . . . . ? C6 C5 C4 C3 -2(2) . . . . ? C5 C4 C3 C2 2(2) . . . . ? C1 C2 C3 C4 -2.7(19) . . . . ? S2 C2 C3 C4 -177.6(10) . . . . ? W2 S4 C7 C12 178.4(9) . . . . ? W2 S4 C7 C8 -7.1(11) . . . . ? C12 C7 C8 C9 0.1(17) . . . . ? S4 C7 C8 C9 -174.6(9) . . . . ? C12 C7 C8 S5 176.1(9) . . . . ? S4 C7 C8 S5 1.4(14) . . . . ? W2 S5 C8 C9 -179.1(8) . . . . ? W2 S5 C8 C7 5.0(10) . . . . ? C7 C8 C9 C10 -0.6(18) . . . . ? S5 C8 C9 C10 -176.6(10) . . . . ? C8 C9 C10 C11 1(2) . . . . ? C9 C10 C11 C12 -1(2) . . . . ? C10 C11 C12 C7 1(2) . . . . ? C8 C7 C12 C11 -0.1(19) . . . . ? S4 C7 C12 C11 174.5(11) . . . . ? W3A S7A C13 C18 173.6(12) . . . . ? W3A S7A C13 C14 -17.4(11) . . . . ? W3A S7A C13 S7B 154(2) . . . . ? W3B S7B C13 C18 -165.3(10) . . . . ? W3B S7B C13 C14 8.9(18) . . . . ? W3B S7B C13 S7A -2.3(17) . . . . ? C18 C13 C14 C15 1(2) . . . . ? S7A C13 C14 C15 -168.4(10) . . . . ? S7B C13 C14 C15 -172.3(13) . . . . ? C18 C13 C14 S8B 171.8(14) . . . . ? S7A C13 C14 S8B 2.0(15) . . . . ? S7B C13 C14 S8B -2(2) . . . . ? C18 C13 C14 S8A 172.5(12) . . . . ? S7A C13 C14 S8A 2.7(17) . . . . ? S7B C13 C14 S8A -1(2) . . . . ? W3B S8B C14 C13 -6.5(16) . . . . ? W3B S8B C14 C15 162.5(12) . . . . ? W3B S8B C14 S8A 175(4) . . . . ? W3A S8A C14 C13 13.0(14) . . . . ? W3A S8A C14 C15 -175.5(9) . . . . ? W3A S8A C14 S8B 15(3) . . . . ? C13 C14 C15 C16 -6(2) . . . . ? S8B C14 C15 C16 -174.0(15) . . . . ? S8A C14 C15 C16 -178.1(12) . . . . ? C14 C15 C16 C17 6(2) . . . . ? C15 C16 C17 C18 -2(2) . . . . ? C16 C17 C18 C13 -3(2) . . . . ? C14 C13 C18 C17 3(2) . . . . ? S7A C13 C18 C17 171.5(12) . . . . ? S7B C13 C18 C17 178.1(14) . . . . ? C23 N1 C19 C20 -64.2(15) . . . . ? C25 N1 C19 C20 174.6(13) . . . . ? C21 N1 C19 C20 55.7(16) . . . . ? C23 N1 C21 C22 174.1(13) . . . . ? C25 N1 C21 C22 -65.1(17) . . . . ? C19 N1 C21 C22 53.6(17) . . . . ? C25 N1 C23 C24 -45.8(16) . . . . ? C19 N1 C23 C24 -165.1(12) . . . . ? C21 N1 C23 C24 73.2(15) . . . . ? C23 N1 C25 C26 -57.9(17) . . . . ? C19 N1 C25 C26 62.1(17) . . . . ? C21 N1 C25 C26 -177.1(14) . . . . ? C29 N2 C27 C28 54.7(17) . . . . ? C33 N2 C27 C28 174.4(13) . . . . ? C31 N2 C27 C28 -66.0(16) . . . . ? C27 N2 C29 C30 48.8(16) . . . . ? C33 N2 C29 C30 -71.5(15) . . . . ? C31 N2 C29 C30 168.5(12) . . . . ? C29 N2 C31 C32 60.8(15) . . . . ? C27 N2 C31 C32 -176.5(12) . . . . ? C33 N2 C31 C32 -57.7(15) . . . . ? C29 N2 C33 C34 -175.5(12) . . . . ? C27 N2 C33 C34 61.9(15) . . . . ? C31 N2 C33 C34 -56.1(15) . . . . ? C41 N3 C35 C36 173.3(11) . . . . ? C37 N3 C35 C36 -63.3(15) . . . . ? C39 N3 C35 C36 54.1(15) . . . . ? C35 N3 C37 C38 -178.0(12) . . . . ? C41 N3 C37 C38 -55.8(15) . . . . ? C39 N3 C37 C38 62.5(15) . . . . ? C35 N3 C39 C40 55.2(14) . . . . ? C41 N3 C39 C40 -65.4(13) . . . . ? C37 N3 C39 C40 173.8(11) . . . . ? C35 N3 C41 C42 66.9(14) . . . . ? C37 N3 C41 C42 -54.6(15) . . . . ? C39 N3 C41 C42 -172.4(11) . . . . ? C45 N4 C43 C44 -55.8(15) . . . . ? C47 N4 C43 C44 -175.3(11) . . . . ? C49 N4 C43 C44 67.6(15) . . . . ? C43 N4 C45 C46 -56.1(16) . . . . ? C47 N4 C45 C46 63.4(14) . . . . ? C49 N4 C45 C46 -178.5(12) . . . . ? C45 N4 C47 C48 175.6(12) . . . . ? C43 N4 C47 C48 -61.9(15) . . . . ? C49 N4 C47 C48 55.9(15) . . . . ? C45 N4 C49 C50 -68.3(17) . . . . ? C43 N4 C49 C50 167.0(13) . . . . ? C47 N4 C49 C50 49.8(16) . . . . ? C57 N5 C51 C52 62.3(14) . . . . ? C55 N5 C51 C52 -176.7(11) . . . . ? C53 N5 C51 C52 -56.2(14) . . . . ? C57 N5 C53 C54 -171.9(11) . . . . ? C55 N5 C53 C54 65.8(14) . . . . ? C51 N5 C53 C54 -52.2(14) . . . . ? C57 N5 C55 C56 -58.4(14) . . . . ? C53 N5 C55 C56 61.3(14) . . . . ? C51 N5 C55 C56 -177.9(11) . . . . ? C55 N5 C57 C58 -55.2(14) . . . . ? C53 N5 C57 C58 -176.9(11) . . . . ? C51 N5 C57 C58 62.4(14) . . . . ? C61 N6 C59 C60 57.1(16) . . . . ? C65 N6 C59 C60 -63.3(16) . . . . ? C63 N6 C59 C60 178.3(12) . . . . ? C65 N6 C61 C62 176.2(13) . . . . ? C59 N6 C61 C62 53.3(16) . . . . ? C63 N6 C61 C62 -63.5(16) . . . . ? C61 N6 C63 C64 -57.5(16) . . . . ? C65 N6 C63 C64 61.4(15) . . . . ? C59 N6 C63 C64 -178.9(13) . . . . ? C61 N6 C65 C66 -179.9(12) . . . . ? C59 N6 C65 C66 -56.7(16) . . . . ? C63 N6 C65 C66 58.5(15) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 3.646 _refine_diff_density_min -2.608 _refine_diff_density_rms 0.185 #==========================================END data_jjw127 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H45 N O2 S3 Si W' _chemical_formula_weight 675.72 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' 0.0000 0.0000 '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 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'Pbca' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.742(5) _cell_length_b 14.364(5) _cell_length_c 26.503(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5993(4) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'blocks' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.498 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 4.123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3710 _exptl_absorpt_correction_T_max 0.4255 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31811 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5271 _reflns_number_gt 4635 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material 'SHELXTL (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0198P)^2^+50.7809P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5271 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0540 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 1.248 _refine_ls_restrained_S_all 1.248 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 1.01140(2) 0.31395(2) 0.411211(13) 0.04300(12) Uani 1 1 d . . . Si1 Si 0.9098(3) 0.2208(2) 0.30693(10) 0.0851(12) Uani 1 1 d . . . S1 S 1.02540(14) 0.36565(15) 0.49755(8) 0.0476(5) Uani 1 1 d . . . S2 S 0.97345(13) 0.16889(14) 0.45556(8) 0.0450(5) Uani 1 1 d . . . S3 S 0.9702(2) 0.45433(18) 0.39652(10) 0.0695(7) Uani 1 1 d . . . O2 O 0.9498(5) 0.2472(4) 0.3612(2) 0.0652(18) Uani 1 1 d . A . O1 O 1.1179(4) 0.3068(5) 0.3924(3) 0.072(2) Uani 1 1 d . . . C1 C 1.0310(5) 0.2676(6) 0.5362(3) 0.046(2) Uani 1 1 d . . . C2 C 1.0043(5) 0.1800(6) 0.5185(3) 0.0459(19) Uani 1 1 d . . . C3 C 1.0056(5) 0.1037(7) 0.5512(4) 0.056(2) Uani 1 1 d . . . H3 H 0.9893 0.0439 0.5394 0.067 Uiso 1 1 calc R . . C4 C 1.0307(7) 0.1155(9) 0.6007(4) 0.073(3) Uani 1 1 d . . . H4 H 1.0305 0.0636 0.6230 0.088 Uiso 1 1 calc R . . C5 C 1.0557(7) 0.2007(9) 0.6183(4) 0.071(3) Uani 