# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H18 O2 S' _chemical_formula_weight 286.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 5.6730(11) _cell_length_b 8.3677(17) _cell_length_c 31.795(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1509.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 3297 _cell_measurement_theta_min 2.5625 _cell_measurement_theta_max 27.8904 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 608 _exptl_absorpt_coefficient_mu 0.213 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9586 _exptl_absorpt_correction_T_max 0.9749 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'rigaku saturn' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7898 _diffrn_reflns_av_R_equivalents 0.1418 _diffrn_reflns_av_sigmaI/netI 0.0980 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.56 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2603 _reflns_number_gt 2424 _reflns_threshold_expression >2sigma(I) _computing_data_collection crystalclear _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+4.7392P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(2) _refine_ls_number_reflns 2603 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0925 _refine_ls_R_factor_gt 0.0834 _refine_ls_wR_factor_ref 0.1904 _refine_ls_wR_factor_gt 0.1875 _refine_ls_goodness_of_fit_ref 1.131 _refine_ls_restrained_S_all 1.131 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group S1 S -0.1030(2) 0.24471(15) 0.86802(4) 0.0250(3) Uani 1 1 d . . . O1 O -0.0912(8) -0.1972(4) 0.86617(12) 0.0368(10) Uani 1 1 d . . . C1 C -0.1525(10) 0.3525(7) 0.97236(17) 0.0289(13) Uani 1 1 d . . . H1 H -0.0119 0.2917 0.9751 0.035 Uiso 1 1 calc R . . C2 C -0.1916(11) 0.4805(7) 0.99906(17) 0.0318(13) Uani 1 1 d . . . H2 H -0.0786 0.5067 1.0200 0.038 Uiso 1 1 calc R . . C3 C -0.3944(12) 0.5698(7) 0.99526(19) 0.0385(14) Uani 1 1 d . . . H3 H -0.4218 0.6582 1.0134 0.046 Uiso 1 1 calc R . . C4 C -0.5568(12) 0.5294(9) 0.9650(2) 0.0490(18) Uani 1 1 d . . . H4 H -0.6975 0.5902 0.9624 0.059 Uiso 1 1 calc R . . C5 C -0.5186(10) 0.4015(7) 0.93815(19) 0.0336(13) Uani 1 1 d . . . H5 H -0.6325 0.3758 0.9173 0.040 Uiso 1 1 calc R . . C6 C -0.3170(9) 0.3118(6) 0.94156(15) 0.0236(11) Uani 1 1 d . . . C7 C -0.2709(10) 0.1700(6) 0.91293(16) 0.0248(11) Uani 1 1 d . . . H7A H -0.4217 0.1227 0.9034 0.030 Uiso 1 1 calc R . . H7B H -0.1799 0.0869 0.9280 0.030 Uiso 1 1 calc R . . C8 C -0.0627(9) 0.0600(6) 0.83897(15) 0.0224(11) Uani 1 1 d . . . H8 H -0.2197 0.0214 0.8289 0.027 Uiso 1 1 calc R . . C9 C 0.0954(10) 0.0912(5) 0.80104(15) 0.0212(10) Uani 1 1 d . . . C10 C 0.3089(10) 0.1748(6) 0.80495(16) 0.0250(11) Uani 1 1 d . . . H10 H 0.3568 0.2152 0.8315 0.030 Uiso 1 1 calc R . . C11 C 0.4481(10) 0.1980(6) 0.77016(17) 0.0278(12) Uani 1 1 d . . . H11 H 0.5914 0.2556 0.7731 0.033 Uiso 1 1 calc R . . C12 C 0.3858(10) 0.1397(6) 0.73080(17) 0.0279(12) Uani 1 1 d . . . C13 C 0.1746(9) 0.0572(6) 0.72727(16) 0.0246(12) Uani 1 1 d . . . H13 H 0.1276 0.0170 0.7006 0.029 Uiso 1 1 calc R . . C14 C 0.0311(9) 0.0324(6) 0.76190(16) 0.0237(11) Uani 1 1 d . . . H14 H -0.1121 -0.0252 0.7588 0.028 Uiso 1 1 calc R . . C15 C 0.5432(11) 0.1651(8) 0.69305(18) 0.0373(14) Uani 1 1 d . . . H15A H 0.5837 0.0615 0.6807 0.056 Uiso 1 1 calc R . . H15B H 0.6876 0.2200 0.7018 0.056 Uiso 1 1 calc R . . H15C H 0.4603 0.2304 0.6722 0.056 Uiso 1 1 calc R . . C16 C 0.0467(9) -0.0672(6) 0.86753(17) 0.0245(11) Uani 1 1 d . . . C17 C -0.0129(16) -0.3302(7) 0.8923(2) 0.057(2) Uani 1 1 d . . . H17A H -0.0192 -0.2989 0.9220 0.085 Uiso 1 1 calc R . . H17B H 0.1493 -0.3588 0.8848 0.085 Uiso 1 1 calc R . . H17C H -0.1162 -0.4224 0.8877 0.085 Uiso 1 1 calc R . . O2 O 0.2197(8) -0.0545(5) 0.88821(13) 0.0391(11) Uani 1 1 d . . . 