data_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H36 O3 W' _chemical_formula_weight 472.31 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' 'W' 'W' -0.8490 6.8722 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.9821(10) _cell_length_b 13.6032(14) _cell_length_c 30.815(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.022(3) _cell_angle_gamma 90.00 _cell_volume 4184.4(8) _cell_formula_units_Z 8 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 9860 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description tablet _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 5.528 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5745 _exptl_absorpt_correction_T_max 0.7696 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD' _diffrn_measurement_method '\w- and \f-scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 179826 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0306 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 0.66 _diffrn_reflns_theta_max 30.58 _reflns_number_total 12832 _reflns_number_gt 11160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens XP' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure was refined as a pseudo-merohedral twin with component ratios 0.446:0.554(1). ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0121P)^2^+21.1847P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment 'rigid methyls' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12832 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0326 _refine_ls_wR_factor_ref 0.0669 _refine_ls_wR_factor_gt 0.0603 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group W1 W 0.272585(18) 0.900638(12) 0.624028(12) 0.01597(4) Uani 1 1 d . . . W2 W 0.752128(18) 0.621819(12) 0.625368(11) 0.01620(4) Uani 1 1 d . . . O1 O 0.4596(3) 0.9117(2) 0.6240(2) 0.0205(6) Uani 1 1 d . . . O2 O 0.2132(7) 0.8350(4) 0.67371(14) 0.0209(10) Uani 1 1 d . . . O3 O 0.2198(6) 0.8339(3) 0.57377(14) 0.0203(11) Uani 1 1 d . . . O4 O 0.9391(3) 0.6118(2) 0.6239(2) 0.0226(7) Uani 1 1 d . . . O5 O 0.6912(6) 0.6854(4) 0.57520(15) 0.0204(12) Uani 1 1 d . . . O6 O 0.6984(6) 0.6907(4) 0.67492(14) 0.0213(12) Uani 1 1 d . . . C1 C 0.2029(4) 1.0197(3) 0.6232(3) 0.0177(8) Uani 1 1 d . . . C2 C 0.1458(5) 1.1228(3) 0.6244(3) 0.0230(9) Uani 1 1 d . . . C3 C 0.1713(9) 1.1712(6) 0.6682(2) 0.0375(19) Uani 1 1 d . . . H3A H 0.1279 1.1327 0.6911 0.045 Uiso 1 1 calc R . . H3B H 0.1345 1.2380 0.6680 0.045 Uiso 1 1 calc R . . H3C H 0.2680 1.1741 0.6736 0.045 Uiso 1 1 calc R . . C4 C 