1 1 d . . . H5 H 1.0738 0.2072 0.6523 0.086 Uiso 1 1 calc R . . C6 C 1.0548(6) 0.2763(8) 0.5874(4) 0.062(3) Uani 1 1 d . . . H6 H 1.0704 0.3356 0.6003 0.074 Uiso 1 1 calc R . . C7 C 0.884(2) 0.1044(18) 0.3060(11) 0.104(10) Uani 0.50 1 d P A 1 H7 H 0.9353 0.0686 0.3162 0.125 Uiso 0.50 1 calc PR A 1 C8 C 0.859(3) 0.0732(18) 0.2518(11) 0.134(14) Uani 0.50 1 d P A 1 H8A H 0.8500 0.0057 0.2514 0.201 Uiso 0.50 1 calc PR A 1 H8B H 0.9052 0.0891 0.2285 0.201 Uiso 0.50 1 calc PR A 1 H8C H 0.8069 0.1049 0.2415 0.201 Uiso 0.50 1 calc PR A 1 C9 C 0.822(2) 0.085(3) 0.3393(16) 0.117(14) Uani 0.50 1 d P A 1 H9A H 0.7743 0.1277 0.3344 0.176 Uiso 0.50 1 calc PR A 1 H9B H 0.8441 0.0915 0.3737 0.176 Uiso 0.50 1 calc PR A 1 H9C H 0.8025 0.0206 0.3341 0.176 Uiso 0.50 1 calc PR A 1 C10 C 1.0194(15) 0.2376(17) 0.2622(10) 0.083(7) Uani 0.50 1 d P A 1 H10 H 1.0009 0.2260 0.2266 0.100 Uiso 0.50 1 calc PR A 1 C11 C 1.086(2) 0.163(2) 0.2736(15) 0.143(14) Uani 0.50 1 d P A 1 H11A H 1.1297 0.1644 0.2474 0.215 Uiso 0.50 1 calc PR A 1 H11B H 1.0585 0.1021 0.2743 0.215 Uiso 0.50 1 calc PR A 1 H11C H 1.1117 0.1762 0.3065 0.215 Uiso 0.50 1 calc PR A 1 C12 C 1.0560(19) 0.3393(17) 0.2627(9) 0.087(8) Uani 0.50 1 d P A 1 H12A H 1.0887 0.3491 0.2937 0.130 Uiso 0.50 1 calc PR A 1 H12B H 1.0091 0.3841 0.2613 0.130 Uiso 0.50 1 calc PR A 1 H12C H 1.0931 0.3483 0.2334 0.130 Uiso 0.50 1 calc PR A 1 C13 C 0.8504(18) 0.3229(19) 0.2915(10) 0.075(7) Uani 0.50 1 d P A 1 H13 H 0.8863 0.3787 0.2990 0.090 Uiso 0.50 1 calc PR A 1 C14 C 0.822(2) 0.328(2) 0.2379(10) 0.123(12) Uani 0.50 1 d P A 1 H14A H 0.7911 0.2712 0.2290 0.185 Uiso 0.50 1 calc PR A 1 H14B H 0.8710 0.3355 0.2158 0.185 Uiso 0.50 1 calc PR A 1 H14C H 0.7837 0.3820 0.2338 0.185 Uiso 0.50 1 calc PR A 1 C15 C 0.7746(16) 0.323(3) 0.3275(12) 0.126(13) Uani 0.50 1 d P A 1 H15A H 0.7316 0.3669 0.3153 0.189 Uiso 0.50 1 calc PR A 1 H15B H 0.7934 0.3415 0.3612 0.189 Uiso 0.50 1 calc PR A 1 H15C H 0.7500 0.2602 0.3290 0.189 Uiso 0.50 1 calc PR A 1 N1 N 0.7626(4) 0.4125(4) 0.5548(3) 0.0431(16) Uani 1 1 d . . . C16 C 0.8364(5) 0.3589(7) 0.5770(4) 0.056(2) Uani 1 1 d . . . H16A H 0.8694 0.4019 0.5986 0.068 Uiso 1 1 calc R . . H16B H 0.8739 0.3394 0.5489 0.068 Uiso 1 1 calc R . . C17 C 0.8146(7) 0.2735(8) 0.6078(4) 0.078(3) Uani 1 1 d . . . H17A H 0.7808 0.2920 0.6372 0.117 Uiso 1 1 calc R . . H17B H 0.8671 0.2434 0.6192 0.117 Uiso 1 1 calc R . . H17C H 0.7820 0.2299 0.5871 0.117 Uiso 1 1 calc R . . C18 C 0.7134(5) 0.3525(6) 0.5183(3) 0.052(2) Uani 1 1 d . . . H18A H 0.6932 0.2965 0.5365 0.062 Uiso 1 1 calc R . . H18B H 0.6627 0.3875 0.5071 0.062 Uiso 1 1 calc R . . C19 C 0.7618(7) 0.3215(7) 0.4725(4) 0.073(3) Uani 1 1 d . . . H19A H 0.7832 0.3761 0.4543 0.109 Uiso 1 1 calc R . . H19B H 0.7241 0.2857 0.4503 0.109 Uiso 1 1 calc R . . H19C H 0.8097 0.2823 0.4828 0.109 Uiso 1 1 calc R . . C20 C 0.8011(6) 0.4960(6) 0.5291(4) 0.053(2) Uani 1 1 d . . . H20A H 0.8439 0.4739 0.5045 0.063 Uiso 1 1 calc R . . H20B H 0.8313 0.5337 0.5547 0.063 Uiso 1 1 calc R . . C21 C 0.7383(7) 0.5584(7) 0.5017(5) 0.081(3) Uani 1 1 d . . . H21A H 0.7132 0.5242 0.4734 0.122 Uiso 1 1 calc R . . H21B H 0.7679 0.6136 0.4890 0.122 Uiso 1 1 calc R . . H21C H 0.6934 0.5775 0.5251 0.122 Uiso 1 1 calc R . . C22 C 0.6999(6) 0.4408(8) 0.5957(4) 0.065(3) Uani 1 1 d . . . H22A H 0.6523 0.4749 0.5797 0.077 Uiso 1 1 calc R . . H22B H 0.6762 0.3838 0.6113 0.077 Uiso 1 1 calc R . . C23 C 0.7376(10) 0.5011(9) 0.6368(4) 0.095(4) Uani 1 1 d . . . H23A H 0.7613 0.5578 0.6218 0.142 Uiso 1 1 calc R . . H23B H 0.7827 0.4667 0.6542 0.142 Uiso 1 1 calc R . . H23C H 0.6931 0.5180 0.6610 0.142 Uiso 1 1 calc R . . C12B C 0.9547(18) 0.1095(17) 0.2217(7) 0.081(7) Uani 0.50 1 d P A 2 H12D H 1.0083 0.0850 0.2085 0.122 Uiso 0.50 1 calc PR A 2 H12E H 0.9400 0.1670 0.2039 0.122 Uiso 0.50 1 calc PR A 2 H12F H 0.9096 0.0634 0.2167 0.122 Uiso 0.50 1 calc PR A 2 C11B C 1.0386(18) 0.098(2) 0.3009(9) 0.090(8) Uani 0.50 1 d P A 2 H11D H 1.0568 0.0394 0.2849 0.135 Uiso 0.50 1 calc PR A 2 H11E H 1.0274 0.0864 0.3368 0.135 Uiso 0.50 1 calc PR A 2 H11F H 1.0834 0.1444 0.2974 0.135 Uiso 0.50 1 calc PR A 2 C7B C 0.781(2) 0.174(3) 0.3298(17) 0.148(18) Uani 0.50 1 d P A 2 H7B H 0.7497 0.2276 0.3451 0.177 Uiso 0.50 1 calc PR A 2 C10B C 0.964(2) 0.130(3) 0.2775(11) 0.123(14) Uani 0.50 1 d P A 2 H10B H 0.9263 0.0785 0.2896 0.147 Uiso 0.50 1 calc PR A 2 C13B C 0.880(4) 0.316(3) 0.2643(11) 0.14(2) Uani 0.50 1 d P A 2 H13B H 0.8548 0.2898 0.2325 0.166 Uiso 0.50 1 calc PR A 2 C9B C 0.784(3) 0.100(3) 0.3653(12) 0.109(12) Uani 0.50 1 d P A 2 H9B1 H 0.7256 0.0825 0.3748 0.163 Uiso 0.50 1 calc PR A 2 H9B2 H 0.8147 0.1203 0.3954 0.163 Uiso 0.50 1 calc PR A 2 H9B3 H 0.8124 0.0463 0.3502 0.163 Uiso 0.50 1 calc PR A 2 C15B C 0.958(3) 0.366(3) 0.2534(13) 0.148(18) Uani 0.50 1 d P A 2 H15D H 0.9442 0.4279 0.2406 0.222 Uiso 0.50 1 calc PR A 2 H15E H 0.9905 0.3315 0.2279 0.222 Uiso 0.50 1 calc PR A 2 H15F H 0.9916 0.3712 0.2843 0.222 Uiso 0.50 1 calc PR A 2 C8B C 0.732(2) 0.141(3) 0.2810(12) 0.171(18) Uani 0.50 1 d P A 2 H8B1 H 0.7562 0.0825 0.2688 0.256 Uiso 0.50 1 calc PR A 2 H8B2 H 0.7369 0.1887 0.2547 0.256 Uiso 0.50 1 calc PR A 2 H8B3 H 0.6716 0.1316 0.2891 0.256 Uiso 0.50 1 calc PR A 2 C14B C 0.822(3) 0.390(2) 0.2860(15) 0.154(18) Uani 0.50 1 d P A 2 H14D H 0.8466 0.4149 0.3171 0.231 Uiso 0.50 1 calc PR A 2 H14E H 0.7659 0.3629 0.2936 0.231 Uiso 0.50 1 calc PR A 2 H14F H 0.8148 0.4405 0.2615 0.231 Uiso 0.50 1 calc PR 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 W1 0.0452(2) 0.03866(19) 0.0451(2) 0.00403(15) 0.00863(15) -0.00186(15) Si1 0.158(3) 0.0666(19) 0.0306(14) -0.0067(13) -0.0206(17) 0.038(2) S1 0.0536(13) 0.0423(11) 0.0469(12) -0.0002(9) 0.0007(10) -0.0096(10) S2 0.0460(11) 0.0351(10) 0.0538(12) 0.0039(9) 0.0027(9) -0.0041(9) S3 0.097(2) 0.0519(14) 0.0598(16) 0.0024(12) -0.0113(14) 0.0012(14) O2 0.099(5) 0.059(4) 0.038(3) -0.010(3) 0.005(3) -0.014(4) O1 0.049(4) 0.064(4) 0.104(6) 0.007(4) 0.016(4) 0.005(3) C1 0.034(4) 0.057(5) 0.047(5) 0.005(4) 0.007(4) 0.006(4) C2 0.034(4) 0.050(5) 0.053(5) 0.009(4) 0.002(4) 0.011(4) C3 0.048(5) 0.056(5) 0.064(6) 0.019(5) 0.015(4) 0.015(4) C4 0.074(7) 0.085(8) 0.060(7) 0.034(6) 0.012(5) 0.022(6) C5 0.077(7) 0.096(9) 0.041(5) 0.013(6) 0.004(5) 0.014(6) C6 0.054(6) 0.082(7) 0.051(5) -0.001(5) -0.001(5) 0.007(5) C7 0.14(3) 0.086(18) 0.09(2) -0.024(15) -0.07(2) -0.039(18) C8 0.24(4) 0.080(18) 0.081(19) -0.017(16) -0.07(2) -0.03(2) C9 0.08(2) 0.15(3) 0.13(3) -0.02(3) 