Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Prof I Parkin' _publ_contact_author_address ; Department of Chemistry Christopher Ingold Laboratory University College London 20 Gordon Street London WC1H 0AJ ; _publ_contact_author_email I.P.PARKIN@UCL.AC.UK _publ_section_title ; Synthesis and characterisation of tungsten(VI) oxo-salicylate complexes for use in the chemical vapour deposition of self cleaning films ; loop_ _publ_author_name 'I. Parkin' 'Warren B. Cross' 'Andrew J. P. White' 'David J. Williams' data_Compound_1 _database_code_depnum_ccdc_archive 'CCDC 258927' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C32.50 H27 O15 Cl W2' _chemical_formula_weight 1060.69 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -5.4734 5.5774 '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 10.9865(7) _cell_length_b 11.6322(9) _cell_length_c 14.8949(11) _cell_angle_alpha 71.128(6) _cell_angle_beta 87.945(5) _cell_angle_gamma 73.363(5) _cell_volume 1722.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 58 _cell_measurement_theta_min 8.82 _cell_measurement_theta_max 24.92 _exptl_crystal_description plates _exptl_crystal_colour Orange _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.045 _exptl_crystal_density_method ? _exptl_crystal_F_000 1014 _exptl_absorpt_coefficient_mu 13.509 _exptl_absorpt_correction_type 'Lamina [1 1 0]' _exptl_absorpt_correction_T_min 0.4546 _exptl_absorpt_correction_T_max 0.7381 _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4949 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 59.98 _reflns_number_total 4669 _reflns_number_observed 3841 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 266 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+3.8436P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00049(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4403 _refine_ls_number_parameters 470 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_obs 0.0453 _refine_ls_wR_factor_all 0.1237 _refine_ls_wR_factor_obs 0.1117 _refine_ls_goodness_of_fit_all 1.050 _refine_ls_goodness_of_fit_obs 1.082 _refine_ls_restrained_S_all 1.079 _refine_ls_restrained_S_obs 1.087 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.31242(4) 0.13797(4) 0.12136(3) 0.0306(2) Uani 1 d . . W2 W 0.09707(4) 0.13633(4) 0.32187(3) 0.0328(2) Uani 1 d . . O1 O 0.4443(7) 0.0175(6) 0.1693(6) 0.042(2) Uani 1 d . . O2 O 0.0232(8) 0.0242(6) 0.3287(5) 0.040(2) Uani 1 d . . O3 O 0.2109(7) 0.1090(6) 0.2279(5) 0.035(2) Uani 1 d . . C4 C 0.3487(9) 0.4312(9) 0.0109(7) 0.031(2) Uani 1 d . . C5 C 0.3776(9) 0.3436(9) -0.0375(8) 0.034(2) Uani 1 d . . O5 O 0.3804(7) 0.2210(6) 0.0051(5) 0.037(2) Uani 1 d . . C6 C 0.4094(11) 0.3775(11) -0.1330(7) 0.040(2) Uani 1 d . . C7 C 0.4042(12) 0.5037(11) -0.1785(8) 0.046(3) Uani 1 d . . H7A H 0.4249(12) 0.5295(11) -0.2431(8) 0.056 Uiso 1 calc R . C8 C 0.3690(12) 0.5938(11) -0.1314(8) 0.046(3) Uani 1 d . . H8A H 0.3611(12) 0.6805(11) -0.1653(8) 0.055 Uiso 1 calc R . C9 C 0.3460(10) 0.5578(10) -0.0373(8) 0.040(2) Uani 1 d . . H9A H 0.3282(10) 0.6179(10) -0.0045(8) 0.049 Uiso 1 calc R . C10 C 0.3315(10) 0.3923(10) 0.1141(8) 0.036(2) Uani 1 d . . O10 O 0.3137(7) 0.4691(7) 0.1589(5) 0.039(2) Uani 1 d . . O11 O 0.3490(7) 0.2707(7) 0.1618(5) 0.039(2) Uani 1 d . . C12 C 0.4457(15) 0.2768(12) -0.1803(9) 0.056(3) Uani 1 d . . H12A H 0.3697(15) 0.2545(12) -0.1923(9) 0.084 Uiso 1 d R . H12B H 0.5080(15) 0.2012(12) -0.1386(9) 0.084 Uiso 1 d R . H12C H 0.4828(15) 0.3092(12) -0.2407(9) 0.084 Uiso 1 d R . C13 C 0.0561(10) 0.2050(10) -0.0419(7) 0.034(2) Uani 1 d . . C14 C 0.1556(10) 0.0935(10) -0.0201(7) 0.034(2) Uani 1 d . . O14 O 0.2430(7) 0.0573(6) 0.0536(5) 0.0334(15) Uani 1 d . . C15 C 0.1672(13) 0.0100(11) -0.0727(9) 0.048(3) Uani 1 d . . C16 C 0.0758(15) 0.0417(14) -0.1434(9) 0.059(3) Uani 1 d . . H16A H 0.0825(15) -0.0125(14) -0.1804(9) 0.071 Uiso 1 calc R . C17 C -0.0260(14) 0.1501(13) -0.1628(9) 0.058(3) Uani 1 d . . H17A H -0.0879(14) 0.1672(13) -0.2119(9) 0.069 Uiso 1 calc R . C18 C -0.0409(11) 0.2340(11) -0.1134(7) 0.040(2) Uani 1 d . . H18A H -0.1121(11) 0.3076(11) -0.1263(7) 0.048 Uiso 1 calc R . C19 C 0.0459(10) 0.2927(9) 0.0123(7) 0.033(2) Uani 1 d . . O19 O 0.1363(6) 0.2918(6) 0.0611(5) 0.0307(14) Uani 1 d . . O20 O -0.0637(7) 0.3761(8) 0.0048(5) 0.044(2) Uani 1 d . . C21 C 0.2790(14) -0.1065(12) -0.0508(10) 0.056(3) Uani 1 d . . H21A H 0.2715(14) -0.1661(12) 0.0116(10) 0.084 Uiso 1 d R . H21B H 0.3577(14) -0.0830(12) -0.0499(10) 0.084 Uiso 1 d R . H21C H 0.2811(14) -0.1468(12) -0.0995(10) 0.084 Uiso 1 d R . C22 C 0.3255(10) 0.1790(10) 0.4594(7) 0.033(2) Uani 1 d . . C23 C 0.2875(11) 0.0681(11) 0.4860(7) 0.037(2) Uani 1 d . . O23 O 0.2166(7) 0.0421(6) 0.4263(5) 0.035(2) Uani 1 d . . C24 C 0.3296(12) -0.0272(11) 0.5755(8) 0.046(3) Uani 1 d . . C25 C 0.4055(14) -0.0028(13) 0.6352(9) 0.058(3) Uani 1 d . . H25A H 0.4348(14) -0.0652(13) 0.6956(9) 0.070 Uiso 1 calc R . C26 C 0.4409(14) 0.1078(13) 0.6113(9) 0.055(3) Uani 1 d . . H26A H 0.4930(14) 0.1211(13) 0.6543(9) 0.066 Uiso 1 calc R . C27 C 0.3989(12) 0.1981(12) 0.5238(9) 0.049(3) Uani 1 d . . H27A H 0.4209(12) 0.2753(12) 0.5072(9) 0.059 Uiso 1 calc R . C28 C 0.2849(11) 0.2759(9) 0.3663(7) 0.035(2) Uani 1 d . . O28 O 0.1966(7) 0.2774(6) 0.3145(5) 0.0338(15) Uani 1 d . . O29 O 0.3456(8) 0.3615(8) 0.3382(6) 0.046(2) Uani 1 d . . C30 C 0.2919(14) -0.1447(12) 0.5993(9) 0.055(3) Uani 1 d . . H30A H 0.2036(14) -0.1244(12) 0.5756(9) 0.082 Uiso 1 d R . H30B H 0.2991(14) -0.1854(12) 0.6685(9) 0.082 Uiso 1 d R . H30C H 0.3479(14) -0.2026(12) 0.5698(9) 0.082 Uiso 1 d R . C31 C -0.0852(11) 0.4349(10) 0.3007(8) 0.039(2) Uani 1 d . . C32 C -0.0609(13) 0.3452(11) 0.3896(8) 0.044(3) Uani 1 d . . O32 O -0.0052(8) 0.2178(7) 0.4036(5) 0.042(2) Uani 1 d . . C33 C -0.0937(18) 0.3821(14) 0.4714(9) 0.066(4) Uani 1 d . . C34 C -0.1436(21) 0.5068(14) 0.4585(11) 0.083(6) Uani 1 d . . H34A H -0.1602(21) 0.5324(14) 0.5133(11) 0.099 Uiso 1 calc R . C35 C -0.1716(17) 0.5982(13) 0.3717(10) 0.069(4) Uani 1 d . . H35A H -0.2122(17) 0.6841(13) 0.3667(10) 0.083 Uiso 1 calc R . C36 C -0.1401(14) 0.5649(12) 0.2899(9) 0.056(3) Uani 1 d . . H36A H -0.1552(14) 0.6277(12) 0.2287(9) 0.067 Uiso 1 calc R . C37 C -0.0603(10) 0.4021(11) 0.2136(8) 0.037(2) Uani 1 d . . O37 O -0.0869(7) 0.4814(7) 0.1336(5) 0.041(2) Uani 1 d . . O38 O -0.0132(7) 0.2794(7) 0.2222(5) 0.0343(15) Uani 1 d . . C39 C -0.0676(23) 0.2785(17) 0.5664(10) 0.090(6) Uani 1 d U . H39A H 0.0237(23) 0.2338(17) 0.5763(10) 0.135 Uiso 1 d R . H39B H -0.1152(23) 0.2184(17) 0.5678(10) 0.135 Uiso 1 d R . H39C H -0.0943(23) 0.3157(17) 0.6168(10) 0.135 Uiso 1 d R . C40 C 0.6658(33) 0.2747(48) 0.6174(31) 0.087(11) Uani 0.50 d PU . Cl1 Cl 0.5964(20) 0.3907(20) 0.5780(13) 0.140(5) Uani 0.50 d PU . Cl2 Cl 0.5100(27) 0.5149(24) 0.4468(15) 0.180(8) Uani 0.50 d PU . 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 0.0336(3) 0.0202(3) 0.0339(3) -0.0087(2) -0.0101(2) -0.0001(2) W2 0.0411(3) 0.0254(3) 0.0304(3) -0.0058(2) -0.0085(2) -0.0101(2) O1 0.045(4) 0.022(3) 0.049(4) -0.009(3) -0.018(3) 0.004(3) O2 0.062(5) 0.022(3) 0.041(4) -0.009(3) 0.001(3) -0.020(3) O3 0.046(4) 0.019(3) 0.040(4) -0.009(3) -0.012(3) -0.006(3) C4 0.037(5) 0.026(5) 0.025(5) -0.006(4) -0.004(4) -0.003(4) C5 0.021(4) 0.028(5) 0.050(6) -0.017(4) -0.002(4) 0.001(4) O5 0.035(4) 0.024(3) 0.047(4) -0.016(3) -0.006(3) 0.003(3) C6 0.043(6) 0.043(6) 0.030(5) -0.015(5) -0.003(4) -0.003(5) C7 0.049(7) 0.042(6) 0.039(6) -0.005(5) 0.005(5) -0.009(5) C8 0.057(7) 0.030(6) 0.037(6) 0.000(5) -0.004(5) -0.005(5) C9 0.039(6) 0.033(6) 0.046(6) -0.014(5) -0.003(5) -0.004(4) C10 0.031(5) 0.036(6) 0.042(6) -0.012(5) -0.006(4) -0.010(4) O10 0.051(4) 0.037(4) 0.030(4) -0.010(3) -0.001(3) -0.014(3) O11 0.044(4) 0.028(4) 0.043(4) -0.011(3) -0.011(3) -0.006(3) C12 0.076(9) 0.047(7) 0.043(7) -0.021(6) 0.005(6) -0.011(6) C13 0.041(5) 0.037(5) 0.024(5) -0.007(4) -0.008(4) -0.012(4) C14 0.048(6) 0.033(5) 0.020(4) -0.001(4) -0.004(4) -0.019(5) O14 0.036(4) 0.028(3) 0.035(4) -0.014(3) -0.008(3) -0.001(3) C15 0.066(8) 0.035(6) 0.047(6) -0.018(5) 0.004(6) -0.018(5) C16 0.083(10) 0.063(8) 0.046(7) -0.025(6) -0.004(7) -0.033(7) C17 0.070(9) 0.060(8) 0.042(6) -0.016(6) -0.023(6) -0.015(6) C18 0.038(6) 0.045(6) 0.031(5) -0.005(5) -0.016(4) -0.010(5) C19 0.037(5) 0.023(5) 0.032(5) -0.006(4) -0.005(4) -0.004(4) O19 0.032(3) 0.022(3) 0.033(4) -0.008(3) -0.009(3) 0.000(3) O20 0.034(4) 0.048(5) 0.039(4) -0.013(3) -0.007(3) 0.002(3) C21 0.067(8) 0.036(6) 0.070(8) -0.029(6) 0.004(7) -0.010(6) C22 0.036(5) 0.036(5) 0.030(5) -0.015(4) -0.008(4) -0.009(4) C23 0.049(6) 0.039(6) 0.025(5) -0.012(4) -0.004(4) -0.012(5) O23 0.053(4) 0.026(3) 0.024(3) -0.002(3) -0.004(3) -0.013(3) C24 0.053(7) 0.041(6) 0.035(6) -0.005(5) -0.014(5) -0.004(5) C25 0.064(8) 0.056(8) 0.036(6) -0.003(5) -0.020(6) 0.000(6) C26 0.068(8) 0.053(8) 0.043(7) -0.015(6) -0.017(6) -0.015(6) C27 0.057(7) 0.048(7) 0.045(7) -0.020(5) -0.007(6) -0.013(6) C28 0.050(6) 0.022(5) 0.032(5) -0.012(4) -0.002(4) -0.005(4) O28 0.036(4) 0.029(4) 0.032(4) -0.005(3) -0.008(3) -0.008(3) O29 0.055(5) 0.047(5) 0.046(4) -0.017(4) -0.011(4) -0.024(4) C30 0.065(8) 0.052(7) 0.035(6) 0.003(5) -0.012(6) -0.018(6) C31 0.046(6) 0.033(6) 0.034(5) -0.009(4) -0.002(5) -0.007(4) C32 0.065(7) 0.034(6) 0.034(6) -0.013(5) 0.002(5) -0.014(5) O32 0.067(5) 0.036(4) 0.026(3) -0.008(3) -0.002(3) -0.020(4) C33 0.113(13) 0.051(8) 0.038(7) -0.019(6) 0.027(7) -0.028(8) C34 0.150(18) 0.046(8) 0.055(8) -0.022(7) 0.030(10) -0.030(9) C35 0.106(12) 0.037(7) 0.052(8) -0.019(6) 0.013(8) 0.003(7) C36 0.070(9) 0.043(7) 0.045(7) -0.014(5) 0.008(6) -0.003(6) C37 0.036(5) 0.046(6) 0.037(6) -0.022(5) 0.004(4) -0.012(5) O37 0.049(4) 0.035(4) 0.027(4) -0.005(3) -0.003(3) 0.001(3) O38 0.040(4) 0.036(4) 0.029(3) -0.014(3) -0.004(3) -0.011(3) C39 0.158(15) 0.068(9) 0.037(7) -0.016(7) 0.011(8) -0.026(9) C40 0.055(17) 0.132(28) 0.107(24) -0.069(22) 0.032(16) -0.043(18) Cl1 0.159(12) 0.170(12) 0.147(11) -0.089(10) 0.042(9) -0.092(10) Cl2 0.205(11) 0.179(11) 0.182(11) -0.057(9) 0.010(9) -0.095(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.685(7) . ? W1 O14 1.887(7) . ? W1 O3 1.903(8) . ? W1 O5 1.931(8) . ? W1 O11 1.970(7) . ? W1 O19 2.203(6) . ? W2 O2 1.698(7) . ? W2 O3 1.886(8) . ? W2 O23 1.888(7) . ? W2 O32 1.918(8) . ? W2 O38 1.954(7) . ? W2 O28 2.192(7) . ? C4 C5 1.391(14) . ? C4 C9 1.41(2) . ? C4 C10 1.476(15) . ? C5 O5 1.352(13) . ? C5 C6 1.41(2) . ? C6 C7 1.39(2) . ? C6 C12 1.51(2) . ? C7 C8 1.40(2) . ? C8 C9 1.36(2) . ? C10 O10 1.249(13) . ? C10 O11 1.322(13) . ? C13 C14 1.39(2) . ? C13 C18 1.423(14) . ? C13 C19 1.471(14) . ? C14 O14 1.359(12) . ? C14 C15 1.41(2) . ? C15 C16 1.37(2) . ? C15 C21 1.50(2) . ? C16 C17 1.38(2) . ? C17 C18 1.37(2) . ? C19 O19 1.247(12) . ? C19 O20 1.294(13) . ? C22 C27 1.38(2) . ? C22 C23 1.40(2) . ? C22 C28 1.462(15) . ? C23 O23 1.359(13) . ? C23 C24 1.42(2) . ? C24 C25 1.38(2) . ? C24 C30 1.47(2) . ? C25 C26 1.38(2) . ? C26 C27 1.38(2) . ? C28 O28 1.254(13) . ? C28 O29 1.304(14) . ? C31 C32 1.37(2) . ? C31 C36 1.41(2) . ? C31 C37 1.462(14) . ? C32 O32 1.380(14) . ? C32 C33 1.42(2) . ? C33 C34 1.35(2) . ? C33 C39 1.50(2) . ? C34 C35 1.36(2) . ? C35 C36 1.40(2) . ? C37 O37 1.231(14) . ? C37 O38 1.336(13) . ? C40 Cl1 1.29(5) . ? Cl1 Cl2 1.32(3) 2_666 ? Cl1 Cl2 2.08(4) . ? Cl2 Cl1 1.32(3) 2_666 ? Cl2 Cl2 1.53(4) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O14 97.7(3) . . ? O1 W1 O3 98.0(3) . . ? O14 W1 O3 97.0(3) . . ? O1 W1 O5 98.3(3) . . ? O14 W1 O5 88.6(3) . . ? O3 W1 O5 161.9(3) . . ? O1 W1 O11 99.5(3) . . ? O14 W1 O11 161.6(3) . . ? O3 W1 O11 87.2(3) . . ? O5 W1 O11 82.4(3) . . ? O1 W1 O19 178.2(3) . . ? O14 W1 O19 81.5(3) . . ? O3 W1 O19 80.6(3) . . ? O5 W1 O19 83.3(3) . . ? O11 W1 O19 81.5(3) . . ? O2 W2 O3 99.1(3) . . ? O2 W2 O23 98.0(3) . . ? O3 W2 O23 95.8(3) . . ? O2 W2 O32 99.3(4) . . ? O3 W2 O32 160.5(3) . . ? O23 W2 O32 88.0(3) . . ? O2 W2 O38 99.6(3) . . ? O3 W2 O38 87.9(3) . . ? O23 W2 O38 161.2(3) . . ? O32 W2 O38 82.7(3) . . ? O2 W2 O28 178.6(3) . . ? O3 W2 O28 80.3(3) . . ? O23 W2 O28 80.8(3) . . ? O32 W2 O28 81.4(3) . . ? O38 W2 O28 81.6(3) . . ? W2 O3 W1 161.9(4) . . ? C5 C4 C9 119.5(10) . . ? C5 C4 C10 121.5(9) . . ? C9 C4 C10 118.8(9) . . ? O5 C5 C4 122.0(10) . . ? O5 C5 C6 116.5(9) . . ? C4 C5 C6 121.4(10) . . ? C5 O5 W1 131.7(6) . . ? C7 C6 C5 117.3(10) . . ? C7 C6 C12 123.8(10) . . ? C5 C6 C12 118.9(10) . . ? C6 C7 C8 121.5(11) . . ? C9 C8 C7 120.4(11) . . ? C8 C9 C4 119.7(10) . . ? O10 C10 O11 118.9(10) . . ? O10 C10 C4 121.6(9) . . ? O11 C10 C4 119.0(9) . . ? C10 O11 W1 129.7(7) . . ? C14 C13 C18 121.1(10) . . ? C14 C13 C19 120.1(9) . . ? C18 C13 C19 118.8(10) . . ? O14 C14 C13 122.5(9) . . ? O14 C14 C15 117.0(10) . . ? C13 C14 C15 120.4(10) . . ? C14 O14 W1 136.8(6) . . ? C16 C15 C14 117.6(12) . . ? C16 C15 C21 123.1(12) . . ? C14 C15 C21 119.3(11) . . ? C15 C16 C17 122.1(12) . . ? C18 C17 C16 122.2(11) . . ? C17 C18 C13 116.5(11) . . ? O19 C19 O20 120.3(9) . . ? O19 C19 C13 123.7(9) . . ? O20 C19 C13 115.9(9) . . ? C19 O19 W1 129.2(6) . . ? C27 C22 C23 119.1(10) . . ? C27 C22 C28 120.0(10) . . ? C23 C22 C28 120.9(9) . . ? O23 C23 C22 122.4(9) . . ? O23 C23 C24 116.8(10) . . ? C22 C23 C24 120.7(10) . . ? C23 O23 W2 136.7(7) . . ? C25 C24 C23 116.9(12) . . ? C25 C24 C30 124.0(11) . . ? C23 C24 C30 119.1(11) . . ? C26 C25 C24 123.3(12) . . ? C27 C26 C25 118.4(12) . . ? C26 C27 C22 121.6(12) . . ? O28 C28 O29 120.7(9) . . ? O28 C28 C22 122.2(10) . . ? O29 C28 C22 117.1(10) . . ? C28 O28 W2 131.9(6) . . ? C32 C31 C36 120.5(11) . . ? C32 C31 C37 122.6(10) . . ? C36 C31 C37 116.9(10) . . ? C31 C32 O32 122.4(10) . . ? C31 C32 C33 120.0(11) . . ? O32 C32 C33 117.5(11) . . ? C32 O32 W2 129.9(7) . . ? C34 C33 C32 117.8(13) . . ? C34 C33 C39 125.0(13) . . ? C32 C33 C39 117.2(13) . . ? C33 C34 C35 123.9(14) . . ? C34 C35 C36 119.5(13) . . ? C35 C36 C31 118.1(12) . . ? O37 C37 O38 119.1(9) . . ? O37 C37 C31 123.0(10) . . ? O38 C37 C31 117.8(10) . . ? C37 O38 W2 131.5(6) . . ? C40 Cl1 Cl2 156.1(23) . 