#Supplementary Material (ESI) for Dalton Transactions #This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'John C. Bollinger' 'Malcolm H. Chisholm' 'Damon R. Click' 'Kirsten Folting' 'Christopher M. Hadad' 'Darin B. Tiedtke' 'Paul J. Wilson' _publ_contact_author ;Prof Malcolm Chisholm Department of Chemistry The Ohio State University Newman & Wolfrom Laboratories 100 West 18th Avenue Columbus OH 43210 UNITED STATES OF AMERICA ; _publ_contact_author_name 'Damon Click' _publ_contact_author_email dclick@chemistry.ohio-state.edu ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_CIF_for_W2(?-O)(OCH2tBu)8 _database_code_CSD 158778 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C40 H88 O9 W2' _chemical_formula_moiety 'C40 H88 O9 W2' _chemical_formula_weight 1080.81 _cell_length_a 12.2210(13) _cell_length_b 19.820(2) _cell_length_c 11.5931(10) _cell_angle_alpha 91.561(6) _cell_angle_beta 111.493(6) _cell_angle_gamma 72.050(6) _cell_volume 2474.0(5) _cell_formula_units_Z 2 _cell_measurement_reflns_used 120 _cell_measurement_theta_min 12.51 _cell_measurement_theta_max 17.34 _cell_measurement_temperature 103 _exptl_crystal_colour grey _exptl_crystal_description plate _exptl_crystal_size_max .30 _exptl_crystal_size_mid .30 _exptl_crystal_size_min .13 _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 4.6953 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.244 _exptl_absorpt_correction_T_max 0.597 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 103 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector 'scintillation counter' _diffrn_detector_area_resol_mean . _diffrn_reflns_number 10252 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_theta_min 3 _diffrn_reflns_theta_max 22.5 _diffrn_reflns_theta_full 22.5 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 4 _diffrn_standards_decay_% 3.3 _diffrn_standards_interval_count 200 _reflns_number_total 6890 _reflns_number_gt 6047 _reflns_threshold_expression 'F > 3\s(F)' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source W W -1.421 6.872 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 6890 _refine_ls_number_parameters 461 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef 0.4645E-6 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack . _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0176 _refine_ls_wR_factor_ref 0.0266 _refine_ls_goodness_of_fit_ref 1.0956 _refine_ls_shift/su_max 0.0725 _refine_diff_density_max 1.64 _refine_diff_density_min -0.75 _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution MULTAN78 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly W1 W 0.09956(2) 0.754520(10) 0.97493(2) 0.01436(8) Uani 1 0 . W2 W -0.11800(2) 0.746153(10) 0.86371(2) 0.01528(8) Uani 1 0 . O3 O 0.0409(3) 0.6719(2) 0.9517(3) 0.0172(15) Uani 1 0 . O4 O 0.9520(3) 0.7855(2) 0.0398(3) 0.0169(15) Uani 1 0 . C5 C -0.1002(5) 0.8560(3) 1.0733(5) 0.020(2) Uani 1 0 . C6 C 0.8823(5) 0.8521(3) 0.1967(5) 0.022(2) Uani 1 0 . C7 C 0.7887(6) 0.8138(3) 0.1844(6) 0.043(3) Uani 1 0 . C8 C 0.0059(6) 0.8141(3) 1.3008(5) 0.039(3) Uani 1 0 . C9 C -0.1704(5) 0.9295(3) 1.2209(5) 0.030(2) Uani 1 0 . O10 O -0.0489(3) 0.8227(2) 0.8270(3) 0.0172(14) Uani 1 0 . C11 C 0.9038(5) 0.8979(3) 0.7883(5) 0.023(2) Uani 1 0 . C12 C 0.9084(5) 0.9126(3) 0.6617(5) 0.024(2) Uani 1 0 . C13 C 0.8306(6) 0.8745(3) 0.5641(5) 0.041(3) Uani 1 0 . C14 C 0.0432(6) 0.8875(3) 0.6691(5) 0.035(2) Uani 1 0 . C15 C -0.1466(5) 0.9931(3) 0.6269(5) 0.032(2) Uani 1 0 . O16 O 0.1453(3) 0.8377(2) 1.0348(3) 0.0191(16) Uani 1 0 . C17 C 0.2338(5) 0.8500(3) 1.1465(5) 0.025(2) Uani 1 0 . C18 C 0.3425(5) 0.8641(3) 1.1255(5) 0.021(2) Uani 1 0 . C19 C 0.2933(5) 0.9289(3) 1.0333(5) 0.037(2) Uani 1 0 . C20 C 0.4124(5) 0.7986(3) 1.0766(6) 0.033(3) Uani 1 0 . C21 C 0.4299(6) 0.8766(3) 1.2509(6) 0.037(3) Uani 1 0 . O22 O 0.1851(3) 0.7258(2) 0.8693(3) 0.0194(16) Uani 1 0 . C23 C 0.1795(5) 0.6779(3) 0.7747(4) 0.020(2) Uani 1 0 . C24 C 0.3077(5) 0.6345(3) 0.7804(5) 0.021(2) Uani 1 0 . C25 C 0.2903(5) 0.5851(3) 0.6770(6) 0.032(3) Uani 1 0 . C26 C 0.3822(5) 0.5914(3) 0.9077(5) 0.035(2) Uani 1 0 . C27 C 0.3749(5) 0.6836(3) 0.7595(5) 0.029(2) Uani 1 0 . O28 O 0.2167(3) 0.7059(2) 1.1323(3) 0.0198(15) Uani 1 0 . C29 C 0.2166(5) 0.6442(3) 1.1937(5) 0.027(2) Uani 1 0 . C30 C 0.3335(5) 0.6163(3) 1.3097(5) 0.025(2) Uani 1 0 . C31 C 0.3235(6) 0.5503(3) 1.3666(5) 0.039(3) Uani 1 0 . C32 C 0.3434(5) 0.6714(3) 1.4058(5) 0.033(2) Uani 1 0 . C33 C 0.4485(5) 0.5957(3) 1.2755(5) 0.034(2) Uani 1 0 . O34 O -0.2736(3) 0.8218(2) 0.8216(3) 0.0217(16) Uani 1 0 . C35 C -0.3937(5) 0.8178(3) 0.8001(6) 0.046(3) Uani 1 0 . C36 C -0.4969(5) 0.8837(3) 0.7352(6) 0.039(3) Uani 1 0 . C37 C -0.6219(5) 0.8770(3) 0.7186(6) 0.040(3) Uani 1 0 . C38 C -0.4783(8) 0.9397(5) 0.8368(9) 0.071(5) Uani 1 0 . C39 C 0.5071(8) 0.9164(7) 0.6277(11) 0.151(6) Uani 1 0 . O40 O -0.1367(3) 0.7126(2) 0.7080(3) 0.0215(16) Uani 1 0 . C41 C 0.8589(5) 0.6443(3) 0.6650(5) 0.028(2) Uani 1 0 . C42 C -0.1816(5) 0.6458(3) 0.5246(5) 0.025(2) Uani 1 0 . C43 C -0.1884(6) 0.5717(3) 0.4901(6) 0.041(3) Uani 1 0 . C44 C -0.3080(6) 0.7020(3) 0.4606(6) 0.042(3) Uani 1 0 . C45 C 0.9150(6) 0.6608(3) 0.4833(5) 0.038(3) Uani 1 0 . O46 O 0.8127(3) 0.6895(2) 0.9287(3) 0.0206(16) Uani 1 0 . C47 C 0.8799(5) 0.6329(3) 0.0277(5) 0.023(2) Uani 1 0 . C48 C 0.7964(5) 0.5927(3) 0.0407(5) 0.024(2) Uani 1 0 . C49 C 0.8786(5) 0.5336(3) 0.1475(5) 0.035(2) Uani 1 0 . C50 C -0.3107(5) 0.6423(3) 1.0727(5) 0.031(2) Uani 1 0 . C51 C -0.2552(5) 0.5598(3) 0.9197(5) 0.032(2) Uani 1 0 . H1 H -0.0457 0.8827 1.0808 0.033 Uiso 1 0 . H2 H 0.8215 0.8791 0.0095 0.033 Uiso 1 0 . H3 H -0.2893 0.8399 1.123 0.0521 Uiso 1 0 . H4 H 0.8168 0.7674 0.1606 0.0521 Uiso 1 0 . H5 H -0.2198 0.8104 1.2621 0.0521 Uiso 1 0 . H6 H 0.9945 0.8144 0.3776 0.0516 Uiso 1 0 . H7 H 0.0365 0.7663 1.2838 0.0516 Uiso 1 0 . H8 H 0.0638 0.8381 1.306 0.0516 Uiso 1 0 . H9 H -0.1148 0.9545 1.2233 0.0431 Uiso 1 0 . H10 H -0.2485 0.9516 1.156 0.0431 Uiso 1 0 . H11 H 0.8193 0.9304 0.2984 0.0431 Uiso 1 0 . H12 H -0.1798 0.9161 0.7826 0.0343 Uiso 1 0 . H13 H 0.9527 0.9213 0.8483 0.0343 Uiso 1 0 . H14 H -0.2544 0.8952 0.5522 0.0481 Uiso 1 0 . H15 H 0.8406 0.8794 0.4875 0.0481 Uiso 1 0 . H16 H 0.8577 0.8254 0.5922 0.0481 Uiso 1 0 . H17 H 0.0786 0.8377 0.6928 0.0444 Uiso 1 0 . H18 H 0.0444 0.8974 0.5899 0.0444 Uiso 1 0 . H19 H 0.0898 0.9119 0.729 0.0444 Uiso 1 0 . H20 H -0.1021 1.0165 0.6909 0.0407 Uiso 1 0 . H21 H -0.1405 1.0042 0.5508 0.0407 Uiso 1 0 . H22 H -0.2314 1.0085 0.6175 0.0407 Uiso 1 0 . H23 H 0.1934 0.8902 1.1794 0.0353 Uiso 1 0 . H24 H 0.266 0.8092 1.2048 0.0353 Uiso 1 0 . H25 H 0.3604 0.938 1.0212 0.0449 Uiso 1 0 . H26 H 0.2379 0.9205 0.9561 0.0449 Uiso 1 0 . H27 H 0.2504 0.9689 1.0645 0.0449 Uiso 1 0 . H28 H 0.4414 0.7581 1.1345 0.0456 Uiso 1 0 . H29 H 0.3579 0.7905 0.9987 0.0456 Uiso 1 0 . H30 H 0.481 0.8069 1.0664 0.0456 Uiso 1 0 . H31 H 0.4605 0.8353 1.3075 0.0471 Uiso 1 0 . H32 H 0.4975 0.8862 1.2406 0.0471 Uiso 1 0 . H33 H 0.3863 0.916 1.2826 0.0471 Uiso 1 0 . H34 H 0.1383 0.6463 0.7852 0.0319 Uiso 1 0 . H35 H 0.134 0.7046 0.6955 0.0319 Uiso 1 0 . H36 H 0.24 0.5586 0.6846 0.0455 Uiso 1 0 . H37 H 0.251 0.6126 0.5984 0.0455 Uiso 1 0 . H38 H 0.3689 0.5534 0.6835 0.0455 Uiso 1 0 . H39 H 0.3392 0.5617 0.9209 0.0453 Uiso 1 0 . H40 H 0.4615 0.5629 0.9102 0.0453 Uiso 1 0 . H41 H 0.3922 0.6231 0.971 0.0453 Uiso 1 0 . H42 H 0.4532 0.6557 0.7585 0.0401 Uiso 1 0 . H43 H 0.3264 0.7118 0.6821 0.0401 Uiso 1 0 . H44 H 0.3869 0.7138 0.8249 0.0401 Uiso 1 0 . H45 H 0.1463 0.6565 1.2166 0.037 Uiso 1 0 . H46 H 0.2123 0.6081 1.1383 0.037 Uiso 1 0 . H47 H 0.252 0.5637 1.3877 0.047 Uiso 1 0 . H48 H 0.3167 0.516 1.3079 0.047 Uiso 1 0 . H49 H 0.3954 0.5304 1.4395 0.047 Uiso 1 0 . H50 H 0.4153 0.6514 1.4786 0.0435 Uiso 1 0 . H51 H 0.3493 0.7126 1.3715 0.0435 Uiso 1 0 . H52 H 0.2717 0.6843 1.4265 0.0435 Uiso 1 0 . H53 H 0.5208 0.5764 1.3483 0.0461 Uiso 1 0 . H54 H 0.4427 0.5611 1.2171 0.0461 Uiso 1 0 . H55 H 0.4533 0.6367 1.2398 0.0461 Uiso 1 0 . H56 H -0.405 0.7796 0.7506 0.0531 Uiso 1 0 . H57 H -0.3975 0.8083 0.8782 0.0531 Uiso 1 0 . H58 H -0.6841 0.9222 0.6903 0.0493 Uiso 1 0 . H59 H -0.6408 0.8442 0.659 0.0493 Uiso 1 0 . H60 H -0.6191 0.8602 0.796 0.0493 Uiso 1 0 . H61 H -0.4782 0.9212 0.9114 0.0857 Uiso 1 0 . H62 H -0.4015 0.9475 0.8525 0.0857 Uiso 1 0 . H63 H -0.5443 0.9833 0.806 0.0857 Uiso 1 0 . H64 H -0.4111 0.9176 0.6464 0.1359 Uiso 1 0 . H65 H -0.5153 0.8897 0.5595 0.1359 Uiso 1 0 . H66 H -0.5492 0.9637 0.6091 0.1359 Uiso 1 0 . H67 H 0.9392 0.6102 0.7023 0.0382 Uiso 1 0 . H68 H -0.1983 0.6307 0.6893 0.0382 Uiso 1 0 . H69 H 0.7528 0.5614 0.5163 0.0506 Uiso 1 0 . H70 H -0.2133 0.5707 0.4024 0.0506 Uiso 1 0 . H71 H 0.8909 0.5372 0.5303 0.0506 Uiso 1 0 . H72 H -0.3042 0.7472 0.4879 0.0513 Uiso 1 0 . H73 H -0.3297 0.7039 0.373 0.0513 Uiso 1 0 . H74 H -0.3685 0.69 0.4811 0.0513 Uiso 1 0 . H75 H -0.0048 0.6295 0.5319 0.0472 Uiso 1 0 . H76 H 0.8965 0.6533 0.3978 0.0472 Uiso 1 0 . H77 H -0.0871 0.7087 0.4944 0.0472 Uiso 1 0 . H78 H -0.0534 0.6007 1.0105 0.0341 Uiso 1 0 . H79 H -0.0879 0.6525 1.1037 0.0341 Uiso 1 0 . H80 H 0.8302 0.5071 0.1597 0.0437 Uiso 1 0 . H81 H 0.9442 0.5028 0.127 0.0437 Uiso 1 0 . H82 H -0.0878 0.5543 1.2216 0.0437 Uiso 1 0 . H83 H -0.2778 0.6624 1.1479 0.042 Uiso 1 0 . H84 H -0.3604 0.6794 1.0072 0.042 Uiso 1 0 . H85 H -0.36 0.6159 1.0828 0.042 Uiso 1 0 . H86 H -0.3027 0.5323 0.9302 0.0425 Uiso 1 0 . H87 H -0.3063 0.5967 0.8542 0.0425 Uiso 1 0 . H88 H -0.1883 0.5301 0.8997 0.0425 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 W1 0.01234(10) 0.01463(10) 0.01442(10) -0.00461(10) 0.00516(10) -0.00214(10) W2 0.01234(10) 0.01606(10) 0.01372(10) -0.00451(10) 0.00404(10) -0.00082(10) O3 0.015(2) 0.014(2) 0.023(2) -0.0060(10) 0.008(2) -0.0035(10) O4 0.015(2) 0.019(2) 0.018(2) -0.003(2) 0.0105(10) -0.0024(10) C5 0.020(3) 0.016(3) 0.025(3) -0.003(2) 0.011(2) -0.003(2) C6 0.023(3) 0.024(3) 0.020(3) -0.007(2) 0.013(2) -0.002(2) C7 0.051(4) 0.037(4) 0.049(4) -0.021(3) 0.035(3) -0.008(3) C8 0.039(4) 0.045(4) 0.022(3) -0.002(3) 0.008(3) -0.001(3) C9 0.038(3) 0.025(3) 0.031(3) -0.002(3) 0.022(3) -0.003(2) O10 0.017(2) 0.012(2) 0.018(2) -0.0040(10) 0.0074(10) 0.0012(10) C11 0.026(3) 0.019(3) 0.019(3) -0.006(2) 0.009(2) -0.002(2) C12 0.022(3) 0.023(3) 0.021(3) -0.006(2) 0.008(2) 0.000(2) C13 0.051(4) 0.044(4) 0.019(3) -0.023(3) 0.014(3) -0.003(3) C14 0.037(3) 0.029(3) 0.036(3) -0.009(3) 0.023(3) 0.003(3) C15 0.027(3) 0.027(3) 0.032(3) -0.012(3) 0.011(3) 0.002(2) O16 0.022(2) 0.016(2) 0.020(2) -0.007(2) 0.010(2) -0.0042(10) C17 0.026(3) 0.029(3) 0.017(3) -0.016(2) 0.006(2) -0.006(2) C18 0.014(3) 0.021(3) 0.024(3) -0.009(2) 0.005(2) -0.004(2) C19 0.032(3) 0.034(3) 0.034(3) -0.015(3) 0.012(3) 0.003(3) C20 0.022(3) 0.035(3) 0.050(4) -0.013(3) 0.019(3) -0.014(3) C21 0.031(3) 0.037(4) 0.038(3) -0.017(3) 