0.01(2) -0.08(2) C10 0.087(17) 0.079(15) 0.083(17) -0.009(13) 0.017(13) 0.002(14) C11 0.15(3) 0.13(3) 0.15(4) 0.00(3) 0.00(3) 0.06(3) C12 0.12(2) 0.085(17) 0.055(14) 0.010(12) 0.008(14) -0.037(16) C13 0.12(2) 0.063(15) 0.044(15) -0.004(12) -0.018(14) 0.023(14) C14 0.15(3) 0.15(3) 0.063(18) 0.008(19) -0.024(19) 0.04(2) C15 0.064(16) 0.20(4) 0.11(2) -0.03(3) 0.013(15) 0.05(2) N1 0.035(4) 0.041(4) 0.054(4) 0.006(3) -0.003(3) -0.003(3) C16 0.036(5) 0.070(6) 0.063(6) 0.019(5) -0.006(4) -0.003(4) C17 0.062(6) 0.084(8) 0.088(8) 0.043(7) -0.011(6) 0.003(6) C18 0.044(5) 0.054(5) 0.056(6) -0.003(4) 0.000(4) -0.011(4) C19 0.081(7) 0.064(6) 0.073(7) -0.019(6) 0.014(6) -0.022(6) C20 0.055(5) 0.041(5) 0.063(6) 0.009(4) -0.006(4) -0.009(4) C21 0.088(8) 0.061(7) 0.096(9) 0.031(7) -0.013(7) 0.000(6) C22 0.061(6) 0.072(7) 0.060(6) 0.002(5) 0.008(5) 0.000(5) C23 0.145(12) 0.079(8) 0.060(7) -0.008(6) 0.013(8) -0.005(8) C12B 0.13(2) 0.072(15) 0.038(11) -0.011(10) -0.016(12) 0.024(15) C11B 0.10(2) 0.11(2) 0.063(15) 0.006(14) 0.002(14) 0.018(16) C7B 0.10(2) 0.15(3) 0.19(4) -0.10(3) -0.09(3) 0.02(3) C10B 0.12(2) 0.16(3) 0.09(2) -0.09(2) -0.055(19) 0.08(2) C13B 0.26(5) 0.13(3) 0.022(13) -0.045(17) -0.04(2) 0.11(3) C9B 0.10(3) 0.14(3) 0.09(2) 0.01(2) -0.019(18) -0.06(2) C15B 0.25(5) 0.12(3) 0.08(2) -0.01(2) 0.04(3) -0.03(3) C8B 0.11(3) 0.30(5) 0.11(2) -0.02(3) -0.06(2) -0.06(3) C14B 0.21(4) 0.11(3) 0.13(3) 0.00(2) -0.05(3) 0.09(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.753(6) . ? W1 O2 1.902(6) . ? W1 S3 2.153(3) . ? W1 S1 2.416(2) . ? W1 S2 2.466(2) . ? Si1 O2 1.615(7) . ? Si1 C7 1.72(2) . ? Si1 C10B 1.75(2) . ? Si1 C13 1.79(3) . ? Si1 C13B 1.83(3) . ? Si1 C10 2.11(2) . ? Si1 C7B 2.22(4) . ? S1 C1 1.744(9) . ? S2 C2 1.744(9) . ? C1 C2 1.407(12) . ? C1 C6 1.412(12) . ? C2 C3 1.398(11) . ? C3 C4 1.381(14) . ? C4 C5 1.367(16) . ? C5 C6 1.360(14) . ? C7 C9 1.34(4) . ? C7 C8 1.55(3) . ? C10 C11 1.52(4) . ? C10 C12 1.57(3) . ? C13 C14 1.49(3) . ? C13 C15 1.53(4) . ? N1 C20 1.507(10) . ? N1 C18 1.510(10) . ? N1 C16 1.511(10) . ? N1 C22 1.520(11) . ? C16 C17 1.513(13) . ? C18 C19 1.502(13) . ? C20 C21 1.518(13) . ? C22 C23 1.514(15) . ? C12B C10B 1.51(3) . ? C11B C10B 1.40(3) . ? C7B C9B 1.42(5) . ? C7B C8B 1.58(4) . ? C13B C15B 1.46(6) . ? C13B C14B 1.52(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 O1 W1 O2 105.1(3) . . ? O1 W1 S3 106.9(2) . . ? O2 W1 S3 101.1(2) . . ? O1 W1 S1 101.5(3) . . ? O2 W1 S1 149.5(2) . . ? S3 W1 S1 84.88(9) . . ? O1 W1 S2 108.5(2) . . ? O2 W1 S2 77.5(2) . . ? S3 W1 S2 143.57(10) . . ? S1 W1 S2 80.23(7) . . ? O2 Si1 C7 109.5(9) . . ? O2 Si1 C10B 112.5(9) . . ? C7 Si1 C10B 52.0(16) . . ? O2 Si1 C13 102.4(9) . . ? C7 Si1 C13 131.9(15) . . ? C10B Si1 C13 140.3(14) . . ? O2 Si1 C13B 118.5(11) . . ? C7 Si1 C13B 130.6(16) . . ? C10B Si1 C13B 114.1(16) . . ? C13 Si1 C13B 27.5(12) . . ? O2 Si1 C10 98.9(8) . . ? C7 Si1 C10 107.4(15) . . ? C10B Si1 C10 55.5(16) . . ? C13 Si1 C10 101.9(12) . . ? C13B Si1 C10 77.3(19) . . ? O2 Si1 C7B 100.6(10) . . ? C7 Si1 C7B 59.4(16) . . ? C10B Si1 C7B 110.0(17) . . ? C13 Si1 C7B 80.4(14) . . ? C13B Si1 C7B 99(2) . . ? C10 Si1 C7B 159.3(11) . . ? C1 S1 W1 108.2(3) . . ? C2 S2 W1 108.1(3) . . ? Si1 O2 W1 159.7(4) . . ? C2 C1 C6 118.6(8) . . ? C2 C1 S1 120.7(6) . . ? C6 C1 S1 120.4(8) . . ? C3 C2 C1 119.3(8) . . ? C3 C2 S2 121.7(7) . . ? C1 C2 S2 119.0(6) . . ? C4 C3 C2 119.9(10) . . ? C5 C4 C3 121.0(10) . . ? C6 C5 C4 120.4(10) . . ? C5 C6 C1 120.7(10) . . ? C9 C7 C8 112(3) . . ? C9 C7 Si1 112(3) . . ? C8 C7 Si1 111(2) . . ? C11 C10 C12 113(3) . . ? C11 C10 Si1 112(2) . . ? C12 C10 Si1 113.7(16) . . ? C14 C13 C15 111(2) . . ? C14 C13 Si1 115(2) . . ? C15 C13 Si1 105(2) . . ? C20 N1 C18 111.7(7) . . ? C20 N1 C16 105.8(6) . . ? C18 N1 C16 110.6(7) . . ? C20 N1 C22 111.8(7) . . ? C18 N1 C22 106.0(6) . . ? C16 N1 C22 111.0(7) . . ? N1 C16 C17 116.7(7) . . ? C19 C18 N1 115.3(7) . . ? N1 C20 C21 115.1(8) . . ? C23 C22 N1 114.2(9) . . ? C9B C7B C8B 110(3) . . ? C9B C7B Si1 112(2) . . ? C8B C7B Si1 108(3) . . ? C11B C10B C12B 117(2) . . ? C11B C10B Si1 117.2(18) . . ? C12B C10B Si1 122(2) . . ? C15B C13B C14B 104(4) . . ? C15B C13B Si1 106(3) . . ? C14B C13B Si1 116(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 O1 W1 S1 C1 -90.6(4) . . . . ? O2 W1 S1 C1 59.9(5) . . . . ? S3 W1 S1 C1 163.2(3) . . . . ? S2 W1 S1 C1 16.6(3) . . . . ? O1 W1 S2 C2 84.4(4) . . . . ? O2 W1 S2 C2 -173.7(4) . . . . ? S3 W1 S2 C2 -81.9(3) . . . . ? S1 W1 S2 C2 -14.6(3) . . . . ? C7 Si1 O2 W1 160.4(19) . . . . ? C10B Si1 O2 W1 105(2) . . . . ? C13 Si1 O2 W1 -56.1(17) . . . . ? C13B Si1 O2 W1 -32(3) . . . . ? C10 Si1 O2 W1 48.3(16) . . . . ? C7B Si1 O2 W1 -138.5(17) . . . . ? O1 W1 O2 Si1 -65.7(14) . . . . ? S3 W1 O2 Si1 45.4(14) . . . . ? S1 W1 O2 Si1 144.3(11) . . . . ? S2 W1 O2 Si1 -171.8(14) . . . . ? W1 S1 C1 C2 -17.6(7) . . . . ? W1 S1 C1 C6 168.4(6) . . . . ? C6 C1 C2 C3 -2.7(12) . . . . ? S1 C1 C2 C3 -176.8(6) . . . . ? C6 C1 C2 S2 179.2(6) . . . . ? S1 C1 C2 S2 5.1(9) . . . . ? W1 S2 C2 C3 -168.1(6) . . . . ? W1 S2 C2 C1 9.9(7) . . . . ? C1 C2 C3 C4 1.8(12) . . . . ? S2 C2 C3 C4 179.9(7) . . . . ? C2 C3 C4 C5 -1.1(15) . . . . ? C3 C4 C5 C6 1.3(17) . . . . ? C4 C5 C6 C1 -2.3(16) . . . . ? C2 C1 C6 C5 3.0(13) . . . . ? S1 C1 C6 C5 177.1(8) . . . . ? O2 Si1 C7 C9 65(3) . . . . ? C10B Si1 C7 C9 168(3) . . . . ? C13 Si1 C7 C9 -64(3) . . . . ? C13B Si1 C7 C9 -101(3) . . . . ? C10 Si1 C7 C9 171(3) . . . . ? C7B Si1 C7 C9 -26(3) . . . . ? O2 Si1 C7 C8 -171(2) . . . . ? C10B Si1 C7 C8 -67(3) . . . . ? C13 Si1 C7 C8 61(4) . . . . ? C13B Si1 C7 C8 24(4) . . . . ? C10 Si1 C7 C8 -64(3) . . . . ? C7B Si1 C7 C8 98(3) . . . . ? O2 Si1 C10 C11 68(2) . . . . ? C7 Si1 C10 C11 -45(2) . . . . ? C10B Si1 C10 C11 -43(2) . . . . ? C13 Si1 C10 C11 173(2) . . . . ? C13B Si1 C10 C11 -174(2) . . . . ? C7B Si1 C10 C11 -92(4) . . . . ? O2 Si1 C10 C12 -61.5(19) . . . . ? C7 Si1 C10 C12 -175.3(18) . . . . ? C10B Si1 C10 C12 -173(2) . . . . ? C13 Si1 C10 C12 43(2) . . . . ? C13B Si1 C10 C12 56(2) . . . . ? C7B Si1 C10 C12 138(4) . . . . ? O2 Si1 C13 C14 167(2) . . . . ? C7 Si1 C13 C14 -62(3) . . . . ? C10B Si1 C13 C14 15(4) . . . . ? C13B Si1 C13 C14 37(4) . . . . ? C10 Si1 C13 C14 65(3) . . . . ? C7B Si1 C13 C14 -94(3) . . . . ? O2 Si1 C13 C15 -70.9(19) . . . . ? C7 Si1 C13 C15 60(3) . . . . ? C10B Si1 C13 C15 138(3) . . . . ? C13B Si1 C13 C15 160(5) . . . . ? C10 Si1 C13 C15 -173.0(19) . . . . ? C7B Si1 C13 C15 28(2) . . . . ? C20 N1 C16 