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 S1 0.0318(7) 0.0121(6) 0.0312(6) 0.0002(5) 0.0055(5) -0.0003(6) O1 0.053(3) 0.0143(18) 0.043(2) 0.0049(16) -0.007(2) -0.0125(18) C1 0.030(3) 0.019(3) 0.038(3) 0.004(2) -0.002(2) 0.002(2) C2 0.034(3) 0.031(3) 0.031(3) -0.006(2) -0.006(2) -0.007(3) C3 0.034(3) 0.032(3) 0.050(3) -0.016(3) 0.004(3) -0.001(3) C4 0.033(4) 0.048(4) 0.065(4) -0.020(3) -0.008(3) 0.018(3) C5 0.018(3) 0.031(3) 0.051(3) -0.009(3) -0.007(3) 0.007(2) C6 0.024(3) 0.020(3) 0.028(2) -0.001(2) 0.005(2) -0.001(2) C7 0.028(3) 0.014(2) 0.033(3) 0.001(2) 0.005(2) -0.001(2) C8 0.021(3) 0.015(3) 0.031(2) -0.0009(19) -0.003(2) -0.001(2) C9 0.022(3) 0.009(2) 0.032(2) 0.0031(19) 0.001(2) 0.004(2) C10 0.028(3) 0.016(2) 0.031(3) 0.000(2) -0.006(2) 0.000(2) C11 0.024(3) 0.019(3) 0.040(3) 0.004(2) 0.001(2) 0.002(2) C12 0.022(3) 0.025(3) 0.037(3) 0.008(2) 0.001(2) 0.011(2) C13 0.024(3) 0.018(3) 0.032(3) -0.002(2) -0.005(2) 0.008(2) C14 0.017(3) 0.018(3) 0.036(3) -0.001(2) -0.005(2) 0.003(2) C15 0.036(4) 0.038(3) 0.038(3) 0.004(3) 0.002(3) 0.003(3) C16 0.025(3) 0.015(2) 0.033(2) -0.004(2) -0.002(2) 0.001(2) C17 0.108(7) 0.015(3) 0.048(4) 0.011(3) -0.013(4) 0.000(4) O2 0.036(3) 0.026(2) 0.055(2) 0.0075(19) -0.014(2) 0.005(2) _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 S1 C8 1.815(5) . ? S1 C7 1.827(5) . ? O1 C16 1.340(6) . ? O1 C17 1.459(7) . ? C1 C2 1.384(8) . ? C1 C6 1.395(8) . ? C1 H1 0.9500 . ? C2 C3 1.377(9) . ? C2 H2 0.9500 . ? C3 C4 1.375(9) . ? C3 H3 0.9500 . ? C4 C5 1.386(8) . ? C4 H4 0.9500 . ? C5 C6 1.373(8) . ? C5 H5 0.9500 . ? C6 C7 1.518(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.525(7) . ? C8 C16 1.531(7) . ? C8 H8 1.0000 . ? C9 C14 1.387(7) . ? C9 C10 1.404(7) . ? C10 C11 1.373(8) . ? C10 H10 0.9500 . ? C11 C12 1.389(8) . ? C11 H11 0.9500 . ? C12 C13 1.388(8) . ? C12 C15 1.511(8) . ? C13 C14 1.385(8) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 O2 1.186(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8 S1 C7 99.9(2) . . ? C16 O1 C17 115.0(5) . . ? C2 C1 C6 120.8(5) . . ? C2 C1 H1 119.6 . . ? C6 C1 H1 119.6 . . ? C3 C2 C1 120.0(5) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 119.2(6) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C3 C4 C5 121.1(6) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 120.3(6) . . ? C6 C5 H5 119.9 . . ? C4 C5 H5 119.9 . . ? C5 C6 C1 118.6(5) . . ? C5 C6 C7 121.6(5) . . ? C1 C6 C7 119.8(5) . . ? C6 C7 S1 106.9(3) . . ? C6 C7 H7A 110.3 . . ? S1 C7 H7A 110.3 . . ? C6 C7 H7B 110.3 . . ? S1 C7 H7B 110.3 . . ? H7A C7 H7B 108.6 . . ? C9 C8 C16 110.4(4) . . ? C9 C8 S1 109.3(3) . . ? C16 C8 S1 110.0(3) . . ? C9 C8 H8 109.0 . . ? C16 C8 H8 109.0 . . ? S1 C8 H8 109.0 . . ? C14 C9 C10 118.9(5) . . ? C14 C9 C8 119.6(5) . . ? C10 C9 C8 121.5(4) . . ? C11 C10 C9 119.7(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 122.0(5) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C13 C12 C11 117.9(5) . . ? C13 C12 C15 121.1(5) . . ? C11 C12 C15 121.1(5) . . ? C14 