0.010(3) -0.006(3) O22 0.019(2) 0.018(2) 0.022(2) -0.010(2) 0.009(2) -0.0071(10) C23 0.020(3) 0.022(3) 0.018(3) -0.009(2) 0.007(2) -0.006(2) C24 0.019(3) 0.023(3) 0.021(3) -0.006(2) 0.009(2) -0.004(2) C25 0.027(3) 0.033(3) 0.042(4) -0.009(3) 0.016(3) -0.012(3) C26 0.025(3) 0.032(3) 0.037(3) -0.007(3) 0.010(3) 0.001(3) C27 0.024(3) 0.031(3) 0.032(3) -0.011(3) 0.015(3) -0.005(3) O28 0.018(2) 0.015(2) 0.019(2) -0.0028(10) 0.006(2) 0.0024(10) C29 0.027(3) 0.022(3) 0.026(3) -0.009(2) 0.011(2) 0.000(2) C30 0.023(3) 0.022(3) 0.020(3) -0.004(2) 0.002(2) 0.001(2) C31 0.041(4) 0.031(3) 0.024(3) -0.014(3) 0.003(3) 0.003(2) C32 0.029(3) 0.033(3) 0.023(3) -0.009(3) 0.001(3) 0.000(2) C33 0.023(3) 0.036(3) 0.033(3) -0.003(3) 0.007(3) -0.001(3) O34 0.011(2) 0.024(2) 0.023(2) -0.005(2) 0.005(2) 0.001(2) C35 0.017(3) 0.035(4) 0.064(4) -0.007(3) 0.009(3) 0.015(3) C36 0.019(3) 0.037(4) 0.041(4) -0.005(3) 0.009(3) 0.013(3) C37 0.020(3) 0.035(4) 0.051(4) -0.009(3) 0.008(3) 0.005(3) C38 0.047(5) 0.061(5) 0.116(8) -0.018(4) 0.036(5) -0.026(5) C39 0.028(5) 0.171(11) 0.134(9) 0.012(6) 0.014(5) 0.110(9) O40 0.020(2) 0.020(2) 0.020(2) -0.006(2) 0.006(2) -0.0032(10) C41 0.031(3) 0.024(3) 0.025(3) -0.015(3) 0.010(3) -0.004(2) C42 0.026(3) 0.028(3) 0.018(3) -0.010(2) 0.006(2) -0.005(2) C43 0.047(4) 0.038(4) 0.036(3) -0.024(3) 0.016(3) -0.015(3) C44 0.033(4) 0.046(4) 0.031(3) -0.017(3) 0.002(3) -0.006(3) C45 0.043(4) 0.044(4) 0.027(3) -0.025(3) 0.017(3) -0.012(3) O46 0.013(2) 0.022(2) 0.021(2) -0.004(2) 0.005(2) 0.0020(10) C47 0.021(3) 0.019(3) 0.025(3) -0.005(2) 0.010(2) 0.001(2) C48 0.021(3) 0.021(3) 0.025(3) -0.008(2) 0.009(2) -0.002(2) C49 0.024(3) 0.035(3) 0.035(3) -0.009(3) 0.012(3) 0.004(3) C50 0.029(3) 0.035(3) 0.032(3) -0.015(3) 0.017(3) -0.009(3) C51 0.028(3) 0.029(3) 0.039(3) -0.013(3) 0.018(3) -0.007(3) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 W2 2.5509(4) . . no C48 C49 1.536(3) . . no W1 O3 1.956(2) . . no C48 C50 1.536(8) . 1_654 no W1 O4 2.117(4) . 1_456 no C48 C51 1.532(3) . 1_654 no W1 O10 2.0965(14) . . no W1 O16 1.9320(15) . . no W1 O22 1.857(4) . . no W1 O28 1.9078(14) . . no W2 O3 1.961(2) . . no W2 O4 2.1343(16) . 1_456 no W2 O10 2.070(3) . . no W2 O34 1.925(2) . . no W2 O40 1.865(2) . . no W2 O46 1.910(3) . 1_455 no O4 C5 1.452(2) . 1_654 no O10 C11 1.4402(8) . 1_455 no O16 C17 1.423(3) . . no O22 C23 1.428(3) . . no O28 C29 1.431(4) . . no O34 C35 1.423(8) . . no O40 C41 1.4410(15) . 1_455 no O46 C47 1.436(2) . 1_556 no C5 C6 1.529(7) . 1_456 no C6 C7 1.521(9) . . no C6 C8 1.522(5) . 1_654 no C6 C9 1.533(2) . 1_654 no C11 C12 1.528(7) . . no C12 C13 1.537(5) . . no C12 C14 1.537(9) . 1_655 no C12 C15 1.5282(6) . 1_655 no C17 C18 1.541(9) . . no C18 C19 1.511(3) . . no C18 C20 1.538(5) . . no C18 C21 1.524(4) . . no C23 C24 1.515(7) . . no C24 C25 1.523(3) . . no C24 C26 1.530(4) . . no C24 C27 1.526(8) . . no C29 C30 1.517(4) . . no C30 C31 1.540(6) . . no C30 C32 1.537(3) . . no C30 C33 1.532(9) . . no C35 C36 1.485(3) . . no C36 C37 1.516(9) . . no C36 C38 1.598(4) . . no C36 C39 1.444(10) . 1_455 no C41 C42 1.516(5) . 1_655 no C42 C43 1.530(2) . . no C42 C44 1.524(5) . . no C42 C45 1.533(10) . 1_455 no C47 C48 1.524(8) . . no C5 H1 0.950(5) . . no C32 H51 0.950(4) . . no C5 H2 0.950(3) . 1_456 no C32 H52 0.950(7) . . no C7 H3 0.949(4) . 1_654 no C33 H53 0.950(3) . . no C7 H4 0.950(2) . . no C33 H54 0.950(2) . . no C7 H5 0.950(6) . 1_654 no C33 H55 0.950(4) . . no C8 H6 0.950(6) . 1_456 no C35 H56 0.950(2) . . no C8 H7 0.9493(19) . . no C35 H57 0.950(5) . . no C8 H8 0.950(7) . . no C37 H58 0.950(2) . . no C9 H9 0.950(6) . . no C37 H59 0.950(2) . . no C9 H10 0.950(4) . . no C37 H60 0.950(5) . . no C9 H11 0.950(5) . 1_456 no C38 H61 0.949(7) . . no C11 H12 0.950(6) . 1_655 no C38 H62 0.949(9) . . no C11 H13 0.950(3) . . no C38 H63 0.949(4) . . no C13 H14 0.950(7) . 1_655 no C39 H64 0.950(9) . 1_655 no C13 H15 0.950(6) . . no C39 H65 0.942(6) . 1_655 no C13 H16 0.9499(14) . . no C39 H66 0.951(3) . 1_655 no C14 H17 0.9499(5) . . no C41 H67 0.950(4) . . no C14 H18 0.950(5) . . no C41 H68 0.950(7) . 1_655 no C14 H19 0.950(3) . . no C43 H69 0.950(8) . 1_455 no C15 H20 0.950(3) . . no C43 H70 0.950(4) . . no C15 H21 0.950(5) . . no C43 H71 0.949(4) . 1_455 no C15 H22 0.950(6) . . no C44 H72 0.9499(15) . . no C17 H23 0.950(4) . . no C44 H73 0.950(4) . . no C17 H24 0.951(2) . . no C44 H74 0.950(8) . . no C19 H25 0.950(7) . . no C45 H75 0.950(4) . 1_655 no C19 H26 0.950(3) . . no C45 H76 0.950(4) . . no C19 H27 0.950(4) . . no C45 H77 0.9496(15) . 1_655 no C20 H28 0.950(3) . . no C47 H78 0.950(5) . 1_654 no C20 H29 0.950(3) . . no C47 H79 0.950(2) . 1_654 no C20 H30 0.950(7) . . no C49 H80 0.950(6) . . no C21 H31 0.950(3) . . no C49 H81 0.950(6) . . no C21 H32 0.950(7) . . no C49 H82 0.950(3) . 1_654 no C21 H33 0.950(4) . . no C50 H83 0.950(2) . . no C23 H34 0.950(5) . . no C50 H84 0.950(2) . . no C23 H35 0.950(2) . . no C50 H85 0.950(6) . . no C25 H36 0.950(6) . . no C51 H86 0.950(6) . . no C25 H37 0.950(3) . . no C51 H87 0.9498(19) . . no C25 H38 0.950(5) . . no C51 H88 0.950(6) . . no C26 H39 0.950(6) . . no C26 H40 0.950(6) . . no C26 H41 0.950(2) . . no C27 H42 0.950(6) . . no C27 H43 0.950(2) . . no C27 H44 0.950(2) . . no C29 H45 0.950(7) . . no C29 H46 0.950(2) . . no C31 H47 0.950(8) . . no C31 H48 0.950(2) . . no C31 H49 0.950(3) . . no C32 H50 0.950(3) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag W2 W1 O3 49.45(7) . . . no W2 W1 O4 53.44(5) . . 1_456 no W2 W1 O10 51.77(9) . . . no W2 W1 O16 127.97(9) . . . no W2 W1 O22 107.42(8) . . . no W2 W1 O28 125.92(11) . . . no O3 W1 O4 77.22(11) . . 1_456 no O3 W1 O10 97.41(8) . . . no O3 W1 O16 165.13(14) . . . no O3 W1 O22 92.61(12) . . . no O3 W1 O28 86.24(8) . . . no O4 W1 O10 75.84(11) 1_456 . . no O4 W1 O16 90.33(13) 1_456 . . no O4 W1 O22 160.54(9) 1_456 . . no O4 W1 O28 92.75(13) 1_456 . . no O10 W1 O16 87.20(6) . . . no O10 W1 O22 89.31(11) . . . no O10 W1 O28 166.82(12) . . . no O16 W1 O22 101.60(14) . . . no O16 W1 O28 86.29(6) . . . no O22 W1 O28 103.22(12) . . . no W1 W2 O3 49.27(7) . . . no W1 W2 O4 52.83(11) . . 1_456 no W1 W2 O10 52.72(5) . . . no W1 W2 O34 127.40(6) . . . no W1 W2 O40 110.99(12) . . . no W1 W2 O46 124.07(6) . . 1_455 no O3 W2 O4 76.71(7) . . 1_456 no O3 W2 O10 98.14(12) . . . no O3 W2 O34 164.68(11) . . . no O3 W2 O40 94.49(9) . . . no O3 W2 O46 84.95(12) . . 1_455 no O4 W2 O10 76.03(10) 1_456 . . no O4 W2 O34 90.18(8) 1_456 . . no O4 W2 O40 163.60(17) 1_456 . . no O4 W2 O46 91.67(10) 1_456 . 1_455 no O10 W2 O34 86.10(12) . . . no O10 W2 O40 91.83(11) . . . no O10 W2 O46 166.14(9) . . 1_455 no O34 W2 O40 100.11(9) . . . no O34 W2 O46 87.60(12) . . 1_455 no O40 W2 O46 101.42(11) . . 1_455 no W1 O3 W2 81.277(14) . . . no W1 O4 W2 73.73(9) 1_654 . 1_654 no W1 O4 C5 125.8(3) 1_654 . 1_654 no W2 O4 C5 125.96(14) 1_654 . 1_654 no W1 O10 W2 75.51(5) . . . no W1 O10 C11 136.29(18) . . 1_455 no W2 O10 C11 136.7(3) . . 1_455 no W1 O16 C17 133.51(8) . . . no W1 O22 C23 134.5(3) . . . no W1 O28 C29 127.0(2) . . . no W2 O34 C35 129.26(8) . . . no W2 O40 C41 131.1(2) . . 1_455 no W2 O46 C47 126.3(3) 1_655 . 1_556 no O4 C5 C6 111.59(19) 1_456 . 1_456 no C5 C6 C7 110.0(3) 1_654 . . no C5 C6 C8 110.4(5) 1_654 . 1_654 no C5 C6 C9 105.7(3) 1_654 . 1_654 no C7 C6 C8 110.5(3) . . 1_654 no C7 C6 C9 109.1(5) . . 1_654 no C8 C6 C9 111.1(2) 1_654 . 1_654 no O10 C11 C12 111.1(3) 1_655 . . no C11 C12 C13 109.5(4) . . . no C11 C12 C14 110.6(3) . . 1_655 no C11 C12 C15 107.4(3) . . 1_655 no C13 C12 C14 110.4(4) . . 1_655 no C13 C12 C15 109.9(2) . . 1_655 no C14 C12 C15 109.0(4) 1_655 . 1_655 no O16 C17 C18 112.5(4) . . . no C17 C18 C19 109.5(4) . . . no C17 C18 C20 109.7(3) . . . no C17 C18 C21 107.5(4) . . . no C19 C18 C20 110.3(4) . . . no C19 C18 C21 110.5(2) . . . no C20 C18 C21 109.3(3) . . . no O22 C23 C24 111.7(3) . . . no C23 C24 C25 107.1(3) . . . no C23 C24 C26 109.5(4) . . . no C23 C24 C27 110.2(2) . . . no C25 C24 C26 110.59(10) . . . no C25 C24 C27 109.6(4) . . . no C26 C24 C27 109.8(3) . . . no O28 C29 C30 111.0(4) . . . no C29 C30 C31 106.3(4) . . . no C29 C30 C32 111.7(2) . . . no C29 C30 C33 110.2(4) . . . no C31 C30 C32 108.7(4) . . . no C31 C30 C33 110.2(3) . . . no C32 C30 C33 109.7(4) . . . no O34 C35 C36 114.0(4) . . . no C35 C36 C37 111.6(4) . . . no C35 C36 C38 102.8(2) . . . no C35 C36 C39 117.3(6) . . 1_455 no C37 C36 C38 103.6(5) . . . no C37 C36 C39 114.9(4) . . 1_455 no C38 C36 C39 104.5(4) . . 1_455 no O40 C41 C42 112.1(2) 1_655 . 1_655 no C41 C42 C43 107.1(3) 1_455 . . no C41 C42 C44 110.7(4) 1_455 . . no C41 C42 C45 110.2(4) 1_455 . 1_455 no C43 C42 C44 110.3(4) . . . no C43 C42 C45 108.4(4) . . 1_455 no C44 C42 C45 110.1(3) . . 1_455 no O46 C47 C48 111.2(3) 1_554 . . no C47 C48 C49 106.2(4) . . . no C47 C48 C50 110.9(2) . . 1_654 no C47 C48 C51 109.9(4) . . 1_654 no C49 C48 C50 109.7(4) . . 1_654 no C49 C48 C51 109.88(9) . . 1_654 no C50 C48 C51 110.1(4) 1_654 . 1_654 no O4 C5 H1 108.9(5) 1_456 . . no O4 C5 H2 108.96(19) 1_456 . 1_456 no C6 C5 H1 108.9(2) 1_456 . . no C6 C5 H2 109.0(5) 1_456 . 1_456 no H1 C5 H2 109.5(2) . . 1_456 no C6 C7 H3 109.4(3) . . 1_654 no C6 C7 H4 109.5(7) . . . no C6 C7 H5 109.4(3) . . 1_654 no H3 C7 H4 109.6(3) 1_654 . . no H3 C7 H5 109.5(8) 1_654 . 1_654 no H4 C7 H5 109.5(3) . . 1_654 no C6 C8 H6 109.4(6) 1_456 . 1_456 no C6 C8 H7 109.5(3) 1_456 . . no C6 C8 H8 109.4(3) 1_456 . . no H6 C8 H7 109.5(3) 1_456 . . no H6 C8 H8 109.4(3) 1_456 . . no H7 C8 H8 109.5(7) . . . no C6 C9 H9 109.5(6) 1_456 . . no C6 C9 H10 109.4(2) 1_456 . . no C6 C9 H11 109.5(3) 1_456 . 1_456 no H9 C9 H10 109.5(3) . . . no H9 C9 H11 109.5(3) . . 1_456 no H10 C9 H11 109.5(7) . . 1_456 no O10 C11 H12 109.1(4) 1_655 . 1_655 no O10 C11 H13 109.1(2) 1_655 . . no C12 C11 H12 109.0(3) . . 1_655 no C12 C11 H13 109.0(5) . . . no H12 C11 H13 109.5(3) 1_655 . . no C12 C13 H14 109.4(3) . . 