0.2127(9) 1.1865(5) 0.5888(2) 0.0388(17) Uani 1 1 d . . . H4A H 0.3098 1.1873 0.5933 0.047 Uiso 1 1 calc R . . H4B H 0.1779 1.2537 0.5904 0.047 Uiso 1 1 calc R . . H4C H 0.1926 1.1587 0.5602 0.047 Uiso 1 1 calc R . . C5 C -0.0048(6) 1.1198(5) 0.6151(2) 0.0369(19) Uani 1 1 d . . . H5A H -0.0202 1.0908 0.5864 0.044 Uiso 1 1 calc R . . H5B H -0.0411 1.1867 0.6158 0.044 Uiso 1 1 calc R . . H5C H -0.0496 1.0797 0.6372 0.044 Uiso 1 1 calc R . . C6 C 0.1342(10) 0.8490(6) 0.7122(2) 0.0217(16) Uani 1 1 d . . . C7 C 0.1131(9) 0.7471(7) 0.7314(3) 0.049(2) Uani 1 1 d . . . H7A H 0.0626 0.7065 0.7109 0.059 Uiso 1 1 calc R . . H7B H 0.0629 0.7527 0.7586 0.059 Uiso 1 1 calc R . . H7C H 0.2003 0.7166 0.7371 0.059 Uiso 1 1 calc R . . C8 C 0.2156(9) 0.9134(7) 0.7428(2) 0.050(2) Uani 1 1 d . . . H8A H 0.3043 0.8841 0.7472 0.060 Uiso 1 1 calc R . . H8B H 0.1694 0.9184 0.7708 0.060 Uiso 1 1 calc R . . H8C H 0.2255 0.9791 0.7302 0.060 Uiso 1 1 calc R . . C9 C 0.0027(8) 0.8946(7) 0.7001(3) 0.044(2) Uani 1 1 d . . . H9A H 0.0184 0.9592 0.6870 0.053 Uiso 1 1 calc R . . H9B H -0.0526 0.9023 0.7261 0.053 Uiso 1 1 calc R . . H9C H -0.0438 0.8522 0.6792 0.053 Uiso 1 1 calc R . . C10 C 0.5655(5) 0.9840(4) 0.6218(3) 0.0282(12) Uani 1 1 d . . . C11 C 0.5536(9) 1.0541(6) 0.6595(3) 0.0402(19) Uani 1 1 d . . . H11A H 0.4671 1.0881 0.6581 0.048 Uiso 1 1 calc R . . H11B H 0.6262 1.1025 0.6582 0.048 Uiso 1 1 calc R . . H11C H 0.5596 1.0173 0.6868 0.048 Uiso 1 1 calc R . . C12 C 0.5516(10) 1.0371(7) 0.5782(3) 0.045(2) Uani 1 1 d . . . H12A H 0.5631 0.9898 0.5545 0.054 Uiso 1 1 calc R . . H12B H 0.6203 1.0883 0.5760 0.054 Uiso 1 1 calc R . . H12C H 0.4626 1.0671 0.5762 0.054 Uiso 1 1 calc R . . C13 C 0.6955(5) 0.9255(4) 0.6229(4) 0.0363(14) Uani 1 1 d . . . H13A H 0.7062 0.8951 0.6515 0.044 Uiso 1 1 calc R . . H13B H 0.7712 0.9696 0.6172 0.044 Uiso 1 1 calc R . . H13C H 0.6928 0.8741 0.6006 0.044 Uiso 1 1 calc R . . C14 C 0.1346(11) 0.8453(7) 0.5360(2) 0.0268(18) Uani 1 1 d . . . C15 C 0.1616(8) 0.7600(6) 0.5065(2) 0.0427(18) Uani 1 1 d . . . H15A H 0.2558 0.7610 0.4975 0.051 Uiso 1 1 calc R . . H15B H 0.1041 0.7647 0.4808 0.051 Uiso 1 1 calc R . . H15C H 0.1427 0.6985 0.5219 0.051 Uiso 1 1 calc R . . C16 C 0.1694(7) 0.9411(5) 0.5139(2) 0.0323(14) Uani 1 1 d . . . H16A H 0.1515 0.9959 0.5337 0.039 Uiso 1 1 calc R . . H16B H 0.1148 0.9486 0.4877 0.039 Uiso 1 1 calc R . . H16C H 0.2645 0.9410 0.5060 0.039 Uiso 1 1 calc R . . C17 C -0.0104(8) 0.8458(6) 0.5511(2) 0.0348(17) Uani 1 1 d . . . H17A H -0.0299 0.7843 0.5665 0.042 Uiso 