C13 C12 121.2(5) . . ? C14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C13 C14 C9 120.4(5) . . ? C13 C14 H14 119.8 . . ? C9 C14 H14 119.8 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 O1 125.0(5) . . ? O2 C16 C8 127.0(5) . . ? O1 C16 C8 108.0(4) . . ? O1 C17 H17A 109.5 . . ? O1 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O1 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.3(9) . . . . ? C1 C2 C3 C4 0.5(9) . . . . ? C2 C3 C4 C5 -0.5(11) . . . . ? C3 C4 C5 C6 0.4(11) . . . . ? C4 C5 C6 C1 -0.2(9) . . . . ? C4 C5 C6 C7 179.4(6) . . . . ? C2 C1 C6 C5 0.2(8) . . . . ? C2 C1 C6 C7 -179.4(5) . . . . ? C5 C6 C7 S1 92.3(6) . . . . ? C1 C6 C7 S1 -88.1(5) . . . . ? C8 S1 C7 C6 179.0(4) . . . . ? C7 S1 C8 C9 -175.0(4) . . . . ? C7 S1 C8 C16 -53.6(4) . . . . ? C16 C8 C9 C14 105.6(5) . . . . ? S1 C8 C9 C14 -133.2(4) . . . . ? C16 C8 C9 C10 -72.7(6) . . . . ? S1 C8 C9 C10 48.4(6) . . . . ? C14 C9 C10 C11 0.6(7) . . . . ? C8 C9 C10 C11 178.9(5) . . . . ? C9 C10 C11 C12 -0.6(8) . . . . ? C10 C11 C12 C13 0.5(8) . . . . ? C10 C11 C12 C15 -179.3(5) . . . . ? C11 C12 C13 C14 -0.5(7) . . . . ? C15 C12 C13 C14 179.4(5) . . . . ? C12 C13 C14 C9 0.5(8) . . . . ? C10 C9 C14 C13 -0.5(7) . . . . ? C8 C9 C14 C13 -178.9(5) . . . . ? C17 O1 C16 O2 -0.7(8) . . . . ? C17 O1 C16 C8 -179.3(5) . . . . ? C9 C8 C16 O2 68.5(7) . . . . ? S1 C8 C16 O2 -52.2(7) . . . . ? C9 C8 C16 O1 -113.0(5) . . . . ? S1 C8 C16 O1 126.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.505 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.081 _database_code_depnum_ccdc_archive 'CCDC 960974' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_r100723a1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H17 O5 P' _chemical_formula_weight 332.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.6316(13) _cell_length_b 9.2654(19) _cell_length_c 26.038(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1599.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3994 _cell_measurement_theta_min 1.564 _cell_measurement_theta_max 27.890 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 0.195 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.9621 _exptl_absorpt_correction_T_max 0.9884 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'rigaku saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_reflns_number 10910 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0400 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.02 _reflns_number_total 2807 _reflns_number_gt 2490 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'crystalclear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement crystalclear _computing_data_reduction crystalclear _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0618P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.104(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(10) _refine_ls_number_reflns 2807 _refine_ls_number_parameters 221 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0458 _refine_ls_R_factor_gt 0.0397 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.61018(10) -0.02428(7) 0.06186(2) 0.0439(2) Uani 1 1 d . . . O1 O 0.6121(3) -0.04908(15) 0.12236(5) 0.0392(4) Uani 1 1 d . . . O2 O 0.4870(3) 0.12038(17) 0.05382(6) 0.0435(4) Uani 1 1 d . . . O3 O 0.8259(3) 0.0008(2) 0.04740(8) 0.0625(5) Uani 1 1 d D . . H3 H 0.907(6) -0.078(3) 0.0442(19) 