1_655 no C12 C13 H15 109.4(6) . . . no C12 C13 H16 109.4(3) . . . no H14 C13 H15 109.5(3) 1_655 . . no H14 C13 H16 109.5(7) 1_655 . . no H15 C13 H16 109.5(4) . . . no C12 C14 H17 109.5(5) 1_455 . . no C12 C14 H18 109.5(3) 1_455 . . no C12 C14 H19 109.4(4) 1_455 . . no H17 C14 H18 109.5(4) . . . no H17 C14 H19 109.5(3) . . . no H18 C14 H19 109.5(6) . . . no C12 C15 H20 109.5(2) 1_455 . . no C12 C15 H21 109.5(4) 1_455 . . no C12 C15 H22 109.5(5) 1_455 . . no H20 C15 H21 109.5(5) . . . no H20 C15 H22 109.5(4) . . . no H21 C15 H22 109.5(3) . . . no O16 C17 H23 108.7(4) . . . no O16 C17 H24 108.7(3) . . . no C18 C17 H23 108.7(3) . . . no C18 C17 H24 108.7(4) . . . no H23 C17 H24 109.4(5) . . . no C18 C19 H25 109.5(4) . . . no C18 C19 H26 109.4(3) . . . no C18 C19 H27 109.5(5) . . . no H25 C19 H26 109.5(6) . . . no H25 C19 H27 109.5(3) . . . no H26 C19 H27 109.5(5) . . . no C18 C20 H28 109.5(5) . . . no C18 C20 H29 109.4(4) . . . no C18 C20 H30 109.4(3) . . . no H28 C20 H29 109.5(3) . . . no H28 C20 H30 109.5(4) . . . no H29 C20 H30 109.5(6) . . . no C18 C21 H31 109.5(3) . . . no C18 C21 H32 109.4(5) . . . no C18 C21 H33 109.5(4) . . . no H31 C21 H32 109.5(5) . . . no H31 C21 H33 109.5(6) . . . no H32 C21 H33 109.5(3) . . . no O22 C23 H34 108.9(5) . . . no O22 C23 H35 108.92(7) . . . no C24 C23 H34 108.90(17) . . . no C24 C23 H35 108.9(5) . . . no H34 C23 H35 109.4(4) . . . no C24 C25 H36 109.4(5) . . . no C24 C25 H37 109.44(8) . . . no C24 C25 H38 109.5(4) . . . no H36 C25 H37 109.5(4) . . . no H36 C25 H38 109.50(5) . . . no H37 C25 H38 109.5(6) . . . no C24 C26 H39 109.5(4) . . . no C24 C26 H40 109.4(5) . . . no C24 C26 H41 109.43(8) . . . no H39 C26 H40 109.509(19) . . . no H39 C26 H41 109.5(6) . . . no H40 C26 H41 109.5(5) . . . no C24 C27 H42 109.46(16) . . . no C24 C27 H43 109.4(4) . . . no C24 C27 H44 109.4(5) . . . no H42 C27 H43 109.5(6) . . . no H42 C27 H44 109.5(4) . . . no H43 C27 H44 109.48(2) . . . no O28 C29 H45 109.1(2) . . . no O28 C29 H46 109.1(4) . . . no C30 C29 H45 109.1(4) . . . no C30 C29 H46 109.1(2) . . . no H45 C29 H46 109.4(5) . . . no C30 C31 H47 109.4(2) . . . no C30 C31 H48 109.5(5) . . . no C30 C31 H49 109.4(5) . . . no H47 C31 H48 109.5(6) . . . no H47 C31 H49 109.5(5) . . . no H48 C31 H49 109.5(3) . . . no C30 C32 H50 109.4(2) . . . no C30 C32 H51 109.4(4) . . . no C30 C32 H52 109.5(4) . . . no H50 C32 H51 109.5(5) . . . no H50 C32 H52 109.5(5) . . . no H51 C32 H52 109.5(3) . . . no C30 C33 H53 109.5(5) . . . no C30 C33 H54 109.4(5) . . . no C30 C33 H55 109.5(3) . . . no H53 C33 H54 109.5(3) . . . no H53 C33 H55 109.5(5) . . . no H54 C33 H55 109.5(5) . . . no O34 C35 H56 108.3(5) . . . no O34 C35 H57 108.3(3) . . . no C36 C35 H56 108.3(3) . . . no C36 C35 H57 108.3(5) . . . no H56 C35 H57 109.5(4) . . . no C36 C37 H58 109.5(4) . . . no C36 C37 H59 109.5(5) . . . no C36 C37 H60 109.4(3) . . . no H58 C37 H59 109.5(3) . . . no H58 C37 H60 109.5(6) . . . no H59 C37 H60 109.5(4) . . . no C36 C38 H61 109.3(4) . . . no C36 C38 H62 109.3(7) . . . no C36 C38 H63 109.3(4) . . . no H61 C38 H62 109.7(4) . . . no H61 C38 H63 109.7(9) . . . no H62 C38 H63 109.6(5) . . . no C36 C39 H64 108.9(6) 1_655 . 1_655 no C36 C39 H65 109.4(5) 1_655 . 1_655 no C36 C39 H66 108.8(8) 1_655 . 1_655 no H64 C39 H65 110.2(9) 1_655 . 1_655 no H64 C39 H66 109.4(5) 1_655 . 1_655 no H65 C39 H66 110.1(6) 1_655 . 1_655 no O40 C41 H67 108.8(3) 1_655 . . no O40 C41 H68 108.8(4) 1_655 . 1_655 no C42 C41 H67 108.8(5) 1_655 . . no C42 C41 H68 108.8(4) 1_655 . 1_655 no H67 C41 H68 109.5(3) . . 1_655 no C42 C43 H69 109.4(5) . . 1_455 no C42 C43 H70 109.4(3) . . . no C42 C43 H71 109.4(4) . . 1_455 no H69 C43 H70 109.5(5) 1_455 . . no H69 C43 H71 109.5(4) 1_455 . 1_455 no H70 C43 H71 109.5(6) . . 1_455 no C42 C44 H72 109.4(4) . . . no C42 C44 H73 109.4(5) . . . no C42 C44 H74 109.4(3) . . . no H72 C44 H73 109.5(4) . . . no H72 C44 H74 109.5(6) . . . no H73 C44 H74 109.5(5) . . . no C42 C45 H75 109.4(4) 1_655 . 1_655 no C42 C45 H76 109.4(5) 1_655 . . no C42 C45 H77 109.4(5) 1_655 . 1_655 no H75 C45 H76 109.5(6) 1_655 . . no H75 C45 H77 109.5(5) 1_655 . 1_655 no H76 C45 H77 109.5(4) . . 1_655 no O46 C47 H78 109.1(4) 1_554 . 1_654 no O46 C47 H79 109.06(7) 1_554 . 1_654 no C48 C47 H78 109.03(18) . . 1_654 no C48 C47 H79 109.0(5) . . 1_654 no H78 C47 H79 109.5(4) 1_654 . 1_654 no C48 C49 H80 109.4(4) . . . no C48 C49 H81 109.4(5) . . . no C48 C49 H82 109.44(8) . . 1_654 no H80 C49 H81 109.49(6) . . . no H80 C49 H82 109.5(6) . . 1_654 no H81 C49 H82 109.5(5) . . 1_654 no C48 C50 H83 109.4(5) 1_456 . . no C48 C50 H84 109.5(5) 1_456 . . no C48 C50 H85 109.41(17) 1_456 . . no H83 C50 H84 109.55(6) . . . no H83 C50 H85 109.5(6) . . . no H84 C50 H85 109.5(5) . . . no C48 C51 H86 109.4(5) 1_456 . . no C48 C51 H87 109.45(9) 1_456 . . no C48 C51 H88 109.4(4) 1_456 . . no H86 C51 H87 109.5(5) . . . no H86 C51 H88 109.49(5) . . . no H87 C51 H88 109.5(6) . . . no # The following lines may be used to test the character set of files sent by # network email or other means. They are not part of the CIF data archive. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ 1===END ############################################################################## # IUMSC CIF Archive file # ############################################################################## data_CIF_for_W2(?-S)(OCH2tBU)8 _database_code_CSD 158779 _audit_creation_method 'minor manual editing of SDT2CIF v. 1.2 BETA output' _chemical_formula_sum 'C40 H88 O8 S1 W2' _chemical_formula_moiety 'C40 H88 O8 S1 W2' _chemical_formula_weight 1096.88 _cell_length_a 14.755(6) _cell_length_b 14.888(6) _cell_length_c 12.172(5) _cell_angle_alpha 92.20(2) _cell_angle_beta 113.168(19) _cell_angle_gamma 93.03(2) _cell_volume 2449.6(17) _cell_formula_units_Z 2 _cell_measurement_reflns_used 26 _cell_measurement_theta_min 9.61 _cell_measurement_theta_max 10.28 _cell_measurement_temperature 108 _exptl_crystal_colour blue _exptl_crystal_description plate _exptl_crystal_size_max .40 _exptl_crystal_size_mid .25 _exptl_crystal_size_min .10 _exptl_crystal_density_diffrn 1.487 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 4.7821 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details Tompa _exptl_absorpt_correction_T_min 0.334 _exptl_absorpt_correction_T_max 0.603 _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x,y,z' '-x,-y,-z' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_ambient_temperature 108 _diffrn_measurement_device_type 'refurbished Picker diffractometer' _diffrn_measurement_method '\q/2\q scans' _diffrn_detector 'scintillation counter' _diffrn_detector_area_resol_mean . _diffrn_reflns_number 8759 _diffrn_reflns_av_R_equivalents 0.022 _diffrn_reflns_theta_min 3.0 _diffrn_reflns_theta_max 22.5 _diffrn_reflns_theta_full 22.5 _diffrn_measured_fraction_theta_max 0.99 _diffrn_measured_fraction_theta_full 0.99 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_standards_number 4 _diffrn_standards_decay_% -7.8 _diffrn_standards_interval_count 310 _reflns_number_total 6376 _reflns_number_gt 5524 _reflns_threshold_expression 'F > 3\s(F)' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source W W -1.421 6.872 'International Tables Vol. IV (1974) Table 2.2B' S S 0.11 0.124 'International Tables Vol. IV (1974) Table 2.2B' O O 0.008 0.006 'International Tables Vol. IV (1974) Table 2.2B' C C 0.002 0.002 'International Tables Vol. IV (1974) Table 2.2B' H H 0 0 'International Tables Vol. IV (1974) Table 2.2B' _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_number_reflns 6376 _refine_ls_number_parameters 461 _refine_ls_hydrogen_treatment noref _refine_ls_extinction_coef 0.5903E-7 _refine_ls_extinction_method Zachariasen _refine_ls_extinction_expression ; Larson, A. C. (1967). Acta Cryst. 23, p. 664. Eq. (3) ; _refine_ls_abs_structure_details none _refine_ls_abs_structure_Flack . _refine_ls_weighting_scheme calc _refine_ls_weighting_details w^-1^=\s^2^(F)+(.07F)^2^ _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0312 _refine_ls_goodness_of_fit_ref 1.289 _refine_ls_shift/su_max 0.027 _refine_diff_density_max 1.90 _refine_diff_density_min -0.92 _computing_data_collection 'NPS, local program' _computing_cell_refinement 'XTEL, local package' _computing_data_reduction 'XTEL, local package' _computing_structure_solution MULTAN78 _computing_structure_refinement 'XTEL, local package' _computing_molecular_graphics 'XTEL, local package' _computing_publication_material 'XTEL, local package' 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_disorder_group _atom_site_disorder_assembly W1 W 0.29292(2) 0.24409(2) 0.11554(2) 0.01527(13) Uani 1 0 . W2 W 0.25961(2) 0.28340(2) 0.89494(2) 0.01521(13) Uani 1 0 . S3 S 0.38955(10) 0.35293(10) 0.06533(10) 0.0224(7) Uani 1 0 . O4 O 0.2724(3) 0.1574(3) 0.9682(4) 0.0190(17) Uani 1 0 . C5 C 0.2122(5) 0.0742(4) 0.9248(6) 0.020(3) Uani 1 0 . C6 C 0.2654(5) 0.0023(4) 0.8849(6) 0.024(3) Uani 1 0 . C7 C 0.2734(6) 0.0278(5) 0.7690(7) 0.035(3) Uani 1 0 . C8 C 0.3675(5) -0.0062(5) -0.0169(7) 0.034(3) Uani 1 0 . C9 C 0.2029(6) 0.9145(5) 0.8640(7) 0.036(3) Uani 1 0 . O10 O 0.1615(3) 0.2785(3) -0.0188(4) 0.0150(15) Uani 1 0 . C11 C 0.0641(5) 0.2335(4) -0.0618(6) 0.019(3) Uani 1 0 . C12 C -0.0090(5) 0.2877(5) -0.0310(6) 0.024(3) Uani 1 0 . C13 C -0.0054(5) 0.3832(5) -0.0669(7) 0.035(3) Uani 1 0 . C14 C 0.0152(5) 0.2843(5) 0.1041(6) 0.032(3) Uani 1 0 . C15 C -0.1107(5) 0.2407(5) -0.1002(6) 0.030(3) Uani 1 0 . O16 O 0.2165(3) 0.1537(3) 0.1601(4) 0.0194(16) Uani 1 0 . C17 C 0.2302(4) 0.1377(4) 0.2793(6) 0.019(3) Uani 1 0 . C18 C 0.2001(5) 0.0413(4) 0.2928(6) 0.021(3) Uani 1 0 . C19 C 0.2626(5) 0.9765(5) 0.2584(6) 0.027(3) Uani 1 0 . C20 C 0.2184(5) 0.0323(5) 0.4248(6) 0.028(3) Uani 1 0 . C21 C 0.0905(5) 0.0187(5) 0.2145(7) 0.032(3) Uani 1 0 . O22 O 0.2740(3) 0.3284(3) 0.2231(4) 0.0196(19) Uani 1 0 . C23 C 0.2661(5) 0.4227(5) 0.2222(6) 0.027(3) Uani 1 0 . C24 C 0.2691(5) 0.4640(5) 0.3405(6) 0.024(3) Uani 1 0 . C25 C 0.2597(6) 0.5649(5) 0.3262(7) 0.041(3) Uani 1 0 . C26 C 0.3683(7) 0.4507(6) 0.4377(7) 0.055(4) Uani 1 0 . C27 C 0.1870(7) 0.4229(6) 0.3694(9) 0.058(5) Uani 1 0 . O28 O 0.4058(3) 0.1887(3) 0.2130(4) 0.0237(16) Uani 1 0 . C29 C 0.5085(5) 0.1909(5) 0.2373(6) 0.027(3) Uani 1 0 . C30 C 0.5690(5) 0.1942(5) 0.3707(6) 0.026(3) Uani 1 0 . C31 C 0.6784(5) 0.2040(5) 0.3919(7) 0.032(3) Uani 1 0 . C32 C 0.5458(6) 0.1095(6) 0.4227(8) 0.044(4) Uani 1 0 . C33 C 0.5456(6) 0.2762(6) 0.4296(7) 0.041(4) Uani 1 0 . O34 O 0.1530(3) 0.2276(3) -0.2464(4) 0.0184(15) Uani 1 0 . C35 C 0.1353(5) 0.2461(4) 0.6334(6) 0.021(3) Uani 1 0 . C36 C 0.0293(5) 0.2243(5) -0.4520(6) 0.023(3) Uani 1 0 . C37 C 0.0211(5) 0.2434(5) -0.5778(6) 0.026(3) Uani 1 0 . C38 C -0.0006(6) 0.1264(5) -0.4494(7) 0.037(3) Uani 1 0 . C39 C 0.9618(5) 0.2832(6) 0.5816(6) 0.035(3) Uani 1 0 . O40 O 0.2195(3) 0.3954(3) -0.1642(4) 0.024(2) Uani 1 0 . C41 C 0.2338(6) 0.4863(5) -0.1173(7) 0.034(3) Uani 1 0 . C42 C 0.2262(6) 0.5519(5) -0.2104(6) 0.030(3) Uani 1 0 . C43 C 0.2445(6) 0.6477(5) -0.1534(7) 0.040(3) Uani 1 0 . C44 C 0.1236(9) 0.5404(7) -0.3083(10) 0.090(6) Uani 1 0 . C45 C 0.3011(11) 0.5342(7) -0.2640(12) 0.091(8) Uani 1 0 . O46 O 0.3470(3) 0.2556(3) -0.1768(4) 0.0226(19) Uani 1 0 . C47 C 0.4500(5) 0.2407(5) 0.8667(6) 0.029(3) Uani 1 0 . C48 C 0.4899(5) 0.2560(5) -0.2299(6) 0.024(3) Uani 1 0 . C49 C 0.5978(6) 0.2338(6) -0.1803(8) 0.045(4) Uani 1 0 . C50 C 0.4328(7) 0.1929(8) -0.3387(9) 0.075(5) Uani 1 0 . C51 C 0.4816(7) 0.3505(6) 0.7369(10) 0.060(5) Uani 1 0 . H1 H 0.1951 0.0523 0.9867 0.0334 Uiso 1 0 . H2 H 0.1538 0.0859 0.8583 0.0334 Uiso 1 0 . H3 H 0.2987 0.0895 -0.224 0.0485 Uiso 1 0 . H4 H 0.3162 0.9906 0.7497 0.0485 Uiso 1 0 . H5 H 0.2095 0.0216 -0.2963 0.0485 Uiso 1 0 . H6 H 0.362 0.9773 0.0551 0.047 