2_666 ? C40 Cl1 Cl2 140.6(22) . . ? Cl2 Cl1 Cl2 47.2(18) 2_666 . ? Cl1 Cl2 Cl2 93.5(26) 2_666 2_666 ? Cl1 Cl2 Cl1 132.8(18) 2_666 . ? Cl2 Cl2 Cl1 39.3(15) 2_666 . ? _refine_diff_density_max 1.283 _refine_diff_density_min -1.511 _refine_diff_density_rms 0.162 #===END data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 258928' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C52 H66 O15 W2' _chemical_formula_weight 1298.75 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -5.4734 5.5774 '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 17.161(2) _cell_length_b 20.482(2) _cell_length_c 25.789(3) _cell_angle_alpha 98.165(9) _cell_angle_beta 98.061(10) _cell_angle_gamma 91.365(11) _cell_volume 8875.2(17) _cell_formula_units_Z 6 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 11.05 _cell_measurement_theta_max 25.02 _exptl_crystal_description prisms _exptl_crystal_colour Red _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.458 _exptl_crystal_density_method ? _exptl_crystal_F_000 3876 _exptl_absorpt_coefficient_mu 7.563 _exptl_absorpt_correction_type Ellipsoidal _exptl_absorpt_correction_T_min 0.0690 _exptl_absorpt_correction_T_max 0.1731 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27332 _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 60.00 _reflns_number_total 26310 _reflns_number_observed 21816 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 1077 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0786P)^2^+5.4584P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000076(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 25233 _refine_ls_number_parameters 1981 _refine_ls_number_restraints 216 _refine_ls_R_factor_all 0.0601 _refine_ls_R_factor_obs 0.0477 _refine_ls_wR_factor_all 0.1363 _refine_ls_wR_factor_obs 0.1237 _refine_ls_goodness_of_fit_all 1.057 _refine_ls_goodness_of_fit_obs 1.095 _refine_ls_restrained_S_all 1.092 _refine_ls_restrained_S_obs 1.096 _refine_ls_shift/esd_max 0.086 _refine_ls_shift/esd_mean 0.002 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W1 W 0.67695(2) 0.89065(2) 0.428433(14) 0.05800(8) Uani 1 d . . W2 W 0.86833(2) 0.80633(2) 0.432642(14) 0.05635(8) Uani 1 d . . O1 O 0.7004(3) 0.9711(3) 0.4267(3) 0.0733(15) Uani 1 d . . O2 O 0.8908(3) 0.7995(3) 0.3705(2) 0.0707(14) Uani 1 d . . O3 O 0.7775(3) 0.8568(3) 0.4232(2) 0.0610(12) Uani 1 d . . C4 C 0.5689(5) 0.8616(4) 0.5271(4) 0.069(2) Uani 1 d . . C5 C 0.5297(5) 0.8794(4) 0.4799(4) 0.067(2) Uani 1 d . . O5 O 0.5698(3) 0.8984(3) 0.4420(2) 0.0641(12) Uani 1 d . . C6 C 0.4465(5) 0.8781(5) 0.4702(4) 0.075(2) Uani 1 d . . C7 C 0.4077(6) 0.8616(6) 0.5114(6) 0.106(4) Uani 1 d . . H7A H 0.3530(6) 0.8621(6) 0.5067(6) 0.127 Uiso 1 calc R . C8 C 0.4448(7) 0.8447(7) 0.5579(5) 0.092(3) Uani 1 d . . C9 C 0.5253(6) 0.8446(5) 0.5652(4) 0.082(2) Uani 1 d . . H9A H 0.5515(6) 0.8328(5) 0.5964(4) 0.098 Uiso 1 calc R . C10 C 0.6560(5) 0.8648(5) 0.5390(4) 0.074(2) Uani 1 d . . O10 O 0.6904(4) 0.8500(4) 0.5810(3) 0.088(2) Uani 1 d . . O11 O 0.6959(3) 0.8872(3) 0.5049(2) 0.0666(13) Uani 1 d . . C12 C 0.4071(5) 0.8970(6) 0.4188(5) 0.092(3) Uani 1 d . . H12A H 0.4427(5) 0.8874(6) 0.3923(5) 0.111 Uiso 1 calc R . C13 C 0.3940(12) 0.9711(8) 0.4257(8) 0.158(7) Uani 1 d U . H13A H 0.3689(12) 0.9829(8) 0.3929(8) 0.238 Uiso 1 calc R . H13B H 0.4438(12) 0.9951(8) 0.4360(8) 0.238 Uiso 1 calc R . H13C H 0.3611(12) 0.9819(8) 0.4526(8) 0.238 Uiso 1 calc R . C14 C 0.3300(9) 0.8585(10) 0.3981(8) 0.143(6) Uani 1 d . . H14A H 0.3074(9) 0.8723(10) 0.3655(8) 0.214 Uiso 1 calc R . H14B H 0.2944(9) 0.8667(10) 0.4237(8) 0.214 Uiso 1 calc R . H14C H 0.3394(9) 0.8122(10) 0.3922(8) 0.214 Uiso 1 calc R . C15 C 0.3996(7) 0.8238(7) 0.6003(6) 0.115(4) Uani 1 d D . H15A H 0.4375(7) 0.8194(7) 0.6316(6) 0.138 Uiso 0.55 calc PR 1 H15D H 0.4359(7) 0.7989(7) 0.6205(6) 0.138 Uiso 0.45 d PR 2 C16 C 0.3550(11) 0.7563(8) 0.5804(8) 0.095(6) Uani 0.55 d PD 1 H16A H 0.3270(11) 0.7440(8) 0.6075(8) 0.142 Uiso 0.55 calc PR 1 H16B H 0.3920(11) 0.7233(8) 0.5721(8) 0.142 Uiso 0.55 calc PR 1 H16C H 0.3183(11) 0.7596(8) 0.5493(8) 0.142 Uiso 0.55 calc PR 1 C17 C 0.3405(16) 0.8754(11) 0.6163(13) 0.137(9) Uani 0.55 d PDU 1 H17A H 0.3131(16) 0.8609(11) 0.6429(13) 0.206 Uiso 0.55 calc PR 1 H17B H 0.3033(16) 0.8806(11) 0.5859(13) 0.206 Uiso 0.55 calc PR 1 H17C H 0.3681(16) 0.9168(11) 0.6302(13) 0.206 Uiso 0.55 calc PR 1 C16A C 0.3163(15) 0.7916(24) 0.5838(24) 0.220(28) Uiso 0.45 d PD 2 H16J H 0.2958(15) 0.7813(24) 0.6146(24) 0.330 Uiso 0.45 calc PR 2 H16K H 0.3184(15) 0.7518(24) 0.5595(24) 0.330 Uiso 0.45 calc PR 2 H16L H 0.2826(15) 0.8216(24) 0.5670(24) 0.330 Uiso 0.45 calc PR 2 C17A C 0.3984(19) 0.8886(11) 0.6394(11) 0.112(8) Uiso 0.45 d PD 2 H17J H 0.3708(19) 0.8803(11) 0.6679(11) 0.167 Uiso 0.45 calc PR 2 H17K H 0.3721(19) 0.9214(11) 0.6211(11) 0.167 Uiso 0.45 calc PR 2 H17L H 0.4514(19) 0.9041(11) 0.6534(11) 0.167 Uiso 0.45 calc PR 2 C18 C 0.5594(4) 0.7646(4) 0.3445(3) 0.061(2) Uani 1 d . . C19 C 0.5700(4) 0.8271(4) 0.3307(3) 0.060(2) Uani 1 d . . O19 O 0.6321(3) 0.8688(3) 0.3565(2) 0.0605(12) Uani 1 d . . C20 C 0.5216(5) 0.8489(5) 0.2893(4) 0.074(2) Uani 1 d . . C21 C 0.4625(6) 0.8045(5) 0.2617(4) 0.081(2) Uani 1 d . . H21A H 0.4285(6) 0.8183(5) 0.2344(4) 0.097 Uiso 1 calc R . C22 C 0.4515(5) 0.7418(6) 0.2725(4) 0.080(2) Uani 1 d . . C23 C 0.4997(5) 0.7219(5) 0.3143(4) 0.074(2) Uani 1 d . . H23A H 0.4926(5) 0.6795(5) 0.3225(4) 0.089 Uiso 1 calc R . C24 C 0.6109(4) 0.7433(4) 0.3893(3) 0.060(2) Uani 1 d . . O24 O 0.6477(3) 0.7829(3) 0.4258(2) 0.0607(12) Uani 1 d . . O25 O 0.6151(4) 0.6799(3) 0.3894(3) 0.077(2) Uani 1 d . . C26 C 0.5359(7) 0.9166(6) 0.2764(5) 0.099(3) Uani 1 d D . H26A H 0.5538(7) 0.9450(6) 0.3101(5) 0.118 Uiso 0.70 calc PR 1 H26D H 0.5725(7) 0.9357(6) 0.3067(5) 0.118 Uiso 0.30 d PR 2 C27 C 0.6021(14) 0.9197(13) 0.2421(12) 0.166(12) Uani 0.70 d PD 1 H27A H 0.6090(14) 0.9641(13) 0.2349(12) 0.250 Uiso 0.70 calc PR 1 H27B H 0.5883(14) 0.8905(13) 0.2094(12) 0.250 Uiso 0.70 calc PR 1 H27C H 0.6503(14) 0.9066(13) 0.2607(12) 0.250 Uiso 0.70 calc PR 1 C28 C 0.4591(11) 0.9448(14) 0.2519(12) 0.161(10) Uani 0.70 d PDU 1 H28A H 0.4701(11) 0.9882(14) 0.2441(12) 0.242 Uiso 0.70 calc PR 1 H28B H 0.4219(11) 0.9471(14) 0.2766(12) 0.242 Uiso 0.70 calc PR 1 H28C H 0.4375(11) 0.9165(14) 0.2199(12) 0.242 Uiso 0.70 calc PR 1 C27A C 0.5195(38) 0.9201(26) 0.2164(7) 0.140(18) Uiso 0.30 d PD 2 H27J H 0.5296(38) 0.9645(26) 0.2104(7) 0.210 Uiso 0.30 calc PR 2 H27K H 0.4655(38) 0.9069(26) 0.2033(7) 0.210 Uiso 0.30 calc PR 2 H27L H 0.5532(38) 0.8911(26) 0.1982(7) 0.210 Uiso 0.30 calc PR 2 C28A C 0.5021(30) 0.9762(17) 0.3083(16) 0.122(14) Uiso 0.30 d PD 2 H28J H 0.5161(30) 1.0160(17) 0.2955(16) 0.183 Uiso 0.30 calc PR 2 H28K H 0.5235(30) 0.9790(17) 0.3451(16) 0.183 Uiso 0.30 calc PR 2 H28L H 0.4458(30) 0.9705(17) 0.3043(16) 0.183 Uiso 0.30 calc PR 2 C29 C 0.3849(6) 0.6950(7) 0.2399(6) 0.104(4) Uani 1 d . . H29A H 0.3703(6) 0.7139(7) 0.2073(6) 0.125 Uiso 1 calc R . C30 C 0.4103(10) 0.6267(9) 0.2220(8) 0.156(7) Uani 1 d . . H30A H 0.4571(10) 0.6298(9) 0.2059(8) 0.233 Uiso 1 calc R . H30B H 0.3691(10) 0.6032(9) 0.1967(8) 0.233 Uiso 1 calc R . H30C H 0.4208(10) 0.6036(9) 0.2519(8) 0.233 Uiso 1 calc R . C31 C 0.3123(8) 0.6967(11) 0.2657(8) 0.164(8) Uani 1 d U . H31A H 0.3001(8) 0.7418(11) 0.2760(8) 0.246 Uiso 1 calc R . H31B H 0.3209(8) 0.6750(11) 0.2965(8) 0.246 Uiso 1 calc R . H31C H 0.2693(8) 0.6746(11) 0.2413(8) 0.246 Uiso 1 calc R . C32 C 0.9522(5) 0.8904(4) 0.5574(3) 0.068(2) Uani 1 d . . C33 C 0.9835(5) 0.8971(4) 0.5112(3) 0.064(2) Uani 1 d . . O33 O 0.9415(3) 0.8774(3) 0.4629(2) 0.0625(12) Uani 1 d . . C34 C 1.0595(5) 0.9269(4) 0.5134(4) 0.068(2) Uani 1 d . . C35 C 1.0991(5) 0.9492(5) 0.5639(4) 0.080(2) Uani 1 d . . H35A H 1.1497(5) 0.9678(5) 0.5666(4) 0.096 Uiso 1 calc R . C36 C 1.0693(6) 0.9457(6) 0.6095(5) 0.094(3) Uani 1 d . . C37 C 0.9951(6) 0.9153(5) 0.6069(4) 0.085(3) Uani 1 d . . H37A H 0.9742(6) 0.9116(5) 0.6378(4) 0.102 Uiso 1 calc R . C38 C 0.8730(5) 0.8593(4) 0.5550(3) 0.066(2) Uani 1 d . . O38 O 0.8404(3) 0.8218(3) 0.5160(2) 0.0632(12) Uani 1 d . . O39 O 0.8374(4) 0.8729(4) 0.5965(2) 0.082(2) Uani 1 d . . C40 C 1.0914(5) 0.9313(5) 0.4631(4) 0.076(2) Uani 1 d . . H40A H 1.0502(5) 0.9474(5) 0.4384(4) 0.091 Uiso 1 calc R . C41 C 1.1126(7) 0.8622(6) 0.4384(5) 0.097(3) Uani 1 d . . H41A H 1.1331(7) 0.8654(6) 0.4060(5) 0.146 Uiso 1 calc R . H41B H 1.0663(7) 0.8333(6) 0.4311(5) 0.146 Uiso 1 calc R . H41C H 1.1517(7) 0.8449(6) 0.4626(5) 0.146 Uiso 1 calc R . C42 C 1.1641(5) 0.9778(5) 0.4700(5) 0.085(3) Uani 1 d . . H42A H 1.1816(5) 0.9785(5) 0.4363(5) 0.127 Uiso 1 calc R . H42B H 1.2053(5) 0.9628(5) 0.4940(5) 0.127 Uiso 1 calc R . H42C H 1.1511(5) 1.0216(5) 0.4839(5) 0.127 Uiso 1 calc R . C43 C 1.1157(8) 0.9735(7) 0.6635(5) 0.123(5) Uani 1 d D . H43A H 1.0802(8) 0.9704(7) 0.6898(5) 0.147 Uiso 0.60 calc PR 1 H43D H 1.1664(8) 0.9845(7) 0.6545(5) 0.147 Uiso 0.40 d PR 2 C44 C 1.1419(22) 1.0467(9) 0.6685(14) 0.177(14) Uani 0.60 d PDU 1 H44A H 1.1706(22) 1.0609(9) 0.7031(14) 0.265 Uiso 0.60 calc PR 1 H44B H 1.0964(22) 1.0726(9) 0.6632(14) 0.265 Uiso 0.60 calc PR 1 H44C H 1.1751(22) 1.0522(9) 0.6422(14) 0.265 Uiso 0.60 calc PR 1 C45 C 1.1861(17) 0.9313(15) 0.6780(13) 0.185(15) Uani 0.60 d PDU 1 H45A H 1.2141(17) 0.9498(15) 0.7119(13) 0.278 Uiso 0.60 calc PR 1 H45B H 1.2207(17) 0.9305(15) 0.6517(13) 0.278 Uiso 0.60 calc PR 1 H45C H 1.1674(17) 0.8871(15) 0.6793(13) 0.278 Uiso 0.60 calc PR 1 C44A C 1.0932(31) 1.0421(13) 0.6878(17) 0.146(16) Uiso 0.40 d PD 2 H44J H 1.1255(31) 1.0552(13) 0.7214(17) 0.219 Uiso 0.40 calc PR 2 H44K H 1.0388(31) 1.0405(13) 0.6927(17) 0.219 Uiso 0.40 calc PR 2 H44L H 1.1013(31) 1.0735(13) 0.6646(17) 0.219 Uiso 0.40 calc PR 2 C45A C 1.1277(35) 0.9248(18) 0.7037(16) 0.168(20) Uiso 0.40 d PD 2 H45J H 1.1573(35) 0.9466(18) 0.7362(16) 0.252 Uiso 0.40 calc PR 2 H45K H 1.1560(35) 0.8880(18) 0.6897(16) 0.252 Uiso 0.40 calc PR 2 H45L H 1.0774(35) 0.9093(18) 0.7104(16) 0.252 Uiso 0.40 calc PR 2 C46 C 0.8648(5) 0.6647(4) 0.4890(3) 0.064(2) Uani 1 d . . C47 C 0.9378(4) 0.6989(4) 0.4907(3) 0.064(2) Uani 1 d . . O47 O 0.9444(3) 0.7489(3) 0.4615(2) 0.0674(13) Uani 1 d . . C48 C 1.0056(6) 0.6818(5) 0.5211(4) 0.081(2) Uani 1 d . . C49 C 0.9973(6) 0.6318(7) 0.5512(5) 0.101(4) Uani 1 d . . H49A H 1.0416(6) 0.6219(7) 0.5735(5) 0.121 Uiso 1 calc R . C50 C 0.9270(6) 0.5948(6) 0.5507(5) 0.098(3) Uani 1 d . . C51 C 0.8609(6) 0.6121(5) 0.5172(4) 0.076(2) Uani 1 d . . H51A H 0.8136(6) 0.5877(5) 0.5140(4) 0.092 Uiso 1 calc R . C52 C 0.7936(4) 0.6798(4) 0.4547(3) 0.060(2) Uani 1 d . . O52 O 0.7307(3) 0.6477(3) 0.4517(3) 0.075(2) Uani 1 d . . O53 O 0.7978(3) 0.7278(3) 0.4262(2) 0.0623(12) Uani 1 d . . C54 C 1.0838(5) 0.7191(6) 0.5225(4) 0.090(3) Uani 1 d D . H54A H 1.0756(5) 0.7484(6) 0.4955(4) 0.108 Uiso 0.65 calc PR 1 H54D H 1.0704(5) 0.7629(6) 0.5165(4) 0.108 Uiso 0.35 d PR 2 C55 C 1.1496(10) 0.6729(11) 0.5078(12) 0.142(10) Uani 0.65 d PDU 1 H55A H 1.1976(10) 0.6986(11) 0.5092(12) 0.213 Uiso 0.65 calc PR 1 H55B H 1.1346(10) 0.6496(11) 0.4726(12) 0.213 Uiso 0.65 calc PR 1 H55C H 1.1575(10) 0.6418(11) 0.5324(12) 0.213 Uiso 0.65 calc PR 1 C56 C 1.1121(11) 0.7633(10) 0.5756(6) 0.107(6) Uani 0.65 d PD 1 H56A H 1.1614(11) 0.7853(10) 0.5739(6) 0.160 Uiso 0.65 calc PR 1 H56B H 1.1187(11) 0.7366(10) 0.6035(6) 0.160 Uiso 0.65 calc PR 1 H56C H 1.0737(11) 0.7955(10) 0.5825(6) 0.160 Uiso 0.65 calc PR 1 C55A C 1.1251(27) 0.6964(26) 0.4738(12) 0.136(16) Uiso 0.35 d PD 2 H55J H 1.1739(27) 0.7215(26) 0.4767(12) 0.204 Uiso 0.35 calc PR 2 H55K H 1.0915(27) 0.7033(26) 0.4421(12) 0.204 Uiso 0.35 calc PR 2 H55L H 1.1353(27) 0.6503(26) 0.4722(12) 0.204 Uiso 0.35 calc PR 2 C56A C 1.1432(25) 0.7218(35) 0.5739(11) 0.174(24) Uiso 0.35 d PD 2 H56J H 1.1902(25) 0.7463(35) 0.5707(11) 0.260 Uiso 0.35 calc PR 2 H56K H 1.1560(25) 0.6777(35) 0.5795(11) 0.260 Uiso 0.35 calc PR 2 H56L H 1.1201(25) 0.7430(35) 0.6033(11) 0.260 Uiso 0.35 calc PR 2 C57 C 0.9262(8) 0.5447(8) 0.5855(8) 0.146(6) Uani 1 d DU . H57A H 0.9294(8) 0.5726(8) 0.6200(8) 0.175 Uiso 0.50 calc PR 1 H57D H 0.9607(8) 0.5593(8) 0.6179(8) 0.175 Uiso 0.50 d PR 2 C58 C 0.9985(14) 0.5032(20) 0.5954(19) 0.171(18) Uani 0.50 d PDU 1 H58A H 0.9888(14) 0.4726(20) 