0.16(2) Uiso 1 1 d D . . O4 O 0.4931(3) -0.1378(2) 0.03507(7) 0.0574(6) Uani 1 1 d . . . C1 C 0.4229(4) -0.0746(2) 0.14547(8) 0.0363(5) Uani 1 1 d . . . C2 C 0.3559(5) -0.2149(2) 0.15049(10) 0.0501(7) Uani 1 1 d . . . H2 H 0.4376 -0.2917 0.1407 0.060 Uiso 1 1 calc R . . C3 C 0.1657(5) -0.2395(3) 0.17019(11) 0.0573(8) Uani 1 1 d . . . H3A H 0.1223 -0.3338 0.1753 0.069 Uiso 1 1 calc R . . C4 C 0.0405(5) -0.1281(3) 0.18232(10) 0.0569(8) Uani 1 1 d . . . H4 H -0.0895 -0.1463 0.1941 0.068 Uiso 1 1 calc R . . C5 C 0.1084(4) 0.0129(3) 0.17700(8) 0.0418(5) Uani 1 1 d . . . C6 C -0.0039(4) 0.1510(3) 0.18399(10) 0.0552(7) Uani 1 1 d . . . H6A H -0.0182 0.1748 0.2201 0.066 Uiso 1 1 calc R . . H6B H -0.1366 0.1461 0.1684 0.066 Uiso 1 1 calc R . . C7 C 0.1303(4) 0.2605(2) 0.15634(10) 0.0473(6) Uani 1 1 d . . . H7A H 0.1177 0.3552 0.1718 0.057 Uiso 1 1 calc R . . H7B H 0.0943 0.2672 0.1203 0.057 Uiso 1 1 calc R . . C8 C 0.3473(4) 0.2015(2) 0.16270(8) 0.0348(5) Uani 1 1 d . . . C9 C 0.3051(3) 0.0395(2) 0.16014(8) 0.0329(5) Uani 1 1 d . . . C10 C 0.4333(4) 0.2440(2) 0.21585(9) 0.0456(6) Uani 1 1 d . . . H10A H 0.3283 0.2433 0.2418 0.055 Uiso 1 1 calc R . . H10B H 0.5396 0.1782 0.2262 0.055 Uiso 1 1 calc R . . C11 C 0.5166(5) 0.3976(3) 0.20796(10) 0.0554(7) Uani 1 1 d . . . H11A H 0.4129 0.4698 0.2134 0.066 Uiso 1 1 calc R . . H11B H 0.6291 0.4168 0.2308 0.066 Uiso 1 1 calc R . . C12 C 0.5833(4) 0.3940(2) 0.15286(9) 0.0450(6) Uani 1 1 d . . . C13 C 0.7135(5) 0.4844(3) 0.12696(13) 0.0605(8) Uani 1 1 d . . . H13 H 0.7690 0.5636 0.1437 0.073 Uiso 1 1 calc R . . C14 C 0.7612(5) 0.4578(3) 0.07662(13) 0.0681(9) Uani 1 1 d . . . H14 H 0.8444 0.5215 0.0589 0.082 Uiso 1 1 calc R . . C15 C 0.6863(5) 0.3368(3) 0.05204(11) 0.0601(8) Uani 1 1 d . . . H15 H 0.7228 0.3163 0.0183 0.072 Uiso 1 1 calc R . . C16 C 0.5565(4) 0.2473(2) 0.07834(8) 0.0417(6) Uani 1 1 d . . . C17 C 0.4968(4) 0.2751(2) 0.12782(8) 0.0358(5) Uani 1 1 d . . . O5 O 0.0851(3) 0.8188(2) 0.03755(8) 0.0646(6) Uani 1 1 d D . . H5A H 0.061(5) 0.766(3) 0.0112(8) 0.090(11) Uiso 1 1 d D . . H5B H 0.204(3) 0.853(4) 0.0397(14) 0.126(17) Uiso 1 1 d D . . 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 P1 0.0304(4) 0.0549(4) 0.0465(4) -0.0191(3) 0.0029(3) 0.0009(3) O1 0.0294(9) 0.0430(8) 0.0453(9) -0.0098(6) -0.0046(7) 0.0070(7) O2 0.0399(10) 0.0556(10) 0.0351(8) -0.0074(7) -0.0039(7) 0.0076(8) O3 0.0340(11) 0.0763(13) 0.0771(13) -0.0197(11) 0.0158(8) 0.0006(11) O4 0.0429(12) 0.0657(12) 0.0635(11) -0.0361(9) 0.0022(8) -0.0034(9) C1 0.0317(13) 0.0394(12) 0.0377(11) 0.0002(9) -0.0073(9) 0.0013(10) C2 0.0538(19) 0.0350(12) 0.0615(16) 0.0034(11) -0.0108(13) 0.0016(13) C3 0.056(2) 0.0458(13) 0.0699(17) 0.0133(13) -0.0093(14) -0.0105(14) C4 0.0460(19) 0.0686(18) 0.0561(16) 0.0170(13) -0.0023(12) -0.0133(15) C5 0.0335(13) 0.0546(13) 0.0374(11) 0.0035(10) -0.0011(9) -0.0005(13) C6 0.0312(16) 0.0765(18) 0.0578(15) -0.0093(13) 0.0054(12) 0.0112(14) C7 0.0359(16) 0.0473(13) 0.0587(15) -0.0074(11) -0.0032(12) 0.0151(12) C8 0.0329(14) 0.0352(10) 0.0364(11) -0.0044(9) -0.0025(9) 0.0053(10) C9 0.0297(12) 0.0373(11) 0.0318(11) -0.0004(9) -0.0028(8) 0.0031(10) C10 0.0452(16) 0.0499(13) 0.0417(12) -0.0103(10) -0.0038(10) 0.0066(12) C11 0.0594(19) 0.0451(13) 0.0617(16) -0.0193(13) -0.0137(13) 0.0080(14) C12 0.0434(16) 0.0310(11) 0.0605(15) -0.0030(10) -0.0132(12) 0.0056(12) C13 0.0492(17) 