C17 176.7(9) . . . . ? C18 N1 C16 C17 -62.2(11) . . . . ? C22 N1 C16 C17 55.2(11) . . . . ? C20 N1 C18 C19 54.1(10) . . . . ? C16 N1 C18 C19 -63.5(10) . . . . ? C22 N1 C18 C19 176.0(8) . . . . ? C18 N1 C20 C21 56.8(11) . . . . ? C16 N1 C20 C21 177.3(9) . . . . ? C22 N1 C20 C21 -61.7(11) . . . . ? C20 N1 C22 C23 -58.7(11) . . . . ? C18 N1 C22 C23 179.3(9) . . . . ? C16 N1 C22 C23 59.2(11) . . . . ? O2 Si1 C7B C9B -57(3) . . . . ? C7 Si1 C7B C9B 50(3) . . . . ? C10B Si1 C7B C9B 62(3) . . . . ? C13 Si1 C7B C9B -158(3) . . . . ? C13B Si1 C7B C9B -178(3) . . . . ? C10 Si1 C7B C9B 104(4) . . . . ? O2 Si1 C7B C8B -178(3) . . . . ? C7 Si1 C7B C8B -72(3) . . . . ? C10B Si1 C7B C8B -59(3) . . . . ? C13 Si1 C7B C8B 81(3) . . . . ? C13B Si1 C7B C8B 61(3) . . . . ? C10 Si1 C7B C8B -17(6) . . . . ? O2 Si1 C10B C11B -6(4) . . . . ? C7 Si1 C10B C11B -104(4) . . . . ? C13 Si1 C10B C11B 143(3) . . . . ? C13B Si1 C10B C11B 132(4) . . . . ? C10 Si1 C10B C11B 79(3) . . . . ? C7B Si1 C10B C11B -117(3) . . . . ? O2 Si1 C10B C12B -163(3) . . . . ? C7 Si1 C10B C12B 99(3) . . . . ? C13 Si1 C10B C12B -14(5) . . . . ? C13B Si1 C10B C12B -25(4) . . . . ? C10 Si1 C10B C12B -78(4) . . . . ? C7B Si1 C10B C12B 85(4) . . . . ? O2 Si1 C13B C15B 62(2) . . . . ? C7 Si1 C13B C15B -134(3) . . . . ? C10B Si1 C13B C15B -74(3) . . . . ? C13 Si1 C13B C15B 121(5) . . . . ? C10 Si1 C13B C15B -31(2) . . . . ? C7B Si1 C13B C15B 169(2) . . . . ? O2 Si1 C13B C14B -52(5) . . . . ? C7 Si1 C13B C14B 112(3) . . . . ? C10B Si1 C13B C14B 172(3) . . . . ? C13 Si1 C13B C14B 7(3) . . . . ? C10 Si1 C13B C14B -146(4) . . . . ? C7B Si1 C13B C14B 55(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.606 _refine_diff_density_min -1.682 _refine_diff_density_rms 0.119 #=========================================END data_jjw129p21overn _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H48 Mo2 N2 O2 S6' _chemical_formula_weight 828.92 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' 0.0000 0.0000 '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 0.0060 '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' 'Mo' 'Mo' -1.6832 0.6857 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'P21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3100(19) _cell_length_b 12.180(2) _cell_length_c 15.660(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.48(3) _cell_angle_gamma 90.00 _cell_volume 1775.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'blocks' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.550 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_absorpt_coefficient_mu 1.087 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7364 _exptl_absorpt_correction_T_max 0.8120 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9754 _diffrn_reflns_av_R_equivalents 0.0262 _diffrn_reflns_av_sigmaI/netI 0.0286 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3123 _reflns_number_gt 2844 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material 'SHELXTL (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1012P)^2^+8.7273P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3123 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.2110 _refine_ls_wR_factor_gt 0.2070 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.213 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Mo1 Mo 1.00360(7) 0.58335(6) 0.06618(4) 0.0397(3) Uani 1 1 d . . . S2 S 1.0280(2) 0.77649(18) 0.03473(15) 0.0498(6) Uani 1 1 d . . . S3 S 0.8632(3) 0.42748(19) 0.05712(17) 0.0559(6) Uani 1 1 d . . . S1 S 0.7887(3) 0.6491(2) 0.13293(16) 0.0539(6) Uani 1 1 d . . . N1 N 0.3922(7) 0.2634(5) 0.1305(4) 0.0371(14) Uani 1 1 d . . . O1 O 1.1213(7) 0.5557(5) 0.1467(4) 0.0605(18) Uani 1 1 d . . . C1 C 0.8000(10) 0.7926(7) 0.1429(6) 0.051(2) Uani 1 1 d . . . C2 C 0.9071(9) 0.8474(7) 0.0997(5) 0.046(2) Uani 1 1 d . . . C6 C 0.7000(12) 0.8469(10) 0.1928(6) 0.067(3) Uani 1 1 d . . . H6 H 0.6279 0.8085 0.2207 0.080 Uiso 1 1 calc R . . C3 C 0.9108(12) 0.9607(8) 0.1066(7) 0.064(3) Uani 1 1 d . . . H3 H 0.9798 1.0003 0.0770 0.077 Uiso 1 1 calc R . . C11 C 0.3537(11) 0.3742(9) 0.0922(7) 0.066(3) Uani 1 1 d . . . H11A H 0.2539 0.3900 0.1045 0.079 Uiso 1 1 calc R . . H11B H 0.3633 0.3699 0.0307 0.079 Uiso 1 1 calc R . . C5 C 0.7107(13) 0.9612(10) 0.2000(7) 0.073(3) Uani 1 1 d . . . H5 H 0.6468 0.9990 0.2346 0.088 Uiso 1 1 calc R . . C13 C 0.3782(14) 0.2658(11) 0.2263(7) 0.080(3) Uani 1 1 d . . . H13A H 0.4415 0.3223 0.2489 0.096 Uiso 1 1 calc R . . H13B H 0.4104 0.1959 0.2491 0.096 Uiso 1 1 calc R . . C9 C 0.5468(11) 0.2346(10) 0.1107(8) 0.076(3) Uani 1 1 d . . . H9A H 0.5715 0.1651 0.1372 0.092 Uiso 1 1 calc R . . H9B H 0.6101 0.2905 0.1340 0.092 Uiso 1 1 calc R . . C7 C 0.2925(12) 0.1802(9) 0.0911(8) 0.074(3) Uani 1 1 d . . . H7A H 0.3038 0.1817 0.0296 0.089 Uiso 1 1 calc R . . H7B H 0.1942 0.2007 0.1035 0.089 Uiso 1 1 calc R . . C4 C 0.8112(13) 1.0166(9) 0.1578(7) 0.071(3) Uani 1 1 d . . . H4 H 0.8155 1.0926 0.1623 0.085 Uiso 1 1 calc R . . C14 C 0.2247(14) 0.2880(11) 0.2579(7) 0.083(4) Uani 1 1 d . . . H14A H 0.1853 0.3500 0.2280 0.124 Uiso 1 1 calc R . . H14B H 0.2273 0.3032 0.3180 0.124 Uiso 1 1 calc R . . H14C H 0.1659 0.2247 0.2473 0.124 Uiso 1 1 calc R . . C10 C 0.5681(15) 0.2262(12) 0.0107(9) 0.100(5) Uani 1 1 d . . . H10A H 0.5235 0.1604 -0.0102 0.150 Uiso 1 1 calc R . . H10B H 0.6689 0.2245 -0.0018 0.150 Uiso 1 1 calc R . . H10C H 0.5249 0.2888 -0.0166 0.150 Uiso 1 1 calc R . . C12 C 0.4459(14) 0.4689(9) 0.1252(10) 0.086(4) Uani 1 1 d . . . H12A H 0.3995 0.5029 0.1729 0.129 Uiso 1 1 calc R . . H12B H 0.4582 0.5220 0.0805 0.129 Uiso 1 1 calc R . . H12C H 0.5381 0.4414 0.1429 0.129 Uiso 1 1 calc R . . C8 C 0.3193(14) 0.0627(9) 0.1232(10) 0.084(4) Uani 1 1 d . . . H8A H 0.4155 0.0409 0.1096 0.126 Uiso 1 1 calc R . . H8B H 0.2524 0.0135 0.0961 0.126 Uiso 1 1 calc R . . H8C H 0.3066 0.0602 0.1840 0.126 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Mo1 0.0402(4) 0.0433(5) 0.0354(4) -0.0085(3) -0.0068(3) 0.0089(3) S2 0.0496(12) 0.0469(12) 0.0529(12) -0.0023(10) 0.0010(10) 0.0066(9) S3 0.0566(14) 0.0513(13) 0.0600(14) -0.0128(11) 0.0177(11) -0.0023(10) S1 0.0493(12) 0.0573(14) 0.0553(13) -0.0054(11) 0.0095(10) 0.0059(10) N1 0.034(3) 0.043(4) 0.034(3) 0.006(3) -0.011(3) 0.002(3) O1 0.070(4) 0.058(4) 0.053(4) -0.018(3) -0.028(3) 0.023(3) C1 0.059(5) 0.048(5) 0.045(5) -0.004(4) -0.010(4) 0.016(4) C2 0.050(5) 0.055(5) 0.035(4) -0.004(4) -0.013(4) 0.012(4) C6 0.069(6) 0.080(7) 0.051(5) -0.014(5) -0.008(5) 