0.6190(19) 0.257 Uiso 0.50 calc PR 1 H58B H 1.0434(14) 0.5317(20) 0.6110(19) 0.257 Uiso 0.50 calc PR 1 H58C H 1.0086(14) 0.4792(20) 0.5624(19) 0.257 Uiso 0.50 calc PR 1 C59 C 0.8488(13) 0.5047(18) 0.5844(24) 0.157(20) Uani 0.50 d PDU 1 H59A H 0.8568(13) 0.4737(18) 0.6091(24) 0.236 Uiso 0.50 calc PR 1 H59B H 0.8326(13) 0.4813(18) 0.5494(24) 0.236 Uiso 0.50 calc PR 1 H59C H 0.8088(13) 0.5341(18) 0.5940(24) 0.236 Uiso 0.50 calc PR 1 C58A C 0.9633(23) 0.4820(13) 0.5604(16) 0.171(19) Uani 0.50 d PD 2 H58J H 0.9629(23) 0.4487(13) 0.5830(16) 0.257 Uiso 0.50 calc PR 2 H58K H 1.0165(23) 0.4926(13) 0.5560(16) 0.257 Uiso 0.50 calc PR 2 H58L H 0.9333(23) 0.4659(13) 0.5264(16) 0.257 Uiso 0.50 calc PR 2 C59A C 0.8452(14) 0.5285(13) 0.6009(16) 0.100(9) Uani 0.50 d PD 2 H59J H 0.8503(14) 0.4952(13) 0.6237(16) 0.151 Uiso 0.50 calc PR 2 H59K H 0.8090(14) 0.5126(13) 0.5695(16) 0.151 Uiso 0.50 calc PR 2 H59L H 0.8259(14) 0.5676(13) 0.6191(16) 0.151 Uiso 0.50 calc PR 2 W1' W 0.59468(2) 0.46250(2) 0.303065(14) 0.05750(8) Uani 1 d . . W2' W 0.76736(2) 0.43927(2) 0.229138(13) 0.05184(7) Uani 1 d . . O1' O 0.5594(3) 0.5368(3) 0.2933(3) 0.0711(14) Uani 1 d . . O2' O 0.7282(3) 0.4142(3) 0.1651(2) 0.0648(13) Uani 1 d . . O3' O 0.6717(3) 0.4571(3) 0.2567(2) 0.0602(12) Uani 1 d . . C4' C 0.6400(5) 0.4396(5) 0.4329(3) 0.069(2) Uani 1 d . . C5' C 0.5619(5) 0.4285(4) 0.4082(4) 0.071(2) Uani 1 d . . O5' O 0.5380(3) 0.4444(3) 0.3598(2) 0.0719(14) Uani 1 d . . C6' C 0.5053(6) 0.4011(5) 0.4346(4) 0.079(2) Uani 1 d . . C7' C 0.5300(8) 0.3871(7) 0.4846(5) 0.101(3) Uani 1 d . . H7'A H 0.4925(8) 0.3704(7) 0.5025(5) 0.122 Uiso 1 calc R . C8' C 0.6074(8) 0.3962(6) 0.5105(4) 0.095(3) Uani 1 d . . C9' C 0.6622(7) 0.4223(5) 0.4844(4) 0.083(2) Uani 1 d . . H9'A H 0.7144(7) 0.4287(5) 0.5004(4) 0.100 Uiso 1 calc R . C10' C 0.7001(5) 0.4711(4) 0.4083(3) 0.067(2) Uani 1 d . . O10' O 0.7690(4) 0.4840(4) 0.4309(3) 0.084(2) Uani 1 d . . O11' O 0.6789(3) 0.4902(3) 0.3624(2) 0.0662(13) Uani 1 d . . C12' C 0.4203(6) 0.3855(6) 0.4074(5) 0.092(3) Uani 1 d . . H12B H 0.4104(6) 0.4131(6) 0.3793(5) 0.110 Uiso 1 calc R . C13' C 0.3607(9) 0.4022(9) 0.4454(7) 0.130(5) Uani 1 d . . H13D H 0.3689(9) 0.4475(9) 0.4614(7) 0.194 Uiso 1 calc R . H13E H 0.3674(9) 0.3743(9) 0.4725(7) 0.194 Uiso 1 calc R . H13F H 0.3083(9) 0.3951(9) 0.4263(7) 0.194 Uiso 1 calc R . C14' C 0.4092(8) 0.3159(9) 0.3822(8) 0.142(6) Uani 1 d . . H14D H 0.4471(8) 0.3064(9) 0.3585(8) 0.212 Uiso 1 calc R . H14E H 0.3570(8) 0.3085(9) 0.3628(8) 0.212 Uiso 1 calc R . H14F H 0.4161(8) 0.2876(9) 0.4090(8) 0.212 Uiso 1 calc R . C15' C 0.6337(12) 0.3827(7) 0.5662(5) 0.137(6) Uani 1 d D . H15B H 0.6853(12) 0.4060(7) 0.5764(5) 0.164 Uiso 0.60 calc PR 1 H15E H 0.6899(12) 0.3813(7) 0.5683(5) 0.164 Uiso 0.40 d PR 2 C16' C 0.6503(22) 0.3110(9) 0.5708(11) 0.153(11) Uani 0.60 d PDU 1 H16D H 0.6666(22) 0.3067(9) 0.6072(11) 0.229 Uiso 0.60 calc PR 1 H16E H 0.6914(22) 0.2971(9) 0.5505(11) 0.229 Uiso 0.60 calc PR 1 H16F H 0.6034(22) 0.2839(9) 0.5575(11) 0.229 Uiso 0.60 calc PR 1 C17' C 0.5819(17) 0.4178(11) 0.6046(8) 0.140(11) Uani 0.60 d PD 1 H17D H 0.5994(17) 0.4086(11) 0.6398(8) 0.209 Uiso 0.60 calc PR 1 H17E H 0.5280(17) 0.4021(11) 0.5939(8) 0.209 Uiso 0.60 calc PR 1 H17F H 0.5858(17) 0.4645(11) 0.6042(8) 0.209 Uiso 0.60 calc PR 1 C16B C 0.6019(22) 0.3129(10) 0.5699(14) 0.108(10) Uiso 0.40 d PD 2 H16M H 0.6177(22) 0.3029(10) 0.6050(14) 0.162 Uiso 0.40 calc PR 2 H16N H 0.6226(22) 0.2814(10) 0.5447(14) 0.162 Uiso 0.40 calc PR 2 H16O H 0.5454(22) 0.3110(10) 0.5623(14) 0.162 Uiso 0.40 calc PR 2 C17B C 0.6432(37) 0.4294(19) 0.6191(12) 0.177(23) Uiso 0.40 d PD 2 H17M H 0.6611(37) 0.4053(19) 0.6475(12) 0.266 Uiso 0.40 calc PR 2 H17N H 0.5935(37) 0.4477(19) 0.6244(12) 0.266 Uiso 0.40 calc PR 2 H17O H 0.6811(37) 0.4645(19) 0.6184(12) 0.266 Uiso 0.40 calc PR 2 C18' C 0.5225(4) 0.2964(4) 0.2652(3) 0.063(2) Uani 1 d . . C19' C 0.4806(4) 0.3491(4) 0.2496(3) 0.064(2) Uani 1 d . . O19' O 0.5145(3) 0.4111(3) 0.2550(2) 0.0677(13) Uani 1 d . . C20' C 0.4006(5) 0.3406(5) 0.2259(4) 0.076(2) Uani 1 d . . C21' C 0.3673(5) 0.2784(6) 0.2184(4) 0.085(3) Uani 1 d . . H21B H 0.3152(5) 0.2717(6) 0.2023(4) 0.102 Uiso 1 calc R . C22' C 0.4072(6) 0.2244(5) 0.2335(5) 0.089(3) Uani 1 d . . C23' C 0.4854(5) 0.2336(5) 0.2555(4) 0.076(2) Uani 1 d . . H23B H 0.5138(5) 0.1975(5) 0.2638(4) 0.092 Uiso 1 calc R . C24' C 0.6062(5) 0.3062(4) 0.2898(3) 0.064(2) Uani 1 d . . O24' O 0.6364(3) 0.3602(3) 0.3106(2) 0.0638(12) Uani 1 d . . O25' O 0.6466(3) 0.2531(3) 0.2886(3) 0.0728(14) Uani 1 d . . C26' C 0.3579(5) 0.4004(6) 0.2111(5) 0.089(3) Uani 1 d . . H26B H 0.3947(5) 0.4269(6) 0.1959(5) 0.107 Uiso 1 calc R . C27' C 0.2880(7) 0.3827(8) 0.1700(6) 0.125(5) Uani 1 d . . H27D H 0.2629(7) 0.4222(8) 0.1620(6) 0.187 Uiso 1 calc R . H27E H 0.2515(7) 0.3549(8) 0.1830(6) 0.187 Uiso 1 calc R . H27F H 0.3043(7) 0.3596(8) 0.1386(6) 0.187 Uiso 1 calc R . C28' C 0.3369(8) 0.4427(8) 0.2597(6) 0.121(5) Uani 1 d . . H28D H 0.3834(8) 0.4531(8) 0.2853(6) 0.182 Uiso 1 calc R . H28E H 0.2987(8) 0.4191(8) 0.2747(6) 0.182 Uiso 1 calc R . H28F H 0.3153(8) 0.4828(8) 0.2500(6) 0.182 Uiso 1 calc R . C29' C 0.3653(8) 0.1559(7) 0.2234(8) 0.124(5) Uani 1 d . . H29B H 0.3113(8) 0.1639(7) 0.2083(8) 0.149 Uiso 1 calc R . C30' C 0.3921(15) 0.1112(9) 0.1837(8) 0.169(8) Uani 1 d U . H30D H 0.3949(15) 0.1323(9) 0.1530(8) 0.253 Uiso 1 calc R . H30E H 0.3563(15) 0.0733(9) 0.1744(8) 0.253 Uiso 1 calc R . H30F H 0.4435(15) 0.0975(9) 0.1966(8) 0.253 Uiso 1 calc R . C31' C 0.3563(15) 0.1324(10) 0.2760(10) 0.188(10) Uani 1 d U . H31D H 0.3377(15) 0.1675(10) 0.2992(10) 0.282 Uiso 1 calc R . H31E H 0.4064(15) 0.1195(10) 0.2921(10) 0.282 Uiso 1 calc R . H31F H 0.3192(15) 0.0953(10) 0.2698(10) 0.282 Uiso 1 calc R . C32' C 0.8795(5) 0.5783(4) 0.2988(4) 0.065(2) Uani 1 d . . C33' C 0.8557(4) 0.5702(4) 0.2443(3) 0.059(2) Uani 1 d . . O33' O 0.7961(3) 0.5261(3) 0.2206(2) 0.0581(11) Uani 1 d . . C34' C 0.8904(5) 0.6092(5) 0.2122(4) 0.071(2) Uani 1 d . . C35' C 0.9490(6) 0.6540(5) 0.2372(5) 0.084(3) Uani 1 d . . H35B H 0.9739(6) 0.6790(5) 0.2164(5) 0.101 Uiso 1 calc R . C36' C 0.9740(6) 0.6648(5) 0.2924(5) 0.091(3) Uani 1 d . . C37' C 0.9366(6) 0.6277(5) 0.3222(4) 0.083(3) Uani 1 d . . H37B H 0.9494(6) 0.6354(5) 0.3588(4) 0.100 Uiso 1 calc R . C38' C 0.8455(4) 0.5347(4) 0.3309(3) 0.060(2) Uani 1 d . . O38' O 0.8164(3) 0.4786(3) 0.3126(2) 0.0633(12) Uani 1 d . . O39' O 0.8493(4) 0.5568(4) 0.3815(2) 0.083(2) Uani 1 d . . C40' C 0.8619(6) 0.6016(5) 0.1528(4) 0.079(2) Uani 1 d . . H40B H 0.8043(6) 0.5980(5) 0.1488(4) 0.095 Uiso 1 calc R . C41' C 0.8872(10) 0.5381(7) 0.1233(5) 0.116(4) Uani 1 d . . H41D H 0.8726(10) 0.5015(7) 0.1400(5) 0.174 Uiso 1 calc R . H41E H 0.9433(10) 0.5403(7) 0.1240(5) 0.174 Uiso 1 calc R . H41F H 0.8616(10) 0.5324(7) 0.0873(5) 0.174 Uiso 1 calc R . C42' C 0.8824(10) 0.6627(8) 0.1294(7) 0.130(5) Uani 1 d . . H42D H 0.8650(10) 0.7011(8) 0.1498(7) 0.195 Uiso 1 calc R . H42E H 0.8568(10) 0.6588(8) 0.0935(7) 0.195 Uiso 1 calc R . H42F H 0.9384(10) 0.6668(8) 0.1302(7) 0.195 Uiso 1 calc R . C43' C 1.0378(7) 0.7165(6) 0.3189(6) 0.117(5) Uani 1 d D . H43B H 1.0337(7) 0.7273(6) 0.3567(6) 0.140 Uiso 0.55 calc PR 1 H43E H 1.0197(7) 0.7373(6) 0.3505(6) 0.140 Uiso 0.45 d PR 2 C44' C 1.0300(14) 0.7801(9) 0.2922(10) 0.118(8) Uani 0.55 d PDU 1 H44D H 1.0706(14) 0.8122(9) 0.3093(10) 0.177 Uiso 0.55 calc PR 1 H44E H 0.9793(14) 0.7978(9) 0.2953(10) 0.177 Uiso 0.55 calc PR 1 H44F H 1.0353(14) 0.7694(9) 0.2554(10) 0.177 Uiso 0.55 calc PR 1 C45' C 1.1182(9) 0.6870(12) 0.3121(13) 0.130(9) Uani 0.55 d PDU 1 H45D H 1.1597(9) 0.7186(12) 0.3285(13) 0.194 Uiso 0.55 calc PR 1 H45E H 1.1218(9) 0.6763(12) 0.2751(13) 0.194 Uiso 0.55 calc PR 1 H45F H 1.1231(9) 0.6478(12) 0.3285(13) 0.194 Uiso 0.55 calc PR 1 C44B C 1.0669(27) 0.7690(25) 0.2877(24) 0.203(29) Uiso 0.45 d PD 2 H44M H 1.1069(27) 0.7975(25) 0.3101(24) 0.305 Uiso 0.45 calc PR 2 H44N H 1.0236(27) 0.7946(25) 0.2759(24) 0.305 Uiso 0.45 calc PR 2 H44O H 1.0883(27) 0.7474(25) 0.2576(24) 0.305 Uiso 0.45 calc PR 2 C45B C 1.1100(18) 0.6804(19) 0.3428(16) 0.138(13) Uiso 0.45 d PD 2 H45M H 1.1509(18) 0.7124(19) 0.3597(16) 0.207 Uiso 0.45 calc PR 2 H45N H 1.1293(18) 0.6517(19) 0.3151(16) 0.207 Uiso 0.45 calc PR 2 H45O H 1.0945(18) 0.6548(19) 0.3684(16) 0.207 Uiso 0.45 calc PR 2 C46' C 0.9025(5) 0.3290(5) 0.2735(4) 0.068(2) Uani 1 d . . C47' C 0.9291(4) 0.3804(4) 0.2476(3) 0.060(2) Uani 1 d . . O47' O 0.8760(3) 0.4206(3) 0.2249(2) 0.0581(11) Uani 1 d . . C48' C 1.0079(4) 0.3893(5) 0.2429(3) 0.067(2) Uani 1 d . . C49' C 1.0600(5) 0.3463(5) 0.2648(4) 0.080(2) Uani 1 d . . H49B H 1.1131(5) 0.3523(5) 0.2621(4) 0.095 Uiso 1 calc R . C50' C 1.0383(5) 0.2951(5) 0.2902(4) 0.079(2) Uani 1 d . . C51' C 0.9590(5) 0.2871(5) 0.2942(4) 0.074(2) Uani 1 d . . H51B H 0.9426(5) 0.2530(5) 0.3110(4) 0.088 Uiso 1 calc R . C52' C 0.8194(5) 0.3168(4) 0.2768(4) 0.065(2) Uani 1 d . . O52' O 0.7967(4) 0.2719(3) 0.2993(3) 0.086(2) Uani 1 d . . O53' O 0.7673(3) 0.3545(3) 0.2556(2) 0.0607(12) Uani 1 d . . C54' C 1.0340(5) 0.4445(5) 0.2159(4) 0.070(2) Uani 1 d . . H54B H 0.9883(5) 0.4717(5) 0.2096(4) 0.084 Uiso 1 calc R . C55' C 1.0565(11) 0.4196(7) 0.1625(6) 0.131(5) Uani 1 d U . H55D H 1.0727(11) 0.4562(7) 0.1465(6) 0.196 Uiso 1 calc R . H55E H 1.0120(11) 0.3963(7) 0.1402(6) 0.196 Uiso 1 calc R . H55F H 1.0991(11) 0.3903(7) 0.1666(6) 0.196 Uiso 1 calc R . C56' C 1.0996(11) 0.4898(8) 0.2494(7) 0.143(6) Uani 1 d U . H56D H 1.1135(11) 0.5239(8) 0.2300(7) 0.215 Uiso 1 calc R . H56E H 1.1449(11) 0.4646(8) 0.2579(7) 0.215 Uiso 1 calc R . H56F H 1.0818(11) 0.5094(8) 0.2815(7) 0.215 Uiso 1 calc R . C57' C 1.0970(6) 0.2489(6) 0.3136(5) 0.097(3) Uani 1 d D . H57B H 1.0705(6) 0.2227(6) 0.3354(5) 0.116 Uiso 0.70 calc PR 1 H57E H 1.1366(6) 0.2616(6) 0.2936(5) 0.116 Uiso 0.30 d PR 2 C58' C 1.1703(10) 0.2844(8) 0.3477(9) 0.129(7) Uani 0.70 d PDU 1 H58D H 1.2046(10) 0.2524(8) 0.3612(9) 0.194 Uiso 0.70 calc PR 1 H58E H 1.1547(10) 0.3133(8) 0.3768(9) 0.194 Uiso 0.70 calc PR 1 H58F H 1.1975(10) 0.3098(8) 0.3267(9) 0.194 Uiso 0.70 calc PR 1 C59' C 1.1252(16) 0.2013(10) 0.2685(7) 0.155(11) Uani 0.70 d PDU 1 H59D H 1.1622(16) 0.1722(10) 0.2834(7) 0.233 Uiso 0.70 calc PR 1 H59E H 1.1500(16) 0.2264(10) 0.2460(7) 0.233 Uiso 0.70 calc PR 1 H59F H 1.0808(16) 0.1758(10) 0.2480(7) 0.233 Uiso 0.70 calc PR 1 C58B C 1.1363(71) 0.2498(33) 0.3714(16) 0.291(67) Uiso 0.30 d PD 2 H58M H 1.1708(71) 0.2138(33) 0.3733(16) 0.437 Uiso 0.30 calc PR 2 H58N H 1.0964(71) 0.2456(33) 0.3935(16) 0.437 Uiso 0.30 calc PR 2 H58O H 1.1661(71) 0.2908(33) 0.3834(16) 0.437 Uiso 0.30 calc PR 2 C59B C 1.0896(33) 0.1779(12) 0.2835(18) 0.111(15) Uiso 0.30 d PD 2 H59M H 1.1282(33) 0.1516(12) 0.3003(18) 0.167 Uiso 0.30 calc PR 2 H59N H 1.0981(33) 0.1787(12) 0.2475(18) 0.167 Uiso 0.30 calc PR 2 H59O H 1.0378(33) 0.1593(12) 0.2838(18) 0.167 Uiso 0.30 calc PR 2 W1" W 0.69619(2) 0.80313(2) -0.024495(14) 0.05537(8) Uani 1 d . . W2" W 0.88081(2) 0.76283(2) -0.082338(14) 0.05975(8) Uani 1 d . . O1" O 0.6706(3) 0.8775(3) -0.0419(3) 0.0706(14) Uani 1 d . . O2" O 0.8523(3) 0.7393(3) -0.1474(2) 0.0722(14) Uani 1 d . . O3" O 0.7820(3) 0.7889(3) -0.0636(2) 0.0643(13) Uani 1 d . . C4" C 0.7148(5) 0.7894(4) 0.1083(3) 0.064(2) Uani 1 d . . C5" C 0.6395(4) 0.7806(4) 0.0774(3) 0.061(2) Uani 1 d . . O5" O 0.6267(3) 0.7956(3) 0.0280(2) 0.0635(13) Uani 1 d . . C6" C 0.5752(5) 0.7573(5) 0.0995(4) 0.072(2) Uani 1 d . . C7" C 0.5888(5) 0.7425(5) 0.1502(4) 0.075(2) Uani 1 d . . H7"A H 0.5467(5) 0.7267(5) 0.1647(4) 0.091 Uiso 1 calc R . C8" C 0.6641(5) 0.7502(5) 0.1815(3) 0.070(2) Uani 1 d . . C9" C 0.7252(5) 0.7742(5) 0.1599(4) 0.071(2) Uani 1 d . . H9"A H 0.7749(5) 0.7807(5) 0.1801(4) 0.085 Uiso 1 calc R . C10" C 0.7823(5) 0.8166(4) 0.0876(3) 0.064(2) Uani 1 d . . O10" O 0.8476(3) 0.8270(4) 0.1155(2) 0.082(2) Uani 1 d . . O11" O 0.7732(3) 0.8320(3) 0.0398(2) 0.0654(13) Uani 1 d . . C12" C 0.4934(5) 0.7501(6) 0.0670(4) 0.087(3) Uani 1 d D . H12C H 0.4961(5) 0.7643(6) 0.0326(4) 0.105 Uiso 0.65 calc PR 1 H12D H 0.5016(5) 0.7426(6) 0.0306(4) 0.105 Uiso 0.35 d PR 2 C13" C 0.4348(9) 0.7925(11) 0.0960(9) 0.136(9) Uani 0.65 d PD 1 H13G H 0.3837(9) 0.7873(11) 0.0750(9) 0.204 Uiso 0.65 calc PR 1 H13H H 0.4526(9) 0.8380(11) 0.1014(9) 0.204 Uiso 0.65 calc PR 1 H13I H 0.4318(9) 0.7784(11) 0.1297(9) 0.204 Uiso 0.65 calc PR 1 C14" C 0.4631(12) 0.6767(7) 0.0584(11) 0.133(9) Uani 0.65 d PD 1 H14G H 0.4115(12) 0.6724(7) 0.0379(11) 0.199 Uiso 0.65 calc PR 1 H14H H 0.4605(12) 0.6626(7) 0.0921(11) 0.199 Uiso 0.65 calc PR 1 H14I H 0.4984(12) 0.6498(7) 0.0399(11) 0.199 Uiso 0.65 calc PR 1 C13C C 0.4526(28) 0.8167(13) 0.0720(24) 0.144(20) Uiso 0.35 d PD 2 H13J H 0.4012(28) 0.8113(13) 0.0513(24) 0.216 Uiso 0.35 calc PR 2 H13K H 0.4835(28) 0.8491(13) 0.0594(24) 0.216 Uiso 0.35 calc PR 2 H13L H 0.4477(28) 0.8310(13) 0.1085(24) 0.216 Uiso 0.35 calc PR 2 C14C C 0.4351(26) 0.6939(17) 0.0737(28) 0.145(23) Uiso 0.35 d PD 2 H14J H 0.3865(26) 0.6961(17) 0.0505(28) 0.218 Uiso 0.35 calc PR 2 H14K H 0.4250(26) 0.6989(17) 0.1097(28) 0.218 Uiso 0.35 calc PR 2 H14L H 0.4575(26) 0.6520(17) 0.0649(28) 0.218 Uiso 0.35 calc PR 2 