0.0338(13) 0.099(2) 0.0064(14) -0.0124(15) -0.0042(13) C14 0.052(2) 0.0542(16) 0.098(2) 0.0297(16) 0.0101(16) -0.0039(14) C15 0.058(2) 0.0644(16) 0.0580(16) 0.0196(13) 0.0096(13) 0.0055(15) C16 0.0401(15) 0.0439(13) 0.0411(13) 0.0055(10) -0.0017(9) 0.0037(11) C17 0.0321(13) 0.0329(11) 0.0423(12) 0.0022(9) -0.0023(10) 0.0070(10) O5 0.0431(13) 0.0789(14) 0.0717(13) -0.0390(11) -0.0056(10) -0.0005(12) _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 P1 O4 1.4818(18) . ? P1 O3 1.4974(19) . ? P1 O2 1.5835(17) . ? P1 O1 1.5919(16) . ? O1 C1 1.411(3) . ? O2 C16 1.415(3) . ? O3 H3 0.912(10) . ? C1 C9 1.369(3) . ? C1 C2 1.381(3) . ? C2 C3 1.381(4) . ? C2 H2 0.9300 . ? C3 C4 1.362(4) . ? C3 H3A 0.9300 . ? C4 C5 1.389(3) . ? C4 H4 0.9300 . ? C5 C9 1.398(3) . ? C5 C6 1.491(4) . ? C6 C7 1.529(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.549(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C17 1.507(3) . ? C8 C9 1.528(3) . ? C8 C10 1.548(3) . ? C10 C11 1.540(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.502(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.379(4) . ? C12 C17 1.403(3) . ? C13 C14 1.371(4) . ? C13 H13 0.9300 . ? C14 C15 1.383(4) . ? C14 H14 0.9300 . ? C15 C16 1.378(4) . ? C15 H15 0.9300 . ? C16 C17 1.372(3) . ? O5 H5A 0.855(10) . ? O5 H5B 0.853(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 O4 P1 O3 119.49(11) . . ? O4 P1 O2 105.55(10) . . ? O3 P1 O2 109.17(11) . . ? O4 P1 O1 111.57(10) . . ? O3 P1 O1 105.29(11) . . ? O2 P1 O1 104.90(8) . . ? C1 O1 P1 116.05(14) . . ? C16 O2 P1 118.39(14) . . ? P1 O3 H3 117(3) . . ? C9 C1 C2 121.1(2) . . ? C9 C1 O1 119.82(18) . . ? C2 C1 O1 119.0(2) . . ? C3 C2 C1 119.0(3) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 121.2(2) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 119.5(3) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C9 120.0(2) . . ? C4 C5 C6 129.3(2) . . ? C9 C5 C6 110.7(2) . . ? C5 C6 C7 102.8(2) . . ? C5 C6 H6A 111.2 . . ? C7 C6 H6A 111.2 . . ? C5 C6 H6B 111.2 . . ? C7 C6 H6B 111.2 . . ? H6A C6 H6B 109.1 . . ? C6 C7 C8 104.87(19) . . ? C6 C7 H7A 110.8 . . ? C8 C7 H7A 110.8 . . ? C6 C7 H7B 110.8 . . ? C8 C7 H7B 110.8 . . ? H7A C7 H7B 108.8 . . ? C17 C8 C9 122.58(18) . . ? C17 C8 C10 100.44(18) . . ? C9 C8 C10 110.88(17) . . ? C17 C8 C7 112.78(18) . . ? C9 C8 C7 99.88(18) . . ? C10 C8 C7 110.38(18) . . ? C1 C9 C5 119.0(2) . . ? C1 C9 C8 131.7(2) . . ? C5 C9 C8 109.3(2) . . ? C11 C10 C8 104.37(19) . . ? C11 C10 H10A 110.9 . . ? C8 C10 H10A 110.9 . . ? C11 C10 H10B 110.9 . . ? C8 C10 H10B 110.9 . . ? H10A C10 H10B 108.9 . . ? C12 C11 C10 102.27(19) . . ? C12 C11 H11A 111.3 . . ? C10 C11 H11A 111.3 . . ? C12 C11 H11B 111.3 . . ? C10 C11 H11B 111.3 . . ? H11A C11 H11B 109.2 . . ? C13 C12 C17 120.4(2) . . ? C13 C12 C11 129.7(2) . . ? C17 C12 C11 109.9(2) . . ? C14 C13 C12 120.2(2) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 120.3(3) . . ? C13 C14 H14 119.8 . . ? C15 C14 H14 119.8 . . ? C16 C15 C14 118.9(3) . . ? C16 C15 H15 120.6 . . ? C14 C15 H15 120.6 . . ? C17 C16 C15 122.3(2) . . ? C17 C16 O2 119.1(2) . . ? C15 C16 O2 118.7(2) . . ? C16 C17 C12 117.8(2) . . ? C16 C17 C8 132.1(2) . . ? C12 C17 C8 110.13(19) . . ? H5A O5 H5B 115.9(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 P1 O1 C1 -49.28(16) . . . . ? O3 P1 O1 C1 179.67(15) . . . . ? O2 P1 O1 C1 64.52(15) . . . . ? O4 P1 O2 C16 