0.022(5) C3 0.077(7) 0.051(5) 0.065(6) -0.007(5) -0.007(5) 0.011(5) C11 0.059(6) 0.069(6) 0.070(7) 0.021(5) -0.003(5) 0.016(5) C5 0.075(7) 0.077(7) 0.067(7) -0.025(6) 0.002(6) 0.032(6) C13 0.101(9) 0.080(8) 0.058(6) 0.010(6) -0.022(6) 0.005(7) C9 0.053(6) 0.072(7) 0.105(9) 0.011(7) -0.007(6) 0.013(5) C7 0.063(6) 0.076(8) 0.083(8) -0.010(6) -0.017(6) -0.012(6) C4 0.083(8) 0.052(6) 0.077(7) -0.017(5) -0.016(6) 0.026(6) C14 0.088(8) 0.103(9) 0.058(6) 0.001(6) 0.027(6) 0.027(7) C10 0.097(10) 0.087(9) 0.116(11) -0.028(8) 0.058(9) -0.007(7) C12 0.078(8) 0.052(6) 0.128(11) 0.012(7) 0.018(7) -0.009(6) C8 0.084(8) 0.055(6) 0.113(10) -0.003(6) -0.009(7) -0.009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Mo1 O1 1.697(6) . ? Mo1 S3 2.307(3) 3_765 ? Mo1 S3 2.308(3) . ? Mo1 S1 2.402(2) . ? Mo1 S2 2.415(2) . ? Mo1 Mo1 2.9018(13) 3_765 ? S2 C2 1.751(9) . ? S3 Mo1 2.307(3) 3_765 ? S1 C1 1.758(9) . ? N1 C7 1.503(12) . ? N1 C13 1.506(13) . ? N1 C9 1.516(12) . ? N1 C11 1.519(11) . ? C1 C2 1.381(13) . ? C1 C6 1.388(13) . ? C2 C3 1.385(14) . ? C6 C5 1.400(17) . ? C3 C4 1.407(15) . ? C11 C12 1.525(17) . ? C5 C4 1.333(17) . ? C13 C14 1.540(17) . ? C9 C10 1.584(18) . ? C7 C8 1.537(16) . ? 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 O1 Mo1 S3 105.2(3) . 3_765 ? O1 Mo1 S3 104.1(3) . . ? S3 Mo1 S3 102.10(8) 3_765 . ? O1 Mo1 S1 106.1(2) . . ? S3 Mo1 S1 146.99(10) 3_765 . ? S3 Mo1 S1 80.08(9) . . ? O1 Mo1 S2 106.5(2) . . ? S3 Mo1 S2 80.38(8) 3_765 . ? S3 Mo1 S2 147.44(9) . . ? S1 Mo1 S2 81.02(8) . . ? O1 Mo1 Mo1 113.8(2) . 3_765 ? S3 Mo1 Mo1 51.07(6) 3_765 3_765 ? S3 Mo1 Mo1 51.03(6) . 3_765 ? S1 Mo1 Mo1 121.99(7) . 3_765 ? S2 Mo1 Mo1 122.52(7) . 3_765 ? C2 S2 Mo1 107.5(3) . . ? Mo1 S3 Mo1 77.90(8) 3_765 . ? C1 S1 Mo1 108.7(3) . . ? C7 N1 C13 111.4(8) . . ? C7 N1 C9 110.1(8) . . ? C13 N1 C9 107.4(8) . . ? C7 N1 C11 107.1(7) . . ? C13 N1 C11 110.7(8) . . ? C9 N1 C11 110.2(7) . . ? C2 C1 C6 122.4(9) . . ? C2 C1 S1 118.7(7) . . ? C6 C1 S1 118.9(9) . . ? C1 C2 C3 117.5(9) . . ? C1 C2 S2 121.1(7) . . ? C3 C2 S2 121.4(8) . . ? C1 C6 C5 118.1(11) . . ? C2 C3 C4 120.6(11) . . ? N1 C11 C12 114.1(9) . . ? C4 C5 C6 120.9(10) . . ? N1 C13 C14 114.3(9) . . ? N1 C9 C10 110.1(9) . . ? N1 C7 C8 113.3(9) . . ? C5 C4 C3 120.5(10) . . ? 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 O1 Mo1 S2 C2 -89.7(4) . . . . ? S3 Mo1 S2 C2 167.2(3) 3_765 . . . ? S3 Mo1 S2 C2 69.7(3) . . . . ? S1 Mo1 S2 C2 14.6(3) . . . . ? Mo1 Mo1 S2 C2 136.9(3) 3_765 . . . ? O1 Mo1 S3 Mo1 -109.3(2) . . . 3_765 ? S3 Mo1 S3 Mo1 0.0 3_765 . . 3_765 ? S1 Mo1 S3 Mo1 146.42(10) . . . 3_765 ? S2 Mo1 S3 Mo1 91.04(15) . . . 3_765 ? O1 Mo1 S1 C1 90.3(4) . . . . ? S3 Mo1 S1 C1 -70.8(4) 3_765 . . . ? S3 Mo1 S1 C1 -167.7(3) . . . . ? S2 Mo1 S1 C1 -14.4(3) . . . . ? Mo1 Mo1 S1 C1 -137.3(3) 3_765 . . . ? Mo1 S1 C1 C2 12.0(7) . . . . ? Mo1 S1 C1 C6 -168.9(7) . . . . ? C6 C1 C2 C3 -1.0(13) . . . . ? S1 C1 C2 C3 178.0(7) . . . . ? C6 C1 C2 S2 -178.0(7) . . . . ? S1 C1 C2 S2 1.1(10) . . . . ? Mo1 S2 C2 C1 -13.4(7) . . . . ? Mo1 S2 C2 C3 169.8(7) . . . . ? C2 C1 C6 C5 -0.9(14) . . . . ? S1 C1 C6 C5 180.0(8) . . . . ? C1 C2 C3 C4 1.9(14) . . . . ? S2 C2 C3 C4 178.8(8) . . . . ? C7 N1 C11 C12 -179.7(10) . . . . ? C13 N1 C11 C12 58.8(12) . . . . ? C9 N1 C11 C12 -59.9(12) . . . . ? C1 C6 C5 C4 2.2(16) . . . . ? C7 N1 C13 C14 -56.3(13) . . . . ? C9 N1 C13 C14 -176.9(10) . . . . ? C11 N1 C13 C14 62.7(13) . . . . ? C7 N1 C9 C10 56.5(12) . . . . ? C13 N1 C9 C10 177.9(9) . . . . ? C11 N1 C9 C10 -61.4(12) . . . . ? C13 N1 C7 C8 -59.3(13) . . . . ? C9 N1 C7 C8 59.7(13) . . . . ? C11 N1 C7 C8 179.5(10) . . . . ? C6 C5 C4 C3 -1.4(17) . . . . ? C2 C3 C4 C5 -0.7(16) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.004 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.178 #==========================================END data_stas54 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H115 N5 O2.50 S10 W2.50' _chemical_formula_weight 1606.69 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' 0.0000 0.0000 '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 0.0060 '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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.9822(9) _cell_length_b 17.7957(9) _cell_length_c 41.0856(19) _cell_angle_alpha 90.00 _cell_angle_beta 103.2160(10) _cell_angle_gamma 90.00 _cell_volume 14223.0(12) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'plate' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6520 _exptl_absorpt_coefficient_mu 4.367 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4081 _exptl_absorpt_correction_T_max 0.6692 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39849 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -48 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12507 _reflns_number_gt 8939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2001)' _computing_cell_refinement 'SMART (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Bruker, 2000)' _computing_publication_material 'SHELXTL (Bruker, 2000)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1097P)^2^+91.9962P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12507 _refine_ls_number_parameters 664 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0901 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1921 _refine_ls_wR_factor_gt 0.1707 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S7 S 0.84619(19) 0.1822(2) 0.44605(8) 0.0816(9) Uani 1 1 d . . . W2 W 0.82481(2) 0.08522(3) 0.412389(11) 0.06172(17) Uani 1 1 d . . . W1 W 0.81694(2) 0.61948(3) 0.424428(10) 0.05573(16) Uani 1 1 d . . . W3 W 0.99444(7) 0.26679(5) 0.25724(2) 0.0489(3) Uani 0.50 1 d P . . S6 S 0.83505(15) 0.08774(18) 0.35417(7) 0.0639(7) Uani 1 1 d . . . S2 S 0.77704(15) 0.59683(18) 0.36385(7) 0.0647(7) Uani 1 1 d . . . S8 S 0.92685(18) 0.0305(2) 0.41657(9) 0.0932(12) Uani 1 1 d . . . S5 S 0.71072(18) 0.1346(3) 0.38166(9) 0.0924(12) Uani 1 1 d . . . S4 S 0.74621(15) 0.52490(19) 0.42755(7) 0.0688(8) Uani 1 1 d . . . S3 S 0.89760(17) 0.6101(2) 0.47149(9) 0.0903(11) Uani 1 1 d . . . S11 S 0.9331(2) 0.3734(2) 0.26280(8) 0.0825(10) Uani 1 1 d . . . S1 S 0.9185(2) 0.6498(3) 0.40288(11) 0.1126(16) Uani 1 1 d . . . S10 S 0.9432(4) 0.1952(3) 0.26935(19) 0.0748(17) Uani 0.50 1 d P . . S9 S 0.8918(4) 0.2120(4) 0.2466(2) 0.090(2) Uani 0.50 1 d P . . C3 C 0.7586(6) 0.1185(7) 0.3274(3) 0.070(3) Uani 1 1 d . . . C5 C 0.7603(7) 0.1175(9) 0.2902(3) 0.090(4) Uani 1 1 d . . . H5A H 0.7195 0.1431 