C15" C 0.6725(5) 0.7312(6) 0.2376(4) 0.078(2) Uani 1 d . . H15C H 0.6278(5) 0.7493(6) 0.2538(4) 0.094 Uiso 1 calc R . C16" C 0.6662(8) 0.6567(7) 0.2360(5) 0.104(3) Uani 1 d . . H16G H 0.6188(8) 0.6392(7) 0.2135(5) 0.156 Uiso 1 calc R . H16H H 0.6649(8) 0.6466(7) 0.2711(5) 0.156 Uiso 1 calc R . H16I H 0.7109(8) 0.6372(7) 0.2224(5) 0.156 Uiso 1 calc R . C17" C 0.7473(7) 0.7615(9) 0.2730(5) 0.120(5) Uani 1 d U . H17G H 0.7496(7) 0.8084(9) 0.2732(5) 0.180 Uiso 1 calc R . H17H H 0.7926(7) 0.7428(9) 0.2597(5) 0.180 Uiso 1 calc R . H17I H 0.7466(7) 0.7522(9) 0.3084(5) 0.180 Uiso 1 calc R . C18" C 0.6082(5) 0.6435(4) -0.0498(3) 0.065(2) Uani 1 d . . C19" C 0.5741(4) 0.6961(4) -0.0727(3) 0.060(2) Uani 1 d . . O19" O 0.6181(3) 0.7522(3) -0.0738(2) 0.0604(12) Uani 1 d . . C20" C 0.4943(4) 0.6919(4) -0.0969(3) 0.061(2) Uani 1 d . . C21" C 0.4534(5) 0.6321(5) -0.0971(4) 0.076(2) Uani 1 d . . H21C H 0.4010(5) 0.6275(5) -0.1129(4) 0.091 Uiso 1 calc R . C22" C 0.4868(6) 0.5777(5) -0.0746(5) 0.087(3) Uani 1 d . . C23" C 0.5641(6) 0.5840(5) -0.0522(5) 0.083(3) Uani 1 d . . H23C H 0.5879(6) 0.5487(5) -0.0384(5) 0.099 Uiso 1 calc R . C24" C 0.6904(5) 0.6492(4) -0.0242(4) 0.066(2) Uani 1 d . . O24" O 0.7271(3) 0.7028(3) -0.0078(2) 0.0623(12) Uani 1 d . . O25" O 0.7235(4) 0.5937(3) -0.0196(3) 0.083(2) Uani 1 d . . C26" C 0.4604(5) 0.7495(5) -0.1191(3) 0.068(2) Uani 1 d . . H26C H 0.4974(5) 0.7651(5) -0.1408(3) 0.081 Uiso 1 calc R . C27" C 0.3797(5) 0.7310(6) -0.1556(4) 0.085(3) Uani 1 d . . H27G H 0.3597(5) 0.7696(6) -0.1692(4) 0.127 Uiso 1 calc R . H27H H 0.3427(5) 0.7143(6) -0.1355(4) 0.127 Uiso 1 calc R . H27I H 0.3872(5) 0.6979(6) -0.1846(4) 0.127 Uiso 1 calc R . C28" C 0.4499(6) 0.8057(5) -0.0764(5) 0.092(3) Uani 1 d . . H28G H 0.4278(6) 0.8420(5) -0.0924(5) 0.138 Uiso 1 calc R . H28H H 0.5000(6) 0.8196(5) -0.0559(5) 0.138 Uiso 1 calc R . H28I H 0.4150(6) 0.7913(5) -0.0538(5) 0.138 Uiso 1 calc R . C29" C 0.4390(7) 0.5129(6) -0.0765(6) 0.113(4) Uani 1 d . . H29C H 0.4704(7) 0.4867(6) -0.0529(6) 0.136 Uiso 1 calc R . C30" C 0.4289(13) 0.4747(8) -0.1293(8) 0.163(8) Uani 1 d . . H30G H 0.4795(13) 0.4686(8) -0.1407(8) 0.245 Uiso 1 calc R . H30H H 0.3967(13) 0.4980(8) -0.1535(8) 0.245 Uiso 1 calc R . H30I H 0.4040(13) 0.4325(8) -0.1286(8) 0.245 Uiso 1 calc R . C31" C 0.3628(8) 0.5260(8) -0.0540(6) 0.124(5) Uani 1 d . . H31G H 0.3743(8) 0.5513(8) -0.0193(6) 0.186 Uiso 1 calc R . H31H H 0.3366(8) 0.4847(8) -0.0518(6) 0.186 Uiso 1 calc R . H31I H 0.3293(8) 0.5502(8) -0.0767(6) 0.186 Uiso 1 calc R . C32" C 1.0065(5) 0.8866(4) -0.0050(4) 0.069(2) Uani 1 d . . C33" C 0.9898(5) 0.8830(5) -0.0593(4) 0.072(2) Uani 1 d . . O33" O 0.9263(3) 0.8468(3) -0.0871(2) 0.0703(14) Uani 1 d . . C34" C 1.0353(6) 0.9191(5) -0.0870(4) 0.082(3) Uani 1 d . . C35" C 1.1006(6) 0.9568(6) -0.0570(5) 0.097(3) Uani 1 d . . H35C H 1.1328(6) 0.9801(6) -0.0748(5) 0.116 Uiso 1 calc R . C36" C 1.1191(6) 0.9611(6) -0.0036(5) 0.090(3) Uani 1 d . . C37" C 1.0714(6) 0.9265(5) 0.0233(4) 0.080(2) Uani 1 d . . H37C H 1.0822(6) 0.9295(5) 0.0599(4) 0.096 Uiso 1 calc R . C38" C 0.9577(5) 0.8499(5) 0.0241(4) 0.070(2) Uani 1 d . . O38" O 0.9158(3) 0.8004(3) 0.0035(2) 0.0660(13) Uani 1 d . . O39" O 0.9601(4) 0.8710(4) 0.0746(3) 0.086(2) Uani 1 d . . C40" C 1.0168(7) 0.9138(6) -0.1464(5) 0.100(3) Uani 1 d D . H40C H 0.9597(7) 0.9065(6) -0.1564(5) 0.120 Uiso 0.55 calc PR 1 H40D H 0.9711(7) 0.8830(6) -0.1578(5) 0.120 Uiso 0.45 d PR 2 C41" C 1.0570(19) 0.8539(10) -0.1727(10) 0.133(11) Uani 0.55 d PD 1 H41G H 1.0451(19) 0.8508(10) -0.2105(10) 0.200 Uiso 0.55 calc PR 1 H41H H 1.0381(19) 0.8144(10) -0.1617(10) 0.200 Uiso 0.55 calc PR 1 H41I H 1.1130(19) 0.8594(10) -0.1623(10) 0.200 Uiso 0.55 calc PR 1 C42" C 1.0418(21) 0.9783(8) -0.1650(10) 0.120(9) Uani 0.55 d PD 1 H42G H 1.0296(21) 0.9740(8) -0.2028(10) 0.180 Uiso 0.55 calc PR 1 H42H H 1.0974(21) 0.9869(8) -0.1546(10) 0.180 Uiso 0.55 calc PR 1 H42I H 1.0139(21) 1.0141(8) -0.1491(10) 0.180 Uiso 0.55 calc PR 1 C41C C 1.0877(24) 0.8835(23) -0.1712(22) 0.176(23) Uiso 0.45 d PD 2 H41J H 1.0766(24) 0.8799(23) -0.2091(22) 0.264 Uiso 0.45 calc PR 2 H41K H 1.0961(24) 0.8405(23) -0.1613(22) 0.264 Uiso 0.45 calc PR 2 H41L H 1.1341(24) 0.9115(23) -0.1586(22) 0.264 Uiso 0.45 calc PR 2 C42C C 0.9939(31) 0.9766(19) -0.1709(23) 0.190(28) Uiso 0.45 d PD 2 H42J H 0.9838(31) 0.9658(19) -0.2088(23) 0.285 Uiso 0.45 calc PR 2 H42K H 1.0363(31) 1.0094(19) -0.1611(23) 0.285 Uiso 0.45 calc PR 2 H42L H 0.9473(31) 0.9935(19) -0.1581(23) 0.285 Uiso 0.45 calc PR 2 C43" C 1.1938(6) 1.0001(5) 0.0237(4) 0.100(4) Uani 1 d D . H43C H 1.1914(6) 1.0435(5) 0.0118(4) 0.121 Uiso 0.50 calc PR 1 H43F H 1.2033(6) 1.0358(5) 0.0046(4) 0.121 Uiso 0.50 d PR 2 C44" C 1.2681(17) 0.9685(20) 0.0055(16) 0.133(15) Uani 0.50 d PDU 1 H44G H 1.3141(17) 0.9942(20) 0.0234(16) 0.200 Uiso 0.50 calc PR 1 H44H H 1.2656(17) 0.9673(20) -0.0320(16) 0.200 Uiso 0.50 calc PR 1 H44I H 1.2708(17) 0.9244(20) 0.0140(16) 0.200 Uiso 0.50 calc PR 1 C45" C 1.2012(18) 1.0130(16) 0.0845(5) 0.085(8) Uani 0.50 d PDU 1 H45G H 1.2496(18) 1.0377(16) 0.0988(5) 0.128 Uiso 0.50 calc PR 1 H45H H 1.2012(18) 0.9716(16) 0.0980(5) 0.128 Uiso 0.50 calc PR 1 H45I H 1.1576(18) 1.0376(16) 0.0948(5) 0.128 Uiso 0.50 calc PR 1 C44C C 1.2636(19) 0.9533(21) 0.0234(18) 0.148(19) Uani 0.50 d PDU 2 H44P H 1.3112(19) 0.9773(21) 0.0405(18) 0.222 Uiso 0.50 calc PR 2 H44Q H 1.2692(19) 0.9363(21) -0.0125(18) 0.222 Uiso 0.50 calc PR 2 H44R H 1.2535(19) 0.9173(21) 0.0420(18) 0.222 Uiso 0.50 calc PR 2 C45C C 1.1915(26) 1.0319(16) 0.0816(7) 0.096(11) Uani 0.50 d PDU 2 H45P H 1.2407(26) 1.0553(16) 0.0956(7) 0.144 Uiso 0.50 calc PR 2 H45Q H 1.1828(26) 0.9979(16) 0.1026(7) 0.144 Uiso 0.50 calc PR 2 H45R H 1.1495(26) 1.0620(16) 0.0826(7) 0.144 Uiso 0.50 calc PR 2 C46" C 0.9918(5) 0.6558(5) -0.0148(4) 0.075(2) Uani 1 d . . C47" C 1.0286(5) 0.6972(5) -0.0403(4) 0.070(2) Uani 1 d . . O47" O 0.9876(3) 0.7341(3) -0.0761(2) 0.0718(15) Uani 1 d . . C48" C 1.1126(5) 0.7054(5) -0.0337(4) 0.080(2) Uani 1 d . . C49" C 1.1515(6) 0.6685(7) 0.0029(5) 0.096(3) Uani 1 d . . H49C H 1.2062(6) 0.6729(7) 0.0092(5) 0.116 Uiso 1 calc R . C50" C 1.1164(6) 0.6267(7) 0.0302(5) 0.101(3) Uani 1 d . . C51" C 1.0339(6) 0.6186(7) 0.0205(5) 0.093(3) Uani 1 d . . H51C H 1.0077(6) 0.5891(7) 0.0372(5) 0.112 Uiso 1 calc R . C52" C 0.9050(5) 0.6440(5) -0.0250(4) 0.076(2) Uani 1 d . . O52" O 0.8716(4) 0.6020(4) -0.0039(3) 0.092(2) Uani 1 d . . O53" O 0.8621(3) 0.6790(3) -0.0567(2) 0.0650(13) Uani 1 d . . C54" C 1.1523(6) 0.7505(6) -0.0644(5) 0.095(3) Uani 1 d . . H54C H 1.1208(6) 0.7896(6) -0.0660(5) 0.113 Uiso 1 calc R . C55" C 1.1526(8) 0.7177(8) -0.1206(6) 0.118(5) Uani 1 d . . H55G H 1.1780(8) 0.7470(8) -0.1396(6) 0.177 Uiso 1 calc R . H55H H 1.0994(8) 0.7076(8) -0.1376(6) 0.177 Uiso 1 calc R . H55I H 1.1807(8) 0.6777(8) -0.1204(6) 0.177 Uiso 1 calc R . C56" C 1.2352(7) 0.7740(8) -0.0380(6) 0.117(4) Uani 1 d . . H56G H 1.2577(7) 0.8025(8) -0.0591(6) 0.175 Uiso 1 calc R . H56H H 1.2672(7) 0.7366(8) -0.0348(6) 0.175 Uiso 1 calc R . H56I H 1.2328(7) 0.7979(8) -0.0034(6) 0.175 Uiso 1 calc R . C57" C 1.1590(8) 0.5868(11) 0.0712(7) 0.156(7) Uani 1 d D . H57C H 1.1340(8) 0.5423(11) 0.0633(7) 0.188 Uiso 0.65 calc PR 1 H57F H 1.1258(8) 0.5541(11) 0.0816(7) 0.188 Uiso 0.35 d PR 2 C58" C 1.2468(11) 0.5785(19) 0.0664(13) 0.178(15) Uani 0.65 d PD 1 H58G H 1.2522(11) 0.5618(19) 0.0304(13) 0.267 Uiso 0.65 calc PR 1 H58H H 1.2681(11) 0.5479(19) 0.0891(13) 0.267 Uiso 0.65 calc PR 1 H58I H 1.2750(11) 0.6204(19) 0.0767(13) 0.267 Uiso 0.65 calc PR 1 C59" C 1.1473(16) 0.6135(17) 0.1284(7) 0.158(12) Uani 0.65 d PD 1 H59G H 1.0921(16) 0.6181(17) 0.1300(7) 0.238 Uiso 0.65 calc PR 1 H59H H 1.1747(16) 0.6557(17) 0.1391(7) 0.238 Uiso 0.65 calc PR 1 H59I H 1.1678(16) 0.5832(17) 0.1515(7) 0.238 Uiso 0.65 calc PR 1 C58C C 1.2204(32) 0.5513(36) 0.0400(31) 0.201(39) Uiso 0.35 d PD 2 H58P H 1.2511(32) 0.5243(36) 0.0619(31) 0.301 Uiso 0.35 calc PR 2 H58Q H 1.2544(32) 0.5835(36) 0.0297(31) 0.301 Uiso 0.35 calc PR 2 H58R H 1.1936(32) 0.5239(36) 0.0089(31) 0.301 Uiso 0.35 calc PR 2 C59C C 1.2016(34) 0.6469(24) 0.1090(24) 0.183(25) Uiso 0.35 d PD 2 H59P H 1.2327(34) 0.6318(24) 0.1385(24) 0.275 Uiso 0.35 calc PR 2 H59Q H 1.1632(34) 0.6762(24) 0.1216(24) 0.275 Uiso 0.35 calc PR 2 H59R H 1.2352(34) 0.6700(24) 0.0902(24) 0.275 Uiso 0.35 calc PR 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W1 0.0453(2) 0.0602(2) 0.0675(2) 0.00957(15) 0.00501(14) -0.00012(13) W2 0.04210(15) 0.0615(2) 0.0627(2) 0.00548(14) 0.00272(13) -0.00280(13) O1 0.060(3) 0.065(3) 0.094(4) 0.015(3) 0.004(3) 0.001(2) O2 0.051(3) 0.091(4) 0.067(3) 0.001(3) 0.009(2) -0.002(3) O3 0.053(3) 0.067(3) 0.061(3) 0.008(2) 0.001(2) -0.006(2) C4 0.059(4) 0.073(5) 0.072(5) 0.003(4) 0.015(4) -0.008(4) C5 0.057(4) 0.057(4) 0.085(5) 0.001(4) 0.019(4) 0.004(3) O5 0.052(3) 0.070(3) 0.070(3) 0.013(3) 0.005(2) 0.006(2) C6 0.048(4) 0.081(6) 0.092(6) -0.003(5) 0.013(4) 0.002(4) C7 0.054(5) 0.115(9) 0.146(11) -0.011(8) 0.042(6) -0.008(5) C8 0.076(6) 0.119(9) 0.082(6) 0.010(6) 0.017(5) -0.012(6) C9 0.068(5) 0.092(6) 0.084(6) 0.005(5) 0.018(4) -0.012(5) C10 0.063(5) 0.074(5) 0.084(6) 0.001(4) 0.014(4) -0.002(4) O10 0.077(4) 0.116(5) 0.073(4) 0.027(4) 0.014(3) 0.000(4) O11 0.055(3) 0.070(3) 0.074(3) 0.008(3) 0.009(2) -0.001(2) C12 0.051(5) 0.096(7) 0.125(9) 0.003(6) 0.011(5) 0.003(4) C13 0.172(13) 0.112(10) 0.171(13) 0.010(10) -0.034(11) 0.023(10) C14 0.091(9) 0.166(15) 0.159(15) 0.024(12) -0.022(9) -0.022(9) C15 0.089(8) 0.149(12) 0.117(9) 0.028(8) 0.044(7) -0.010(7) C16 0.073(10) 0.121(16) 0.100(13) 0.029(12) 0.037(10) -0.006(11) C17 0.146(17) 0.145(17) 0.141(16) 0.039(14) 0.068(14) 0.024(14) C18 0.045(3) 0.082(5) 0.054(4) 0.008(3) 0.004(3) 0.005(3) C19 0.043(3) 0.074(5) 0.064(4) 0.010(4) 0.008(3) 0.007(3) O19 0.050(3) 0.065(3) 0.067(3) 0.016(2) 0.006(2) 0.001(2) C20 0.064(5) 0.078(5) 0.076(5) 0.011(4) -0.004(4) 0.010(4) C21 0.067(5) 0.097(7) 0.076(5) 0.016(5) -0.003(4) 0.016(5) C22 0.051(4) 0.104(7) 0.080(6) 0.009(5) -0.007(4) -0.002(4) C23 0.054(4) 0.085(6) 0.081(5) 0.011(4) 0.007(4) -0.005(4) C24 0.040(3) 0.067(5) 0.072(5) 0.014(4) 0.008(3) -0.005(3) O24 0.049(3) 0.067(3) 0.065(3) 0.013(2) 0.003(2) 0.001(2) O25 0.071(3) 0.062(3) 0.090(4) 0.012(3) -0.012(3) -0.011(3) C26 0.100(8) 0.089(7) 0.099(8) 0.021(6) -0.020(6) 0.009(6) C27 0.209(31) 0.130(19) 0.186(27) 0.066(19) 0.072(25) 0.006(19) C28 0.147(16) 0.148(16) 0.189(18) 0.058(14) -0.014(14) 0.040(13) C29 0.062(5) 0.123(9) 0.115(9) 0.011(7) -0.022(6) -0.007(6) C30 0.117(11) 0.138(13) 0.174(16) -0.060(12) -0.019(11) -0.022(10) C31 0.077(8) 0.219(18) 0.171(15) -0.045(13) 0.018(9) -0.059(10) C32 0.055(4) 0.075(5) 0.069(5) 0.004(4) 0.000(4) -0.005(4) C33 0.052(4) 0.062(4) 0.073(5) 0.005(4) -0.001(3) -0.003(3) O33 0.046(2) 0.070(3) 0.070(3) 0.011(2) 0.003(2) -0.005(2) C34 0.052(4) 0.066(5) 0.082(5) 0.001(4) 0.003(4) -0.002(3) C35 0.061(5) 0.089(6) 0.081(6) 0.000(5) -0.007(4) -0.008(4) C36 0.075(6) 0.100(7) 0.096(7) 0.006(6) -0.014(5) -0.015(5) C37 0.087(6) 0.095(7) 0.067(5) 0.010(5) -0.007(5) -0.017(5) C38 0.057(4) 0.072(5) 0.066(5) 0.016(4) 0.000(4) 0.003(4) O38 0.053(3) 0.070(3) 0.066(3) 0.011(3) 0.007(2) -0.004(2) O39 0.076(4) 0.110(5) 0.057(3) 0.007(3) 0.009(3) -0.010(3) C40 0.053(4) 0.084(6) 0.086(6) 0.011(5) 0.000(4) -0.013(4) C41 0.080(6) 0.087(7) 0.118(9) -0.015(6) 0.027(6) -0.020(5) C42 0.060(5) 0.078(6) 0.115(8) 0.010(5) 0.011(5) -0.008(4) C43 0.110(9) 0.153(13) 0.089(8) 0.017(8) -0.035(7) -0.028(9) C44 0.211(30) 0.154(24) 0.138(22) -0.036(19) -0.008(22) -0.019(22) C45 0.177(25) 0.233(31) 0.119(19) 0.009(20) -0.065(19) 0.050(23) C46 0.062(4) 0.061(4) 0.067(4) 0.005(3) 0.003(4) 0.007(3) C47 0.048(4) 0.062(4) 0.074(5) 0.001(4) -0.003(3) 0.004(3) O47 0.047(3) 0.071(3) 0.080(3) 0.003(3) 0.002(2) 0.000(2) C48 0.067(5) 0.090(6) 0.082(6) 0.018(5) -0.007(4) 0.014(4) C49 0.067(6) 0.120(9) 0.114(8) 0.044(7) -0.020(6) 0.010(6) C50 0.069(6) 0.104(8) 0.122(9) 0.045(7) -0.008(6) 0.008(5) C51 0.064(5) 0.074(5) 0.087(6) 0.012(4) 0.000(4) 0.003(4) C52 0.051(4) 0.063(4) 0.064(4) 0.007(3) 0.006(3) 0.001(3) O52 0.057(3) 0.072(3) 0.094(4) 0.023(3) -0.004(3) -0.010(3) O53 0.048(3) 0.065(3) 0.071(3) 0.006(2) 0.000(2) -0.001(2) C54 0.054(5) 0.116(8) 0.100(7) 0.036(6) -0.007(5) 0.001(5) C55 0.095(13) 0.148(19) 0.177(22) -0.026(17) 0.051(15) -0.026(13) C56 0.091(11) 0.104(13) 0.113(14) -0.016(11) 0.010(10) -0.015(10) C57 0.123(10) 0.151(12) 0.172(13) 0.082(11) -0.006(9) -0.001(9) C58 0.134(25) 0.195(31) 0.206(32) 0.132(27) -0.009(22) 0.012(22) C59 0.160(29) 0.096(26) 0.208(37) 0.062(25) -0.038(24) 0.009(19) C58A 0.188(40) 0.114(25) 0.239(51) 0.093(30) 0.043(37) 0.079(28) C59A 0.114(19) 0.056(14) 0.138(25) 0.041(15) 0.014(16) -0.018(12) W1' 0.0453(2) 0.0610(2) 0.0663(2) 0.01065(15) 0.00770(14) 0.00010(13) W2' 0.04036(14) 0.0572(2) 0.0560(2) 0.00814(13) 0.00058(12) 0.00038(12) O1' 0.056(3) 0.068(3) 0.091(4) 0.013(3) 0.013(3) 0.004(2) O2' 0.052(3) 0.077(3) 0.063(3) 0.004(3) 0.005(2) 0.000(2) O3' 0.046(2) 0.063(3) 0.070(3) 0.014(2) -0.002(2) 0.000(2) C4' 0.077(5) 0.077(5) 0.055(4) 0.009(4) 0.014(4) -0.002(4) C5' 0.068(5) 0.068(5) 0.079(5) 