175.89(16) . . . . ? O3 P1 O2 C16 -54.50(18) . . . . ? O1 P1 O2 C16 57.92(18) . . . . ? P1 O1 C1 C9 -85.7(2) . . . . ? P1 O1 C1 C2 91.0(2) . . . . ? C9 C1 C2 C3 0.7(4) . . . . ? O1 C1 C2 C3 -176.1(2) . . . . ? C1 C2 C3 C4 3.2(4) . . . . ? C2 C3 C4 C5 -3.0(4) . . . . ? C3 C4 C5 C9 -1.1(4) . . . . ? C3 C4 C5 C6 175.0(2) . . . . ? C4 C5 C6 C7 -162.4(2) . . . . ? C9 C5 C6 C7 14.0(3) . . . . ? C5 C6 C7 C8 -30.7(2) . . . . ? C6 C7 C8 C17 166.61(18) . . . . ? C6 C7 C8 C9 34.8(2) . . . . ? C6 C7 C8 C10 -81.9(2) . . . . ? C2 C1 C9 C5 -4.6(3) . . . . ? O1 C1 C9 C5 172.08(19) . . . . ? C2 C1 C9 C8 174.6(2) . . . . ? O1 C1 C9 C8 -8.8(3) . . . . ? C4 C5 C9 C1 4.8(3) . . . . ? C6 C5 C9 C1 -171.9(2) . . . . ? C4 C5 C9 C8 -174.5(2) . . . . ? C6 C5 C9 C8 8.7(2) . . . . ? C17 C8 C9 C1 28.4(4) . . . . ? C10 C8 C9 C1 -89.9(3) . . . . ? C7 C8 C9 C1 153.7(2) . . . . ? C17 C8 C9 C5 -152.3(2) . . . . ? C10 C8 C9 C5 89.4(2) . . . . ? C7 C8 C9 C5 -27.0(2) . . . . ? C17 C8 C10 C11 35.1(2) . . . . ? C9 C8 C10 C11 166.2(2) . . . . ? C7 C8 C10 C11 -84.1(2) . . . . ? C8 C10 C11 C12 -31.8(2) . . . . ? C10 C11 C12 C13 -161.9(3) . . . . ? C10 C11 C12 C17 16.0(3) . . . . ? C17 C12 C13 C14 -0.7(4) . . . . ? C11 C12 C13 C14 177.1(3) . . . . ? C12 C13 C14 C15 -2.8(4) . . . . ? C13 C14 C15 C16 2.7(4) . . . . ? C14 C15 C16 C17 1.0(4) . . . . ? C14 C15 C16 O2 -177.3(2) . . . . ? P1 O2 C16 C17 -86.5(2) . . . . ? P1 O2 C16 C15 91.9(2) . . . . ? C15 C16 C17 C12 -4.3(4) . . . . ? O2 C16 C17 C12 173.9(2) . . . . ? C15 C16 C17 C8 174.7(2) . . . . ? O2 C16 C17 C8 -7.0(4) . . . . ? C13 C12 C17 C16 4.2(3) . . . . ? C11 C12 C17 C16 -174.0(2) . . . . ? C13 C12 C17 C8 -175.1(2) . . . . ? C11 C12 C17 C8 6.7(3) . . . . ? C9 C8 C17 C16 31.4(4) . . . . ? C10 C8 C17 C16 154.7(2) . . . . ? C7 C8 C17 C16 -87.9(3) . . . . ? C9 C8 C17 C12 -149.4(2) . . . . ? C10 C8 C17 C12 -26.2(2) . . . . ? C7 C8 C17 C12 91.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.248 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.053 _database_code_depnum_ccdc_archive 'CCDC 960975' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H25 O5 P' _chemical_formula_sum 'C29 H25 O5 P' _chemical_formula_weight 484.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_H-M_alt 'C 2' _space_group_name_Hall 'C 2y' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 25.330(4) _cell_length_b 6.6640(8) _cell_length_c 16.090(2) _cell_angle_alpha 90 _cell_angle_beta 121.291(16) _cell_angle_gamma 90 _cell_volume 2320.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 3570 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 28.10 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.386 _exptl_crystal_F_000 1016 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.120 _exptl_absorpt_coefficient_mu 0.159 _shelx_estimated_absorpt_T_min 0.975 _shelx_estimated_absorpt_T_max 0.981 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.679 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.222 _diffrn_reflns_number 10436 _diffrn_reflns_av_unetI/netI 0.0920 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.481 _diffrn_reflns_theta_max 28.160 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.982 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.982 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.810 _diffrn_reflns_point_group_measured_fraction_full 0.852 _reflns_number_total 