1 1 calc R . . H17B H -0.0699 0.8518 0.5260 0.042 Uiso 1 1 calc R . . H17C H -0.0250 0.9015 0.5707 0.042 Uiso 1 1 calc R . . C18 C 0.6827(5) 0.5020(4) 0.6269(3) 0.0233(10) Uani 1 1 d . . . C19 C 0.6269(6) 0.3996(4) 0.6296(2) 0.0249(12) Uani 1 1 d . . . C20 C 0.6727(11) 0.3402(6) 0.5900(3) 0.046(2) Uani 1 1 d . . . H20A H 0.6447 0.3740 0.5634 0.055 Uiso 1 1 calc R . . H20B H 0.6322 0.2746 0.5908 0.055 Uiso 1 1 calc R . . H20C H 0.7706 0.3341 0.5903 0.055 Uiso 1 1 calc R . . C21 C 0.4742(6) 0.4006(5) 0.6294(3) 0.0404(17) Uani 1 1 d . . . H21A H 0.4417 0.4442 0.6525 0.048 Uiso 1 1 calc R . . H21B H 0.4405 0.3339 0.6344 0.048 Uiso 1 1 calc R . . H21C H 0.4421 0.4245 0.6013 0.048 Uiso 1 1 calc R . . C22 C 0.6731(11) 0.3485(6) 0.6713(3) 0.051(2) Uani 1 1 d . . . H22A H 0.7707 0.3408 0.6708 0.061 Uiso 1 1 calc R . . H22B H 0.6308 0.2837 0.6734 0.061 Uiso 1 1 calc R . . H22C H 0.6475 0.3884 0.6965 0.061 Uiso 1 1 calc R . . C23 C 1.0452(5) 0.5396(4) 0.6226(4) 0.0368(15) Uani 1 1 d . . . C24 C 1.0370(11) 0.4727(8) 0.6607(4) 0.061(3) Uani 1 1 d . . . H24A H 1.0371 0.5116 0.6875 0.074 Uiso 1 1 calc R . . H24B H 1.1143 0.4283 0.6607 0.074 Uiso 1 1 calc R . . H24C H 0.9543 0.4340 0.6591 0.074 Uiso 1 1 calc R . . C25 C 1.1760(5) 0.5974(5) 0.6220(4) 0.0399(15) Uani 1 1 d . . . H25A H 1.1792 0.6388 0.5960 0.048 Uiso 1 1 calc R . . H25B H 1.2518 0.5515 0.6217 0.048 Uiso 1 1 calc R . . H25C H 1.1813 0.6389 0.6480 0.048 Uiso 1 1 calc R . . C26 C 1.0276(10) 0.4842(7) 0.5789(3) 0.060(3) Uani 1 1 d . . . H26A H 0.9424 0.4484 0.5791 0.071 Uiso 1 1 calc R . . H26B H 1.1016 0.4377 0.5750 0.071 Uiso 1 1 calc R . . H26C H 1.0277 0.5316 0.5549 0.071 Uiso 1 1 calc R . . C27 C 0.6179(11) 0.6718(6) 0.5351(2) 0.0235(17) Uani 1 1 d . . . C28 C 0.5849(8) 0.7715(6) 0.5174(2) 0.0334(16) Uani 1 1 d . . . H28A H 0.5242 0.8055 0.5374 0.040 Uiso 1 1 calc R . . H28B H 0.5414 0.7645 0.4891 0.040 Uiso 1 1 calc R . . H28C H 0.6675 0.8098 0.5142 0.040 Uiso 1 1 calc R . . C29 C 0.4912(9) 0.6125(6) 0.5441(3) 0.0354(18) Uani 1 1 d . . . H29A H 0.5157 0.5481 0.5560 0.042 Uiso 1 1 calc R . . H29B H 0.4413 0.6035 0.5170 0.042 Uiso 1 1 calc R . . H29C H 0.4352 0.6478 0.5650 0.042 Uiso 1 1 calc R . . C30 C 0.7115(10) 0.6146(6) 0.5045(2) 0.040(2) Uani 1 1 d . . . H30A H 0.7912 0.6543 0.4983 0.048 Uiso 1 1 calc R . . H30B H 0.6644 0.6003 0.4773 0.048 Uiso 1 1 calc R . . H30C H 0.7385 0.5528 0.5183 0.048 Uiso 1 1 calc R . . C31 C 0.6226(11) 0.6786(7) 0.7147(2) 0.0262(18) Uani 1 1 d . . . C32 C 0.6036(9) 0.7845(6) 0.7319(2) 0.0425(19) Uani 