0.007(4) 0.020(4) 0.005(4) O5' 0.059(3) 0.084(4) 0.075(4) 0.014(3) 0.015(3) -0.002(3) C6' 0.081(6) 0.077(5) 0.085(6) 0.015(5) 0.032(5) 0.003(4) C7' 0.102(8) 0.121(9) 0.092(7) 0.033(7) 0.037(6) -0.007(7) C8' 0.112(8) 0.103(8) 0.075(6) 0.020(5) 0.022(6) -0.001(6) C9' 0.092(6) 0.084(6) 0.074(6) 0.014(5) 0.008(5) -0.002(5) C10' 0.065(5) 0.069(5) 0.063(5) 0.005(4) 0.000(4) -0.001(4) O10' 0.080(4) 0.101(5) 0.067(3) 0.014(3) -0.003(3) -0.018(3) O11' 0.053(3) 0.077(3) 0.067(3) 0.010(3) 0.006(2) -0.009(2) C12' 0.067(5) 0.093(7) 0.125(9) 0.030(6) 0.035(6) 0.006(5) C13' 0.106(9) 0.145(13) 0.155(13) 0.037(10) 0.061(10) 0.022(9) C14' 0.083(8) 0.160(15) 0.170(15) -0.024(12) 0.028(9) 0.002(8) C15' 0.214(19) 0.121(11) 0.089(8) 0.042(8) 0.042(10) 0.001(11) C16' 0.180(19) 0.167(19) 0.113(15) 0.036(14) 0.009(14) 0.040(15) C17' 0.241(36) 0.118(17) 0.058(10) 0.002(10) 0.027(15) -0.014(20) C18' 0.050(4) 0.067(5) 0.070(5) 0.007(4) 0.007(3) -0.006(3) C19' 0.047(4) 0.070(5) 0.075(5) 0.012(4) 0.007(3) -0.007(3) O19' 0.047(3) 0.072(3) 0.084(4) 0.020(3) 0.002(2) -0.006(2) C20' 0.054(4) 0.090(6) 0.081(5) 0.002(5) 0.003(4) -0.004(4) C21' 0.055(5) 0.097(7) 0.095(7) 0.003(5) 0.000(4) -0.015(5) C22' 0.068(5) 0.083(6) 0.109(8) 0.001(5) 0.003(5) -0.022(5) C23' 0.066(5) 0.070(5) 0.092(6) 0.008(4) 0.011(4) -0.002(4) C24' 0.054(4) 0.071(5) 0.069(5) 0.020(4) 0.011(3) -0.001(4) O24' 0.053(3) 0.064(3) 0.072(3) 0.011(3) 0.001(2) 0.002(2) O25' 0.062(3) 0.066(3) 0.091(4) 0.020(3) 0.006(3) 0.003(3) C26' 0.049(4) 0.097(7) 0.115(8) 0.011(6) -0.009(5) -0.002(4) C27' 0.076(7) 0.147(12) 0.137(12) -0.006(10) -0.007(7) 0.010(7) C28' 0.082(7) 0.127(11) 0.133(11) -0.020(9) -0.018(7) 0.014(7) C29' 0.088(8) 0.087(8) 0.191(16) -0.002(9) 0.026(9) -0.021(6) C30' 0.240(22) 0.115(12) 0.141(14) 0.002(10) 0.020(14) -0.041(13) C31' 0.223(21) 0.143(15) 0.197(20) 0.042(14) 0.023(17) -0.072(15) C32' 0.054(4) 0.063(4) 0.076(5) 0.001(4) 0.015(4) -0.003(3) C33' 0.040(3) 0.061(4) 0.075(5) 0.004(3) 0.009(3) -0.001(3) O33' 0.050(2) 0.059(3) 0.065(3) 0.010(2) 0.002(2) 0.003(2) C34' 0.065(5) 0.072(5) 0.080(5) 0.017(4) 0.020(4) 0.003(4) C35' 0.071(5) 0.080(6) 0.105(7) 0.016(5) 0.021(5) -0.015(4) C36' 0.072(6) 0.083(6) 0.112(8) -0.010(6) 0.025(5) -0.024(5) C37' 0.067(5) 0.083(6) 0.092(6) -0.009(5) 0.011(5) -0.015(4) C38' 0.046(3) 0.073(5) 0.054(4) 0.002(3) -0.002(3) -0.007(3) O38' 0.055(3) 0.068(3) 0.063(3) 0.010(2) -0.005(2) -0.008(2) O39' 0.080(4) 0.099(5) 0.062(3) -0.003(3) 0.004(3) -0.024(3) C40' 0.073(5) 0.082(6) 0.089(6) 0.025(5) 0.018(5) -0.003(4) C41' 0.154(13) 0.107(9) 0.096(8) 0.017(7) 0.043(8) -0.001(8) C42' 0.153(13) 0.122(11) 0.136(12) 0.061(10) 0.051(10) 0.019(10) C43' 0.100(8) 0.101(8) 0.143(11) -0.018(8) 0.037(8) -0.046(7) C44' 0.136(15) 0.096(12) 0.123(14) -0.005(10) 0.051(12) -0.062(11) C45' 0.082(12) 0.146(16) 0.151(17) -0.004(14) 0.016(12) -0.041(12) C46' 0.045(4) 0.079(5) 0.077(5) 0.016(4) -0.001(3) 0.006(3) C47' 0.047(4) 0.064(4) 0.066(4) 0.006(3) 0.001(3) 0.005(3) O47' 0.046(2) 0.065(3) 0.061(3) 0.009(2) 0.001(2) 0.003(2) C48' 0.043(4) 0.086(5) 0.072(5) 0.010(4) 0.009(3) 0.009(3) C49' 0.049(4) 0.086(6) 0.099(7) 0.010(5) 0.000(4) 0.009(4) C50' 0.052(4) 0.085(6) 0.101(7) 0.025(5) -0.003(4) 0.017(4) C51' 0.056(4) 0.073(5) 0.092(6) 0.018(4) 0.003(4) 0.009(4) C52' 0.050(4) 0.067(5) 0.078(5) 0.021(4) 0.002(3) 0.000(3) O52' 0.061(3) 0.086(4) 0.120(5) 0.048(4) 0.004(3) 0.007(3) O53' 0.045(2) 0.062(3) 0.074(3) 0.011(2) 0.003(2) 0.002(2) C54' 0.057(4) 0.078(5) 0.075(5) 0.012(4) 0.007(4) 0.003(4) C55' 0.180(13) 0.105(8) 0.119(9) 0.010(7) 0.071(9) 0.003(9) C56' 0.168(14) 0.124(11) 0.127(11) 0.022(9) -0.004(10) -0.070(11) C57' 0.063(5) 0.104(8) 0.127(9) 0.043(7) -0.002(5) 0.026(5) C58' 0.114(12) 0.103(11) 0.155(14) 0.034(10) -0.053(11) 0.027(9) C59' 0.209(25) 0.108(14) 0.146(18) 0.026(13) -0.006(17) 0.090(16) W1" 0.04281(15) 0.0605(2) 0.0614(2) 0.00881(14) 0.00495(13) -0.01054(13) W2" 0.0469(2) 0.0694(2) 0.0613(2) 0.00542(15) 0.00836(13) -0.01011(14) O1" 0.056(3) 0.070(3) 0.085(4) 0.016(3) 0.007(3) -0.012(2) O2" 0.062(3) 0.084(4) 0.069(3) 0.002(3) 0.015(3) -0.012(3) O3" 0.055(3) 0.065(3) 0.070(3) 0.013(2) 0.000(2) -0.013(2) C4" 0.052(4) 0.077(5) 0.060(4) -0.001(4) 0.011(3) -0.010(3) C5" 0.046(4) 0.075(5) 0.058(4) 0.005(3) 0.007(3) -0.008(3) O5" 0.041(2) 0.085(4) 0.062(3) 0.011(3) 0.002(2) -0.006(2) C6" 0.052(4) 0.091(6) 0.073(5) 0.005(4) 0.016(4) -0.006(4) C7" 0.051(4) 0.105(7) 0.069(5) 0.011(5) 0.008(4) -0.011(4) C8" 0.056(4) 0.096(6) 0.061(4) 0.012(4) 0.013(3) 0.001(4) C9" 0.048(4) 0.089(6) 0.071(5) 0.004(4) 0.007(3) -0.004(4) C10" 0.050(4) 0.079(5) 0.060(4) 0.004(4) 0.003(3) -0.011(3) O10" 0.055(3) 0.119(5) 0.068(3) 0.012(3) 0.000(3) -0.029(3) O11" 0.045(2) 0.082(4) 0.065(3) 0.006(3) 0.004(2) -0.021(2) C12" 0.051(4) 0.140(9) 0.071(5) 0.019(6) 0.008(4) -0.016(5) C13" 0.054(9) 0.178(24) 0.163(23) 0.016(19) -0.024(11) 0.013(12) C14" 0.083(13) 0.137(18) 0.150(22) -0.029(16) -0.026(14) -0.040(13) C15" 0.058(4) 0.116(7) 0.066(5) 0.020(5) 0.017(4) 0.016(5) C16" 0.111(9) 0.110(9) 0.097(8) 0.037(7) 0.005(6) 0.012(7) C17" 0.087(7) 0.198(15) 0.076(6) 0.029(8) 0.008(6) -0.013(8) C18" 0.052(4) 0.064(4) 0.076(5) 0.010(4) 0.004(3) -0.010(3) C19" 0.053(4) 0.063(4) 0.059(4) 0.004(3) 0.002(3) -0.014(3) O19" 0.045(2) 0.068(3) 0.069(3) 0.019(2) 0.003(2) -0.015(2) C20" 0.046(4) 0.071(5) 0.064(4) 0.008(4) 0.006(3) -0.008(3) C21" 0.050(4) 0.083(6) 0.088(6) 0.013(5) -0.009(4) -0.015(4) C22" 0.069(5) 0.071(6) 0.115(8) 0.014(5) 0.000(5) -0.023(4) C23" 0.067(5) 0.070(5) 0.108(7) 0.018(5) 0.002(5) -0.020(4) C24" 0.049(4) 0.075(5) 0.076(5) 0.020(4) 0.007(3) -0.008(4) O24" 0.045(2) 0.068(3) 0.072(3) 0.013(2) 0.001(2) -0.005(2) O25" 0.061(3) 0.065(3) 0.123(5) 0.030(3) 0.003(3) -0.006(3) C26" 0.052(4) 0.082(5) 0.066(5) 0.010(4) 0.002(3) -0.009(4) C27" 0.058(5) 0.117(8) 0.078(6) 0.025(5) -0.005(4) -0.008(5) C28" 0.069(5) 0.083(6) 0.116(8) 0.009(6) -0.013(5) 0.010(5) C29" 0.089(7) 0.089(7) 0.151(12) 0.027(8) -0.019(7) -0.043(6) C30" 0.183(18) 0.108(11) 0.173(17) 0.009(11) -0.041(14) -0.051(12) C31" 0.100(9) 0.135(11) 0.141(12) 0.062(10) -0.006(8) -0.043(8) C32" 0.048(4) 0.075(5) 0.080(5) 0.005(4) 0.009(4) -0.016(4) C33" 0.063(5) 0.073(5) 0.079(5) 0.008(4) 0.011(4) -0.011(4) O33" 0.051(3) 0.084(4) 0.075(3) 0.012(3) 0.011(2) -0.012(3) C34" 0.076(6) 0.080(6) 0.091(6) 0.014(5) 0.020(5) -0.021(5) C35" 0.072(6) 0.113(8) 0.109(8) 0.019(6) 0.027(6) -0.032(6) C36" 0.065(5) 0.088(7) 0.114(8) 0.009(6) 0.015(5) -0.028(5) C37" 0.068(5) 0.084(6) 0.082(6) 0.000(5) 0.011(4) -0.026(4) C38" 0.046(4) 0.085(6) 0.073(5) 0.002(4) 0.008(3) -0.013(4) O38" 0.046(3) 0.077(3) 0.071(3) 0.004(3) 0.004(2) -0.017(2) O39" 0.073(4) 0.105(5) 0.071(4) -0.006(3) 0.008(3) -0.036(3) C40" 0.098(8) 0.114(9) 0.090(7) 0.021(6) 0.023(6) -0.028(7) C41" 0.186(31) 0.116(20) 0.087(15) -0.014(14) 0.013(17) -0.009(21) C42" 0.172(29) 0.116(18) 0.080(13) 0.024(12) 0.043(16) -0.031(17) C43" 0.075(6) 0.089(7) 0.131(10) 0.001(6) 0.016(6) -0.042(6) C44" 0.074(18) 0.117(20) 0.204(32) 0.005(22) 0.028(19) -0.032(15) C45" 0.062(12) 0.062(13) 0.123(15) 0.020(10) -0.020(10) -0.027(11) C44C 0.061(16) 0.171(35) 0.202(33) -0.013(26) 0.027(18) -0.015(19) C45C 0.088(16) 0.073(17) 0.126(17) 0.035(11) -0.004(12) 0.000(12) C46" 0.051(4) 0.094(6) 0.080(5) 0.012(5) 0.005(4) 0.006(4) C47" 0.049(4) 0.083(5) 0.073(5) -0.007(4) 0.011(4) -0.009(4) O47" 0.057(3) 0.087(4) 0.068(3) -0.003(3) 0.012(3) -0.010(3) C48" 0.052(4) 0.095(6) 0.087(6) -0.006(5) 0.012(4) 0.005(4) C49" 0.048(4) 0.126(9) 0.111(8) 0.009(7) 0.002(5) 0.013(5) C50" 0.063(6) 0.129(10) 0.111(8) 0.024(7) 0.006(6) 0.017(6) C51" 0.057(5) 0.123(9) 0.100(7) 0.030(6) -0.001(5) 0.005(5) C52" 0.054(4) 0.093(6) 0.077(5) 0.010(5) 0.006(4) -0.008(4) O52" 0.058(3) 0.110(5) 0.115(5) 0.051(4) 0.005(3) -0.006(3) O53" 0.046(3) 0.073(3) 0.075(3) 0.011(3) 0.004(2) -0.003(2) C54" 0.051(5) 0.111(8) 0.120(8) -0.001(6) 0.027(5) -0.011(5) C55" 0.094(8) 0.139(11) 0.119(10) -0.016(8) 0.045(7) -0.004(7) C56" 0.074(7) 0.138(11) 0.135(11) 0.017(9) 0.012(7) -0.023(7) C57" 0.082(8) 0.209(20) 0.171(17) 0.055(15) -0.036(10) 0.031(10) C58" 0.120(20) 0.196(35) 0.223(39) 0.057(31) 0.006(24) 0.083(23) C59" 0.144(22) 0.227(34) 0.104(17) 0.061(19) -0.022(15) 0.032(22) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag W1 O1 1.695(6) . ? W1 O3 1.890(5) . ? W1 O19 1.893(5) . ? W1 O5 1.926(5) . ? W1 O11 1.965(6) . ? W1 O24 2.241(5) . ? W2 O2 1.688(6) . ? W2 O3 1.897(5) . ? W2 O33 1.903(5) . ? W2 O47 1.922(6) . ? W2 O53 1.964(5) . ? W2 O38 2.247(6) . ? C4 C9 1.392(13) . ? C4 C5 1.405(13) . ? C4 C10 1.482(12) . ? C5 O5 1.365(10) . ? C5 C6 1.413(12) . ? C6 C7 1.40(2) . ? C6 C12 1.51(2) . ? C7 C8 1.37(2) . ? C8 C9 1.37(2) . ? C8 C15 1.53(2) . ? C10 O10 1.238(12) . ? C10 O11 1.312(11) . ? C12 C14 1.51(2) . ? C12 C13 1.53(2) . ? C15 C17 1.536(10) . ? C15 C16A 1.539(10) . ? C15 C17A 1.550(10) . ? C15 C16 1.550(10) . ? C18 C19 1.390(12) . ? C18 C23 1.401(12) . ? C18 C24 1.477(11) . ? C19 O19 1.381(10) . ? C19 C20 1.389(12) . ? C20 C21 1.390(14) . ? C20 C26 1.494(15) . ? C21 C22 1.37(2) . ? C22 C23 1.380(14) . ? C22 C29 1.542(14) . ? C24 O24 1.238(10) . ? C24 O25 1.303(10) . ? C26 C27 1.540(10) . ? C26 C28 1.541(9) . ? C26 C28A 1.545(10) . ? C26 C27A 1.545(10) . ? C29 C31 1.49(2) . ? C29 C30 1.50(2) . ? C32 C33 1.396(13) . ? C32 C37 1.403(13) . ? C32 C38 1.477(12) . ? C33 O33 1.350(10) . ? C33 C34 1.418(11) . ? C34 C35 1.389(13) . ? C34 C40 1.490(14) . ? C35 C36 1.36(2) . ? C36 C37 1.392(15) . ? C36 C43 1.530(15) . ? C38 O38 1.232(10) . ? C38 O39 1.304(11) . ? C40 C42 1.526(12) . ? C40 C41 1.542(15) . ? C43 C44 1.536(10) . ? C43 C44A 1.537(10) . ? C43 C45 1.537(10) . ? C43 C45A 1.538(10) . ? C46 C51 1.390(13) . ? C46 C47 1.412(12) . ? C46 C52 1.470(11) . ? C47 O47 1.366(11) . ? C47 C48 1.390(12) . ? C48 C49 1.39(2) . ? C48 C54 1.523(14) . ? C49 C50 1.40(2) . ? C50 C51 1.411(14) . ? C50 C57 1.46(2) . ? C52 O52 1.238(10) . ? C52 O53 1.313(10) . ? C54 C56 1.539(9) . ? C54 C55 1.543(10) . ? C54 C56A 1.547(10) . ? C54 C55A 1.548(10) . ? C57 C58 1.533(10) . ? C57 C59 1.538(10) . ? C57 C59A 1.538(10) . ? C57 C58A 1.546(10) . ? W1' O1' 1.690(6) . ? W1' O3' 1.899(5) . ? W1' O19' 1.902(6) . ? W1' O5' 1.938(6) . ? W1' O11' 1.961(5) . ? W1' O24' 2.256(6) . ? W2' O2' 1.695(5) . ? W2' O33' 1.885(5) . ? W2' O3' 1.900(5) . ? W2' O47' 1.927(5) . ? W2' O53' 1.954(5) . ? W2' O38' 2.226(5) . ? C4' C5' 1.400(13) . ? C4' C9' 1.425(13) . ? C4' C10' 1.466(12) . ? C5' O5' 1.346(11) . ? C5' C6' 1.410(13) . ? C6' C7' 1.37(2) . ? C6' C12' 1.53(2) . ? C7' C8' 1.40(2) . ? C8' C9' 1.37(2) . ? C8' C15' 1.51(2) . ? C10' O10' 1.248(11) . ? C10' O11' 1.306(10) . ? C12' C14' 1.48(2) . ? C12' C13' 1.53(2) . ? C15' C16' 1.520(10) . ? C15' C16B 1.537(10) . ? C15' C17B 1.538(10) . ? C15' C17' 1.539(10) . ? C18' C19' 1.387(12) . ? C18' C23' 1.394(12) . ? C18' C24' 1.483(11) . ? C19' O19' 1.366(10) . ? C19' C20' 1.419(12) . ? C20' C21' 1.361(14) . ? C20' C26' 1.508(15) . ? C21' C22' 1.39(2) . ? C22' C23' 1.379(14) . ? C22' C29' 1.53(2) . ? C24' O24' 1.227(10) . ? C24' O25' 1.303(10) . ? C26' C27' 1.49(2) . ? C26' C28' 1.51(2) . ? C29' C30' 1.41(2) . ? C29' C31' 1.53(3) . ? C32' C33' 1.393(12) . ? C32' C37' 1.401(12) . ? C32' C38' 1.464(12) . ? C33' O33' 1.363(9) . ? C33' C34' 1.408(12) . ? C34' C35' 1.368(14) . ? C34' C40' 1.525(14) . ? C35' C36' 1.41(2) . ? C36' C37' 1.36(2) . ? C36' C43' 1.522(14) . ? C38' O38' 1.244(10) . ? C38' O39' 1.311(10) . ? C40' C41' 1.51(2) . ? C40' C42' 1.52(2) . ? C43' C45' 1.541(10) . ? C43' C44B 1.545(10) . ? C43' C45B 1.556(10) . ? C43' C44' 1.557(10) . ? C46' C51' 1.409(12) . ? C46' C47' 1.423(12) . ? C46' C52' 1.458(11) . ? C47' O47' 1.369(9) . ? C47' C48' 1.386(11) . ? C48' C49' 1.391(13) . ? C48' C54' 1.499(13) . ? C49' C50' 1.383(15) . ? C50' C51' 1.387(13) . ? C50' C57' 1.521(12) . ? C52' O52' 1.236(10) . ? C52' O53' 1.310(10) . ? C54' C55' 1.51(2) . ? C54' C56' 1.53(2) . ? C57' C58' 1.534(9) . ? C57' C59B 1.540(10) . ? C57' C58B 1.547(10) . ? C57' C59' 1.547(10) . ? W1" O1" 1.699(6) . ? W1" O19" 1.892(5) . ? W1" O3" 1.903(6) . ? W1" O5" 1.946(5) . ? W1" O11" 1.978(5) . ? W1" O24" 2.220(6) . ? W2" O2" 1.678(6) . ? W2" O3" 1.896(6) . ? W2" O33" 1.898(6) . ? W2" O47" 1.930(6) . ? W2" O53" 1.960(6) . ? W2" O38" 2.230(6) . ? C4" C9" 1.398(13) . ? C4" C5" 1.413(11) . ? C4" C10" 1.471(11) . ? C5" O5" 1.342(10) . ? C5" C6" 1.415(11) . ? C6" C7" 1.373(13) . ? C6" C12" 1.523(12) . ? C7" C8" 1.417(12) . ? C8" C9" 1.367(12) . ? C8" C15" 1.537(12) . ? C10" O10" 1.241(10) . ? C10" O11" 1.304(10) . ? C12" C13C 1.547(10) . ? C12" C13" 1.547(9) . ? C12" C14C 1.550(10) . ? C12" C14" 1.554(9) . ? C15" C16" 1.52(2) . ? C15" C17" 1.53(2) . ? C18" C19" 1.401(12) . ? C18" C23" 1.408(12) . ? C18" C24" 1.467(11) . ? C19" O19" 1.366(9) . ? C19" C20" 1.418(11) . ? C20" C21" 1.396(12) . ? C20" C26" 1.480(12) . ? C21" C22" 1.423(15) . ? C22" C23" 1.367(14) . ? C22" C29" 1.534(13) . ? C24" O24" 1.242(10) . ? C24" O25" 1.295(11) . ? C26" C28" 1.508(14) . ? C26" C27" 1.567(11) . ? C29" C30" 1.46(2) . ? C29" C31" 1.52(2) . ? C32" C33" 1.379(13) . ? C32" C37" 1.415(12) . ? C32" C38" 