Uiso 1 0 . H7 H 0.4009 0.9485 0.9587 0.047 Uiso 1 0 . H8 H 0.4067 0.0496 -0.0015 0.047 Uiso 1 0 . H9 H 0.1366 -0.0791 -0.1932 0.0487 Uiso 1 0 . H10 H 0.2297 -0.1324 -0.1668 0.0487 Uiso 1 0 . H11 H 0.1989 0.8968 0.9366 0.0487 Uiso 1 0 . H12 H 0.0404 0.2238 -0.1463 0.0309 Uiso 1 0 . H13 H 0.0688 0.1767 0.9729 0.0309 Uiso 1 0 . H14 H 0.0583 0.4132 0.9778 0.0483 Uiso 1 0 . H15 H -0.0179 0.3831 -0.1502 0.0483 Uiso 1 0 . H16 H 0.9461 0.4161 0.9472 0.0483 Uiso 1 0 . H17 H 0.0015 0.2241 0.1223 0.0436 Uiso 1 0 . H18 H 0.084 0.301 0.1498 0.0436 Uiso 1 0 . H19 H -0.0228 0.3238 0.1283 0.0436 Uiso 1 0 . H20 H -0.159 0.2722 -0.0837 0.0427 Uiso 1 0 . H21 H 0.8748 0.2398 0.8168 0.0427 Uiso 1 0 . H22 H -0.1122 0.1806 -0.0766 0.0427 Uiso 1 0 . H23 H 0.2983 0.1504 0.3301 0.0318 Uiso 1 0 . H24 H 0.1919 0.1769 0.304 0.0318 Uiso 1 0 . H25 H 0.2481 0.916 0.2732 0.0406 Uiso 1 0 . H26 H 0.2496 -0.0215 0.1747 0.0406 Uiso 1 0 . H27 H 0.3315 0.9924 0.3031 0.0406 Uiso 1 0 . H28 H 0.1953 0.9739 0.4345 0.0406 Uiso 1 0 . H29 H 0.2872 0.0419 0.472 0.0406 Uiso 1 0 . H30 H 0.1841 0.0762 0.4486 0.0406 Uiso 1 0 . H31 H 0.0516 0.0578 0.2389 0.0455 Uiso 1 0 . H32 H 0.0789 0.0273 0.1331 0.0455 Uiso 1 0 . H33 H 0.0723 0.9582 0.2224 0.0455 Uiso 1 0 . H34 H 0.3185 0.4502 0.2061 0.0397 Uiso 1 0 . H35 H 0.2045 0.4342 0.1598 0.0397 Uiso 1 0 . H36 H 0.2668 0.5956 0.3993 0.0544 Uiso 1 0 . H37 H 0.3107 0.5901 0.3027 0.0544 Uiso 1 0 . H38 H 0.1973 0.5759 0.2656 0.0544 Uiso 1 0 . H39 H 0.3783 0.388 0.4462 0.0678 Uiso 1 0 . H40 H 0.4205 0.4776 0.4176 0.0678 Uiso 1 0 . H41 H 0.3743 0.4781 0.512 0.0678 Uiso 1 0 . H42 H 0.1239 0.4317 0.3071 0.0724 Uiso 1 0 . H43 H 0.1919 0.3594 0.3772 0.0724 Uiso 1 0 . H44 H 0.1884 0.4497 0.4428 0.0724 Uiso 1 0 . H45 H 0.5208 0.1378 0.2006 0.04 Uiso 1 0 . H46 H 0.5265 0.2423 0.205 0.04 Uiso 1 0 . H47 H 0.7191 0.1993 0.4744 0.0452 Uiso 1 0 . H48 H 0.6935 0.1579 0.3458 0.0452 Uiso 1 0 . H49 H 0.6946 0.2613 0.3684 0.0452 Uiso 1 0 . H50 H 0.4773 0.103 0.4085 0.0578 Uiso 1 0 . H51 H 0.561 0.0571 0.3862 0.0578 Uiso 1 0 . H52 H 0.5838 0.111 0.5068 0.0578 Uiso 1 0 . H53 H 0.584 0.2814 0.5135 0.0539 Uiso 1 0 . H54 H 0.5595 0.3305 0.3962 0.0539 Uiso 1 0 . H55 H 0.477 0.2734 0.4163 0.0539 Uiso 1 0 . H56 H 0.152 0.3084 -0.3692 0.0341 Uiso 1 0 . H57 H 0.1768 0.2113 0.6079 0.0341 Uiso 1 0 . H58 H 0.0416 0.3045 -0.5788 0.039 Uiso 1 0 . H59 H 0.063 0.2056 -0.5989 0.039 Uiso 1 0 . H60 H 0.955 0.2307 0.3671 0.039 Uiso 1 0 . H61 H -0.0673 0.1119 -0.5046 0.0486 Uiso 1 0 . H62 H 0.0411 0.0886 0.5285 0.0486 Uiso 1 0 . H63 H 0.0048 0.1129 -0.3712 0.0486 Uiso 1 0 . H64 H 0.9849 0.3457 0.5886 0.0481 Uiso 1 0 . H65 H -0.1041 0.2763 -0.4781 0.0481 Uiso 1 0 . H66 H -0.0395 0.2682 -0.3435 0.0481 Uiso 1 0 . H67 H 0.1859 0.4971 -0.0856 0.0476 Uiso 1 0 . H68 H 0.2984 0.4955 -0.0543 0.0476 Uiso 1 0 . H69 H 0.3098 0.6565 -0.0908 0.0526 Uiso 1 0 . H70 H 0.2379 0.6908 0.7895 0.0526 Uiso 1 0 . H71 H 0.1981 0.6585 0.8829 0.0526 Uiso 1 0 . H72 H 0.1149 0.5816 -0.369 0.1013 Uiso 1 0 . H73 H 0.1082 0.4805 -0.3445 0.1013 Uiso 1 0 . H74 H 0.0739 0.5518 -0.2756 0.1013 Uiso 1 0 . H75 H 0.2923 0.4744 -0.2986 0.1052 Uiso 1 0 . H76 H 0.2998 0.5758 -0.3215 0.1052 Uiso 1 0 . H77 H 0.3686 0.5409 -0.2005 0.1052 Uiso 1 0 . H78 H 0.4851 0.2822 -0.0657 0.0415 Uiso 1 0 . H79 H 0.4591 0.1812 0.8912 0.0415 Uiso 1 0 . H80 H 0.6033 0.1723 -0.158 0.0606 Uiso 1 0 . H81 H 0.6252 0.2406 -0.2391 0.0606 Uiso 1 0 . H82 H 0.636 0.272 0.8888 0.0606 Uiso 1 0 . H83 H 0.3645 0.2043 0.6276 0.085 Uiso 1 0 . H84 H 0.4584 0.2004 -0.3997 0.085 Uiso 1 0 . H85 H 0.4379 0.1313 0.6813 0.085 Uiso 1 0 . H86 H 0.5085 0.3626 -0.3201 0.074 Uiso 1 0 . H87 H 0.4147 0.3663 -0.2923 0.074 Uiso 1 0 . H88 H 0.5184 0.3909 0.8083 0.074 Uiso 1 0 . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 W1 0.0146(2) 0.0198(2) 0.0113(2) 0.00336(10) 0.00490(10) 0.00084(10) W2 0.0149(2) 0.0192(2) 0.0118(2) 0.00305(10) 0.00543(10) 0.00084(10) S3 0.0213(10) 0.0290(10) 0.0156(10) -0.0033(10) 0.0068(10) -0.0008(10) O4 0.028(3) 0.015(2) 0.015(2) 0.004(2) 0.011(2) 0.001(2) C5 0.027(4) 0.017(4) 0.019(4) 0.002(3) 0.011(3) 0.006(3) C6 0.025(4) 0.021(4) 0.029(4) 0.006(3) 0.014(3) 0.003(3) C7 0.044(5) 0.036(5) 0.034(4) 0.004(4) 0.025(4) -0.007(4) C8 0.033(4) 0.022(4) 0.052(5) 0.014(3) 0.021(4) 0.006(4) C9 0.044(5) 0.033(4) 0.040(5) 0.008(4) 0.026(4) -0.006(4) O10 0.012(2) 0.017(2) 0.015(2) 0.002(2) 0.004(2) -0.002(2) C11 0.015(3) 0.019(4) 0.019(4) 0.005(3) 0.003(3) 0.000(3) C12 0.019(4) 0.031(4) 0.024(4) 0.006(3) 0.009(3) -0.001(3) C13 0.024(4) 0.025(4) 0.044(5) 0.007(3) 0.003(4) -0.006(4) C14 0.022(4) 0.047(5) 0.025(4) 0.009(3) 0.009(3) -0.009(3) C15 0.021(4) 0.040(5) 0.027(4) 0.004(3) 0.009(3) -0.005(3) O16 0.020(2) 0.029(3) 0.008(2) 0.007(2) 0.004(2) 0.003(2) C17 0.012(3) 0.026(4) 0.015(4) 0.003(3) 0.002(3) 0.002(3) C18 0.016(3) 0.025(4) 0.019(4) 0.002(3) 0.004(3) 0.001(3) C19 0.029(4) 0.023(4) 0.027(4) 0.005(3) 0.008(3) 0.003(3) C20 0.037(4) 0.027(4) 0.026(4) 0.006(3) 0.017(3) 0.007(3) C21 0.030(4) 0.033(4) 0.035(4) -0.002(3) 0.014(4) 0.006(4) O22 0.025(3) 0.020(3) 0.013(2) 0.006(2) 0.008(2) -0.002(2) C23 0.029(4) 0.023(4) 0.030(4) 0.004(3) 0.013(3) -0.001(3) C24 0.020(4) 0.029(4) 0.019(4) 0.005(3) 0.003(3) -0.004(3) C25 0.051(5) 0.028(4) 0.037(5) 0.009(4) 0.009(4) -0.005(4) C26 0.066(6) 0.050(6) 0.030(5) 0.030(5) -0.000(4) -0.016(4) C27 0.073(7) 0.052(6) 0.074(7) -0.019(5) 0.061(6) -0.030(5) O28 0.016(2) 0.036(3) 0.018(2) 0.007(2) 0.004(2) 0.005(2) C29 0.020(4) 0.040(5) 0.023(4) 0.011(3) 0.009(3) 0.006(3) C30 0.026(4) 0.028(4) 0.023(4) 0.006(3) 0.010(3) 0.002(3) C31 0.024(4) 0.037(5) 0.031(4) 0.009(3) 0.005(3) 0.002(3) C32 0.033(5) 0.047(5) 0.045(5) 0.002(4) 0.005(4) 0.019(4) C33 0.033(5) 0.045(5) 0.042(5) -0.001(4) 0.014(4) -0.019(4) O34 0.021(2) 0.022(2) 0.014(2) 0.009(2) 0.008(2) 0.002(2) C35 0.020(4) 0.026(4) 0.016(4) -0.001(3) 0.008(3) 0.000(3) C36 0.021(4) 0.030(4) 0.018(4) -0.001(3) 0.008(3) 0.002(3) C37 0.027(4) 0.030(4) 0.016(4) 0.002(3) 0.003(3) 0.004(3) C38 0.041(5) 0.040(5) 0.027(4) -0.008(4) 0.012(4) 0.003(4) C39 0.025(4) 0.052(5) 0.025(4) 0.012(4) 0.007(3) 0.002(4) O40 0.027(3) 0.022(3) 0.022(3) 0.003(2) 0.006(2) 0.003(2) C41 0.059(5) 0.019(4) 0.028(4) 0.005(4) 0.021(4) -0.001(3) C42 0.043(5) 0.024(4) 0.030(4) 0.005(3) 0.020(4) -0.002(3) C43 0.055(5) 0.027(4) 0.043(5) 0.004(4) 0.027(4) 0.001(4) C44 0.091(9) 0.035(6) 0.080(8) 0.021(6) -0.034(7) 0.001(5) C45 0.156(12) 0.039(6) 0.142(11) 0.002(7) 0.130(11) -0.008(6) O46 0.018(3) 0.034(3) 0.017(2) 0.005(2) 0.009(2) -0.000(2) C47 0.019(4) 0.046(5) 0.024(4) 0.012(3) 0.009(3) 0.010(3) C48 0.021(4) 0.030(4) 0.023(4) 0.004(3) 0.012(3) 0.001(3) C49 0.033(5) 0.067(6) 0.048(5) 0.024(4) 0.027(4) 0.020(4) C50 0.044(6) 0.127(10) 0.060(7) -0.030(6) 0.039(5) -0.054(7) C51 0.053(6) 0.058(6) 0.103(8) 0.023(5) 0.058(6) 0.045(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 W2 2.6282(11) . 1_554 no C48 C49 1.523(10) . . no W1 S3 2.3557(16) . . no C48 C50 1.513(7) . . no W1 O4 2.081(3) . 1_554 no C48 C51 1.477(3) . 1_554 no W1 O10 2.090(3) . . no W1 O16 1.938(3) . . no W1 O22 1.888(3) . . no W1 O28 1.878(3) . . no W2 S3 2.3548(15) . 1_556 no W2 O4 2.0942(17) . . no W2 O10 2.096(4) . 1_556 no W2 O34 1.936(3) . 1_556 no W2 O40 1.8744(17) . 1_556 no W2 O46 1.874(5) . 1_556 no O4 C5 1.437(4) . . no O10 C11 1.438(7) . . no O16 C17 1.415(6) . . no O22 C23 1.4153(13) . . no O28 C29 1.424(9) . . no O34 C35 1.421(6) . 1_554 no O40 C41 1.420(2) . . no O46 C47 1.431(8) . 1_554 no C5 C6 1.531(8) . . no C6 C7 1.522(9) . . no C6 C8 1.526(9) . 1_556 no C6 C9 1.512(6) . 1_545 no C11 C12 1.530(9) . . no C12 C13 1.507(3) . . no C12 C14 1.542(8) . . no C12 C15 1.517(8) . . no C17 C18 1.514(3) . . no C18 C19 1.525(8) . 1_545 no C18 C20 1.533(8) . . no C18 C21 1.530(9) . . no C23 C24 1.528(8) . . no C24 C25 1.5260(17) . . no C24 C26 1.506(10) . . no C24 C27 1.496(13) . . no C29 C30 1.511(8) . . no C30 C31 1.529(11) . . no C30 C32 1.514(6) . . no C30 C33 1.516(7) . . no C35 C36 1.507(8) . 1_556 no C36 C37 1.527(8) . . no C36 C38 1.506(3) . . no C36 C39 1.522(9) . 1_454 no C41 C42 1.500(6) . . no C42 C43 1.524(3) . . no C42 C44 1.510(12) . . no C42 C45 1.517(17) . . no C47 C48 1.528(10) . 1_556 no C5 H1 0.947(6) . . no C32 H51 0.962(5) . . no C5 H2 0.952(5) . . no C32 H52 0.953(6) . . no C7 H3 0.961(3) . 1_556 no C33 H53 0.951(6) . . no C7 H4 0.950(7) . 1_545 no C33 H54 0.967(5) . . no C7 H5 0.961(7) . 1_556 no C33 H55 0.959(8) . . no C8 H6 0.952(6) . 1_545 no C35 H56 0.9526(18) . 1_556 no C8 H7 0.959(6) . 1_544 no C35 H57 0.953(6) . . no C8 H8 0.955(4) . . no C37 H58 0.945(2) . . no C9 H9 0.964(7) . 1_566 no C37 H59 0.955(6) . . no C9 H10 0.954(6) . 1_566 no C37 H60 0.945(6) . 1_454 no C9 H11 0.954(7) . . no C38 H61 0.956(7) . . no C11 H12 0.950(5) . . no C38 H62 0.961(8) . 1_554 no C11 H13 0.954(2) . 1_554 no C38 H63 0.954(7) . . no C13 H14 0.956(6) . 1_554 no C39 H64 0.963(2) . . no C13 H15 0.956(6) . . no C39 H65 0.955(6) . 1_656 no C13 H16 0.954(7) . 1_454 no C39 H66 0.954(7) . 1_656 no C14 H17 0.962(3) . . no C41 H67 0.946(9) . . no C14 H18 0.958(6) . . no C41 H68 0.958(7) . . no C14 H19 0.949(6) . . no C43 H69 0.963(7) . . no C15 H20 0.954(7) . . no C43 H70 0.944(5) . 1_554 no C15 H21 0.947(6) . 1_454 no C43 H71 0.966(9) . 1_554 no C15 H22 0.951(2) . . no C44 H72 0.952(6) . . no C17 H23 0.953(5) . . no C44 H73 0.955(3) . . no C17 H24 0.952(5) . . no C44 H74 0.980(12) . . no C19 H25 0.955(2) . . no C45 H75 0.950(3) . . no C19 H26 0.961(6) . 1_565 no C45 H76 0.947(7) . . no C19 H27 0.956(6) . . no C45 H77 0.988(11) . . no C20 H28 0.947(3) . 1_545 no C47 H78 0.959(4) . 1_556 no C20 H29 0.949(7) . . no C47 H79 0.945(2) . . no C20 H30 0.950(6) . . no C49 H80 0.964(2) . . no C21 H31 0.955(7) . . no C49 H81 0.957(8) . . no C21 H32 0.951(6) . . no C49 H82 0.952(5) . 1_554 no C21 H33 0.946(3) . 1_545 no C50 H83 0.955(9) . 1_554 no C23 H34 0.947(7) . . no C50 H84 0.965(13) . . no C23 H35 0.957(6) . . no C50 H85 0.958(3) . 1_554 no C25 H36 0.950(6) . . no C51 H86 0.944(9) . 1_556 no C25 H37 0.969(8) . . no C51 H87 0.954(9) . 1_556 no C25 H38 0.954(7) . . no C51 H88 0.983(6) . . no C26 H39 0.956(2) . . no C26 H40 0.968(9) . . no C26 H41 0.947(7) . . no C27 H42 0.962(8) . . no C27 H43 0.9569(13) . . no C27 H44 0.957(8) . . no C29 H45 0.954(4) . . no C29 H46 0.946(4) . . no C31 H47 0.953(5) . . no C31 H48 0.959(5) . . no C31 H49 0.959(3) . . no C32 H50 0.956(9) . . no loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag W2 W1 S3 56.07(4) 1_554 . . no W2 W1 O4 51.22(6) 1_554 . 1_554 no W2 W1 O10 51.22(12) 1_554 . . no W2 W1 O16 125.11(9) 1_554 . . no W2 W1 O22 120.86(8) 1_554 . . no W2 W1 O28 122.95(14) 1_554 . . no S3 W1 O4 93.39(11) . . 