1 1 d . . . H32A H 0.6914 0.8150 0.7364 0.051 Uiso 1 1 calc R . . H32B H 0.5548 0.7826 0.7595 0.051 Uiso 1 1 calc R . . H32C H 0.5524 0.8230 0.7107 0.051 Uiso 1 1 calc R . . C33 C 0.4900(10) 0.6343(7) 0.7043(3) 0.046(2) Uani 1 1 d . . . H33A H 0.4391 0.6792 0.6857 0.055 Uiso 1 1 calc R . . H33B H 0.4403 0.6228 0.7313 0.055 Uiso 1 1 calc R . . H33C H 0.5033 0.5717 0.6892 0.055 Uiso 1 1 calc R . . C34 C 0.7073(10) 0.6195(7) 0.7455(2) 0.050(2) Uani 1 1 d . . . H34A H 0.7138 0.5516 0.7350 0.060 Uiso 1 1 calc R . . H34B H 0.6662 0.6199 0.7743 0.060 Uiso 1 1 calc R . . H34C H 0.7971 0.6483 0.7471 0.060 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 0.01824(8) 0.01628(8) 0.01338(7) 0.00060(10) -0.00058(11) -0.00054(6) W2 0.01972(9) 0.01437(7) 0.01451(7) -0.00138(9) 0.00142(12) -0.00036(6) O1 0.0197(14) 0.0191(17) 0.0227(16) 0.000(2) 0.002(2) -0.0038(11) O2 0.023(2) 0.023(2) 0.0170(19) 0.0023(15) 0.0038(17) 0.000(2) O3 0.022(2) 0.021(2) 0.0179(19) -0.0025(15) 0.0009(17) 0.003(2) O4 0.0187(14) 0.0207(17) 0.0285(18) 0.005(2) 0.003(2) 0.0030(12) O5 0.024(3) 0.018(2) 0.020(2) 0.0003(16) 0.0027(17) -0.0004(18) O6 0.025(3) 0.024(3) 0.0149(19) -0.0028(16) 0.0074(17) 0.000(2) C1 0.0169(18) 0.022(2) 0.014(2) 0.006(2) 0.001(3) 0.0007(15) C2 0.028(2) 0.020(2) 0.021(2) -0.003(3) 0.001(3) 0.0001(17) C3 0.049(5) 0.032(4) 0.031(4) -0.015(3) -0.008(3) 0.011(3) C4 0.059(5) 0.019(3) 0.039(4) 0.004(2) 0.011(3) 0.000(3) C5 0.030(3) 0.030(3) 0.050(5) 0.005(3) -0.008(3) 0.007(2) C6 0.023(4) 0.025(4) 0.018(3) 0.003(2) 0.009(2) 0.006(3) C7 0.056(5) 0.056(5) 0.035(4) 0.024(4) 0.025(4) 0.014(4) C8 0.046(5) 0.081(6) 0.024(3) -0.020(3) 0.002(3) -0.001(4) C9 0.028(4) 0.068(6) 0.036(4) 0.020(4) 0.016(3) 0.013(4) C10 0.023(2) 0.020(2) 0.042(4) -0.006(3) 0.000(3) -0.0059(17) C11 0.036(4) 0.035(4) 0.050(4) -0.017(3) -0.003(3) -0.005(3) C12 0.039(4) 0.032(4) 0.064(5) 0.012(4) 0.015(4) -0.002(3) C13 0.015(2) 0.031(3) 0.062(4) -0.002(4) 0.005(4) -0.0055(18) C14 0.026(4) 0.035(4) 0.020(3) -0.004(3) -0.001(3) 0.001(3) C15 0.059(5) 0.041(4) 0.028(3) -0.016(3) -0.016(3) 0.013(4) C16 0.034(3) 0.040(4) 0.023(3) 0.006(3) -0.004(2) -0.004(3) C17 0.026(3) 0.040(4) 0.039(4) -0.002(3) -0.001(3) -0.006(3) C18 0.023(2) 0.026(3) 0.021(2) 0.000(3) -0.003(3) -0.0014(17) C19 0.039(3) 0.018(2) 0.018(3) -0.003(2) 0.004(3) -0.0035(19) C20 0.064(6) 0.023(4) 0.050(5) -0.013(3) 0.018(4) -0.010(3) C21 0.042(3) 0.031(3) 0.048(5) -0.001(4) 0.008(4) -0.014(2) C22 0.072(6) 0.025(4) 0.057(5) 0.020(3) -0.022(4) -0.015(4) C23 0.024(2) 0.021(3) 