1.463(12) . ? C33" O33" 1.358(10) . ? C33" C34" 1.395(13) . ? C34" C35" 1.413(15) . ? C34" C40" 1.51(2) . ? C35" C36" 1.36(2) . ? C36" C37" 1.386(14) . ? C36" C43" 1.522(13) . ? C38" O38" 1.238(10) . ? C38" O39" 1.306(11) . ? C40" C42" 1.539(9) . ? C40" C41" 1.541(10) . ? C40" C42C 1.548(10) . ? C40" C41C 1.554(10) . ? C43" C45" 1.541(10) . ? C43" C44" 1.544(10) . ? C43" C45C 1.549(10) . ? C43" C44C 1.552(10) . ? C46" C47" 1.344(14) . ? C46" C51" 1.405(15) . ? C46" C52" 1.484(12) . ? C47" O47" 1.399(12) . ? C47" C48" 1.430(12) . ? C48" C49" 1.40(2) . ? C48" C54" 1.51(2) . ? C49" C50" 1.36(2) . ? C50" C51" 1.405(15) . ? C50" C57" 1.54(2) . ? C52" O52" 1.248(12) . ? C52" O53" 1.323(12) . ? C54" C55" 1.51(2) . ? C54" C56" 1.524(15) . ? C57" C59" 1.539(10) . ? C57" C58" 1.541(10) . ? C57" C58C 1.548(10) . ? C57" C59C 1.555(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 W1 O3 98.2(3) . . ? O1 W1 O19 97.1(3) . . ? O3 W1 O19 98.3(2) . . ? O1 W1 O5 99.5(3) . . ? O3 W1 O5 161.4(2) . . ? O19 W1 O5 85.3(2) . . ? O1 W1 O11 101.4(3) . . ? O3 W1 O11 88.8(2) . . ? O19 W1 O11 159.0(2) . . ? O5 W1 O11 82.0(2) . . ? O1 W1 O24 176.5(3) . . ? O3 W1 O24 80.3(2) . . ? O19 W1 O24 80.1(2) . . ? O5 W1 O24 82.4(2) . . ? O11 W1 O24 81.8(2) . . ? O2 W2 O3 98.6(3) . . ? O2 W2 O33 97.0(3) . . ? O3 W2 O33 97.5(2) . . ? O2 W2 O47 99.0(3) . . ? O3 W2 O47 161.2(2) . . ? O33 W2 O47 86.8(2) . . ? O2 W2 O53 100.4(3) . . ? O3 W2 O53 88.1(2) . . ? O33 W2 O53 160.7(2) . . ? O47 W2 O53 82.3(2) . . ? O2 W2 O38 176.6(3) . . ? O3 W2 O38 80.2(2) . . ? O33 W2 O38 80.0(2) . . ? O47 W2 O38 82.5(2) . . ? O53 W2 O38 82.8(2) . . ? W1 O3 W2 162.4(3) . . ? C9 C4 C5 119.6(8) . . ? C9 C4 C10 118.8(9) . . ? C5 C4 C10 121.5(8) . . ? O5 C5 C4 121.9(7) . . ? O5 C5 C6 117.6(9) . . ? C4 C5 C6 120.5(8) . . ? C5 O5 W1 133.6(5) . . ? C7 C6 C5 115.8(10) . . ? C7 C6 C12 125.6(9) . . ? C5 C6 C12 118.6(9) . . ? C8 C7 C6 124.6(10) . . ? C9 C8 C7 117.9(10) . . ? C9 C8 C15 119.5(11) . . ? C7 C8 C15 122.5(11) . . ? C8 C9 C4 121.5(11) . . ? O10 C10 O11 120.7(8) . . ? O10 C10 C4 121.4(9) . . ? O11 C10 C4 117.9(9) . . ? C10 O11 W1 135.3(6) . . ? C6 C12 C14 112.7(11) . . ? C6 C12 C13 109.8(11) . . ? C14 C12 C13 110.2(13) . . ? C8 C15 C17 111.4(14) . . ? C8 C15 C16A 119.3(27) . . ? C8 C15 C17A 103.3(15) . . ? C16A C15 C17A 110.9(14) . . ? C8 C15 C16 110.8(11) . . ? C17 C15 C16 109.1(12) . . ? C19 C18 C23 118.4(8) . . ? C19 C18 C24 120.8(7) . . ? C23 C18 C24 120.7(8) . . ? O19 C19 C20 117.5(8) . . ? O19 C19 C18 120.4(7) . . ? C20 C19 C18 122.1(8) . . ? C19 O19 W1 133.4(5) . . ? C19 C20 C21 116.5(9) . . ? C19 C20 C26 119.6(8) . . ? C21 C20 C26 123.9(9) . . ? C22 C21 C20 123.7(9) . . ? C21 C22 C23 118.5(9) . . ? C21 C22 C29 120.9(9) . . ? C23 C22 C29 120.6(10) . . ? C22 C23 C18 120.8(9) . . ? O24 C24 O25 120.7(7) . . ? O24 C24 C18 122.7(7) . . ? O25 C24 C18 116.6(7) . . ? C24 O24 W1 129.2(5) . . ? C20 C26 C27 112.7(13) . . ? C20 C26 C28 111.4(13) . . ? C27 C26 C28 112.3(12) . . ? C20 C26 C28A 119.2(21) . . ? C20 C26 C27A 113.1(23) . . ? C28A C26 C27A 110.8(14) . . ? C31 C29 C30 114.5(15) . . ? C31 C29 C22 111.9(11) . . ? C30 C29 C22 114.2(10) . . ? C33 C32 C37 119.9(8) . . ? C33 C32 C38 121.0(8) . . ? C37 C32 C38 119.1(8) . . ? O33 C33 C32 121.3(7) . . ? O33 C33 C34 117.7(8) . . ? C32 C33 C34 121.0(8) . . ? C33 O33 W2 135.3(5) . . ? C35 C34 C33 115.8(9) . . ? C35 C34 C40 125.1(8) . . ? C33 C34 C40 119.1(8) . . ? C36 C35 C34 124.8(9) . . ? C35 C36 C37 119.0(10) . . ? C35 C36 C43 121.5(10) . . ? C37 C36 C43 119.5(12) . . ? C36 C37 C32 119.5(10) . . ? O38 C38 O39 120.0(8) . . ? O38 C38 C32 122.6(8) . . ? O39 C38 C32 117.4(8) . . ? C38 O38 W2 129.6(5) . . ? C34 C40 C42 113.6(8) . . ? C34 C40 C41 109.9(9) . . ? C42 C40 C41 108.6(8) . . ? C36 C43 C44 113.8(15) . . ? C36 C43 C44A 115.8(22) . . ? C36 C43 C45 111.3(15) . . ? C44 C43 C45 111.1(13) . . ? C36 C43 C45A 115.6(23) . . ? C44A C43 C45A 113.1(15) . . ? C51 C46 C47 119.5(8) . . ? C51 C46 C52 118.6(8) . . ? C47 C46 C52 121.8(8) . . ? O47 C47 C48 117.7(8) . . ? O47 C47 C46 121.0(7) . . ? C48 C47 C46 121.2(9) . . ? C47 O47 W2 131.9(5) . . ? C49 C48 C47 116.9(9) . . ? C49 C48 C54 122.5(9) . . ? C47 C48 C54 120.5(9) . . ? C48 C49 C50 124.9(9) . . ? C49 C50 C51 115.8(10) . . ? C49 C50 C57 119.2(10) . . ? C51 C50 C57 125.0(11) . . ? C46 C51 C50 121.5(9) . . ? O52 C52 O53 119.8(7) . . ? O52 C52 C46 121.3(8) . . ? O53 C52 C46 118.8(7) . . ? C52 O53 W2 133.7(5) . . ? C48 C54 C56 113.6(11) . . ? C48 C54 C55 112.5(11) . . ? C56 C54 C55 109.7(11) . . ? C48 C54 C56A 116.1(25) . . ? C48 C54 C55A 113.1(21) . . ? C56A C54 C55A 109.9(14) . . ? C50 C57 C58 119.5(18) . . ? C50 C57 C59 118.5(22) . . ? C58 C57 C59 112.0(14) . . ? C50 C57 C59A 115.3(16) . . ? C50 C57 C58A 108.9(17) . . ? C59A C57 C58A 111.6(14) . . ? O1' W1' O3' 99.3(3) . . ? O1' W1' O19' 96.1(3) . . ? O3' W1' O19' 96.2(2) . . ? O1' W1' O5' 99.7(3) . . ? O3' W1' O5' 160.0(2) . . ? O19' W1' O5' 87.7(3) . . ? O1' W1' O11' 100.0(3) . . ? O3' W1' O11' 88.7(2) . . ? O19' W1' O11' 162.2(2) . . ? O5' W1' O11' 82.1(2) . . ? O1' W1' O24' 175.9(3) . . ? O3' W1' O24' 80.0(2) . . ? O19' W1' O24' 79.9(2) . . ? O5' W1' O24' 81.4(2) . . ? O11' W1' O24' 84.1(2) . . ? O2' W2' O33' 96.4(3) . . ? O2' W2' O3' 98.0(2) . . ? O33' W2' O3' 98.3(2) . . ? O2' W2' O47' 99.4(2) . . ? O33' W2' O47' 85.7(2) . . ? O3' W2' O47' 161.6(2) . . ? O2' W2' O53' 99.7(3) . . ? O33' W2' O53' 161.4(2) . . ? O3' W2' O53' 88.7(2) . . ? O47' W2' O53' 82.5(2) . . ? O2' W2' O38' 176.4(2) . . ? O33' W2' O38' 80.6(2) . . ? O3' W2' O38' 80.7(2) . . ? O47' W2' O38' 82.3(2) . . ? O53' W2' O38' 83.7(2) . . ? W1' O3' W2' 160.9(3) . . ? C5' C4' C9' 119.8(9) . . ? C5' C4' C10' 122.0(8) . . ? C9' C4' C10' 118.2(8) . . ? O5' C5' C4' 122.0(8) . . ? O5' C5' C6' 118.2(9) . . ? C4' C5' C6' 119.9(9) . . ? C5' O5' W1' 132.5(5) . . ? C7' C6' C5' 117.5(10) . . ? C7' C6' C12' 121.7(9) . . ? C5' C6' C12' 120.8(9) . . ? C6' C7' C8' 124.8(10) . . ? C9' C8' C7' 117.5(10) . . ? C9' C8' C15' 118.0(13) . . ? C7' C8' C15' 124.5(12) . . ? C8' C9' C4' 120.6(10) . . ? O10' C10' O11' 118.9(8) . . ? O10' C10' C4' 122.7(8) . . ? O11' C10' C4' 118.3(7) . . ? C10' O11' W1' 134.5(5) . . ? C14' C12' C13' 110.8(11) . . ? C14' C12' C6' 111.2(10) . . ? C13' C12' C6' 112.0(12) . . ? C8' C15' C16' 114.8(15) . . ? C8' C15' C16B 107.5(18) . . ? C8' C15' C17B 130.1(23) . . ? C16B C15' C17B 113.5(14) . . ? C8' C15' C17' 110.6(14) . . ? C16' C15' C17' 116.9(13) . . ? C19' C18' C23' 118.7(8) . . ? C19' C18' C24' 120.5(7) . . ? C23' C18' C24' 120.7(8) . . ? O19' C19' C18' 121.9(7) . . ? O19' C19' C20' 116.6(8) . . ? C18' C19' C20' 121.4(8) . . ? C19' O19' W1' 136.4(5) . . ? C21' C20' C19' 117.0(9) . . ? C21' C20' C26' 124.4(8) . . ? C19' C20' C26' 118.6(8) . . ? C20' C21' C22' 123.4(9) . . ? C23' C22' C21' 118.5(9) . . ? C23' C22' C29' 121.5(11) . . ? C21' C22' C29' 119.9(10) . . ? C22' C23' C18' 120.9(10) . . ? O24' C24' O25' 121.2(7) . . ? O24' C24' C18' 123.3(8) . . ? O25' C24' C18' 115.6(7) . . ? C24' O24' W1' 129.8(5) . . ? C27' C26' C20' 112.6(10) . . ? C27' C26' C28' 111.8(10) . . ? C20' C26' C28' 110.9(11) . . ? C30' C29' C31' 118.3(17) . . ? C30' C29' C22' 114.5(14) . . ? C31' C29' C22' 110.0(14) . . ? C33' C32' C37' 119.4(8) . . ? C33' C32' C38' 119.8(7) . . ? C37' C32' C38' 120.7(8) . . ? O33' C33' C32' 121.1(7) . . ? O33' C33' C34' 117.9(7) . . ? C32' C33' C34' 120.9(7) . . ? C33' O33' W2' 134.0(5) . . ? C35' C34' C33' 116.6(9) . . ? C35' C34' C40' 122.9(8) . . ? C33' C34' C40' 120.4(8) . . ? C34' C35' C36' 124.5(9) . . ? C37' C36' C35' 116.9(9) . . ? C37' C36' C43' 120.2(11) . . ? C35' C36' C43' 122.9(10) . . ? C36' C37' C32' 121.5(10) . . ? O38' C38' O39' 120.2(7) . . ? O38' C38' C32' 123.2(7) . . ? O39' C38' C32' 116.6(7) . . ? C38' O38' W2' 128.3(5) . . ? C41' C40' C42' 113.5(10) . . ? C41' C40' C34' 112.5(9) . . ? C42' C40' C34' 111.9(10) . . ? C36' C43' C45' 107.6(12) . . ? C36' C43' C44B 120.2(27) . . ? C36' C43' C45B 108.4(19) . . ? C44B C43' C45B 108.9(14) . . ? C36' C43' C44' 110.3(13) . . ? C45' C43' C44' 109.3(12) . . ? C51' C46' C47' 117.9(7) . . ? C51' C46' C52' 119.8(8) . . ? C47' C46' C52' 122.3(7) . . ? O47' C47' C48' 118.6(7) . . ? O47' C47' C46' 120.0(7) . . ? C48' C47' C46' 121.4(7) . . ? C47' O47' W2' 135.2(5) . . ? C47' C48' C49' 117.2(8) . . ? C47' C48' C54' 119.9(8) . . ? C49' C48' C54' 122.9(8) . . ? C50' C49' C48' 124.5(8) . . ? C49' C50' C51' 117.1(8) . . ? C49' C50' C57' 123.0(9) . . ? C51' C50' C57' 119.9(9) . . ? C50' C51' C46' 122.0(9) . . ? O52' C52' O53' 118.9(7) . . ? O52' C52' C46' 122.0(8) . . ? O53' C52' C46' 119.1(7) . . ? C52' O53' W2' 137.2(5) . . ? C48' C54' C55' 112.0(9) . . ? C48' C54' C56' 113.6(9) . . ? C55' C54' C56' 110.6(11) . . ? C50' C57' C58' 113.9(10) . . ? C50' C57' C59B 113.9(22) . . ? C50' C57' C58B 129.9(33) . . ? C59B C57' C58B 110.6(15) . . ? C50' C57' C59' 109.7(11) . . ? C58' C57' C59' 107.6(11) . . ? O1" W1" O19" 96.2(3) . . ? O1" W1" O3" 98.3(3) . . ? O19" W1" O3" 97.8(2) . . ? O1" W1" O5" 99.9(3) . . ? O19" W1" O5" 86.6(2) . . ? O3" W1" O5" 160.7(2) . . ? O1" W1" O11" 100.3(3) . . ? O19" W1" O11" 161.2(2) . . ? O3" W1" O11" 88.6(2) . . ? O5" W1" O11" 81.8(2) . . ? O1" W1" O24" 175.9(3) . . ? O19" W1" O24" 80.4(2) . . ? O3" W1" O24" 80.0(2) . . ? O5" W1" O24" 82.2(2) . . ? O11" W1" O24" 83.4(2) . . ? O2" W2" O3" 98.3(3) . . ? O2" W2" O33" 97.2(3) . . ? O3" W2" O33" 99.5(2) . . ? O2" W2" O47" 99.9(3) . . ? O3" W2" O47" 160.4(2) . . ? O33" W2" O47" 85.3(3) . . ? O2" W2" O53" 99.5(3) . . ? O3" W2" O53" 88.0(2) . . ? O33" W2" O53" 160.5(2) . . ? O47" W2" O53" 81.9(2) . . ? O2" W2" O38" 176.3(3) . . ? O3" W2" O38" 79.7(2) . . ? O33" W2" O38" 80.2(2) . . ? O47" W2" O38" 82.5(2) . . ? O53" W2" O38" 83.5(2) . . ? W2" O3" W1" 161.1(3) . . ? C9" C4" C5" 119.9(7) . . ? C9" C4" C10" 119.2(7) . . ? C5" C4" C10" 120.9(7) . . ? O5" C5" C4" 121.8(7) . . ? O5" C5" C6" 118.8(7) . . ? C4" C5" C6" 119.3(8) . . ? C5" O5" W1" 132.3(5) . . ? C7" C6" C5" 118.4(8) . . ? C7" C6" C12" 122.1(8) . . ? C5" C6" C12" 119.4(8) . . ? C6" C7" C8" 123.0(8) . . ? C9" C8" C7" 117.7(8) . . ? C9" C8" C15" 123.9(8) . . ? C7" C8" C15" 118.4(8) . . ? C8" C9" C4" 121.6(8) . . ? O10" C10" O11" 119.2(7) . . ? O10" C10" C4" 120.9(8) . . ? O11" C10" C4" 119.9(7) . . ? C10" O11" W1" 133.5(5) . . ? C6" C12" C13C 110.5(23) . . ? C6" C12" C13" 110.6(9) . . ? C6" C12" C14C 119.8(26) . . ? C13C C12" C14C 109.7(14) . . ? C6" C12" C14" 109.8(10) . . ? C13" C12" C14" 108.5(11) . . ? C16" C15" C17" 111.5(10) . . ? C16" C15" C8" 111.5(9) . . ? C17" C15" C8" 113.0(9) . . ? C19" C18" C23" 120.2(8) . . ? C19" C18" C24" 120.6(7) . . ? C23" C18" C24" 119.2(8) . . ? O19" C19" C18" 120.4(7) . . ? O19" C19" C20" 118.2(7) . . ? C18" C19" C20" 121.3(7) . . ? C19" O19" W1" 133.7(5) . . ? C21" C20" C19" 115.7(8) . . ? C21" C20" C26" 125.0(7) . . ? C19" C20" C26" 119.3(7) . . ? C20" C21" C22" 124.1(8) . . ? C23" C22" C21" 117.9(8) . . ? C23" C22" C29" 120.3(10) . . ? C21" C22" C29" 121.8(9) . . ? C22" C23" C18" 120.7(10) . . ? O24" C24" O25" 121.2(7) . . ? O24" C24" C18" 123.5(8) . . ? O25" C24" C18" 115.3(7) . . ? C24" O24" W1" 129.1(5) . . ? C20" C26" C28" 112.1(8) . . ? C20" C26" C27" 112.1(8) . . ? C28" C26" C27" 109.3(8) . . ? C30" C29" C31" 114.4(13) . . ? C30" C29" C22" 111.1(13) . . ? C31" C29" C22" 110.7(12) . . ? C33" C32" C37" 120.0(8) . . ? C33" C32" C38" 121.1(7) . . ? C37" C32" C38" 119.0(8) . . ? O33" C33" C32" 121.0(8) . . ? O33" C33" C34" 117.9(9) . . ? C32" C33" C34" 121.1(8) . . ? C33" O33" W2" 133.0(6) . . ? C33" C34" C35" 116.6(10) . . ? C33" C34" C40" 120.2(9) . . ? C35" C34" C40" 123.1(9) . . ? C36" C35" C34" 123.9(9) . . ? C35" C36" C37" 118.4(9) . . ? C35" C36" C43" 118.7(9) . . ? C37" C36" C43" 122.8(11) . . ? C36" C37" C32" 120.0(10) . . ? O38" C38" O39" 119.6(8) . . ? O38" C38" C32" 123.3(8) . . ? O39" C38" C32" 117.1(7) . . ? C38" O38" W2" 128.5(6) . . ? C34" C40" C42" 110.6(13) . . ? C34" C40" C41" 109.8(14) . . ? C42" C40" C41" 111.7(12) . . ? C34" C40" C42C 118.7(25) . . ? C34" C40" C41C 108.7(24) . . ? C42C C40" C41C 108.9(14) . . ? C36" C43" C45" 114.4(13) . . ? C36" C43" C44" 111.5(18) . . ? C45" C43" C44" 111.1(14) . . ? C36" C43" C45C 115.1(19) . . ? C36" C43" C44C 108.5(19) . . ? C45C C43" C44C 108.1(13) . . ? C47" C46" C51" 121.6(9) . . ? C47" C46" C52" 121.7(9) . . ? C51" C46" C52" 116.6(9) . . ? C46" C47" O47" 122.2(7) . . ? C46" C47" C48" 122.2(10) . . ? O47" C47" C48" 115.5(8) . . ? C47" O47" W2" 130.9(5) . . ? C49" C48" C47" 113.8(10) . . ? C49" C48" C54" 125.3(9) . . ? C47" C48" C54" 120.9(10) . . ? C50" C49" C48" 125.9(9) . . ? C49" C50" C51" 117.9(11) . . ? C49" C50" C57" 126.0(11) . . ? C51" C50" C57" 116.1(12) . . ? C46" C51" C50" 118.6(11) . . ? O52" C52" O53" 119.4(8) . . ? O52" C52" C46" 121.4(9) . . ? O53" C52" C46" 119.2(8) . . ? C52" O53" W2" 133.9(5) . . ? C48" C54" C55" 110.5(10) . . ? C48" C54" C56" 112.8(11) . . ? C55" C54" C56" 111.1(10) . . ? C59" C57" C58" 111.5(13) . . ? C59" C57" C50" 112.8(15) . . ? C58" C57" C50" 113.4(17) . . ? C50" C57" C58C 101.8(40) . . ? C50" C57" C59C 96.5(32) . . ? C58C C57" C59C 108.2(14) . . ? _refine_diff_density_max 1.046 _refine_diff_density_min -1.167 _refine_diff_density_rms 0.117 #===END data_Compound_3 _database_code_depnum_ccdc_archive 'CCDC 258929' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C26 H33 O7 Cl W' _chemical_formula_weight 676.82 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' W W -5.4734 5.5774 '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 12.3643(11) _cell_length_b 14.9782(15) _cell_length_c 17.039(2) _cell_angle_alpha 69.847(8) _cell_angle_beta 71.662(10) _cell_angle_gamma 82.612(9) _cell_volume 2811.