4627 _reflns_number_gt 3636 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.522 _reflns_Friedel_fraction_max 0.607 _reflns_Friedel_fraction_full 0.674 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _refine_special_details ; ENTER TEXT OF LETTER ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0582P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0069(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details ; Flack x determined using 796 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack -0.05(13) _chemical_absolute_configuration ? _refine_ls_number_reflns 4627 _refine_ls_number_parameters 326 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0814 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1415 _refine_ls_wR_factor_gt 0.1290 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.78282(5) 0.42323(18) 0.69212(8) 0.0274(3) Uani 1 1 d . . . . . O1 O 0.75939(14) 0.5352(5) 0.7545(2) 0.0281(7) Uani 1 1 d . . . . . O2 O 0.85617(13) 0.4154(5) 0.75994(19) 0.0255(6) Uani 1 1 d . . . . . O3 O 0.76339(16) 0.2077(5) 0.6826(2) 0.0341(8) Uani 1 1 d . . . . . H3 H 0.7692 0.1504 0.6415 0.051 Uiso 1 1 calc R U . . . O4 O 0.76203(15) 0.5448(5) 0.6041(2) 0.0319(8) Uani 1 1 d . . . . . O5 O 0.77446(17) 0.9539(6) 0.5836(2) 0.0352(8) Uani 1 1 d . . . . . C1 C 0.8805(2) 0.6470(7) 0.9393(3) 0.0254(10) Uani 1 1 d . . . . . C2 C 0.8315(2) 0.4980(6) 0.9249(3) 0.0236(9) Uani 1 1 d . . . . . C3 C 0.7742(2) 0.4554(7) 0.8454(3) 0.0249(9) Uani 1 1 d . . . . . C4 C 0.7312(2) 0.3385(7) 0.8524(3) 0.0266(10) Uani 1 1 d . . . . . C5 C 0.7507(2) 0.2488(7) 0.9427(3) 0.0278(10) Uani 1 1 d . . . . . H5 H 0.7225 0.1676 0.9499 0.033 Uiso 1 1 calc R U . . . C6 C 0.8098(2) 0.2754(7) 1.0213(3) 0.0296(10) Uani 1 1 d . . . . . H6 H 0.8226 0.2075 1.0808 0.035 Uiso 1 1 calc R U . . . C7 C 0.8503(2) 0.4017(7) 1.0130(3) 0.0261(9) Uani 1 1 d . . . . . C8 C 0.9158(2) 0.4543(7) 1.0882(3) 0.0288(10) Uani 1 1 d . . . . . H8A H 0.9401 0.3331 1.1221 0.035 Uiso 1 1 calc R U . . . H8B H 0.9176 0.5498 1.1367 0.035 Uiso 1 1 calc R U . . . C9 C 0.9389(2) 0.5510(7) 1.0266(3) 0.0272(10) Uani 1 1 d . . . . . H9A H 0.9570 0.4489 1.0039 0.033 Uiso 1 1 calc R U . . . H9B H 0.9705 0.6545 1.0643 0.033 Uiso 1 1 calc R U . . . C10 C 0.8927(2) 0.7097(7) 0.8603(3) 0.0252(9) Uani 1 1 d . . . . . C11 C 0.8868(2) 0.6014(6) 0.7823(3) 0.0241(9) Uani 1 1 d . . . . . C12 C 0.9086(2) 0.6777(7) 0.7247(3) 0.0254(10) Uani 1 1 d . . . . . C13 C 0.9346(2) 0.8686(7) 0.7472(3) 0.0277(10) Uani 1 1 d . . . . . H13 H 0.9512 0.9220 0.7107 0.033 Uiso 1 1 calc R U . . . C14 C 0.9373(2) 0.9827(7) 0.8206(3) 0.0301(11) Uani 1 1 d . . . . . H14 H 0.9540 1.1144 0.8328 0.036 Uiso 1 1 calc R U . . . C15 C 0.9152(2) 0.9032(7) 0.8761(3) 0.0269(9) Uani 1 1 d . . . . . C16 C 0.9100(2) 1.0005(7) 0.9553(3) 0.0314(11) Uani 1 1 d . . . . . H16A H 0.8910 1.1352 0.9354 0.038 Uiso 1 1 calc R U . . . H16B H 0.9510 1.0129 1.0156 0.038 Uiso 1 1 calc R U . . . C17 C 0.8684(2) 0.8561(7) 0.9691(3) 0.0312(11) Uani 1 1 d . . . . . H17A H 0.8245 0.8947 0.9272 0.037 Uiso 1 1 calc R U . . . H17B H 0.8792 0.8553 1.0377 0.037 Uiso 1 1 calc R U . . . C18 C 0.6665(2) 0.3119(8) 0.7713(3) 0.0309(11) Uani 1 1 d . . . . . C19 C 0.6382(2) 0.1265(9) 0.7568(3) 0.0374(12) Uani 1 1 d . . . . . H19 H 0.6616 0.0143 0.7943 0.045 Uiso 1 1 calc R U . . . C20 C 0.5756(3) 0.1038(10) 0.6876(4) 0.0468(16) Uani 