0.066(5) 0.001(4) 0.009(4) 0.0055(19) C24 0.039(5) 0.043(5) 0.103(8) 0.040(5) 0.006(5) 0.013(4) C25 0.021(2) 0.041(3) 0.059(4) 0.008(4) 0.004(4) 0.007(2) C26 0.046(5) 0.049(6) 0.083(7) -0.030(5) 0.021(5) 0.002(4) C27 0.028(4) 0.024(4) 0.019(3) 0.004(2) -0.003(3) 0.003(3) C28 0.037(4) 0.033(4) 0.030(4) 0.010(3) -0.006(3) -0.001(3) C29 0.035(4) 0.036(4) 0.035(4) 0.009(3) -0.007(3) -0.013(3) C30 0.045(5) 0.048(5) 0.027(4) -0.013(3) -0.001(4) 0.008(4) C31 0.025(4) 0.039(5) 0.015(3) -0.001(3) 0.007(3) -0.003(3) C32 0.052(5) 0.042(5) 0.034(4) -0.014(3) 0.017(3) -0.003(3) C33 0.028(4) 0.066(6) 0.042(5) -0.020(4) 0.015(3) -0.013(4) C34 0.055(5) 0.072(6) 0.023(4) 0.020(3) 0.005(4) 0.015(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 C1 1.763(4) . ? W1 O2 1.869(5) . ? W1 O3 1.871(5) . ? W1 O1 1.872(3) . ? W2 C18 1.772(5) . ? W2 O6 1.870(4) . ? W2 O4 1.871(3) . ? W2 O5 1.873(5) . ? O1 C10 1.446(5) . ? O2 C6 1.437(9) . ? O3 C14 1.450(10) . ? O4 C23 1.445(6) . ? O5 C27 1.447(10) . ? O6 C31 1.450(9) . ? C1 C2 1.515(6) . ? C2 C3 1.523(10) . ? C2 C5 1.530(8) . ? C2 C4 1.549(9) . ? C6 C9 1.499(13) . ? C6 C7 1.522(11) . ? C6 C8 1.523(12) . ? C10 C11 1.510(11) . ? C10 C13 1.523(7) . ? C10 C12 1.531(12) . ? C14 C15 1.499(10) . ? C14 C16 1.510(11) . ? C14 C17 1.521(13) . ? C18 C19 1.503(7) . ? C19 C21 1.525(8) . ? C19 C22 1.531(10) . ? C19 C20 1.535(9) . ? C23 C24 1.489(13) . ? C23 C25 1.525(8) . ? C23 C26 1.554(14) . ? C27 C28 1.499(10) . ? C27 C29 1.525(13) . ? C27 C30 1.539(11) . ? C31 C33 1.489(14) . ? C31 C34 1.504(12) . ? C31 C32 1.547(11) . ? 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 C1 W1 O2 109.0(3) . . ? C1 W1 O3 108.8(3) . . ? O2 W1 O3 110.92(14) . . ? C1 W1 O1 108.62(17) . . ? O2 W1 O1 110.8(3) . . ? O3 W1 O1 108.6(3) . . ? C18 W2 O6 109.1(3) . . ? C18 W2 O4 108.91(18) . . ? O6 W2 O4 110.0(3) . . ? C18 W2 O5 108.6(3) . . ? O6 W2 O5 110.45(14) . . ? O4 W2 O5 109.7(3) . . ? C10 O1 W1 141.6(3) . . ? C6 O2 W1 141.9(5) . . ? C14 O3 W1 141.1(5) . . ? C23 O4 W2 141.3(3) . . ? C27 O5 W2 144.0(5) . . ? C31 O6 W2 141.5(5) . . ? C2 C1 W1 177.5(6) . . ? C1 C2 C3 111.0(7) . . ? C1 C2 C5 109.9(4) . . ? C3 C2 C5 110.0(6) . . ? C1 C2 C4 109.7(5) . . ? C3 C2 C4 108.3(5) . . ? C5 C2 C4 107.9(6) . . ? O2 C6 C9 109.3(6) . . ? O2 C6 C7 106.1(6) . . ? C9 C6 C7 110.7(8) . . ? O2 C6 C8 107.1(7) . . ? C9 C6 C8 112.5(8) . . ? C7 C6 C8 110.9(7) . . ? O1 C10 C11 109.6(6) . . ? O1 C10 C13 105.5(4) . . ? C11 C10 C13 112.3(8) . . ? O1 C10 C12 107.3(7) . . ? C11 C10 C12 111.8(6) . . ? C13 C10 C12 110.1(8) . . ? O3 