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27 _cell_measurement_theta_min 10.59 _cell_measurement_theta_max 27.80 _exptl_crystal_description 'platy needles' _exptl_crystal_colour Red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method ? _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 8.826 _exptl_absorpt_correction_type 'Lamina [1 1 1]' _exptl_absorpt_correction_T_min 0.3216 _exptl_absorpt_correction_T_max 0.8687 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7987 _diffrn_reflns_av_R_equivalents 0.0201 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 59.99 _reflns_number_total 7592 _reflns_number_observed 5951 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 442 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0689P)^2^+2.2696P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00014(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7150 _refine_ls_number_parameters 730 _refine_ls_number_restraints 137 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_obs 0.0480 _refine_ls_wR_factor_all 0.1333 _refine_ls_wR_factor_obs 0.1208 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_goodness_of_fit_obs 1.091 _refine_ls_restrained_S_all 1.057 _refine_ls_restrained_S_obs 1.096 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group W W 0.22731(4) 0.50020(3) 0.28722(3) 0.0717(2) Uani 1 d . . Cl Cl 0.1983(3) 0.6180(2) 0.1645(2) 0.0924(7) Uani 1 d . . O O 0.1432(7) 0.4187(6) 0.2892(6) 0.096(2) Uani 1 d . . O1 O 0.2593(7) 0.4374(6) 0.3939(5) 0.091(2) Uani 1 d . . C1 C 0.2440(9) 0.4584(7) 0.4694(7) 0.080(3) Uani 1 d . . C2 C 0.3054(10) 0.4033(9) 0.5268(8) 0.092(3) Uani 1 d . . C3 C 0.2837(12) 0.4184(10) 0.6038(9) 0.101(4) Uani 1 d . . H3A H 0.3222(12) 0.3813(10) 0.6433(9) 0.122 Uiso 1 calc R . C4 C 0.2038(14) 0.4894(11) 0.6270(9) 0.110(4) Uani 1 d . . C5 C 0.1453(10) 0.5425(9) 0.5693(7) 0.087(3) Uani 1 d . . H5A H 0.0919(10) 0.5885(9) 0.5835(7) 0.104 Uiso 1 calc R . C6 C 0.1658(9) 0.5279(7) 0.4892(7) 0.076(2) Uani 1 d . . C7 C 0.1036(8) 0.5877(7) 0.4294(6) 0.069(2) Uani 1 d . . O7 O 0.0325(7) 0.6494(5) 0.4471(4) 0.085(2) Uani 1 d . . O8 O 0.1157(6) 0.5723(5) 0.3537(4) 0.075(2) Uani 1 d . . C9 C 0.3960(11) 0.3333(10) 0.5048(10) 0.128(6) Uani 1 d D . H9A H 0.4269(11) 0.3096(10) 0.5549(10) 0.153 Uiso 0.70 calc PR 1 H9B H 0.3805(11) 0.3245(10) 0.4562(10) 0.153 Uiso 0.30 d PR 2 C10 C 0.3524(16) 0.2459(13) 0.5002(14) 0.118(7) Uani 0.70 d PD 1 H10A H 0.4154(16) 0.2040(13) 0.4858(14) 0.177 Uiso 0.70 calc PR 1 H10B H 0.3134(16) 0.2645(13) 0.4562(14) 0.177 Uiso 0.70 calc PR 1 H10C H 0.3007(16) 0.2137(13) 0.5558(14) 0.177 Uiso 0.70 calc PR 1 C11 C 0.4974(14) 0.3758(14) 0.4269(16) 0.123(9) Uani 0.70 d PD 1 H11A H 0.5519(14) 0.3261(14) 0.4170(16) 0.184 Uiso 0.70 calc PR 1 H11B H 0.5323(14) 0.4216(14) 0.4386(16) 0.184 Uiso 0.70 calc PR 1 H11C H 0.4720(14) 0.4064(14) 0.3760(16) 0.184 Uiso 0.70 calc PR 1 C10A C 0.3961(37) 0.2305(15) 0.5634(25) 0.100(11) Uiso 0.30 d PD 2 H10D H 0.4616(37) 0.1972(15) 0.5376(25) 0.149 Uiso 0.30 calc PR 2 H10E H 0.3281(37) 0.2007(15) 0.5700(25) 0.149 Uiso 0.30 calc PR 2 H10F H 0.3987(37) 0.2287(15) 0.6197(25) 0.149 Uiso 0.30 calc PR 2 C11A C 0.5158(29) 0.3734(40) 0.4702(48) 0.168(38) Uiso 0.30 d PD 2 H11D H 0.5707(29) 0.3253(40) 0.4571(48) 0.251 Uiso 0.30 calc PR 2 H11E H 0.5307(29) 0.3933(40) 0.5136(48) 0.251 Uiso 0.30 calc PR 2 H11F H 0.5211(29) 0.4270(40) 0.4181(48) 0.251 Uiso 0.30 calc PR 2 C12 C 0.1822(18) 0.4957(13) 0.7162(9) 0.153(7) Uani 1 d DU . H12A H 0.2551(18) 0.4778(13) 0.7295(9) 0.184 Uiso 0.55 calc PR 1 H12B H 0.1098(18) 0.5288(13) 0.7204(9) 0.184 Uiso 0.45 d PR 2 C13 C 0.1566(32) 0.5963(15) 0.7196(19) 0.148(13) Uani 0.55 d PD 1 H13A H 0.1435(32) 0.5958(15) 0.7783(19) 0.222 Uiso 0.55 calc PR 1 H13B H 0.0899(32) 0.6210(15) 0.7011(19) 0.222 Uiso 0.55 calc PR 1 H13C H 0.2202(32) 0.6357(15) 0.6816(19) 0.222 Uiso 0.55 calc PR 1 C14 C 0.0980(29) 0.4246(21) 0.7881(16) 0.161(19) Uani 0.55 d PD 1 H14A H 0.0888(29) 0.4334(21) 0.8431(16) 0.241 Uiso 0.55 calc PR 1 H14B H 0.1260(29) 0.3612(21) 0.7906(16) 0.241 Uiso 0.55 calc PR 1 H14C H 0.0257(29) 0.4344(21) 0.7761(16) 0.241 Uiso 0.55 calc PR 1 C13A C 0.2456(37) 0.5595(26) 0.7382(27) 0.151(16) Uiso 0.45 d PD 2 H13D H 0.2169(37) 0.5513(26) 0.7995(27) 0.227 Uiso 0.45 calc PR 2 H13E H 0.2348(37) 0.6246(26) 0.7052(27) 0.227 Uiso 0.45 calc PR 2 H13F H 0.3254(37) 0.5429(26) 0.7238(27) 0.227 Uiso 0.45 calc PR 2 C14A C 0.1403(37) 0.4059(21) 0.7922(22) 0.116(14) Uiso 0.45 d PD 2 H14D H 0.1291(37) 0.4176(21) 0.8462(22) 0.173 Uiso 0.45 calc PR 2 H14E H 0.1958(37) 0.3555(21) 0.7879(22) 0.173 Uiso 0.45 calc PR 2 H14F H 0.0695(37) 0.3881(21) 0.7904(22) 0.173 Uiso 0.45 calc PR 2 O21 O 0.3652(6) 0.4592(5) 0.2224(5) 0.078(2) Uani 1 d . . C21 C 0.4706(8) 0.4952(7) 0.1703(6) 0.068(2) Uani 1 d . . C22 C 0.5387(8) 0.4420(8) 0.1176(6) 0.074(2) Uani 1 d . . C23 C 0.6400(10) 0.4835(9) 0.0593(7) 0.086(3) Uani 1 d . . H23A H 0.6839(10) 0.4528(9) 0.0205(7) 0.103 Uiso 1 calc R . C24 C 0.6795(10) 0.5677(10) 0.0555(8) 0.095(3) Uani 1 d . . C25 C 0.6139(10) 0.6140(9) 0.1131(8) 0.090(3) Uani 1 d . . H25A H 0.6397(10) 0.6697(9) 0.1131(8) 0.108 Uiso 1 calc R . C26 C 0.5084(8) 0.5771(7) 0.1717(6) 0.067(2) Uani 1 d . . C27 C 0.4423(9) 0.6249(7) 0.2354(7) 0.072(2) Uani 1 d . . O27 O 0.3445(6) 0.6050(5) 0.2807(4) 0.076(2) Uani 1 d . . O28 O 0.4952(6) 0.6889(6) 0.2439(6) 0.089(2) Uani 1 d . . C29 C 0.4982(9) 0.3458(8) 0.1283(7) 0.083(3) Uani 1 d . . H29A H 0.4157(9) 0.3503(8) 0.1372(7) 0.100 Uiso 1 calc R . C30 C 0.5220(16) 0.2741(11) 0.2108(8) 0.119(5) Uani 1 d . . H30A H 0.4972(16) 0.2124(11) 0.2193(8) 0.179 Uiso 1 calc R . H30B H 0.4814(16) 0.2938(11) 0.2605(8) 0.179 Uiso 1 calc R . H30C H 0.6023(16) 0.2712(11) 0.2043(8) 0.179 Uiso 1 calc R . C31 C 0.5558(12) 0.3120(10) 0.0487(8) 0.100(4) Uani 1 d . . H31A H 0.5270(12) 0.2511(10) 0.0592(8) 0.150 Uiso 1 calc R . H31B H 0.6367(12) 0.3067(10) 0.0395(8) 0.150 Uiso 1 calc R . H31C H 0.5394(12) 0.3572(10) -0.0022(8) 0.150 Uiso 1 calc R . C32 C 0.7887(12) 0.6150(11) -0.0081(9) 0.123(5) Uani 1 d D . H32A H 0.8338(12) 0.6211(11) 0.0279(9) 0.147 Uiso 0.60 calc PR 1 H32B H 0.8106(12) 0.6584(11) 0.0143(9) 0.147 Uiso 0.40 d PR 2 C33 C 0.7682(19) 0.7161(11) -0.0640(13) 0.112(8) Uani 0.60 d PD 1 H33A H 0.8396(19) 0.7430(11) -0.1031(13) 0.168 Uiso 0.60 calc PR 1 H33B H 0.7333(19) 0.7541(11) -0.0270(13) 0.168 Uiso 0.60 calc PR 1 H33C H 0.7188(19) 0.7149(11) -0.0972(13) 0.168 Uiso 0.60 calc PR 1 C34 C 0.8618(24) 0.5559(17) -0.0627(19) 0.159(14) Uani 0.60 d PDU 1 H34A H 0.9293(24) 0.5899(17) -0.1014(19) 0.238 Uiso 0.60 calc PR 1 H34B H 0.8195(24) 0.5437(17) -0.0964(19) 0.238 Uiso 0.60 calc PR 1 H34C H 0.8829(24) 0.4966(17) -0.0250(19) 0.238 Uiso 0.60 calc PR 1 C33A C 0.7825(45) 0.6791(32) -0.0983(18) 0.162(21) Uiso 0.40 d PD 2 H33D H 0.8562(45) 0.7049(32) -0.1328(18) 0.243 Uiso 0.40 calc PR 2 H33E H 0.7282(45) 0.7300(32) -0.0924(18) 0.243 Uiso 0.40 calc PR 2 H33F H 0.7593(45) 0.6426(32) -0.1266(18) 0.243 Uiso 0.40 calc PR 2 C34A C 0.8802(33) 0.5371(24) -0.0199(25) 0.111(12) Uiso 0.40 d PD 2 H34D H 0.9500(33) 0.5660(24) -0.0601(25) 0.167 Uiso 0.40 calc PR 2 H34E H 0.8551(33) 0.4955(24) -0.0425(25) 0.167 Uiso 0.40 calc PR 2 H34F H 0.8924(33) 0.5012(24) 0.0354(25) 0.167 Uiso 0.40 calc PR 2 W' W 0.21515(3) 0.95830(3) 0.19647(3) 0.0637(2) Uani 1 d . . Cl' Cl 0.2499(3) 0.8643(2) 0.1084(2) 0.0936(8) Uani 1 d . . O' O 0.3061(6) 1.0434(6) 0.1267(5) 0.088(2) Uani 1 d . . O1' O 0.1850(6) 1.0023(5) 0.2917(5) 0.085(2) Uani 1 d D . C1' C 0.2030(10) 0.9686(9) 0.3724(7) 0.050(4) Uani 0.55 d PD 1 C2' C 0.1577(12) 1.0224(12) 0.4295(10) 0.078(6) Uani 0.55 d PD 1 C3' C 0.1780(14) 0.9838(14) 0.5105(11) 0.090(6) Uani 0.55 d PD 1 H3'A H 0.1491(14) 1.0172(14) 0.5499(11) 0.108 Uiso 0.55 calc PR 1 C4' C 0.2371(14) 0.9004(13) 0.5372(10) 0.102(9) Uani 0.55 d PD 1 C5' C 0.2813(12) 0.8503(11) 0.4798(10) 0.090(7) Uani 0.55 d PD 1 H5'A H 0.3228(12) 0.7941(11) 0.4956(10) 0.108 Uiso 0.55 calc PR 1 C6' C 0.2634(10) 0.8844(9) 0.3966(8) 0.054(3) Uani 0.55 d PD 1 C7' C 0.3158(11) 0.8274(13) 0.3391(11) 0.077(7) Uani 0.55 d PD 1 O7' O 0.3602(22) 0.7493(15) 0.3637(16) 0.117(9) Uani 0.55 d PDU 1 C1B C 0.2214(15) 0.9816(16) 0.3647(11) 0.100(13) Uiso 0.45 d PD 2 C2B C 0.1858(12) 1.0393(11) 0.4180(10) 0.052(5) Uiso 0.45 d PD 2 C3B C 0.2230(18) 1.0131(17) 0.4919(13) 0.092(9) Uiso 0.45 d PD 2 H3BA H 0.1993(18) 1.0508(17) 0.5280(13) 0.110 Uiso 0.45 calc PR 2 C4B C 0.2912(22) 0.9367(23) 0.5150(16) 0.159(20) Uiso 0.45 d PD 2 C5B C 0.3268(19) 0.8796(19) 0.4624(18) 0.176(24) Uiso 0.45 d PD 2 H5BA H 0.3743(19) 0.8269(19) 0.4765(18) 0.211 Uiso 0.45 calc PR 2 C6B C 0.2899(15) 0.9022(14) 0.3866(12) 0.116(14) Uiso 0.45 d PD 2 C7B C 0.3345(12) 0.8377(14) 0.3352(11) 0.064(7) Uiso 0.45 d PD 2 O7B O 0.3880(18) 0.7640(15) 0.3564(14) 0.063(5) Uiso 0.45 d PD 2 O8' O 0.3136(5) 0.8649(5) 0.2573(4) 0.0689(15) Uani 1 d D . C9' C 0.0908(17) 1.1149(16) 0.3911(20) 0.162(17) Uani 0.55 d PDU 1 H9'A H 0.0290(17) 1.0970(16) 0.3753(20) 0.195 Uiso 0.55 calc PR 1 C10' C 0.1648(33) 1.1885(21) 0.3098(19) 0.166(15) Uani 0.55 d PDU 1 H10G H 0.1992(33) 1.1599(21) 0.2650(19) 0.249 Uiso 0.55 calc PR 1 H10H H 0.2233(33) 1.2094(21) 0.3251(19) 0.249 Uiso 0.55 calc PR 1 H10I H 0.1179(33) 1.2421(21) 0.2887(19) 0.249 Uiso 0.55 calc PR 1 C11' C 0.0384(42) 1.1652(31) 0.4599(24) 0.162(21) Uani 0.55 d PDU 1 H11G H -0.0085(42) 1.1216(31) 0.5119(24) 0.243 Uiso 0.55 calc PR 1 H11H H -0.0072(42) 1.2189(31) 0.4372(24) 0.243 Uiso 0.55 calc PR 1 H11I H 0.0982(42) 1.1863(31) 0.4737(24) 0.243 Uiso 0.55 calc PR 1 C12' C 0.2570(17) 0.8607(18) 0.6275(13) 0.128(10) Uani 0.55 d PDU 1 H12C H 0.3058(17) 0.8033(18) 0.6307(13) 0.154 Uiso 0.55 calc PR 1 C13' C 0.1407(19) 0.8349(22) 0.6950(15) 0.136(12) Uani 0.55 d PD 1 H13G H 0.1066(19) 0.7883(22) 0.6838(15) 0.204 Uiso 0.55 calc PR 1 H13H H 0.0924(19) 0.8909(22) 0.6911(15) 0.204 Uiso 0.55 calc PR 1 H13I H 0.1501(19) 0.8094(22) 0.7525(15) 0.204 Uiso 0.55 calc PR 1 C14' C 0.3141(28) 0.9346(26) 0.6430(24) 0.165(15) Uani 0.55 d PDU 1 H14G H 0.3868(28) 0.9494(26) 0.5999(24) 0.248 Uiso 0.55 calc PR 1 H14H H 0.3246(28) 0.9097(26) 0.7002(24) 0.248 Uiso 0.55 calc PR 1 H14I H 0.2669(28) 0.9912(26) 0.6388(24) 0.248 Uiso 0.55 calc PR 1 C9B C 0.1116(14) 1.1240(13) 0.3934(14) 0.067(6) Uiso 0.45 d PD 2 H9BA H 0.0568(14) 1.1158(13) 0.3657(14) 0.081 Uiso 0.45 calc PR 2 C10B C 0.2196(20) 1.1794(22) 0.3287(17) 0.099(8) Uiso 0.45 d PD 2 H10J H 0.1979(20) 1.2432(22) 0.2996(17) 0.148 Uiso 0.45 calc PR 2 H10K H 0.2566(20) 1.1482(22) 0.2863(17) 0.148 Uiso 0.45 calc PR 2 H10L H 0.2709(20) 1.1812(22) 0.3604(17) 0.148 Uiso 0.45 calc PR 2 C11B C 0.0623(34) 1.1732(29) 0.4630(20) 0.094(10) Uiso 0.45 d PD 2 H11J H 0.0157(34) 1.2269(29) 0.4419(20) 0.141 Uiso 0.45 calc PR 2 H11K H 0.1235(34) 1.1943(29) 0.4753(20) 0.141 Uiso 0.45 calc PR 2 H11L H 0.0170(34) 1.1292(29) 0.5155(20) 0.141 Uiso 0.45 calc PR 2 C12B C 0.3379(29) 0.9007(31) 0.5942(19) 0.175(20) Uiso 0.45 d PD 2 H12D H 0.3756(29) 0.8389(31) 0.5949(19) 0.210 Uiso 0.45 calc PR 2 C13B C 0.2332(31) 0.8833(37) 0.6738(28) 0.156(17) Uiso 0.45 d PD 2 H13J H 0.1814(31) 0.8440(37) 0.6692(28) 0.234 Uiso 0.45 calc PR 2 H13K H 0.1962(31) 0.9430(37) 0.6765(28) 0.234 Uiso 0.45 calc PR 2 H13L H 0.2560(31) 0.8518(37) 0.7258(28) 0.234 Uiso 0.45 calc PR 2 C14B C 0.4227(40) 0.9628(45) 0.5986(40) 0.236(32) Uiso 0.45 d PD 2 H14J H 0.4877(40) 0.9725(45) 0.5478(40) 0.353 Uiso 0.45 calc PR 2 H14K H 0.4469(40) 0.9319(45) 0.6501(40) 0.353 Uiso 0.45 calc PR 2 H14L H 0.3871(40) 1.0231(45) 0.6008(40) 0.353 Uiso 0.45 calc PR 2 O21' O 0.0851(5) 1.0152(5) 0.1640(4) 0.070(2) Uani 1 d . . C21' C -0.0239(7) 0.9934(7) 0.1734(6) 0.062(2) Uani 1 d . . C22' C -0.0834(8) 1.0629(7) 0.1215(6) 0.066(2) Uani 1 d . . C23' C -0.1915(8) 1.0395(9) 0.1272(7) 0.080(3) Uani 1 d . . H23B H -0.2326(8) 1.0837(9) 0.0933(7) 0.096 Uiso 1 calc R . C24' C -0.2407(8) 0.9527(8) 0.1816(7) 0.073(2) Uani 1 d . . C25' C -0.1793(8) 0.8879(8) 0.2331(6) 0.071(2) Uani 1 d . . H25B H -0.2115(8) 0.8300(8) 0.2706(6) 0.085 Uiso 1 calc R . C26' C -0.0703(8) 0.9077(7) 0.2299(6) 0.068(2) Uani 1 d . . C27' C -0.0102(8) 0.8368(7) 0.2885(6) 0.066(2) Uani 1 d . . O27' O 0.0879(6) 0.8483(5) 0.2870(4) 0.075(2) Uani 1 d . . O28' O -0.0662(6) 0.7619(5) 0.3400(5) 0.083(2) Uani 1 d . . C29' C -0.0293(8) 1.1560(7) 0.0608(6) 0.068(2) Uani 1 d . . H29B H 0.0249(8) 1.1691(7) 0.0866(6) 0.082 Uiso 1 calc R . C30' C -0.1098(15) 1.2408(10) 0.0493(11) 0.139(7) Uani 1 d . . H30D H -0.1524(15) 1.2457(10) 0.1055(11) 0.208 Uiso 1 calc R . H30E H -0.1612(15) 1.2332(10) 0.0201(11) 0.208 