1_554 no S3 W1 O10 92.83(10) . . . no S3 W1 O16 178.51(11) . . . no S3 W1 O22 91.14(11) . . . no S3 W1 O28 91.65(12) . . . no O4 W1 O10 75.00(13) 1_554 . . no O4 W1 O16 86.99(14) 1_554 . . no O4 W1 O22 163.81(16) 1_554 . . no O4 W1 O28 92.19(14) 1_554 . . no O10 W1 O16 88.66(14) . . . no O10 W1 O22 89.28(14) . . . no O10 W1 O28 166.64(8) . . . no O16 W1 O22 88.87(14) . . . no O16 W1 O28 86.89(15) . . . no O22 W1 O28 103.21(14) . . . no W1 W2 S3 56.10(4) 1_556 . 1_556 no W1 W2 O4 50.76(9) 1_556 . . no W1 W2 O10 51.01(8) 1_556 . 1_556 no W1 W2 O34 124.67(10) 1_556 . 1_556 no W1 W2 O40 123.05(12) 1_556 . 1_556 no W1 W2 O46 121.71(10) 1_556 . 1_556 no S3 W2 O4 93.07(9) 1_556 . . no S3 W2 O10 92.70(9) 1_556 . 1_556 no S3 W2 O34 179.18(8) 1_556 . 1_556 no S3 W2 O40 91.52(10) 1_556 . 1_556 no S3 W2 O46 91.57(11) 1_556 . 1_556 no O4 W2 O10 74.58(14) . . 1_556 no O4 W2 O34 87.70(10) . . 1_556 no O4 W2 O40 165.9(2) . . 1_556 no O4 W2 O46 90.93(14) . . 1_556 no O10 W2 O34 87.76(16) 1_556 . 1_556 no O10 W2 O40 91.93(16) 1_556 . 1_556 no O10 W2 O46 165.09(4) 1_556 . 1_556 no O34 W2 O40 87.79(11) 1_556 . 1_556 no O34 W2 O46 88.15(17) 1_556 . 1_556 no O40 W2 O46 102.24(16) 1_556 . 1_556 no W1 S3 W2 67.82(5) . . 1_554 no W1 O4 W2 78.03(5) 1_556 . . no W1 O4 C5 130.3(4) 1_556 . . no W2 O4 C5 130.8(3) . . . no W1 O10 W2 77.78(15) . . 1_554 no W1 O10 C11 129.58(18) . . . no W2 O10 C11 127.7(3) 1_554 . . no W1 O16 C17 124.7(2) . . . no W1 O22 C23 132.3(4) . . . no W1 O28 C29 139.0(3) . . . no W2 O34 C35 125.6(3) 1_554 . 1_554 no W2 O40 C41 136.7(3) 1_554 . . no W2 O46 C47 134.8(3) 1_554 . 1_554 no O4 C5 C6 112.3(5) . . . no C5 C6 C7 109.3(3) . . . no C5 C6 C8 109.8(4) . . 1_556 no C5 C6 C9 106.7(6) . . 1_545 no C7 C6 C8 110.9(6) . . 1_556 no C7 C6 C9 110.0(4) . . 1_545 no C8 C6 C9 109.9(3) 1_556 . 1_545 no O10 C11 C12 112.8(2) . . . no C11 C12 C13 110.4(5) . . . no C11 C12 C14 108.9(4) . . . no C11 C12 C15 106.6(3) . . . no C13 C12 C14 111.8(3) . . . no C13 C12 C15 110.5(4) . . . no C14 C12 C15 108.6(5) . . . no O16 C17 C18 112.5(3) . . . no C17 C18 C19 110.4(5) . . 1_545 no C17 C18 C20 107.7(3) . . . no C17 C18 C21 110.3(3) . . . no C19 C18 C20 108.8(4) 1_545 . . no C19 C18 C21 109.9(3) 1_545 . . no C20 C18 C21 109.7(6) . . . no O22 C23 C24 112.6(4) . . . no C23 C24 C25 106.7(4) . . . no C23 C24 C26 108.6(6) . . . no C23 C24 C27 111.1(4) . . . no C25 C24 C26 108.5(4) . . . no C25 C24 C27 110.7(6) . . . no C26 C24 C27 111.1(5) . . . no O28 C29 C30 110.5(6) . . . no C29 C30 C31 108.3(6) . . . no C29 C30 C32 110.4(3) . . . no C29 C30 C33 109.1(4) . . . no C31 C30 C32 110.7(4) . . . no C31 C30 C33 108.4(4) . . . no C32 C30 C33 109.9(6) . . . no O34 C35 C36 113.2(5) 1_556 . 1_556 no C35 C36 C37 108.0(6) 1_554 . . no C35 C36 C38 110.2(4) 1_554 . . no C35 C36 C39 110.1(4) 1_554 . 1_454 no C37 C36 C38 109.4(4) . . . no C37 C36 C39 109.4(4) . . 1_454 no C38 C36 C39 109.8(6) . . 1_454 no O40 C41 C42 112.2(4) . . . no C41 C42 C43 109.4(4) . . . no C41 C42 C44 109.0(6) . . . no C41 C42 C45 109.9(5) . . . no C43 C42 C44 109.1(5) . . . no C43 C42 C45 110.2(6) . . . no C44 C42 C45 109.1(6) . . . no O46 C47 C48 110.8(4) 1_556 . 1_556 no C47 C48 C49 108.0(5) 1_554 . . no C47 C48 C50 109.5(6) 1_554 . . no C47 C48 C51 110.4(5) 1_554 . 1_554 no C49 C48 C50 108.5(5) . . . no C49 C48 C51 110.3(5) . . 1_554 no C50 C48 C51 110.1(4) . . 1_554 no O4 C5 H1 108.7(4) . . . no O4 C5 H2 108.38(18) . . . no C6 C5 H1 109.1(2) . . . no C6 C5 H2 108.9(4) . . . no H1 C5 H2 109.5(7) . . . no C6 C7 H3 110.4(4) . . 1_556 no C6 C7 H4 111.1(4) . . 1_545 no C6 C7 H5 110.6(7) . . 1_556 no H3 C7 H4 108.5(8) 1_556 . 1_545 no H3 C7 H5 107.6(4) 1_556 . 1_556 no H4 C7 H5 108.5(5) 1_545 . 1_556 no C6 C8 H6 110.6(7) 1_554 . 1_545 no C6 C8 H7 110.1(4) 1_554 . 1_544 no C6 C8 H8 110.3(3) 1_554 . . no H6 C8 H7 108.6(3) 1_545 . 1_544 no H6 C8 H8 108.9(4) 1_545 . . no H7 C8 H8 108.3(8) 1_544 . . no C6 C9 H9 110.4(3) 1_565 . 1_566 no C6 C9 H10 110.9(7) 1_565 . 1_566 no C6 C9 H11 110.9(4) 1_565 . . no H9 C9 H10 107.9(5) 1_566 . 1_566 no H9 C9 H11 107.9(8) 1_566 . . no H10 C9 H11 108.8(3) 1_566 . . no O10 C11 H12 108.3(5) . . . no O10 C11 H13 108.3(4) . . 1_554 no C12 C11 H12 108.9(5) . . . no C12 C11 H13 109.3(6) . . 1_554 no H12 C11 H13 109.1(2) . . 1_554 no C12 C13 H14 110.5(4) . . 1_554 no C12 C13 H15 109.9(3) . . . no C12 C13 H16 110.7(6) . . 1_454 no H14 C13 H15 108.5(7) 1_554 . . no H14 C13 H16 108.6(3) 1_554 . 1_454 no H15 C13 H16 108.6(5) . . 1_454 no C12 C14 H17 110.2(3) . . . no C12 C14 H18 110.3(7) . . . no C12 C14 H19 111.0(4) . . . no H17 C14 H18 107.8(5) . . . no H17 C14 H19 108.6(7) . . . no H18 C14 H19 108.9(4) . . . no C12 C15 H20 109.6(3) . . . no C12 C15 H21 109.3(6) . . 1_454 no C12 C15 H22 109.7(5) . . . no H20 C15 H21 109.4(5) . . 1_454 no H20 C15 H22 109.1(7) . . . no H21 C15 H22 109.7(3) 1_454 . . no O16 C17 H23 108.9(6) . . . no O16 C17 H24 109.0(3) . . . no C18 C17 H23 108.5(3) . . . no C18 C17 H24 108.8(6) . . . no H23 C17 H24 109.0(3) . . . no C18 C19 H25 110.9(7) 1_565 . . no C18 C19 H26 110.3(4) 1_565 . 1_565 no C18 C19 H27 110.7(3) 1_565 . . no H25 C19 H26 108.2(3) . . 1_565 no H25 C19 H27 108.6(4) . . . no H26 C19 H27 108.1(7) 1_565 . . no C18 C20 H28 109.4(3) . . 1_545 no C18 C20 H29 109.1(7) . . . no C18 C20 H30 109.2(4) . . . no H28 C20 H29 109.8(4) 1_545 . . no H28 C20 H30 109.7(8) 1_545 . . no H29 C20 H30 109.6(4) . . . no C18 C21 H31 109.4(4) . . . no C18 C21 H32 109.4(7) . . . no C18 C21 H33 109.9(4) . . 1_545 no H31 C21 H32 109.0(4) . . . no H31 C21 H33 109.4(8) . . 1_545 no H32 C21 H33 109.7(4) . . 1_545 no O22 C23 H34 109.0(6) . . . no O22 C23 H35 108.4(3) . . . no C24 C23 H34 109.2(4) . . . no C24 C23 H35 108.5(6) . . . no H34 C23 H35 109.1(5) . . . no C24 C25 H36 111.1(5) . . . no C24 C25 H37 110.1(6) . . . no C24 C25 H38 110.9(4) . . . no H36 C25 H37 107.9(5) . . . no H36 C25 H38 109.2(8) . . . no H37 C25 H38 107.6(5) . . . no C24 C26 H39 110.7(5) . . . no C24 C26 H40 110.0(5) . . . no C24 C26 H41 111.2(8) . . . no H39 C26 H40 107.4(8) . . . no H39 C26 H41 109.2(6) . . . no H40 C26 H41 108.2(6) . . . no C24 C27 H42 110.7(7) . . . no C24 C27 H43 111.1(9) . . . no C24 C27 H44 110.9(5) . . . no H42 C27 H43 107.9(5) . . . no H42 C27 H44 107.9(10) . . . no H43 C27 H44 108.3(7) . . . no O28 C29 H45 108.7(4) . . . no O28 C29 H46 109.3(4) . . . no C30 C29 H45 109.2(4) . . . no C30 C29 H46 109.6(4) . . . no H45 C29 H46 109.5(7) . . . no C30 C31 H47 110.8(6) . . . no C30 C31 H48 110.6(4) . . . no C30 C31 H49 110.5(5) . . . no H47 C31 H48 108.4(5) . . . no H47 C31 H49 108.5(4) . . . no H48 C31 H49 108.0(7) . . . no C30 C32 H50 110.7(5) . . . no C30 C32 H51 110.4(7) . . . no C30 C32 H52 110.8(4) . . . no H50 C32 H51 108.0(4) . . . no H50 C32 H52 108.7(8) . . . no H51 C32 H52 108.1(5) . . . no C30 C33 H53 111.3(5) . . . no C30 C33 H54 110.4(7) . . . no C30 C33 H55 110.9(4) . . . no H53 C33 H54 108.0(4) . . . no H53 C33 H55 108.7(8) . . . no H54 C33 H55 107.4(5) . . . no O34 C35 H56 108.8(3) 1_556 . 1_556 no O34 C35 H57 108.5(4) 1_556 . . no C36 C35 H56 108.4(4) 1_556 . 1_556 no C36 C35 H57 108.8(4) 1_556 . . no H56 C35 H57 109.0(7) 1_556 . . no C36 C37 H58 109.2(4) . . . no C36 C37 H59 109.0(4) . . . no C36 C37 H60 109.4(6) . . 1_454 no H58 C37 H59 109.4(7) . . . no H58 C37 H60 110.3(4) . . 1_454 no H59 C37 H60 109.4(4) . . 1_454 no C36 C38 H61 110.6(4) . . . no C36 C38 H62 110.5(7) . . 1_554 no C36 C38 H63 110.7(4) . . . no H61 C38 H62 108.1(4) . . 1_554 no H61 C38 H63 108.7(8) . . . no H62 C38 H63 108.2(4) 1_554 . . no C36 C39 H64 110.2(7) 1_656 . . no C36 C39 H65 110.9(5) 1_656 . 1_656 no C36 C39 H66 110.9(4) 1_656 . 1_656 no H64 C39 H65 108.0(4) . . 1_656 no H64 C39 H66 108.1(5) . . 1_656 no H65 C39 H66 108.8(7) 1_656 . 1_656 no O40 C41 H67 109.2(5) . . . no O40 C41 H68 108.6(5) . . . no C42 C41 H67 109.3(5) . . . no C42 C41 H68 108.5(6) . . . no H67 C41 H68 109.1(5) . . . no C42 C43 H69 110.4(5) . . . no C42 C43 H70 111.5(5) . . 1_554 no C42 C43 H71 110.3(6) . . 1_554 no H69 C43 H70 108.9(7) . . 1_554 no H69 C43 H71 107.1(6) . . 1_554 no H70 C43 H71 108.6(6) 1_554 . 1_554 no C42 C44 H72 112.0(8) . . . no C42 C44 H73 111.8(7) . . . no C42 C44 H74 110.5(6) . . . no H72 C44 H73 108.9(7) . . . no H72 C44 H74 106.8(8) . . . no H73 C44 H74 106.6(9) . . . no C42 C45 H75 112.0(11) . . . no C42 C45 H76 112.2(9) . . . no C42 C45 H77 109.8(8) . . . no H75 C45 H76 109.7(9) . . . no H75 C45 H77 106.3(10) . . . no H76 C45 H77 106.5(12) . . . no O46 C47 H78 108.6(5) 1_556 . 1_556 no O46 C47 H79 109.3(5) 1_556 . . no C48 C47 H78 108.9(5) 1_556 . 1_556 no C48 C47 H79 110.1(5) 1_556 . . no H78 C47 H79 109.1(5) 1_556 . . no C48 C49 H80 110.4(6) . . . no C48 C49 H81 110.8(6) . . . no C48 C49 H82 110.8(5) . . 1_554 no H80 C49 H81 107.8(6) . . . no H80 C49 H82 108.2(6) . . 1_554 no H81 C49 H82 108.8(7) . . 1_554 no C48 C50 H83 111.2(8) . . 1_554 no C48 C50 H84 110.6(7) . . . no C48 C50 H85 111.0(7) . . 1_554 no H83 C50 H84 107.8(8) 1_554 . . no H83 C50 H85 108.4(8) 1_554 . 1_554 no H84 C50 H85 107.6(9) . . 1_554 no C48 C51 H86 112.3(6) 1_556 . 1_556 no C48 C51 H87 111.6(6) 1_556 . 1_556 no C48 C51 H88 109.4(5) 1_556 . . no H86 C51 H87 109.7(7) 1_556 . 1_556 no H86 C51 H88 107.2(7) 1_556 . . no H87 C51 H88 106.4(6) 1_556 . . no # The following lines may be used to test the character set of files sent by # network email or other means. They are not part of the CIF data archive. # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ 2===END data_CIF_for_W2(?