0.2772 0.135 Uiso 1 1 calc R . . H5B H 0.7607 0.0654 0.2826 0.135 Uiso 1 1 calc R . . H5C H 0.8017 0.1433 0.2871 0.135 Uiso 1 1 calc R . . C4 C 0.7053(6) 0.1403(8) 0.3392(3) 0.075(4) Uani 1 1 d . . . C1 C 0.8369(9) 0.6330(8) 0.3425(3) 0.085(4) Uani 1 1 d . . . C2 C 0.8112(9) 0.6285(9) 0.3045(3) 0.108(6) Uani 1 1 d . . . H2A H 0.8493 0.6389 0.2938 0.163 Uiso 1 1 calc R . . H2B H 0.7747 0.6656 0.2971 0.163 Uiso 1 1 calc R . . H2C H 0.7931 0.5780 0.2982 0.163 Uiso 1 1 calc R . . N6 N 0.8508(5) 0.3534(5) 0.3534(2) 0.058(2) Uani 1 1 d . . . O1 O 0.7750(4) 0.7033(5) 0.42860(18) 0.074(2) Uani 1 1 d . . . N3 N 0.8922(5) 0.8645(5) 0.5023(2) 0.056(2) Uani 1 1 d . . . O2 O 0.7788(5) 0.0205(5) 0.4300(2) 0.090(3) Uani 1 1 d . . . N5 N 0.7139(6) 0.8649(6) 0.3475(2) 0.073(3) Uani 1 1 d . . . N4 N 0.8690(5) 0.3888(6) 0.5208(2) 0.069(3) Uani 1 1 d . . . C7 C 0.9705(6) 0.4586(6) 0.2550(3) 0.065(3) Uani 1 1 d . . . C14 C 0.8013(7) 0.4177(9) 0.5032(4) 0.096(4) Uani 1 1 d . . . H14A H 0.7782 0.4397 0.5199 0.116 Uiso 1 1 calc R . . H14B H 0.8084 0.4586 0.4880 0.116 Uiso 1 1 calc R . . C12 C 0.9091(9) 0.3474(10) 0.5006(3) 0.102(5) Uani 1 1 d . . . H12A H 0.8851 0.2997 0.4929 0.122 Uiso 1 1 calc R . . H12B H 0.9545 0.3344 0.5150 0.122 Uiso 1 1 calc R . . C22 C 0.7481(8) 0.3417(9) 0.3797(4) 0.100(5) Uani 1 1 d . . . H22A H 0.7594 0.3946 0.3849 0.150 Uiso 1 1 calc R . . H22B H 0.7365 0.3174 0.3991 0.150 Uiso 1 1 calc R . . H22C H 0.7088 0.3384 0.3605 0.150 Uiso 1 1 calc R . . C11 C 0.9617(8) 0.8249(11) 0.4605(4) 0.111(5) Uani 1 1 d . . . H11A H 0.9937 0.8604 0.4742 0.167 Uiso 1 1 calc R . . H11B H 0.9514 0.8415 0.4371 0.167 Uiso 1 1 calc R . . H11C H 0.9825 0.7748 0.4621 0.167 Uiso 1 1 calc R . . C15 C 0.7560(10) 0.3624(9) 0.4839(4) 0.108(5) Uani 1 1 d . . . H15A H 0.7820 0.3311 0.4715 0.162 Uiso 1 1 calc R . . H15B H 0.7188 0.3880 0.4681 0.162 Uiso 1 1 calc R . . H15C H 0.7366 0.3308 0.4989 0.162 Uiso 1 1 calc R . . C24 C 0.7640(11) 0.3349(15) 0.2987(5) 0.153(9) Uani 1 1 d . . . H24A H 0.7913 0.2953 0.2914 0.230 Uiso 1 1 calc R . . H24B H 0.7424 0.3661 0.2796 0.230 Uiso 1 1 calc R . . H24C H 0.7284 0.3119 0.3084 0.230 Uiso 1 1 calc R . . C8 C 0.9338(9) 0.5287(8) 0.2627(4) 0.104(5) Uani 1 1 d . . . H8A H 0.9570 0.5732 0.2565 0.157 Uiso 1 1 calc R . . H8B H 0.9347 0.5303 0.2866 0.157 Uiso 1 1 calc R . . H8C H 0.8860 0.5278 0.2498 0.157 Uiso 1 1 calc R . . C23 C 0.8065(9) 0.3792(16) 0.3227(4) 0.164(11) Uani 1 1 d . . . H23A H 0.7762 0.4175 0.3293 0.197 Uiso 1 1 calc R . . H23B H 0.8367 0.4066 0.3107 0.197 Uiso 1 1 calc R . . C13 C 0.9206(8) 0.3901(10) 0.4702(3) 0.104(5) Uani 1 1 d . . . H13A H 0.8861 0.3746 0.4503 0.157 Uiso 1 1 calc R . . H13B H 0.9667 0.3790 0.4669 0.157 Uiso 1 1 calc R . . H13C H 0.9164 0.4442 0.4737 0.157 Uiso 1 1 calc R . . C20 C 0.9543(8) 0.2677(10) 0.3678(4) 0.117(6) Uani 1 1 d . . . H20A H 0.9620 0.2974 0.3884 0.176 Uiso 1 1 calc R . . H20B H 0.9974 0.2636 0.3604 0.176 Uiso 1 1 calc R . . H20C H 0.9382 0.2174 0.3721 0.176 Uiso 1 1 calc R . . C21 C 0.8093(9) 0.3025(10) 0.3715(4) 0.112(6) Uani 1 1 d . . . H21A H 0.7929 0.2583 0.3572 0.135 Uiso 1 1 calc R . . H21B H 0.8397 0.2841 0.3925 0.135 Uiso 1 1 calc R . . C9 C 0.8973(10) 0.6542(10) 0.3595(4) 0.110(6) Uani 1 1 d . . . O3 O 1.0319(10) 0.2561(9) 0.2995(3) 0.082(5) Uani 0.50 1 d P . . C18 C 0.6784(10) 0.9372(11) 0.3490(7) 0.153(8) Uani 1 1 d . . . H18A H 0.6840 0.9520 0.3727 0.184 Uiso 1 1 calc R . . H18B H 0.7003 0.9764 0.3378 0.184 Uiso 1 1 calc R . . C19 C 0.9029(9) 0.3042(10) 0.3421(4) 0.109(5) Uani 1 1 d . . . H19A H 0.8775 0.2647 0.3273 0.131 Uiso 1 1 calc R . . H19B H 0.9271 0.3353 0.3285 0.131 Uiso 1 1 calc R . . C10 C 0.8941(13) 0.8219(13) 0.4730(5) 0.157(9) Uani 1 1 d . . . H10A H 0.8561 0.8394 0.4547 0.188 Uiso 1 1 calc R . . H10B H 0.8847 0.7687 0.4775 0.188 Uiso 1 1 calc R . . C17 C 0.6801(10) 0.8064(11) 0.3661(5) 0.131(7) Uani 1 1 d . . . H17A H 0.7080 0.7599 0.3695 0.157 Uiso 1 1 calc R . . H17B H 0.6337 0.7937 0.3527 0.157 Uiso 1 1 calc R . . C25 C 0.8846(11) 0.4158(11) 0.3731(5) 0.130(7) Uani 1 1 d . . . H25A H 0.8477 0.4507 0.3758 0.156 Uiso 1 1 calc R . . H25B H 0.9050 0.3954 0.3956 0.156 Uiso 1 1 calc R . . C16 C 0.7839(11) 0.8749(19) 0.3665(6) 0.200(14) Uani 1 1 d . . . H16A H 0.7995 0.9211 0.3571 0.239 Uiso 1 1 calc R . . H16B H 0.7787 0.8890 0.3891 0.239 Uiso 1 1 calc R . . N7 N 0.0538(5) 0.0251(7) 0.3351(3) 0.081(3) Uani 1 1 d . . . C31 C 0.7630(7) 0.8612(11) 0.4872(4) 0.119(6) Uani 1 1 d . . . H31A H 0.7652 0.9082 0.4750 0.178 Uiso 1 1 calc R . . H31B H 0.7245 0.8635 0.4983 0.178 Uiso 1 1 calc R . . H31C H 0.7562 0.8190 0.4715 0.178 Uiso 1 1 calc R . . C26 C 0.8526(10) 0.3389(11) 0.5474(4) 0.117(6) Uani 1 1 d . . . H26A H 0.8480 0.3731 0.5658 0.141 Uiso 1 1 calc R . . H26B H 0.8059 0.3193 0.5379 0.141 Uiso 1 1 calc R . . C28 C 0.9167(8) 0.4503(11) 0.5387(4) 0.112(6) Uani 1 1 d . . . H28A H 0.9602 0.4259 0.5503 0.135 Uiso 1 1 calc R . . H28B H 0.9277 0.4836 0.5213 0.135 Uiso 1 1 calc R . . C42 C 0.6384(7) 0.1694(12) 0.3188(4) 0.119(6) Uani 1 1 d . . . H42A H 0.6412 0.1740 0.2954 0.178 Uiso 1 1 calc R . . H42B H 0.6288 0.2187 0.3273 0.178 Uiso 1 1 calc R . . H42C H 0.6014 0.1344 0.3205 0.178 Uiso 1 1 calc R . . C35 C 0.9604(9) 0.7687(9) 0.5420(4) 0.105(5) Uani 1 1 d . . . H35A H 0.9151 0.7447 0.5379 0.158 Uiso 1 1 calc R . . H35B H 0.9820 0.7667 0.5659 0.158 Uiso 1 1 calc R . . H35C H 0.9894 0.7422 0.5294 0.158 Uiso 1 1 calc R . . C33 C 0.8952(9) 1.0042(8) 0.5179(4) 0.105(5) Uani 1 1 d . . . H33A H 0.8761 1.0513 0.5074 0.158 Uiso 1 1 calc R . . H33B H 0.9426 1.0126 0.5305 0.158 Uiso 1 1 calc R . . H33C H 0.8674 0.9866 0.5332 0.158 Uiso 1 1 calc R . . C29 C 0.8935(10) 0.4986(12) 0.5635(4) 0.137(7) Uani 1 1 d . . . H29A H 0.8534 0.5279 0.5522 0.206 Uiso 1 1 calc R . . H29B H 0.9307 0.5328 0.5738 0.206 Uiso 1 1 calc R . . H29C H 0.8812 0.4670 0.5807 0.206 Uiso 1 1 calc R . . C32 C 0.8948(11) 0.9485(11) 0.4925(5) 0.130(6) Uani 1 1 d . . . H32A H 0.9364 0.9560 0.4837 0.156 Uiso 1 1 calc R . . H32B H 0.8546 0.9585 0.4739 0.156 Uiso 1 1 calc R . . C40 C 0.0876(11) 0.1207(14) 0.3831(5) 0.170(11) Uani 1 1 d . . . H40A H 0.1252 0.0870 0.3935 0.255 Uiso 1 1 calc R . . H40B H 0.0536 0.1227 0.3969 0.255 Uiso 1 1 calc R . . H40C H 0.1059 0.1712 0.3812 0.255 Uiso 1 1 calc R . . C34 C 0.9517(12) 0.8554(14) 0.5300(5) 0.156(9) Uani 1 1 d . . . H34A H 0.9464 0.8875 0.5489 0.187 Uiso 1 1 calc R . . H34B H 0.9936 0.8719 0.5229 0.187 Uiso 1 1 calc R . . C30 C 0.8318(11) 