Uiso 1 calc R . H30F H -0.0670(15) 1.2975(10) 0.0149(11) 0.208 Uiso 1 calc R . C31' C 0.0391(17) 1.1456(12) -0.0256(10) 0.144(7) Uani 1 d U . H31D H 0.0895(17) 1.0912(12) -0.0164(10) 0.215 Uiso 1 calc R . H31E H 0.0829(17) 1.2017(12) -0.0604(10) 0.215 Uiso 1 calc R . H31F H -0.0113(17) 1.1374(12) -0.0553(10) 0.215 Uiso 1 calc R . C32' C -0.3615(9) 0.9303(10) 0.1886(8) 0.099(4) Uani 1 d D . H32C H -0.3947(9) 0.8825(10) 0.2452(8) 0.119 Uiso 0.50 calc PR 1 H32D H -0.3771(9) 0.8674(10) 0.2297(8) 0.119 Uiso 0.50 d PR 2 C33' C -0.3442(34) 0.8894(38) 0.1149(29) 0.129(17) Uani 0.50 d PD 1 H33G H -0.2965(34) 0.8331(38) 0.1240(29) 0.193 Uiso 0.50 calc PR 1 H33H H -0.3085(34) 0.9357(38) 0.0600(29) 0.193 Uiso 0.50 calc PR 1 H33I H -0.4167(34) 0.8737(38) 0.1143(29) 0.193 Uiso 0.50 calc PR 1 C34' C -0.4366(28) 1.0199(20) 0.1774(29) 0.166(23) Uani 0.50 d PD 1 H34G H -0.4456(28) 1.0436(20) 0.2248(29) 0.249 Uiso 0.50 calc PR 1 H34H H -0.5099(28) 1.0053(20) 0.1773(29) 0.249 Uiso 0.50 calc PR 1 H34I H -0.4016(28) 1.0672(20) 0.1231(29) 0.249 Uiso 0.50 calc PR 1 C33B C -0.3792(31) 0.9194(37) 0.1077(20) 0.116(14) Uani 0.50 d PD 2 H33J H -0.3211(31) 0.8776(37) 0.0860(20) 0.173 Uiso 0.50 calc PR 2 H33K H -0.3750(31) 0.9805(37) 0.0635(20) 0.173 Uiso 0.50 calc PR 2 H33L H -0.4527(31) 0.8932(37) 0.1228(20) 0.173 Uiso 0.50 calc PR 2 C34B C -0.4532(25) 0.9967(21) 0.2243(24) 0.118(13) Uani 0.50 d PDU 2 H34J H -0.4410(25) 1.0029(21) 0.2751(24) 0.177 Uiso 0.50 calc PR 2 H34K H -0.5270(25) 0.9708(21) 0.2398(24) 0.177 Uiso 0.50 calc PR 2 H34L H -0.4492(25) 1.0581(21) 0.1805(24) 0.177 Uiso 0.50 calc PR 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 W 0.0641(3) 0.0695(3) 0.0755(3) -0.0312(2) -0.0057(2) 0.0038(2) Cl 0.103(2) 0.095(2) 0.0774(14) -0.0307(13) -0.0236(13) 0.0048(14) O 0.079(5) 0.078(5) 0.128(7) -0.046(5) -0.013(4) 0.002(4) O1 0.086(5) 0.082(5) 0.085(5) -0.028(4) -0.008(4) 0.028(4) C1 0.064(5) 0.071(6) 0.079(6) -0.014(5) 0.002(4) 0.000(4) C2 0.071(6) 0.096(8) 0.087(7) -0.011(6) -0.019(5) 0.007(5) C3 0.094(8) 0.111(10) 0.090(8) -0.013(7) -0.039(6) 0.006(7) C4 0.127(11) 0.114(10) 0.081(7) -0.014(7) -0.038(7) -0.005(8) C5 0.089(7) 0.082(7) 0.077(6) -0.022(5) -0.010(5) -0.007(5) C6 0.075(6) 0.069(6) 0.071(5) -0.016(4) -0.010(4) -0.007(4) C7 0.059(5) 0.074(6) 0.063(5) -0.019(4) -0.003(4) -0.004(4) O7 0.095(5) 0.074(4) 0.072(4) -0.030(3) -0.008(3) 0.022(4) O8 0.068(4) 0.076(4) 0.069(4) -0.018(3) -0.014(3) 0.009(3) C9 0.088(9) 0.132(13) 0.125(11) -0.022(10) -0.018(8) 0.040(9) C10 0.102(14) 0.111(15) 0.117(15) -0.042(12) -0.002(11) 0.021(12) C11 0.059(10) 0.120(17) 0.149(21) -0.028(14) 0.001(11) 0.014(9) C12 0.211(16) 0.157(14) 0.088(8) -0.035(9) -0.045(10) -0.004(12) C13 0.170(33) 0.178(34) 0.100(19) -0.071(22) -0.007(20) -0.028(26) C14 0.137(31) 0.255(52) 0.057(13) -0.012(19) -0.024(15) -0.007(31) O21 0.070(4) 0.078(4) 0.080(4) -0.032(3) -0.007(3) 0.002(3) C21 0.068(5) 0.075(6) 0.066(5) -0.032(4) -0.019(4) 0.007(4) C22 0.062(5) 0.097(7) 0.063(5) -0.039(5) -0.012(4) 0.017(5) C23 0.081(7) 0.096(8) 0.076(6) -0.042(6) -0.008(5) 0.013(6) C24 0.072(7) 0.104(9) 0.089(7) -0.035(6) 0.008(5) -0.001(6) C25 0.071(6) 0.096(8) 0.092(7) -0.030(6) -0.011(5) 0.004(5) C26 0.061(5) 0.067(5) 0.064(5) -0.020(4) -0.010(4) 0.006(4) C27 0.070(6) 0.070(6) 0.082(6) -0.033(5) -0.024(5) 0.010(4) O27 0.074(4) 0.078(4) 0.078(4) -0.040(3) -0.007(3) -0.002(3) O28 0.072(4) 0.091(5) 0.110(6) -0.045(4) -0.027(4) 0.006(4) C29 0.074(6) 0.094(7) 0.093(7) -0.055(6) -0.018(5) 0.013(5) C30 0.168(15) 0.100(10) 0.079(7) -0.030(7) -0.019(8) -0.005(9) C31 0.113(9) 0.109(9) 0.084(7) -0.048(7) -0.028(7) 0.025(7) C32 0.084(9) 0.129(12) 0.120(11) -0.027(9) 0.006(8) -0.015(8) C33 0.112(17) 0.129(19) 0.090(13) -0.042(14) 0.006(12) -0.060(15) C34 0.086(16) 0.189(27) 0.154(25) -0.067(21) 0.048(17) -0.018(16) W' 0.0546(2) 0.0733(3) 0.0694(3) -0.0277(2) -0.0231(2) 0.0029(2) Cl' 0.121(2) 0.094(2) 0.0790(15) -0.0415(14) -0.0353(15) 0.006(2) O' 0.066(4) 0.098(5) 0.098(5) -0.027(4) -0.023(4) -0.011(4) O1' 0.095(5) 0.083(5) 0.100(5) -0.051(4) -0.050(4) 0.035(4) C1' 0.045(7) 0.063(9) 0.051(8) -0.027(6) -0.015(5) -0.006(6) C2' 0.061(10) 0.088(14) 0.092(14) -0.056(11) 0.007(9) -0.028(10) C3' 0.095(15) 0.123(18) 0.074(12) -0.066(13) -0.013(11) -0.012(14) C4' 0.158(24) 0.095(16) 0.053(9) -0.030(10) -0.043(13) 0.043(17) C5' 0.128(18) 0.095(14) 0.059(9) -0.048(10) -0.040(11) 0.051(14) C6' 0.055(8) 0.062(9) 0.051(8) -0.033(6) -0.014(6) 0.016(7) C7' 0.049(9) 0.086(14) 0.107(17) -0.050(12) -0.016(9) -0.003(9) O7' 0.138(17) 0.105(14) 0.119(13) -0.051(10) -0.058(12) 0.051(13) O8' 0.071(4) 0.075(4) 0.067(4) -0.030(3) -0.022(3) 0.005(3) C9' 0.204(25) 0.129(20) 0.154(22) -0.092(17) -0.011(15) 0.023(16) C10' 0.183(22) 0.144(20) 0.169(21) -0.075(17) -0.038(16) 0.037(17) C11' 0.180(35) 0.174(29) 0.167(27) -0.143(25) -0.010(21) 0.020(23) C12' 0.166(19) 0.145(17) 0.083(12) -0.070(12) -0.031(12) 0.044(15) C13' 0.157(28) 0.158(29) 0.076(14) -0.037(16) -0.028(16) 0.032(23) C14' 0.184(30) 0.201(32) 0.165(26) -0.096(24) -0.093(23) 0.021(24) O21' 0.059(3) 0.081(4) 0.071(4) -0.017(3) -0.027(3) -0.004(3) C21' 0.056(5) 0.069(5) 0.063(5) -0.025(4) -0.019(4) 0.002(4) C22' 0.063(5) 0.074(6) 0.074(5) -0.035(4) -0.029(4) 0.003(4) C23' 0.060(5) 0.099(8) 0.084(6) -0.033(6) -0.025(5) 0.006(5) C24' 0.058(5) 0.088(7) 0.079(6) -0.028(5) -0.026(4) -0.006(4) C25' 0.053(5) 0.085(6) 0.072(5) -0.025(5) -0.007(4) -0.014(4) C26' 0.055(5) 0.081(6) 0.065(5) -0.024(4) -0.016(4) 0.009(4) C27' 0.060(5) 0.070(5) 0.069(5) -0.030(4) -0.011(4) 0.005(4) O27' 0.065(4) 0.080(4) 0.073(4) -0.014(3) -0.024(3) 0.005(3) O28' 0.063(4) 0.082(5) 0.083(4) -0.011(4) -0.009(3) -0.005(3) C29' 0.060(5) 0.075(6) 0.068(5) -0.021(4) -0.020(4) 0.004(4) C30' 0.124(12) 0.085(9) 0.149(13) -0.007(9) -0.009(10) 0.035(9) C31' 0.176(16) 0.125(12) 0.096(9) -0.049(9) 0.034(10) -0.036(11) C32' 0.060(6) 0.118(10) 0.120(9) -0.031(8) -0.030(6) -0.014(6) C33' 0.063(22) 0.182(43) 0.178(36) -0.067(32) -0.067(20) -0.020(20) C34' 0.053(17) 0.253(60) 0.198(49) -0.073(42) -0.047(24) 0.001(25) C33B 0.069(25) 0.188(41) 0.093(19) -0.029(21) -0.028(15) -0.047(23) C34B 0.083(18) 0.087(16) 0.178(31) -0.065(19) 0.000(18) -0.013(13) _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 W O 1.687(9) . ? W O21 1.875(6) . ? W O1 1.876(8) . ? W O8 1.957(6) . ? W O27 2.223(7) . ? W Cl 2.320(3) . ? O1 C1 1.378(14) . ? C1 C6 1.382(14) . ? C1 C2 1.40(2) . ? C2 C3 1.35(2) . ? C2 C9 1.48(2) . ? C3 C4 1.43(2) . ? C4 C5 1.37(2) . ? C4 C12 1.49(2) . ? C5 C6 1.40(2) . ? C6 C7 1.457(15) . ? C7 O7 1.239(11) . ? C7 O8 1.347(12) . ? C9 C10 1.513(10) . ? C9 C10A 1.519(10) . ? C9 C11 1.521(10) . ? C9 C11A 1.529(10) . ? C12 C13A 1.514(10) . ? C12 C13 1.516(10) . ? C12 C14 1.518(10) . ? C12 C14A 1.520(10) . ? O21 C21 1.379(12) . ? C21 C26 1.378(14) . ? C21 C22 1.413(12) . ? C22 C23 1.39(2) . ? C22 C29 1.52(2) . ? C23 C24 1.38(2) . ? C24 C25 1.39(2) . ? C24 C32 1.52(2) . ? C25 C26 1.410(15) . ? C26 C27 1.479(13) . ? C27 O27 1.221(12) . ? C27 O28 1.299(13) . ? C29 C30 1.53(2) . ? C29 C31 1.542(14) . ? C32 C34 1.517(10) . ? C32 C33 1.525(10) . ? C32 C33A 1.527(10) . ? C32 C34A 1.536(10) . ? W' O' 1.669(8) . ? W' O1' 1.870(7) . ? W' O21' 1.871(6) . ? W' O8' 1.968(6) . ? W' O27' 2.227(7) . ? W' Cl' 2.306(3) . ? O1' C1' 1.372(13) . ? O1' C1B 1.38(2) . ? C1' C6' 1.38(2) . ? C1' C2' 1.41(2) . ? C2' C3' 1.39(2) . ? C2' C9' 1.57(3) . ? C3' C4' 1.37(2) . ? C4' C5' 1.37(2) . ? C4' C12' 1.53(3) . ? C5' C6' 1.41(2) . ? C6' C7' 1.46(2) . ? C7' O7' 1.22(2) . ? C7' O8' 1.32(2) . ? C1B C6B 1.38(2) . ? C1B C2B 1.40(2) . ? C2B C3B 1.39(2) . ? C2B C9B 1.48(2) . ? C3B C4B 1.35(3) . ? C4B C5B 1.38(3) . ? C4B C12B 1.53(3) . ? C5B C6B 1.42(3) . ? C6B C7B 1.46(2) . ? C7B O7B 1.21(2) . ? C7B O8' 1.35(2) . ? C9' C11' 1.538(10) . ? C9' C10' 1.543(10) . ? C12' C14' 1.521(10) . ? C12' C13' 1.528(10) . ? C9B C11B 1.534(10) . ? C9B C10B 1.554(10) . ? C12B C14B 1.522(11) . ? C12B C13B 1.524(10) . ? O21' C21' 1.375(11) . ? C21' C26' 1.376(14) . ? C21' C22' 1.408(13) . ? C22' C23' 1.390(14) . ? C22' C29' 1.507(14) . ? C23' C24' 1.39(2) . ? C24' C25' 1.390(14) . ? C24' C32' 1.531(14) . ? C25' C26' 1.397(13) . ? C26' C27' 1.487(13) . ? C27' O27' 1.237(12) . ? C27' O28' 1.285(12) . ? C29' C31' 1.50(2) . ? C29' C30' 1.506(15) . ? C32' C34' 1.521(10) . ? C32' C33' 1.525(10) . ? C32' C33B 1.526(10) . ? C32' C34B 1.529(10) . ? 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 O W O21 97.4(3) . . ? O W O1 99.2(4) . . ? O21 W O1 92.9(3) . . ? O W O8 100.9(3) . . ? O21 W O8 161.7(3) . . ? O1 W O8 84.1(3) . . ? O W O27 177.4(3) . . ? O21 W O27 80.0(3) . . ? O1 W O27 81.3(3) . . ? O8 W O27 81.7(3) . . ? O W Cl 96.6(3) . . ? O21 W Cl 92.6(2) . . ? O1 W Cl 162.5(3) . . ? O8 W Cl 85.5(2) . . ? O27 W Cl 83.3(2) . . ? C1 O1 W 135.3(6) . . ? O1 C1 C6 120.6(10) . . ? O1 C1 C2 117.6(10) . . ? C6 C1 C2 121.7(11) . . ? C3 C2 C1 117.7(11) . . ? C3 C2 C9 119.1(12) . . ? C1 C2 C9 123.1(12) . . ? C2 C3 C4 122.4(12) . . ? C5 C4 C3 118.6(13) . . ? C5 C4 C12 123.8(16) . . ? C3 C4 C12 117.4(14) . . ? C4 C5 C6 120.1(12) . . ? C1 C6 C5 119.4(11) . . ? C1 C6 C7 122.6(10) . . ? C5 C6 C7 118.0(10) . . ? O7 C7 O8 116.9(9) . . ? O7 C7 C6 123.0(9) . . ? O8 C7 C6 120.0(8) . . ? C7 O8 W 133.4(6) . . ? C2 C9 C10 114.1(13) . . ? C2 C9 C10A 122.5(19) . . ? C2 C9 C11 114.6(12) . . ? C10 C9 C11 112.6(12) . . ? C2 C9 C11A 113.1(31) . . ? C10A C9 C11A 110.7(15) . . ? C4 C12 C13A 124.6(21) . . ? C4 C12 C13 113.3(17) . . ? C4 C12 C14 114.7(18) . . ? C13 C12 C14 112.7(14) . . ? C4 C12 C14A 116.2(22) . . ? C13A C12 C14A 112.8(14) . . ? C21 O21 W 138.6(6) . . ? C26 C21 O21 121.7(8) . . ? C26 C21 C22 122.0(9) . . ? O21 C21 C22 116.3(9) . . ? C23 C22 C21 115.7(10) . . ? C23 C22 C29 125.2(9) . . ? C21 C22 C29 119.1(9) . . ? C24 C23 C22 124.1(9) . . ? C23 C24 C25 118.1(11) . . ? C23 C24 C32 125.1(11) . . ? C25 C24 C32 116.8(13) . . ? C24 C25 C26 120.4(12) . . ? C21 C26 C25 119.2(9) . . ? C21 C26 C27 121.1(9) . . ? C25 C26 C27 119.6(10) . . ? O27 C27 O28 120.1(9) . . ? O27 C27 C26 123.6(9) . . ? O28 C27 C26 116.2(9) . . ? C27 O27 W 131.0(6) . . ? C22 C29 C30 107.6(10) . . ? C22 C29 C31 113.2(10) . . ? C30 C29 C31 110.4(10) . . ? C24 C32 C34 113.9(14) . . ? C24 C32 C33 112.5(13) . . ? C34 C32 C33 112.0(13) . . ? C24 C32 C33A 116.8(25) . . ? C24 C32 C34A 108.4(21) . . ? C33A C32 C34A 108.3(14) . . ? O' W' O1' 95.9(4) . . ? O' W' O21' 97.2(3) . . ? O1' W' O21' 95.2(3) . . ? O' W' O8' 102.5(3) . . ? O1' W' O8' 83.3(3) . . ? O21' W' O8' 160.3(3) . . ? O' W' O27' 177.5(3) . . ? O1' W' O27' 84.6(3) . . ? O21' W' O27' 80.3(3) . . ? O8' W' O27' 80.0(3) . . ? O' W' Cl' 96.5(3) . . ? O1' W' Cl' 164.3(2) . . ? O21' W' Cl' 92.8(2) . . ? O8' W' Cl' 84.6(2) . . ? O27' W' Cl' 83.5(2) . . ? C1' O1' W' 135.9(7) . . ? C1B O1' W' 137.3(12) . . ? O1' C1' C6' 120.7(10) . . ? O1' C1' C2' 117.9(12) . . ? C6' C1' C2' 121.4(11) . . ? C3' C2' C1' 114.9(13) . . ? C3' C2' C9' 131.0(16) . . ? C1' C2' C9' 114.1(16) . . ? C4' C3' C2' 125.5(14) . . ? C3' C4' C5' 118.2(15) . . ? C3' C4' C12' 123.5(16) . . ? C5' C4' C12' 118.3(16) . . ? C4' C5' C6' 119.7(14) . . ? C1' C6' C5' 120.2(11) . . ? C1' C6' C7' 123.8(12) . . ? C5' C6' C7' 115.9(12) . . ? O7' C7' O8' 120.4(18) . . ? O7' C7' C6' 123.0(20) . . ? O8' C7' C6' 116.6(14) . . ? O1' C1B C6B 119.8(18) . . ? O1' C1B C2B 120.0(18) . . ? C6B C1B C2B 120.2(14) . . ? C3B C2B C1B 117.1(15) . . ? C3B C2B C9B 123.7(18) . . ? C1B C2B C9B 119.2(17) . . ? C4B C3B C2B 124.5(18) . . ? C3B C4B C5B 118.6(20) . . ? C3B C4B C12B 129.4(30) . . ? C5B C4B C12B 112.0(29) . . ? C4B C5B C6B 119.3(19) . . ? C1B C6B C5B 120.3(16) . . ? C1B C6B C7B 125.3(18) . . ? C5B C6B C7B 114.4(20) . . ? O7B C7B O8' 118.4(18) . . ? O7B C7B C6B 126.2(21) . . ? O8' C7B C6B 115.5(17) . . ? C7' O8' W' 135.2(8) . . ? C7B O8' W' 137.6(10) . . ? C11' C9' C10' 106.8(13) . . ? C11' C9' C2' 110.3(29) . . ? C10' C9' C2' 114.1(19) . . ? C14' C12' C13' 111.2(14) . . ? C14' C12' C4' 110.0(21) . . ? C13' C12' C4' 107.3(16) . . ? C2B C9B C11B 114.9(24) . . ? C2B C9B C10B 88.8(15) . . ? C11B C9B C10B 106.6(13) . . ? C14B C12B C13B 111.4(16) . . ? C14B C12B C4B 117.5(36) . . ? C13B C12B C4B 105.3(30) . . ? C21' O21' W' 140.5(6) . . ? O21' C21' C26' 121.1(8) . . ? O21' C21' C22' 116.2(8) . . ? C26' C21' C22' 122.7(8) . . ? C23' C22' C21' 116.6(10) . . ? C23' C22' C29' 122.5(9) . . ? C21' C22' C29' 120.9(8) . . ? C22' C23' C24' 122.7(10) . . ? C25' C24' C23' 118.1(9) . . ? C25' C24' C32' 120.3(10) . . ? C23' C24' C32' 121.5(10) . . ? C24' C25' C26' 121.5(9) . . ? C21' C26' C25' 118.3(9) . . ? C21' C26' C27' 122.6(9) . . ? C25' C26' C27' 119.1(9) . . ? O27' C27' O28' 122.1(9) . . ? O27' C27' C26' 122.5(9) . . ? O28' C27' C26' 115.4(9) . . ? C27' O27' W' 131.2(6) . . ? C31' C29' C30' 111.2(12) . . ? C31' C29' C22' 110.0(10) . . ? C30' C29' C22' 115.4(10) . . ? C34' C32' C33' 111.7(14) . . ? C33B C32' C34B 110.4(14) . . ? C34' C32' C24' 110.8(17) . . ? C33' C32' C24' 103.9(18) . . ? C33B C32' C24' 116.7(17) . . ? C34B C32' C24' 113.5(17) . . ? _refine_diff_density_max 0.707 _refine_diff_density_min -0.875 _refine_diff_density_rms 0.094 #===END