-Se)(OCH2tBu)8 _database_code_CSD 158780 _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C40 H88 O8 Se W2' _chemical_formula_sum 'C40 H88 O8 Se W2' _chemical_formula_weight 1143.76 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 '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 12.258(2) _cell_length_b 14.780(3) _cell_length_c 14.777(3) _cell_angle_alpha 93.239(5) _cell_angle_beta 113.413(5) _cell_angle_gamma 91.936(5) _cell_volume 2448.1(8) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 783 _cell_measurement_theta_min 3 _cell_measurement_theta_max 25 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.552 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1148 _exptl_absorpt_coefficient_mu 5.480 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.3412 _exptl_absorpt_correction_T_max 0.6683 _exptl_absorpt_process_details SADABS _diffrn_ambient_temperature 113(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 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_measurement_method '\w scans' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_number 230 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 717 _diffrn_standards_decay_% -0.1 _diffrn_reflns_number 41540 _diffrn_reflns_av_R_equivalents 0.064 _diffrn_reflns_av_sigmaI/netI 0.1917 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 30.00 _diffrn_measured_fraction_theta_max 0.266 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.266 _reflns_number_total 13788 _reflns_number_gt 7554 _reflns_threshold_expression 'I > 2\s(I)' _diffrn_measurement_details ; 0.30 degree frames measured for 10.14 seconds each ; _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SMART (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XTEL (local library)' _computing_publication_material 'XTEL (local library)' _refine_special_details ; The data collection crystal was twinned, as no single crystal could be located in the sample. The twinning was resolved with the use of Bruker's Gemini software version 1.02. The structure was solved with and refined on F^2^ against all completely overlapped and non-overlapped reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [\s^2^(Fo^2^)+(0.05Fo^2^)^2^]^-1^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13788 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1002 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1214 _refine_ls_wR_factor_gt 0.0999 _refine_ls_goodness_of_fit_ref 0.721 _refine_ls_restrained_S_all 0.721 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.741 _refine_diff_density_min -1.309 _refine_diff_density_rms 0.155 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 0.61792(3) 0.246582(15) 0.295080(16) 0.01484(11) Uani 1 1 d . . . W2 W 0.39746(3) 0.286138(15) 0.262265(16) 0.01470(11) Uani 1 1 d . . . Se3 Se 0.57262(8) 0.36352(4) 0.40058(5) 0.0215(2) Uani 1 1 d . . . O4 O 0.4818(5) 0.2812(3) 0.1648(3) 0.0161(9) Uiso 1 1 d . . . C5 C 0.4395(8) 0.2346(4) 0.0669(4) 0.0162(12) Uiso 1 1 d . . . H5A H 0.3521 0.2227 0.0414 0.019 Uiso 1 1 calc R . . H5B H 0.4758 0.1753 0.0714 0.019 Uiso 1 1 calc R . . C6 C 0.4695(8) 0.2894(4) -0.0055(5) 0.0223(14) Uiso 1 1 d . . . C7 C 0.5994(9) 0.2897(6) 0.0157(7) 0.041(2) Uiso 1 1 d . . . H7A H 0.6454 0.3196 0.0816 0.061 Uiso 1 1 calc R . . H7B H 0.6154 0.3226 -0.0339 0.061 Uiso 1 1 calc R . . H7C H 0.6225 0.2270 0.0133 0.061 Uiso 1 1 calc R . . C8 C 0.4288(8) 0.3866(4) -0.0027(5) 0.0263(15) Uiso 1 1 d . . . H8A H 0.4747 0.4177 0.0626 0.039 Uiso 1 1 calc R . . H8B H 0.3439 0.3840 -0.0154 0.039 Uiso 1 1 calc R . . H8C H 0.4418 0.4198 -0.0535 0.039 Uiso 1 1 calc R . . C9 C 0.3962(8) 0.2424(5) -0.1090(5) 0.0286(16) Uiso 1 1 d . . . H9A H 0.4212 0.1804 -0.1123 0.043 Uiso 1 1 calc R . . H9B H 0.4095 0.2765 -0.1591 0.043 Uiso 1 1 calc R . . H9C H 0.3115 0.2403 -0.1214 0.043 Uiso 1 1 calc R . . O10 O 0.4719(5) 0.1607(3) 0.2764(3) 0.0164(9) Uiso 1 1 d . . . C11 C 0.4297(7) 0.0760(4) 0.2149(4) 0.0157(12) Uiso 1 1 d . . . H11A H 0.4944 0.0529 0.1976 0.019 Uiso 1 1 calc R . . H11B H 0.3622 0.0874 0.1527 0.019 Uiso 1 1 calc R . . C12 C 0.3891(8) 0.0034(5) 0.2683(5) 0.0251(15) Uiso 1 1 d . . . C13 C 0.4917(8) -0.0060(5) 0.3709(5) 0.0246(15) Uiso 1 1 d . . . H13A H 0.4671 -0.0515 0.4058 0.037 Uiso 1 1 calc R . . H13B H 0.5102 0.0526 0.4099 0.037 Uiso 1 1 calc R . . H13C H 0.5626 -0.0250 0.3615 0.037 Uiso 1 1 calc R . . C14 C 0.3695(9) -0.0859(5) 0.2059(5) 0.0297(16) Uiso 1 1 d . . . H14A H 0.3054 -0.0809 0.1408 0.044 Uiso 1 1 calc R . . H14B H 0.3475 -0.1347 0.2389 0.044 Uiso 1 1 calc R . . H14C H 0.4430 -0.0995 0.1980 0.044 Uiso 1 1 calc R . . C15 C 0.2784(9) 0.0278(6) 0.2790(7) 0.040(2) Uiso 1 1 d . . . H15A H 0.2149 0.0321 0.2134 0.060 Uiso 1 1 calc R . . H15B H 0.2924 0.0863 0.3176 0.060 Uiso 1 1 calc R . . H15C H 0.2546 -0.0191 0.3131 0.060 Uiso 1 1 calc R . . O16 O 0.6573(6) 0.1550(3) 0.2163(4) 0.0195(11) Uiso 1 1 d . . . C17 C 0.7757(8) 0.1404(5) 0.2304(6) 0.0202(16) Uiso 1 1 d . . . H17A H 0.8280 0.1536 0.3013 0.024 Uiso 1 1 calc R . . H17B H 0.8011 0.1830 0.1922 0.024 Uiso 1 1 calc R . . C18 C 0.7912(7) 0.0425(4) 0.1981(4) 0.0167(12) Uiso 1 1 d . . . C19 C 0.7125(8) 0.0211(5) 0.0897(5) 0.0285(16) Uiso 1 1 d . . . H19A H 0.6289 0.0260 0.0793 0.043 Uiso 1 1 calc R . . H19B H 0.7242 -0.0408 0.0692 0.043 Uiso 1 1 calc R . . H19C H 0.7335 0.0642 0.0503 0.043 Uiso 1 1 calc R . . C20 C 0.7559(8) -0.0230(5) 0.2599(5) 0.0267(15) Uiso 1 1 d . . . H20A H 0.6718 -0.0177 0.2476 0.040 Uiso 1 1 calc R . . H20B H 0.8051 -0.0079 0.3302 0.040 Uiso 1 1 calc R . . H20C H 0.7681 -0.0854 0.2414 0.040 Uiso 1 1 calc R . . C21 C 0.9236(8) 0.0345(5) 0.2165(6) 0.0319(17) Uiso 1 1 d . . . H21A H 0.9456 0.0770 0.1772 0.048 Uiso 1 1 calc R . . H21B H 0.9357 -0.0277 0.1971 0.048 Uiso 1 1 calc R . . H21C H 0.9733 0.0489 0.2869 0.048 Uiso 1 1 calc R . . O22 O 0.7249(5) 0.3297(3) 0.2750(3) 0.0205(10) Uiso 1 1 d . . . C23 C 0.7251(8) 0.4244(4) 0.2648(5) 0.0227(14) Uiso 1 1 d . . . H23A H 0.7071 0.4554 0.3180 0.027 Uiso 1 1 calc R . . H23B H 0.6614 0.4366 0.2007 0.027 Uiso 1 1 calc R . . C24 C 0.8435(8) 0.4634(5) 0.2696(5) 0.0242(15) Uiso 1 1 d . . . C25 C 0.8322(10) 0.5658(6) 0.2555(7) 0.042(2) Uiso 1 1 d . . . H25A H 0.8127 0.5951 0.3079 0.063 Uiso 1 1 calc R . . H25B H 0.7689 0.5743 0.1910 0.063 Uiso 1 1 calc R . . H25C H 0.9078 0.5929 0.2588 0.063 Uiso 1 1 calc R . . C26 C 0.8748(10) 0.4218(7) 0.1877(7) 0.049(2) Uiso 1 1 d . . . H26A H 0.8833 0.3566 0.1947 0.074 Uiso 1 1 calc R . . H26B H 0.9500 0.4508 0.1920 0.074 Uiso 1 1 calc R . . H26C H 0.8114 0.4313 0.1235 0.074 Uiso 1 1 calc R . . C27 C 0.9399(10) 0.4522(6) 0.3718(7) 0.044(2) Uiso 1 1 d . . . H27A H 0.9163 0.4799 0.4226 0.066 Uiso 1 1 calc R . . H27B H 1.0151 0.4821 0.3773 0.066 Uiso 1 1 calc R . . H27C H 0.9503 0.3875 0.3812 0.066 Uiso 1 1 calc R . . O28 O 0.7173(5) 0.1902(3) 0.4065(3) 0.0232(10) Uiso 1 1 d . . . C29 C 0.7405(8) 0.1890(5) 0.5103(5) 0.0280(15) Uiso 1 1 d . . . H29A H 0.7024 0.1333 0.5219 0.034 Uiso 1 1 calc R . . H29B H 0.7073 0.2422 0.5317 0.034 Uiso 1 1 calc R . . C30 C 0.8758(9) 0.1916(4) 0.5695(5) 0.0226(14) Uiso 1 1 d . . . C31 C 0.8974(9) 0.1985(5) 0.6775(6) 0.0316(17) Uiso 1 1 d . . . H31A H 0.8600 0.1449 0.6923 0.047 Uiso 1 1 calc R . . H31B H 0.8630 0.2532 0.6927 0.047 Uiso 1 1 calc R . . H31C H 0.9833 0.2018 0.7178 0.047 Uiso 1 1 calc R . . C32 C 0.9330(9) 0.2768(5) 0.5465(6) 0.039(2) Uiso 1 1 d . . . H32A H 0.9179 0.2730 0.4761 0.059 Uiso 1 1 calc R . . H32B H 1.0190 0.2805 0.5861 0.059 Uiso 1 1 calc R . . H32C H 0.8983 0.3309 0.5626 0.059 Uiso 1 1 calc R . . C33 C 0.9288(9) 0.1060(5) 0.5437(6) 0.0312(18) Uiso 1 1 d . . . H33A H 0.8899 0.0520 0.5563 0.047 Uiso 1 1 calc R . . H33B H 1.0144 0.1082 0.5847 0.047 Uiso 1 1 calc R . . H33C H 0.9158 0.1034 0.4737 0.047 Uiso 1 1 calc R . . O34 O 0.2575(6) 0.2294(3) 0.1543(4) 0.0168(11) Uiso 1 1 d . . . C35 C 0.1400(8) 0.2475(5) 0.1388(5) 0.0193(15) Uiso 1 1 d . . . H35A H 0.1367 0.3129 0.1555 0.023 Uiso 1 1 calc R . . H35B H 0.1157 0.2128 0.1838 0.023 Uiso 1 1 calc R . . C36 C 0.0519(8) 0.2226(4) 0.0321(5) 0.0188(13) Uiso 1 1 d . . . C37 C 0.0842(9) 0.2797(5) -0.0367(6) 0.0356(18) Uiso 1 1 d . . . H37A H 0.1643 0.2668 -0.0316 0.053 Uiso 1 1 calc R . . H37B H 0.0825 0.3442 -0.0181 0.053 Uiso 1 1 calc R . . H37C H 0.0267 0.2651 -0.1050 0.053 Uiso 1 1 calc R . . C38 C -0.0718(8) 0.2421(4) 0.0233(5) 0.0239(14) Uiso 1 1 d . . . H38A H -0.0744 0.3069 0.0401 0.036 Uiso 1 1 calc R . . H38B H -0.0922 0.2064 0.0689 0.036 Uiso 1 1 calc R . . H38C H -0.1291 0.2258 -0.0446 0.036 Uiso 1 1 calc R . . C39 C 0.0566(9) 0.1211(5) 0.0047(6) 0.0334(18) Uiso 1 1 d . . . H39A H 0.1367 0.1091 0.0093 0.050 Uiso 1 1 calc R . . H39B H -0.0015 0.1049 -0.0630 0.050 Uiso 1 1 calc R . . H39C H 0.0376 0.0846 0.0505 0.050 Uiso 1 1 calc R . . O40 O 0.3277(5) 0.2579(3) 0.3500(3) 0.0212(10) Uiso 1 1 d . . . C41 C 0.3674(9) 0.2423(5) 0.4511(6) 0.0332(18) Uiso 1 1 d . . . H41A H 0.4381 0.2835 0.4896 0.040 Uiso 1 1 calc R . . H41B H 0.3916 0.1791 0.4603 0.040 Uiso 1 1 calc R . . C42 C 0.2703(9) 0.2577(5) 0.4904(5) 0.0250(15) Uiso 1 1 d . . . C43 C 0.2369(11) 0.3539(6) 0.4810(7) 0.052(2) Uiso 1 1 d . . . H43A H 0.3071 0.3944 0.5195 0.078 Uiso 1 1 calc R . . H43B H 0.1749 0.3633 0.5061 0.078 Uiso 1 1 calc R . . H43C H 0.2068 0.3670 0.4113 0.078 Uiso 1 1 calc R . . C44 C 0.3221(10) 0.2387(6) 0.5998(7) 0.045(2) Uiso 1 1 d . . . H44A H 0.3851 0.2853 0.6376 0.067 Uiso 1 1 calc R . . H44B H 0.3555 0.1789 0.6072 0.067 Uiso 1 1 calc R . . H44C H 0.2590 0.2396 0.6247 0.067 Uiso 1 1 calc R . . C45 C 0.1606(13) 0.1954(10) 0.4349(11) 0.091(4) Uiso 1 1 d . . . H45A H 0.1285 0.2066 0.3646 0.137 Uiso 1 1 calc R . . H45B H 0.1004 0.2070 0.4615 0.137 Uiso 1 1 calc R . . H45C H 0.1818 0.1321 0.4426 0.137 Uiso 1 1 calc R . . O46 O 0.3361(5) 0.3982(3) 0.2209(3) 0.0220(10) Uiso 1 1 d . . . C47 C 0.3807(9) 0.4901(5) 0.2329(6) 0.0342(18) Uiso 1 1 d . . . H47A H 0.4138 0.5010 0.1830 0.041 Uiso 1 1 calc R . . H47B H 0.4456 0.5027 0.2994 0.041 Uiso 1 1 calc R . . C48 C 0.2786(8) 0.5549(4) 0.2205(5) 0.0222(14) Uiso 1 1 d . . . C49 C 0.2269(10) 0.5366(7) 0.2962(7) 0.052(2) Uiso 1 1 d . . . H49A H 0.1903 0.4747 0.2830 0.079 Uiso 1 1 calc R . . H49B H 0.1666 0.5800 0.2916 0.079 Uiso 1 1 calc R . . H49C H 0.2907 0.5434 0.3627 0.079 Uiso 1 1 calc R . . C50 C 0.1894(10) 0.5391(6) 0.1161(7) 0.048(2) Uiso 1 1 d . . . H50A H 0.2284 0.5499 0.0709 0.072 Uiso 1 1 calc R . . H50B H 0.1255 0.5806 0.1047 0.072 Uiso 1 1 calc R . . H50C H 0.1559 0.4762 0.1042 0.072 Uiso 1 1 calc R . . C51 C 0.3371(9) 0.6509(5) 0.2398(6) 0.0361(18) Uiso 1 1 d . . . H51A H 0.3713 0.6612 0.1912 0.054 Uiso 1 1 calc R . . H51B H 0.4004 0.6582 0.3065 0.054 Uiso 1 1 calc R . . H51C H 0.2773 0.6951 0.2339 0.054 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 0.0140(3) 0.01659(11) 0.01414(11) 0.00106(8) 0.00585(12) 0.00110(11) W2 0.0144(3) 0.01497(11) 0.01509(11) 0.00087(8) 0.00631(12) 0.00102(11) Se3 0.0167(7) 0.0261(3) 0.0208(3) -0.0063(2) 0.0078(3) -0.0007(3) _geom_special_details ; All esds 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. ; 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 O28 1.876(5) . ? W1 O22 1.886(6) . ? W1 O16 1.933(6) . ? W1 O10 2.075(5) . ? W1 O4 2.090(4) . ? W1 Se3 2.4847(8) . ? W1 W2 2.6414(7) . ? W2 O40 1.873(6) . ? W2 O46 1.875(4) . ? W2 O34 1.941(5) . ? W2 O10 2.078(4) . ? W2 O4 2.079(5) . ? W2 Se3 2.4855(8) . ? O4 C5 1.450(7) . ? C5 C6 1.526(10) . ? C6 C7 1.495(13) . ? C6 C9 1.540(9) . ? C6 C8 1.541(9) . ? O10 C11 1.454(7) . ? C11 C12 1.547(10) . ? C12 C15 1.481(13) . ? C12 C14 1.521(9) . ? C12 C13 1.556(10) . ? O16 C17 1.407(11) . ? C17 C18 1.539(9) . ? C18 C19 1.514(9) . ? C18 C20 1.530(10) . ? C18 C21 1.545(13) . ? O22 C23 1.416(7) . ? C23 C24 1.516(13) . ? C24 C26 1.514(13) . ? C24 C27 1.526(11) . ? C24 C25 1.542(10) . ? O28 C29 1.446(8) . ? C29 C30 1.534(13) . ? C30 C31 1.506(10) . ? C30 C33 1.537(11) . ? C30 C32 1.540(12) . ? O34 C35 1.404(10) . ? C35 C36 1.530(9) . ? C36 C38 1.509(12) . ? C36 C37 1.516(11) . ? C36 C39 1.541(9) . ? O40 C41 1.410(9) . ? C41 C42 1.536(13) . ? C42 C43 1.491(11) . ? C42 C45 1.511(16) . ? C42 C44 1.531(11) . ? O46 C47 1.421(9) . ? C47 C48 1.560(11) . ? C48 C50 1.493(11) . ? C48 C49 1.520(14) . ? C48 C51 1.528(11) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? 