0.8499(14) 0.5140(5) 0.151(8) Uani 1 1 d . . . H30A H 0.8316 0.8835 0.5332 0.181 Uiso 1 1 calc R . . H30B H 0.8337 0.7975 0.5223 0.181 Uiso 1 1 calc R . . C48 C 0.9348(12) 0.4593(12) 0.3643(6) 0.164(10) Uani 1 1 d . . . H48A H 0.9782 0.4312 0.3686 0.245 Uiso 1 1 calc R . . H48B H 0.9411 0.5055 0.3776 0.245 Uiso 1 1 calc R . . H48C H 0.9209 0.4721 0.3405 0.245 Uiso 1 1 calc R . . C43 C 0.8396(11) 0.8299(17) 0.3724(5) 0.181(11) Uani 1 1 d . . . H43A H 0.8486 0.8116 0.3955 0.271 Uiso 1 1 calc R . . H43B H 0.8795 0.8583 0.3690 0.271 Uiso 1 1 calc R . . H43C H 0.8312 0.7871 0.3570 0.271 Uiso 1 1 calc R . . C41 C 0.9562(11) 0.6793(14) 0.3455(5) 0.160(9) Uani 1 1 d . . . H41A H 0.9931 0.6419 0.3508 0.240 Uiso 1 1 calc R . . H41B H 0.9733 0.7277 0.3554 0.240 Uiso 1 1 calc R . . H41C H 0.9410 0.6847 0.3212 0.240 Uiso 1 1 calc R . . C46 C 0.7104(12) 0.827(2) 0.3164(5) 0.26(2) Uani 1 1 d . . . H46A H 0.6615 0.8205 0.3049 0.316 Uiso 1 1 calc R . . H46B H 0.7313 0.7769 0.3209 0.316 Uiso 1 1 calc R . . C45 C 0.6045(12) 0.9336(19) 0.3330(6) 0.221(16) Uani 1 1 d . . . H45A H 0.5972 0.9499 0.3096 0.332 Uiso 1 1 calc R . . H45B H 0.5790 0.9666 0.3449 0.332 Uiso 1 1 calc R . . H45C H 0.5882 0.8818 0.3337 0.332 Uiso 1 1 calc R . . C27 C 0.8868(17) 0.2829(13) 0.5617(8) 0.243(19) Uani 1 1 d . . . H27A H 0.9358 0.2907 0.5627 0.365 Uiso 1 1 calc R . . H27B H 0.8712 0.2371 0.5490 0.365 Uiso 1 1 calc R . . H27C H 0.8798 0.2777 0.5845 0.365 Uiso 1 1 calc R . . C47 C 0.7468(15) 0.870(2) 0.2935(5) 0.230(17) Uani 1 1 d . . . H47A H 0.7482 0.9236 0.2991 0.345 Uiso 1 1 calc R . . H47B H 0.7220 0.8629 0.2703 0.345 Uiso 1 1 calc R . . H47C H 0.7939 0.8509 0.2965 0.345 Uiso 1 1 calc R . . C36 C 0.0820(15) 0.0519(19) 0.3047(8) 0.26(2) Uani 1 1 d . . . H36A H 0.0412 0.0552 0.2858 0.308 Uiso 1 1 calc R . . H36B H 0.0972 0.1044 0.3100 0.308 Uiso 1 1 calc R . . C44 C 0.6741(12) 0.8391(16) 0.4012(5) 0.178(11) Uani 1 1 d . . . H44A H 0.7194 0.8377 0.4167 0.267 Uiso 1 1 calc R . . H44B H 0.6416 0.8086 0.4102 0.267 Uiso 1 1 calc R . . H44C H 0.6578 0.8911 0.3984 0.267 Uiso 1 1 calc R . . C39 C 0.061(3) 0.098(3) 0.3565(7) 0.46(5) Uani 1 1 d . . . H39A H 0.0785 0.1345 0.3419 0.554 Uiso 1 1 calc R . . H39B H 0.0129 0.1127 0.3547 0.554 Uiso 1 1 calc R . . C37 C -0.021(2) 0.013(3) 0.3260(12) 0.43(5) Uani 1 1 d . . . H37A H -0.0289 -0.0401 0.3316 0.515 Uiso 1 1 calc R . . H37B H -0.0412 0.0446 0.3410 0.515 Uiso 1 1 calc R . . C52 C -0.0602(18) 0.025(2) 0.2926(9) 0.257(16) Uiso 1 1 d . . . H52A H -0.1093 0.0258 0.2925 0.385 Uiso 1 1 calc R . . H52B H -0.0509 -0.0146 0.2779 0.385 Uiso 1 1 calc R . . H52C H -0.0474 0.0740 0.2845 0.385 Uiso 1 1 calc R . . C51 C 0.0655(10) -0.0790(14) 0.3808(5) 0.159(10) Uani 1 1 d . . . H51A H 0.0182 -0.0639 0.3805 0.239 Uiso 1 1 calc R . . H51B H 0.0953 -0.0668 0.4026 0.239 Uiso 1 1 calc R . . H51C H 0.0669 -0.1332 0.3769 0.239 Uiso 1 1 calc R . . C49 C 0.1299(12) 0.0216(13) 0.2920(4) 0.152(8) Uani 1 1 d . . . H49A H 0.1745 0.0441 0.3024 0.229 Uiso 1 1 calc R . . H49B H 0.1197 0.0306 0.2678 0.229 Uiso 1 1 calc R . . H49C H 0.1316 -0.0326 0.2963 0.229 Uiso 1 1 calc R . . C50 C 0.0908(18) -0.036(2) 0.3529(9) 0.240(15) Uiso 1 1 d . . . H50A H 0.1375 -0.0176 0.3631 0.288 Uiso 1 1 calc R . . H50B H 0.0959 -0.0742 0.3360 0.288 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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 S7 0.092(2) 0.091(2) 0.0596(18) -0.0017(16) 0.0134(17) 0.0223(19) W2 0.0651(3) 0.0771(3) 0.0473(3) 0.0115(2) 0.0217(2) 0.0175(2) W1 0.0503(3) 0.0705(3) 0.0484(3) -0.0089(2) 0.01538(19) 0.0068(2) W3 0.0573(6) 0.0530(4) 0.0372(8) 0.0033(3) 0.0124(5) -0.0012(4) S6 0.0603(16) 0.085(2) 0.0516(15) 0.0087(14) 0.0234(13) 0.0097(14) S2 0.0668(17) 0.082(2) 0.0472(15) -0.0042(13) 0.0172(13) 0.0102(15) S8 0.073(2) 0.135(3) 0.071(2) 0.007(2) 0.0168(17) 0.048(2) S5 0.070(2) 0.143(3) 0.071(2) 0.020(2) 0.0311(17) 0.038(2) S4 0.0579(16) 0.086(2) 0.0647(17) 0.0027(15) 0.0179(14) -0.0003(15) S3 0.0596(18) 0.132(3) 0.070(2) -0.026(2) -0.0048(16) 0.0142(19) S11 0.105(3) 0.088(2) 0.0674(19) -0.0156(16) 0.0466(19) -0.025(2) S1 0.076(2) 0.175(4) 0.101(3) -0.060(3) 0.051(2) -0.050(3) S10 0.077(4) 0.055(3) 0.102(5) 0.020(3) 0.042(4) -0.001(3) S9 0.073(4) 0.075(4) 0.132(7) -0.003(4) 0.042(5) -0.021(4) C3 0.065(7) 0.088(8) 0.057(7) 0.011(6) 0.017(6) 0.000(6) C5 0.080(9) 0.125(12) 0.065(8) 0.009(8) 0.015(7) 0.002(8) C4 0.060(7) 0.111(11) 0.055(7) 0.012(6) 0.014(6) 0.003(7) C1 0.123(12) 0.079(9) 0.072(9) -0.009(7) 0.061(9) 0.001(8) C2 0.153(15) 0.121(13) 0.070(9) -0.008(8) 0.063(10) 0.020(11) N6 0.072(6) 0.059(5) 0.048(5) 0.004(4) 0.024(4) 0.026(5) O1 0.090(6) 0.080(5) 0.055(4) -0.001(4) 0.021(4) 0.023(5) N3 0.056(5) 0.065(6) 0.045(5) 0.005(4) 0.009(4) 0.021(4) O2 0.083(6) 0.102(7) 0.089(6) 0.035(5) 0.028(5) 0.020(5) N5 0.090(8) 0.076(7) 0.057(6) 0.001(5) 0.022(5) 0.017(6) N4 0.065(6) 0.084(7) 0.066(6) -0.004(5) 0.028(5) 0.012(5) C7 0.087(8) 0.056(6) 0.055(6) 0.003(5) 0.022(6) 0.000(6) C14 0.081(10) 0.119(12) 0.087(10) 0.010(9) 0.016(8) 0.012(9) C12 0.105(11) 0.143(14) 0.062(8) 0.002(8) 0.028(8) 0.050(10) C22 0.104(11) 0.109(11) 0.096(10) 0.009(9) 0.043(9) 0.042(9) C11 0.096(11) 0.158(16) 0.092(11) 0.000(10) 0.046(9) 0.035(11) C15 0.136(15) 0.094(11) 0.085(10) 0.004(8) 0.009(10) -0.032(10) C24 0.126(16) 0.25(3) 0.080(12) 0.010(15) 0.027(12) 0.036(17) C8 0.151(15) 0.076(9) 0.094(10) -0.002(8) 0.043(10) 0.036(9) C23 0.076(11) 0.35(4) 0.063(10) -0.002(15) 0.009(9) 0.013(16) C13 0.118(12) 0.156(15) 0.049(7) -0.008(8) 0.037(8) 0.044(11) C20 0.097(11) 0.127(14) 0.135(14) 0.031(11) 0.042(10) 0.071(11) C21 0.143(15) 0.130(14) 0.073(9) 0.010(9) 0.045(10) 0.045(12) C9 0.138(15) 0.117(13) 0.101(12) -0.026(9) 0.080(12) -0.053(11) O3 0.119(14) 0.081(11) 0.039(8) 0.009(7) 0.004(8) 0.019(10) C18 0.111(15) 0.113(15) 0.24(3) 0.026(16) 0.047(16) -0.005(12) C19 0.104(11) 0.137(14) 0.089(10) -0.026(10) 0.027(9) 0.030(11) C10 0.22(3) 0.144(18) 0.112(15) -0.007(13) 0.054(16) 0.059(18) C17 0.127(15) 0.129(16) 0.145(17) 0.033(13) 0.049(13) 0.015(12) C25 0.146(18) 0.114(14) 0.117(14) -0.018(12) 0.005(13) 0.045(13) C16 0.099(16) 0.40(5) 0.112(17) 0.00(2) 0.045(13) 0.05(2) N7 0.050(5) 0.118(9) 0.076(7) 0.019(6) 0.012(5) 0.034(6) C31 0.062(9) 0.188(19) 0.097(11) -0.024(11) -0.001(8) 0.037(10) C26 0.144(15) 0.138(15) 0.087(11) 0.023(10) 0.063(11) 0.056(13) C28 0.089(11) 0.169(17) 0.086(10) -0.018(11) 0.034(9) 0.004(11) C42 0.068(9) 0.193(18) 0.089(10) 0.049(11) 0.005(8) 0.026(10) C35 