C14 C15 107.3(8) . . ? O3 C14 C16 108.6(7) . . ? C15 C14 C16 110.7(7) . . ? O3 C14 C17 108.2(6) . . ? C15 C14 C17 111.2(8) . . ? C16 C14 C17 110.7(8) . . ? C19 C18 W2 177.8(7) . . ? C18 C19 C21 111.2(5) . . ? C18 C19 C22 110.9(6) . . ? C21 C19 C22 108.0(7) . . ? C18 C19 C20 109.4(6) . . ? C21 C19 C20 107.5(7) . . ? C22 C19 C20 109.9(6) . . ? O4 C23 C24 110.7(8) . . ? O4 C23 C25 106.2(4) . . ? C24 C23 C25 111.8(9) . . ? O4 C23 C26 105.8(8) . . ? C24 C23 C26 112.4(7) . . ? C25 C23 C26 109.7(9) . . ? O5 C27 C28 107.8(7) . . ? O5 C27 C29 109.5(6) . . ? C28 C27 C29 111.2(8) . . ? O5 C27 C30 106.3(7) . . ? C28 C27 C30 111.5(7) . . ? C29 C27 C30 110.3(7) . . ? O6 C31 C33 109.2(7) . . ? O6 C31 C34 107.5(7) . . ? C33 C31 C34 114.8(9) . . ? O6 C31 C32 104.3(6) . . ? C33 C31 C32 110.0(8) . . ? C34 C31 C32 110.5(7) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 W1 O1 C10 -3.6(11) . . . . ? O2 W1 O1 C10 -123.3(9) . . . . ? O3 W1 O1 C10 114.6(9) . . . . ? C1 W1 O2 C6 -2.9(10) . . . . ? O3 W1 O2 C6 -122.7(9) . . . . ? O1 W1 O2 C6 116.6(9) . . . . ? C1 W1 O3 C14 -5.3(9) . . . . ? O2 W1 O3 C14 114.7(9) . . . . ? O1 W1 O3 C14 -123.4(8) . . . . ? C18 W2 O4 C23 2.0(12) . . . . ? O6 W2 O4 C23 121.5(11) . . . . ? O5 W2 O4 C23 -116.8(11) . . . . ? C18 W2 O5 C27 -7.6(9) . . . . ? O6 W2 O5 C27 -127.2(9) . . . . ? O4 W2 O5 C27 111.4(9) . . . . ? C18 W2 O6 C31 2.5(9) . . . . ? O4 W2 O6 C31 -116.9(9) . . . . ? O5 W2 O6 C31 121.8(9) . . . . ? O2 W1 C1 C2 56(10) . . . . ? O3 W1 C1 C2 178(100) . . . . ? O1 W1 C1 C2 -64(10) . . . . ? W1 C1 C2 C3 -6(10) . . . . ? W1 C1 C2 C5 -128(10) . . . . ? W1 C1 C2 C4 114(10) . . . . ? W1 O2 C6 C9 48.8(12) . . . . ? W1 O2 C6 C7 168.1(7) . . . . ? W1 O2 C6 C8 -73.5(11) . . . . ? W1 O1 C10 C11 60.3(12) . . . . ? W1 O1 C10 C13 -178.6(8) . . . . ? W1 O1 C10 C12 -61.3(11) . . . . ? W1 O3 C14 C15 172.7(6) . . . . ? W1 O3 C14 C16 53.0(11) . . . . ? W1 O3 C14 C17 -67.2(10) . . . . ? O6 W2 C18 C19 -65(15) . . . . ? O4 W2 C18 C19 56(15) . . . . ? O5 W2 C18 C19 175(100) . . . . ? W2 C18 C19 C21 127(15) . . . . ? W2 C18 C19 C22 7(15) . . . . ? W2 C18 C19 C20 -115(15) . . . . ? W2 O4 C23 C24 -58.5(14) . . . . ? W2 O4 C23 C25 180.0(9) . . . . ? W2 O4 C23 C26 63.5(13) . . . . ? W2 O5 C27 C28 165.8(6) . . . . ? W2 O5 C27 C29 44.7(12) . . . . ? W2 O5 C27 C30 -74.4(11) . . . . ? W2 O6 C31 C33 -49.7(12) . . . . ? W2 O6 C31 C34 75.4(11) . . . . ? W2 O6 C31 C32 -167.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.846 _refine_diff_density_min -1.514 _refine_diff_density_rms 0.177