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 O28 W1 O22 102.6(2) . . ? O28 W1 O16 87.1(2) . . ? O22 W1 O16 88.8(2) . . ? O28 W1 O10 92.4(2) . . ? O22 W1 O10 164.05(17) . . ? O16 W1 O10 86.6(2) . . ? O28 W1 O4 166.4(2) . . ? O22 W1 O4 89.9(2) . . ? O16 W1 O4 87.98(19) . . ? O10 W1 O4 74.67(18) . . ? O28 W1 Se3 91.40(15) . . ? O22 W1 Se3 90.93(14) . . ? O16 W1 Se3 178.33(16) . . ? O10 W1 Se3 94.04(13) . . ? O4 W1 Se3 93.67(12) . . ? O28 W1 W2 123.72(18) . . ? O22 W1 W2 121.68(15) . . ? O16 W1 W2 123.55(18) . . ? O10 W1 W2 50.57(12) . . ? O4 W1 W2 50.52(14) . . ? Se3 W1 W2 57.91(2) . . ? O40 W2 O46 102.5(2) . . ? O40 W2 O34 89.0(2) . . ? O46 W2 O34 87.2(2) . . ? O40 W2 O10 90.5(2) . . ? O46 W2 O10 166.1(2) . . ? O34 W2 O10 88.02(19) . . ? O40 W2 O4 164.90(17) . . ? O46 W2 O4 91.9(2) . . ? O34 W2 O4 87.0(2) . . ? O10 W2 O4 74.82(18) . . ? O40 W2 Se3 90.59(15) . . ? O46 W2 Se3 90.97(15) . . ? O34 W2 Se3 178.00(16) . . ? O10 W2 Se3 93.93(13) . . ? O4 W2 Se3 93.90(13) . . ? O40 W2 W1 121.59(16) . . ? O46 W2 W1 123.40(18) . . ? O34 W2 W1 123.93(18) . . ? O10 W2 W1 50.46(15) . . ? O4 W2 W1 50.86(12) . . ? Se3 W2 W1 57.88(2) . . ? W1 Se3 W2 64.21(2) . . ? C5 O4 W2 128.0(5) . . ? C5 O4 W1 128.3(4) . . ? W2 O4 W1 78.63(14) . . ? O4 C5 C6 112.3(5) . . ? C7 C6 C5 111.3(6) . . ? C7 C6 C9 109.9(7) . . ? C5 C6 C9 106.0(6) . . ? C7 C6 C8 111.5(7) . . ? C5 C6 C8 109.8(6) . . ? C9 C6 C8 108.3(6) . . ? C11 O10 W1 128.5(5) . . ? C11 O10 W2 130.4(4) . . ? W1 O10 W2 78.97(15) . . ? O10 C11 C12 111.5(5) . . ? C15 C12 C14 110.9(8) . . ? C15 C12 C11 111.0(6) . . ? C14 C12 C11 106.6(6) . . ? C15 C12 C13 111.2(7) . . ? C14 C12 C13 108.4(6) . . ? C11 C12 C13 108.5(7) . . ? C17 O16 W1 122.3(5) . . ? O16 C17 C18 112.5(7) . . ? C19 C18 C20 109.5(6) . . ? C19 C18 C17 109.9(5) . . ? C20 C18 C17 108.9(6) . . ? C19 C18 C21 110.5(6) . . ? C20 C18 C21 110.0(6) . . ? C17 C18 C21 108.0(6) . . ? C23 O22 W1 132.9(5) . . ? O22 C23 C24 112.3(6) . . ? C26 C24 C23 112.3(7) . . ? C26 C24 C27 112.0(8) . . ? C23 C24 C27 109.2(7) . . ? C26 C24 C25 107.2(7) . . ? C23 C24 C25 107.7(7) . . ? C27 C24 C25 108.3(7) . . ? C29 O28 W1 138.9(5) . . ? O28 C29 C30 108.5(7) . . ? C31 C30 C29 107.2(8) . . ? C31 C30 C33 110.5(6) . . ? C29 C30 C33 111.2(6) . . ? C31 C30 C32 109.2(6) . . ? C29 C30 C32 108.8(6) . . ? C33 C30 C32 109.9(8) . . ? C35 O34 W2 124.2(4) . . ? O34 C35 C36 112.7(7) . . ? C38 C36 C37 109.3(6) . . ? C38 C36 C35 108.8(6) . . ? C37 C36 C35 109.3(7) . . ? C38 C36 C39 109.9(6) . . ? C37 C36 C39 109.9(6) . . ? C35 C36 C39 109.7(5) . . ? C41 O40 W2 136.8(6) . . ? O40 C41 C42 111.8(7) . . ? C43 C42 C45 109.2(9) . . ? C43 C42 C44 109.2(7) . . ? C45 C42 C44 109.5(9) . . ? C43 C42 C41 109.8(8) . . ? C45 C42 C41 111.5(8) . . ? C44 C42 C41 107.6(7) . . ? C47 O46 W2 137.0(5) . . ? O46 C47 C48 109.9(8) . . ? C50 C48 C49 113.2(9) . . ? C50 C48 C51 110.7(6) . . ? C49 C48 C51 110.5(7) . . ? C50 C48 C47 107.2(7) . . ? C49 C48 C47 109.3(6) . . ? C51 C48 C47 105.5(7) . . ? O4 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? O4 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O10 C11 H11A 109.3 . . ? C12 C11 H11A 109.3 . . ? O10 C11 H11B 109.3 . . ? C12 C11 H11B 109.3 . . ? H11A C11 H11B 108.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O16 C17 H17A 109.1 . . ? C18 C17 H17A 109.1 . . ? O16 C17 H17B 109.1 . . ? C18 C17 H17B 109.1 . . ? H17A C17 H17B 107.8 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O22 C23 H23A 109.1 . . ? C24 C23 H23A 109.1 . . ? O22 C23 H23B 109.1 . . ? C24 C23 H23B 109.1 . . ? H23A C23 H23B 107.9 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O28 C29 H29A 110.0 . . ? C30 C29 H29A 110.0 . . ? O28 C29 H29B 110.0 . . ? C30 C29 H29B 110.0 . . ? H29A C29 H29B 108.4 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O34 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? O34 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O40 C41 H41A 109.3 . . ? C42 C41 H41A 109.3 . . ? O40 C41 H41B 109.3 . . ? C42 C41 H41B 109.3 . . ? H41A C41 H41B 107.9 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O46 C47 H47A 109.7 . . ? C48 C47 H47A 109.7 . . ? O46 C47 H47B 109.7 . . ? C48 C47 H47B 109.7 . . ? H47A C47 H47B 108.2 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? 3===END data_CIF_for_W2(?-Te)(OCH2tBu)8 _database_code_CSD 158781 _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C40 H88 O8 Te W2' _chemical_formula_sum 'C40 H88 O8 Te W2' _chemical_formula_weight 1192.40 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Te' 'Te' -0.5308 1.6751 '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 12.458(5) _cell_length_b 14.694(6) _cell_length_c 14.772(6) _cell_angle_alpha 93.734(10) _cell_angle_beta 113.951(11) _cell_angle_gamma 90.990(10) _cell_volume 2463.1(18) _cell_formula_units_Z 2 _cell_measurement_temperature 114(2) _cell_measurement_reflns_used 422 _cell_measurement_theta_min 3.36 _cell_measurement_theta_max 21.59 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 5.289 _exptl_absorpt_correction_type semi-empirical _exptl_absorpt_correction_T_min .083 _exptl_absorpt_correction_T_max .295 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; The data collection crystal was twinned, as all other crystals of the sample seemed to be as well. In the case of the data collection crystal, the two twin domains are related by a 180-degree rotation about the 0 1 -1 direct-space vector. Information and statistics in this file reflect a data set from which all partially overlapped reflections have been removed. ; _diffrn_measurement_details ' 0.30 degree frames measured for 30.15 seconds each' _diffrn_reflns_special_details ; Multiple measurements of the same reflection (i.e. identical indices) were averaged, but Friedel pairs were not averaged because of the twinning. ; _diffrn_ambient_temperature 114(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 'three-circle goniometer with fixed chi' _diffrn_measurement_device_type 'Bruker Platform goniometer' _diffrn_measurement_method '\w scans' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker SMART 6000' _diffrn_detector_area_resol_mean 44.52 _diffrn_standards_number 150 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 2132 _diffrn_standards_decay_% -0.05 _diffrn_reflns_number 39903 _diffrn_reflns_av_R_equivalents 0.075 _diffrn_reflns_av_sigmaI/netI 0.1307 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.50 _diffrn_measured_fraction_theta_max 0.308 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.308 _reflns_number_total 10392 _reflns_number_gt 6402 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Bruker, 1999)' _computing_cell_refinement 'SAINT (Bruker, 1999)' _computing_data_reduction 'SAINT (Bruker, 1999), XTEL (local package)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XTEL (local package)' _computing_publication_material 'XTEL (local package)' _refine_special_details ; Refinement of F^2^ against all completely overlapped and non-overlapped 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. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; calc [\s^2^(Fo^2^)+(0.0300Fo^2^)^2^]^-1^ ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10392 _refine_ls_number_parameters 221 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1047 _refine_ls_goodness_of_fit_ref 0.950 _refine_ls_restrained_S_all 0.950 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.083 _refine_diff_density_min -1.389 _refine_diff_density_rms 0.143 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 0.39825(4) 0.78780(3) 0.26747(3) 0.01322(15) Uani 1 1 d . . . W2 W 0.61751(5) 0.74793(3) 0.29858(3) 0.01386(15) Uani 1 1 d . . . Te3 Te 0.57967(8) 0.87505(6) 0.42104(6) 0.0213(2) Uani 1 1 d . . . O4 O 0.4757(8) 0.6629(5) 0.2784(5) 0.0164(19) Uiso 1 1 d . . . C5 C 0.4369(14) 0.5798(9) 0.2153(10) 0.025(3) Uiso 1 1 d . . . H5A H 0.5015 0.5581 0.1980 0.029 Uiso 1 1 calc R . . H5B H 0.3699 0.5920 0.1529 0.029 Uiso 1 1 calc R . . C6 C 0.3989(12) 0.5048(9) 0.2659(9) 0.026(3) Uiso 1 1 d . . . C7 C 0.2827(12) 0.5234(9) 0.2834(10) 0.034(3) Uiso 1 1 d . . . H7A H 0.2156 0.5251 0.2191 0.051 Uiso 1 1 calc R . . H7B H 0.2929 0.5820 0.3222 0.051 Uiso 1 1 calc R . . H7C H 0.2683 0.4744 0.3197 0.051 Uiso 1 1 calc R . . C8 C 0.4953(13) 0.4904(10) 0.3785(10) 0.036(4) Uiso 1 1 d . . . H8A H 0.4646 0.4435 0.4071 0.053 Uiso 1 1 calc R . . H8B H 0.5099 0.5480 0.4199 0.053 Uiso 1 1 calc R . . H8C H 0.5689 0.4711 0.3759 0.053 Uiso 1 1 calc R . . C9 C 0.3796(13) 0.4119(10) 0.2023(10) 0.039(4) Uiso 1 1 d . . . H9A H 0.3074 0.4127 0.1416 0.058 Uiso 1 1 calc R . . H9B H 0.3727 0.3620 0.2408 0.058 Uiso 1 1 calc R . . H9C H 0.4467 0.4026 0.1846 0.058 Uiso 1 1 calc R . . O10 O 0.4776(8) 0.7837(5) 0.1679(5) 0.0133(18) Uiso 1 1 d . . . C11 C 0.4367(12) 0.7372(7) 0.0700(8) 0.008(3) Uiso 1 1 d . . . H11A H 0.3512 0.7227 0.0460 0.009 Uiso 1 1 calc R . . H11B H 0.4759 0.6785 0.0753 0.009 Uiso 1 1 calc R . . C12 C 0.4573(14) 0.7886(10) -0.0063(10) 0.028(3) Uiso 1 1 d . . . C13 C 0.4181(14) 0.8874(9) 0.0077(11) 0.039(4) Uiso 1 1 d . . . H13A H 0.3592 0.9046 -0.0557 0.058 Uiso 1 1 calc R . . H13B H 0.4865 0.9305 0.0306 0.058 Uiso 1 1 calc R . . H13C H 0.3842 0.8890 0.0572 0.058 Uiso 1 1 calc R . . C14 C 0.3862(12) 0.7452(9) -0.1056(10) 0.028(3) Uiso 1 1 d . . . H14A H 0.4167 0.6854 -0.1133 0.042 Uiso 1 1 calc R . . H14B H 0.3902 0.7838 -0.1559 0.042 Uiso 1 1 calc R . . H14C H 0.3044 0.7372 -0.1141 0.042 Uiso 1 1 calc R . . C15 C 0.5912(12) 0.7986(10) 0.0179(10) 0.039(4) Uiso 1 1 d . . . H15A H 0.6149 0.7442 -0.0101 0.059 Uiso 1 1 calc R . . H15B H 0.6362 0.8051 0.0901 0.059 Uiso 1 1 calc R . . H15C H 0.6067 0.8528 -0.0111 0.059 Uiso 1 1 calc R . . O16 O 0.2621(7) 0.7312(5) 0.1557(5) 0.0117(16) Uiso 1 1 d . . . C17 C 0.1436(11) 0.7477(8) 0.1425(8) 0.018(3) Uiso 1 1 d . . . H17A H 0.1367 0.8138 0.1561 0.021 Uiso 1 1 calc R . . H17B H 0.1246 0.7144 0.1907 0.021 Uiso 1 1 calc R . . C18 C 0.0564(11) 0.7172(8) 0.0380(8) 0.009(3) Uiso 1 1 d . . . C19 C 0.0634(13) 0.6179(9) 0.0140(10) 0.030(3) Uiso 1 1 d . . . H19A H -0.0078 0.5960 -0.0438 0.045 Uiso 1 1 calc R . . H19B H 0.0703 0.5841 0.0711 0.045 Uiso 1 1 calc R . . H19C H 0.1324 0.6083 -0.0008 0.045 Uiso 1 1 calc R . . C20 C 0.0845(14) 0.7708(10) -0.0373(10) 0.031(4) Uiso 1 1 d . . . H20A H 0.1590 0.7515 -0.0382 0.047 Uiso 1 1 calc R . . H20B H 0.0909 0.8363 -0.0176 0.047 Uiso 1 1 calc R . . H20C H 0.0213 0.7585 -0.1037 0.047 Uiso 1 1 calc R . . C21 C -0.0649(11) 0.7366(8) 0.0305(8) 0.024(3) Uiso 1 1 d . . . H21A H -0.1235 0.7096 -0.0333 0.036 Uiso 1 1 calc R . . H21B H -0.0731 0.8028 0.0350 0.036 Uiso 1 1 calc R . . H21C H -0.0773 0.7101 0.0849 0.036 Uiso 1 1 calc R . . O22 O 0.3290(8) 0.7563(5) 0.3565(6) 0.0122(18) Uiso 1 1 d . . . C23 C 0.3701(14) 0.7353(10) 0.4548(10) 0.029(4) Uiso 1 1 d . . . H23A H 0.4434 0.7719 0.4956 0.034 Uiso 1 1 calc R . . H23B H 0.3871 0.6698 0.4598 0.034 Uiso 1 1 calc R . . C24 C 0.2735(12) 0.7574(9) 0.4926(9) 0.024(3) Uiso 1 1 d . . . C25 C 0.2424(17) 0.8547(11) 0.4816(13) 0.043(4) Uiso 1 1 d . . . H25A H 0.1740 0.8648 0.4972 0.064 Uiso 1 1 calc R . . H25B H 0.2235 0.8690 0.4130 0.064 Uiso 1 1 calc R . . H25C H 0.3091 0.8943 0.5271 0.064 Uiso 1 1 calc R . . C26 C 0.1662(16) 0.6943(12) 0.4341(13) 0.060(5) Uiso 1 1 d . . . H26A H 0.1030 0.7093 0.4551 0.091 Uiso 1 1 calc R . . H26B H 0.1867 0.6309 0.4466 0.091 Uiso 1 1 calc R . . H26C H 0.1399 0.7021 0.3631 0.091 Uiso 1 1 calc R . . C27 C 0.3173(16) 0.7397(11) 0.6006(11) 0.040(4) Uiso 1 1 d . . . H27A H 0.3994 0.7623 0.6354 0.060 Uiso 1 1 calc R . . H27B H 0.3118 0.6739 0.6066 0.060 Uiso 1 1 calc R . . H27C H 0.2692 0.7712 0.6301 0.060 Uiso 1 1 calc R . . O28 O 0.3305(8) 0.9020(6) 0.2246(6) 0.021(2) Uiso 1 1 d . . . C29 C 0.3749(12) 0.9938(8) 0.2388(9) 0.018(3) Uiso 1 1 d . . . H29A H 0.4173 1.0035 0.1960 0.022 Uiso 1 1 calc R . . H29B H 0.4298 1.0088 0.3090 0.022 Uiso 1 1 calc R . . C30 C 0.2659(12) 1.0549(8) 0.2100(9) 0.016(3) Uiso 1 1 d . . . C31 C 0.3241(13) 1.1535(9) 0.2337(10) 0.024(3) Uiso 1 1 d . . . H31A H 0.2674 1.1960 0.1938 0.036 Uiso 1 1 calc R . . H31B H 0.3931 1.1545 0.2176 0.036 Uiso 1 1 calc R . . H31C H 0.3484 1.1720 0.3044 0.036 Uiso 1 1 calc R . . C32 C 0.1962(15) 1.0372(10) 0.2690(11) 0.035(4) Uiso 1 1 d . . . H32A H 0.1228 1.0693 0.2425 0.053 Uiso 1 1 calc R . . H32B H 0.2418 1.0592 0.3386 0.053 Uiso 1 1 calc R . . H32C H 0.1782 0.9715 0.2647 0.053 Uiso 1 1 calc R . . C33 C 0.1949(14) 1.0357(10) 0.1016(10) 0.041(4) Uiso 1 1 d . . . H33A H 0.1503 0.9773 0.0895 0.062 Uiso 1 1 calc R . . H33B H 0.2473 1.0326 0.0669 0.062 Uiso 1 1 calc R . . H33C H 0.1403 1.0845 0.0769 0.062 Uiso 1 1 calc R . . O34 O 0.6532(7) 0.6573(5) 0.2144(6) 0.0143(17) Uiso 1 1 d . . . C35 C 0.7690(11) 0.6426(8) 0.2270(9) 0.021(3) Uiso 1 1 d . . . H35A H 0.8215 0.6571 0.2979 0.025 Uiso 1 1 calc R . . H35B H 0.7911 0.6857 0.1880 0.025 Uiso 1 1 calc R . . C36 C 0.7915(13) 0.5441(8) 0.1956(9) 0.022(3) Uiso 1 1 d . . . C37 C 0.7490(12) 0.4768(8) 0.2549(9) 0.018(3) Uiso 1 1 d . . . H37A H 0.7686 0.4144 0.2418 0.027 Uiso 1 1 calc R . . H37B H 0.6638 0.4794 0.2335 0.027 Uiso 1 1 calc R . . H37C H 0.7885 0.4948 0.3263 0.027 Uiso 1 1 calc R . . C38 C 0.9129(11) 0.5344(8) 0.2148(8) 0.022(3) Uiso 1 1 d . . . H38A H 0.9609 0.5453 0.2863 0.033 Uiso 1 1 calc R . . H38B H 0.9370 0.5788 0.1791 0.033 Uiso 1 1 calc R . . H38C H 0.9238 0.4725 0.1921 0.033 Uiso 1 1 calc R . . C39 C 0.7054(13) 0.5220(10) 0.0854(10) 0.034(3) Uiso 1 1 d . . . H39A H 0.7261 0.5615 0.0434 0.051 Uiso 1 1 calc R . . H39B H 0.6249 0.5325 0.0778 0.051 Uiso 1 1 calc R . . H39C H 0.7110 0.4580 0.0654 0.051 Uiso 1 1 calc R . . O40 O 0.7199(7) 0.8325(5) 0.2759(6) 0.0124(18) Uiso 1 1 d . . . C41 C 0.7262(13) 0.9267(9) 0.2661(10) 0.023(3) Uiso 1 1 d . . . H41A H 0.7108 0.9601 0.3197 0.028 Uiso 1 1 calc R . . H41B H 0.6638 0.9407 0.2018 0.028 Uiso 1 1 calc R . . C42 C 0.8390(11) 0.9594(8) 0.2707(8) 0.021(3) Uiso 1 1 d . . . C43 C 0.9388(18) 0.9418(14) 0.3674(13) 0.053(5) Uiso 1 1 d . . . H43A H 0.9324 0.8782 0.3816 0.080 Uiso 1 1 calc R . . H43B H 0.9350 0.9827 0.4211 0.080 Uiso 1 1 calc R . . H43C H 1.0138 0.9532 0.3624 0.080 Uiso 1 1 calc R . . C44 C 0.8290(15) 1.0630(10) 0.2610(12) 0.044(4) Uiso 1 1 d . . . H44A H 0.9057 1.0905 0.2713 0.067 Uiso 1 1 calc R . . H44B H 0.8037 1.0903 0.3110 0.067 Uiso 1 1 calc R . . H44C H 0.7712 1.0739 0.1945 0.067 Uiso 1 1 calc R . . C45 C 0.8668(14) 0.9151(10) 0.1887(10) 0.042(4) Uiso 1 1 d . . . H45A H 0.8755 0.8496 0.1969 0.063 Uiso 1 1 calc R . . H45B H 0.9402 0.9428 0.1913 0.063 Uiso 1 1 calc R . . H45C H 0.8027 0.9240 0.1244 0.063 Uiso 1 1 calc R . . O46 O 0.7192(8) 0.6871(6) 0.4102(6) 0.021(2) Uiso 1 1 d . . . C47 C 0.7451(13) 0.6814(9) 0.5108(9) 0.021(3) Uiso 1 1 d . . . H47A H 0.7105 0.6235 0.5204 0.025 Uiso 1 1 calc R . . H47B H 0.7113 0.7328 0.5354 0.025 Uiso 1 1 calc R . . C48 C 0.8806(13) 0.6850(8) 0.5692(8) 0.016(3) Uiso 1 1 d . . . C49 C 0.9337(14) 0.7744(10) 0.5492(11) 0.031(4) Uiso 1 1 d . . . H49A H 1.0198 0.7742 0.5804 0.046 Uiso 1 1 calc R . . H49B H 0.9073 0.8273 0.5771 0.046 Uiso 1 1 calc R . . H49C H 0.9075 0.7779 0.4774 0.046 Uiso 1 1 calc R . . C50 C 0.9310(12) 0.6032(9) 0.5387(10) 0.034(3) Uiso 1 1 d . . . H50A H 1.0158 0.6039 0.5794 0.051 Uiso 1 1 calc R . . H50B H 0.9170 0.6041 0.4686 0.051 Uiso 1 1 calc R . . H50C H 0.8933 0.5477 0.5482 0.051 Uiso 1 1 calc R . . C51 C 0.9046(13) 0.6868(9) 0.6781(9) 0.030(3) Uiso 1 1 d . . . H51A H 0.8692 0.6314 0.6903 0.046 Uiso 1 1 calc R . . H51B H 0.8705 0.7406 0.6967 0.046 Uiso 1 1 calc R . . H51C H 0.9897 0.6894 0.7179 0.046 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 0.0147(4) 0.0123(3) 0.0123(2) -0.00022(19) 0.0052(2) 0.0025(2) W2 0.0154(4) 0.0142(3) 0.0118(2) -0.00044(19) 0.0055(2) 0.0027(2) Te3 0.0177(6) 0.0256(5) 0.0179(4) -0.0093(4) 0.0062(4) -0.0002(4) _geom_special_details ; All esds are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances and angles. ; 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 O22 1.917(8) . ? W1 O28 1.919(8) . ? W1 O16 1.947(7) . ? W1 O4 2.072(8) . ? W1 O10 2.078(8) . ? W1 W2 2.6620(13) . ? W1 Te3 2.6936(12) . ? W2 O40 1.905(8) . ? W2 O46 1.913(8) . ? W2 O34 1.942(7) . ? W2 O4 2.054(8) . ? W2 O10 2.116(8) . ? W2 Te3 2.6955(12) . ? O4 C5 1.435(15) . ? C5 C6 1.541(18) . ? C6 C9 1.563(17) . ? C6 C7 1.596(19) . ? C6 C8 1.639(18) . ? O10 C11 1.442(13) . ? C11 C12 1.498(16) . ? C12 C14 1.465(17) . ? C12 C15 1.56(2) . ? C12 C13 1.568(19) . ? O16 C17 1.436(14) . ? C17 C18 1.516(15) . ? C18 C19 1.491(17) . ? C18 C21 1.504(18) . ? C18 C20 1.549(17) . ? O22 C23 1.389(14) . ? C23 C24 1.549(19) . ? C24 C25 1.49(2) . ? C24 C27 1.504(18) . ? C24 C26 1.52(2) . ? O28 C29 1.418(14) . ? C29 C30 1.567(18) . ? C30 C33 1.486(17) . ? C30 C32 1.488(19) . ? C30 C31 1.562(17) . ? O34 C35 1.400(14) . ? C35 C36 1.555(16) . ? C36 C38 1.433(18) . ? C36 C39 1.551(17) . ? C36 C37 1.580(17) . ? O40 C41 1.406(14) . ? C41 C42 1.451(19) . ? C42 C45 1.502(17) . ? C42 C43 1.51(2) . ? C42 C44 1.541(18) . ? O46 C47 1.395(14) . ? C47 C48 1.552(19) . ? C48 C50 1.492(18) . ? C48 C51 1.510(16) . ? C48 C49 1.559(18) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? 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 O22 W1 O28 102.5(3) . . ? O22 W1 O16 90.0(3) . . ? O28 W1 O16 86.0(3) . . ? O22 W1 O4 91.3(3) . . ? O28 W1 O4 164.9(3) . . ? O16 W1 O4 87.8(3) . . ? O22 W1 O10 164.4(3) . . ? O28 W1 O10 91.8(3) . . ? O16 W1 O10 84.6(3) . . ? O4 W1 O10 73.9(3) . . ? O22 W1 W2 122.0(3) . . ? O28 W1 W2 124.4(3) . . ? O16 W1 W2 122.3(2) . . ? O4 W1 W2 49.5(2) . . ? O10 W1 W2 51.2(2) . . ? O22 W1 Te3 89.8(2) . . ? O28 W1 Te3 90.9(3) . . ? O16 W1 Te3 176.7(2) . . ? O4 W1 Te3 95.5(2) . . ? O10 W1 Te3 96.5(2) . . ? W2 W1 Te3 60.43(3) . . ? O40 W2 O46 104.1(3) . . ? O40 W2 O34 88.0(3) . . ? O46 W2 O34 87.6(4) . . ? O40 W2 O4 162.4(3) . . ? O46 W2 O4 92.4(3) . . ? O34 W2 O4 86.4(3) . . ? O40 W2 O10 89.5(3) . . ? O46 W2 O10 165.1(3) . . ? O34 W2 O10 86.9(3) . . ? O4 W2 O10 73.5(3) . . ? O40 W2 W1 121.4(2) . . ? O46 W2 W1 123.7(3) . . ? O34 W2 W1 122.5(2) . . ? O4 W2 W1 50.1(2) . . ? O10 W2 W1 50.0(2) . . ? O40 W2 Te3 90.3(2) . . ? O46 W2 Te3 90.5(3) . . ? O34 W2 Te3 177.1(2) . . ? O4 W2 Te3 95.9(2) . . ? O10 W2 Te3 95.5(2) . . ? W1 W2 Te3 60.36(3) . . ? W1 Te3 W2 59.20(3) . . ? C5 O4 W2 127.2(8) . . ? C5 O4 W1 130.4(8) . . ? W2 O4 W1 80.4(3) . . ? O4 C5 C6 111.7(10) . . ? C5 C6 C9 109.2(11) . . ? C5 C6 C7 115.2(11) . . ? C9 C6 C7 108.5(11) . . ? C5 C6 C8 113.7(11) . . ? C9 C6 C8 107.7(11) . . ? C7 C6 C8 102.1(10) . . ? C11 O10 W1 128.9(7) . . ? C11 O10 W2 127.2(7) . . ? W1 O10 W2 78.8(3) . . ? O10 C11 C12 115.5(9) . . ? C14 C12 C11 109.5(11) . . ? C14 C12 C15 113.8(12) . . ? C11 C12 C15 110.9(11) . . ? C14 C12 C13 111.8(12) . . ? C11 C12 C13 104.5(11) . . ? C15 C12 C13 105.9(12) . . ? C17 O16 W1 122.5(6) . . ? O16 C17 C18 111.5(9) . . ? C19 C18 C21 109.9(10) . . ? C19 C18 C17 111.3(10) . . ? C21 C18 C17 108.1(9) . . ? C19 C18 C20 108.1(10) . . ? C21 C18 C20 110.1(10) . . ? C17 C18 C20 109.3(10) . . ? C23 O22 W1 136.1(9) . . ? O22 C23 C24 107.9(11) . . ? C25 C24 C27 108.9(12) . . ? C25 C24 C26 110.5(13) . . ? C27 C24 C26 108.5(13) . . ? C25 C24 C23 111.1(12) . . ? C27 C24 C23 109.3(12) . . ? C26 C24 C23 108.5(11) . . ? C29 O28 W1 134.7(8) . . ? O28 C29 C30 106.5(10) . . ? C33 C30 C32 111.9(12) . . ? C33 C30 C31 110.9(11) . . ? C32 C30 C31 112.5(11) . . ? C33 C30 C29 107.1(11) . . ? C32 C30 C29 111.5(11) . . ? C31 C30 C29 102.5(11) . . ? C35 O34 W2 121.7(6) . . ? O34 C35 C36 115.2(10) . . ? C38 C36 C39 114.3(11) . . ? C38 C36 C35 111.3(10) . . ? C39 C36 C35 107.4(11) . . ? C38 C36 C37 111.7(10) . . ? C39 C36 C37 104.5(11) . . ? C35 C36 C37 107.1(10) . . ? C41 O40 W2 137.1(9) . . ? O40 C41 C42 113.3(12) . . ? C41 C42 C45 112.3(11) . . ? C41 C42 C43 112.1(12) . . ? C45 C42 C43 107.1(13) . . ? C41 C42 C44 105.3(11) . . ? C45 C42 C44 110.2(11) . . ? C43 C42 C44 109.8(12) . . ? C47 O46 W2 140.4(9) . . ? O46 C47 C48 108.6(11) . . ? C50 C48 C51 110.5(11) . . ? C50 C48 C47 110.2(11) . . ? C51 C48 C47 106.8(11) . . ? C50 C48 C49 110.7(12) . . ? C51 C48 C49 109.5(11) . . ? C47 C48 C49 109.1(10) . . ? O4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? O4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 107.9 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O10 C11 H11A 108.4 . . ? C12 C11 H11A 108.4 . . ? O10 C11 H11B 108.4 . . ? C12 C11 H11B 108.4 . . ? H11A C11 H11B 107.5 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? O16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O22 C23 H23A 110.1 . . ? C24 C23 H23A 110.1 . . ? O22 C23 H23B 110.1 . . ? C24 C23 H23B 110.1 . . ? H23A C23 H23B 108.4 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C24 C27 H27A 109.5 . . ? C24 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C24 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O28 C29 H29A 110.4 . . ? C30 C29 H29A 110.4 . . ? O28 C29 H29B 110.4 . . ? C30 C29 H29B 110.4 . . ? H29A C29 H29B 108.6 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O34 C35 H35A 108.5 . . ? C36 C35 H35A 108.5 . . ? O34 C35 H35B 108.5 . . ? C36 C35 H35B 108.5 . . ? H35A C35 H35B 107.5 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O40 C41 H41A 108.9 . . ? C42 C41 H41A 108.9 . . ? O40 C41 H41B 108.9 . . ? C42 C41 H41B 108.9 . . ? H41A C41 H41B 107.7 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C42 C45 H45A 109.5 . . ? C42 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C42 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? O46 C47 H47A 110.0 . . ? C48 C47 H47A 110.0 . . ? O46 C47 H47B 110.0 . . ? C48 C47 H47B 110.0 . . ? H47A C47 H47B 108.3 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? 4===END