0.114(12) 0.095(11) 0.089(10) 0.010(8) -0.013(9) 0.038(9) C33 0.136(14) 0.066(9) 0.115(12) 0.002(8) 0.029(11) 0.016(9) C29 0.118(14) 0.162(18) 0.122(14) -0.052(13) 0.006(11) 0.039(13) C32 0.133(16) 0.136(16) 0.129(15) 0.005(13) 0.046(13) 0.027(13) C40 0.138(18) 0.22(3) 0.125(17) -0.039(16) -0.027(14) 0.088(18) C34 0.15(2) 0.20(3) 0.114(16) 0.019(15) 0.029(15) -0.032(17) C30 0.121(16) 0.20(2) 0.138(18) -0.026(16) 0.048(14) -0.007(15) C48 0.17(2) 0.118(16) 0.24(3) -0.010(16) 0.13(2) -0.003(15) C43 0.097(14) 0.31(3) 0.131(17) 0.08(2) 0.026(13) 0.064(18) C41 0.140(17) 0.24(3) 0.126(15) -0.064(16) 0.087(14) -0.057(17) C46 0.14(2) 0.57(6) 0.070(12) -0.06(2) 0.011(13) 0.14(3) C45 0.120(18) 0.38(4) 0.17(2) 0.13(3) 0.038(16) 0.10(2) C27 0.36(4) 0.141(19) 0.33(4) 0.13(2) 0.28(4) 0.14(2) C47 0.18(2) 0.43(5) 0.073(13) 0.05(2) 0.015(15) -0.07(3) C36 0.24(3) 0.32(4) 0.29(3) 0.17(3) 0.23(3) 0.16(3) C44 0.17(2) 0.28(3) 0.099(14) 0.040(17) 0.055(14) 0.07(2) C39 0.77(11) 0.46(7) 0.082(18) -0.17(3) -0.06(4) 0.21(7) C37 0.29(5) 0.65(10) 0.41(6) 0.44(7) 0.21(5) 0.23(6) C51 0.122(15) 0.21(2) 0.171(19) 0.089(17) 0.092(15) 0.060(15) C49 0.19(2) 0.19(2) 0.099(13) 0.006(13) 0.082(14) 0.052(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S7 W2 2.192(4) . ? W2 O2 1.731(9) . ? W2 S8 2.231(3) . ? W2 S6 2.447(3) . ? W2 S5 2.500(3) . ? W1 O1 1.738(8) . ? W1 S4 2.220(3) . ? W1 S3 2.222(3) . ? W1 S1 2.452(3) . ? W1 S2 2.467(3) . ? W3 W3 0.6811(12) 2_755 ? W3 O3 1.738(14) . ? W3 S10 1.775(6) . ? W3 S9 2.223(7) . ? W3 S10 2.234(6) 2_755 ? W3 O3 2.278(14) 2_755 ? W3 S11 2.298(4) . ? W3 S9 2.511(7) 2_755 ? W3 S11 2.630(4) 2_755 ? S6 C3 1.754(12) . ? S2 C1 1.759(14) . ? S5 C4 1.727(12) . ? S11 C7 1.751(11) . ? S11 W3 2.630(4) 2_755 ? S1 C9 1.738(17) . ? S10 W3 2.234(6) 2_755 ? S9 W3 2.511(7) 2_755 ? C3 C4 1.326(17) . ? C3 C5 1.535(17) . ? C4 C42 1.498(17) . ? C1 C9 1.30(2) . ? C1 C2 1.53(2) . ? N6 C23 1.441(19) . ? N6 C25 1.45(2) . ? N6 C19 1.512(16) . ? N6 C21 1.533(19) . ? N3 C30 1.42(2) . ? N3 C10 1.43(2) . ? N3 C34 1.45(2) . ? N3 C32 1.55(2) . ? N5 C46 1.43(2) . ? N5 C16 1.45(2) . ? N5 C18 1.48(2) . ? N5 C17 1.54(2) . ? N4 C14 1.473(17) . ? N4 C12 1.478(15) . ? N4 C26 1.502(18) . ? N4 C28 1.52(2) . ? C7 C7 1.34(2) 2_755 ? C7 C8 1.516(16) . ? C14 C15 1.44(2) . ? C12 C13 1.53(2) . ? C22 C21 1.511(19) . ? C11 C10 1.55(3) . ? C24 C23 1.39(3) . ? C20 C19 1.45(2) . ? C9 C41 1.49(2) . ? O3 W3 2.278(14) 2_755 ? C18 C45 1.47(3) . ? C17 C44 1.58(3) . ? C25 C48 1.38(3) . ? C16 C43 1.35(3) . ? N7 C50 1.42(3) . ? N7 C37 1.47(5) . ? N7 C36 1.56(2) . ? N7 C39 1.56(3) . ? C31 C30 1.57(3) . ? C26 C27 1.27(2) . ? C28 C29 1.49(2) . ? C35 C34 1.62(3) . ? C33 C32 1.44(2) . ? C40 C39 1.17(3) . ? C46 C47 1.52(4) . ? C36 C49 1.31(2) . ? C37 C52 1.44(5) . ? C51 C50 1.55(3) . ? 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 O2 W2 S7 107.8(3) . . ? O2 W2 S8 103.9(3) . . ? S7 W2 S8 104.62(15) . . ? O2 W2 S6 126.2(3) . . ? S7 W2 S6 123.68(12) . . ? S8 W2 S6 78.70(11) . . ? O2 W2 S5 86.3(3) . . ? S7 W2 S5 93.75(14) . . ? S8 W2 S5 154.77(12) . . ? S6 W2 S5 76.72(10) . . ? O1 W1 S4 108.5(3) . . ? O1 W1 S3 104.4(3) . . ? S4 W1 S3 103.72(15) . . ? O1 W1 S1 107.7(3) . . ? S4 W1 S1 141.08(14) . . ? S3 W1 S1 80.53(16) . . ? O1 W1 S2 100.8(3) . . ? S4 W1 S2 82.60(11) . . ? S3 W1 S2 150.26(12) . . ? S1 W1 S2 76.99(12) . . ? W3 W3 O3 136.1(7) 2_755 . ? W3 W3 S10 124.7(3) 2_755 . ? O3 W3 S10 77.6(7) . . ? W3 W3 S9 107.3(3) 2_755 . ? O3 W3 S9 108.5(7) . . ? S10 W3 S9 34.4(3) . . ? W3 W3 S10 40.8(2) 2_755 2_755 ? O3 W3 S10 105.4(6) . 2_755 ? S10 W3 S10 98.6(4) . 2_755 ? S9 W3 S10 104.2(3) . 2_755 ? W3 W3 O3 31.9(5) 2_755 2_755 ? O3 W3 O3 163.7(7) . 2_755 ? S10 W3 O3 102.3(5) . 2_755 ? S9 W3 O3 76.9(5) . 2_755 ? S10 W3 O3 58.4(5) 2_755 2_755 ? W3 W3 S11 112.01(13) 2_755 . ? O3 W3 S11 96.3(6) . . ? S10 W3 S11 102.1(2) . . ? S9 W3 S11 83.9(2) . . ? S10 W3 S11 152.8(2) 2_755 . ? O3 W3 S11 99.6(5) 2_755 . ? W3 W3 S9 57.6(3) 2_755 2_755 ? O3 W3 S9 80.2(6) . 2_755 ? S10 W3 S9 109.1(3) . 2_755 ? S9 W3 S9 128.7(4) . 2_755 ? S10 W3 S9 30.0(3) 2_755 2_755 ? O3 W3 S9 84.5(5) 2_755 2_755 ? S11 W3 S9 146.9(2) . 2_755 ? W3 W3 S11 54.10(12) 2_755 2_755 ? O3 W3 S11 104.5(6) . 2_755 ? S10 W3 S11 177.9(3) . 2_755 ? S9 W3 S11 143.5(3) . 2_755 ? S10 W3 S11 81.38(18) 2_755 2_755 ? O3 W3 S11 75.8(4) 2_755 2_755 ? S11 W3 S11 77.26(15) . 2_755 ? S9 W3 S11 71.94(19) 2_755 2_755 ? C3 S6 W2 111.4(4) . . ? C1 S2 W1 110.1(6) . . ? C4 S5 W2 111.7(4) . . ? C7 S11 W3 116.0(4) . . ? C7 S11 W3 106.2(4) . 2_755 ? W3 S11 W3 13.89(3) . 2_755 ? C9 S1 W1 110.7(6) . . ? W3 S10 W3 14.52(7) . 2_755 ? W3 S9 W3 15.00(6) . 2_755 ? C4 C3 C5 124.8(11) . . ? C4 C3 S6 121.2(9) . . ? C5 C3 S6 114.0(9) . . ? C3 C4 C42 125.9(12) . . ? C3 C4 S5 118.9(10) . . ? C42 C4 S5 115.2(10) . . ? C9 C1 C2 127.9(14) . . ? C9 C1 S2 119.5(11) . . ? C2 C1 S2 112.4(13) . . ? C23 N6 C25 111.1(15) . . ? C23 N6 C19 104.1(11) . . ? C25 N6 C19 110.5(12) . . ? C23 N6 C21 108.7(13) . . ? C25 N6 C21 114.7(13) . . ? C19 N6 C21 107.0(11) . . ? C30 N3 C10 112.1(16) . . ? C30 N3 C34 108.8(14) . . ? C10 N3 C34 115.1(15) . . ? C30 N3 C32 110.2(14) . . ? C10 N3 C32 106.5(13) . . ? C34 N3 C32 103.9(14) . . ? C46 N5 C16 112.6(15) . . ? C46 N5 C18 121.3(18) . . ? C16 N5 C18 106.5(17) . . ? C46 N5 C17 101(2) . . ? C16 N5 C17 107.1(15) . . ? C18 N5 C17 107.4(13) . . ? C14 N4 C12 116.9(11) . . ? C14 N4 C26 103.7(11) . . ? C12 N4 C26 110.5(11) . . ? C14 N4 C28 112.9(12) . . ? C12 N4 C28 105.6(11) . . ? C26 N4 C28 106.9(12) . . ? C7 C7 C8 124.5(8) 2_755 . ? C7 C7 S11 120.0(4) 2_755 . ? C8 C7 S11 115.4(10) . . ? C15 C14 N4 115.0(14) . . ? N4 C12 C13 114.5(12) . . ? C24 C23 N6 126(2) . . ? C22 C21 N6 113.1(12) . . ? C1 C9 C41 126.6(16) . . ? C1 C9 S1 120.9(11) . . ? C41 C9 S1 112.3(15) . . ? W3 O3 W3 11.96(18) . 2_755 ? C45 C18 N5 113(2) . . ? C20 C19 N6 117.4(12) . . ? N3 C10 C11 117.0(19) . . ? N5 C17 C44 109.8(17) . . ? C48 C25 N6 124.0(19) . . ? C43 C16 N5 133(3) . . ? C50 N7 C37 113(2) . . ? C50 N7 C36 114.0(17) . . ? C37 N7 C36 112(2) . . ? C50 N7 C39 112(2) . . ? C37 N7 C39 103(3) . . ? C36 N7 C39 101(3) . . ? C27 C26 N4 128.0(15) . . ? C29 C28 N4 119.1(14) . . ? C33 C32 N3 118.1(15) . . ? N3 C34 C35 110.8(16) . . ? N3 C30 C31 114.5(17) . . ? N5 C46 C47 113(3) . . ? C49 C36 N7 129(2) . . ? C40 C39 N7 141(4) . . ? C52 C37 N7 121(3) . . ? N7 C50 C51 122(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 3.626 _refine_diff_density_min -0.874 _refine_diff_density_rms 0.185