1 1 d . . . . . H20 H 0.5564 -0.0234 0.6784 0.056 Uiso 1 1 calc R U . . . C21 C 0.5417(3) 0.2653(11) 0.6327(4) 0.0493(16) Uani 1 1 d . . . . . H21 H 0.4990 0.2501 0.5858 0.059 Uiso 1 1 calc R U . . . C22 C 0.5697(2) 0.4486(11) 0.6457(4) 0.0466(14) Uani 1 1 d . . . . . H22 H 0.5463 0.5598 0.6071 0.056 Uiso 1 1 calc R U . . . C23 C 0.6320(2) 0.4724(8) 0.7150(4) 0.0387(12) Uani 1 1 d . . . . . H23 H 0.6509 0.5999 0.7237 0.046 Uiso 1 1 calc R U . . . C24 C 0.9018(2) 0.5700(7) 0.6394(3) 0.0277(10) Uani 1 1 d . . . . . C25 C 0.9197(3) 0.3723(7) 0.6443(3) 0.0359(12) Uani 1 1 d . . . . . H25 H 0.9360 0.3009 0.7038 0.043 Uiso 1 1 calc R U . . . C26 C 0.9142(3) 0.2767(8) 0.5637(4) 0.0412(13) Uani 1 1 d . . . . . H26 H 0.9263 0.1404 0.5678 0.049 Uiso 1 1 calc R U . . . C27 C 0.8910(3) 0.3806(8) 0.4777(3) 0.0385(13) Uani 1 1 d . . . . . H27 H 0.8870 0.3157 0.4221 0.046 Uiso 1 1 calc R U . . . C28 C 0.8738(2) 0.5772(8) 0.4722(3) 0.0361(12) Uani 1 1 d . . . . . H28 H 0.8587 0.6488 0.4130 0.043 Uiso 1 1 calc R U . . . C29 C 0.8783(2) 0.6726(8) 0.5518(3) 0.0299(10) Uani 1 1 d . . . . . H29 H 0.8654 0.8082 0.5468 0.036 Uiso 1 1 calc R U . . . H1 H 0.759(3) 0.819(12) 0.585(5) 0.07(2) Uiso 1 1 d . . . . . H2 H 0.761(3) 0.982(10) 0.529(4) 0.06(2) Uiso 1 1 d . . . . . 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 P1 0.0278(6) 0.0297(6) 0.0255(5) -0.0011(5) 0.0144(5) -0.0037(5) O1 0.0276(18) 0.0338(19) 0.0256(15) 0.0026(13) 0.0158(14) -0.0006(14) O2 0.0247(16) 0.0269(16) 0.0263(14) -0.0012(14) 0.0142(12) -0.0038(14) O3 0.037(2) 0.035(2) 0.0364(19) -0.0096(15) 0.0228(16) -0.0090(16) O4 0.0321(19) 0.040(2) 0.0235(15) 0.0020(13) 0.0141(14) -0.0022(15) O5 0.041(2) 0.036(2) 0.0298(18) -0.0015(16) 0.0189(16) 0.0018(17) C1 0.027(2) 0.024(2) 0.028(2) -0.0002(18) 0.017(2) -0.0026(18) C2 0.028(2) 0.021(2) 0.026(2) -0.0026(17) 0.0172(19) 0.0004(17) C3 0.030(2) 0.025(3) 0.0247(19) -0.0012(17) 0.0174(18) 0.0013(18) C4 0.027(2) 0.031(3) 0.028(2) -0.0028(18) 0.018(2) -0.0018(19) C5 0.030(3) 0.023(2) 0.034(2) -0.0012(18) 0.019(2) -0.0033(19) C6 0.034(3) 0.028(3) 0.027(2) 0.0017(18) 0.016(2) -0.0012(19) C7 0.028(2) 0.025(2) 0.028(2) -0.0016(19) 0.0165(18) 0.0028(19) C8 0.027(2) 0.035(3) 0.026(2) -0.0001(19) 0.0142(18) 0.001(2) C9 0.021(2) 0.031(3) 0.029(2) 0.0000(19) 0.0125(19) -0.0019(19) C10 0.025(2) 0.024(2) 0.027(2) -0.0018(18) 0.0141(18) -0.0008(18) C11 0.023(2) 0.022(2) 0.026(2) 0.0003(17) 0.0112(19) -0.0025(17) C12 0.024(2) 0.026(2) 0.028(2) 0.0016(18) 0.0144(19) 0.0020(18) C13 0.028(3) 0.028(3) 0.026(2) 0.0035(17) 0.0139(19) 0.0009(18) C14 0.034(3) 0.022(2) 0.034(2) 0.0029(18) 0.017(2) -0.0007(19) C15 0.023(2) 0.027(2) 0.029(2) -0.0023(19) 0.0116(17) 0.0008(19) C16 0.039(3) 0.022(2) 0.032(2) -0.0033(18) 0.017(2) 0.000(2) C17 0.033(3) 0.028(3) 0.036(2) -0.0052(19) 0.020(2) -0.003(2) C18 0.032(3) 0.041(3) 0.025(2) -0.006(2) 0.018(2) -0.007(2) C19 0.044(3) 0.048(3) 0.026(2) -0.007(2) 0.022(2) -0.015(3) C20 0.043(3) 0.071(4) 0.031(3) -0.020(3) 0.023(3) -0.030(3) C21 0.024(3) 0.086(5) 0.039(3) -0.011(3) 0.018(2) -0.016(3) C22 0.025(3) 0.077(4) 0.033(2) 0.001(3) 0.012(2) 0.001(3) C23 0.033(3) 0.045(3) 0.038(3) -0.003(2) 0.019(2) -0.002(2) C24 0.023(2) 0.032(3) 0.032(2) 0.0024(19) 0.017(2) -0.0027(19) C25 0.053(3) 0.029(3) 0.036(3) 0.005(2) 0.031(3) 0.006(2) C26 0.062(4) 0.031(3) 0.044(3) -0.002(2) 0.037(3) 0.000(3) C27 0.051(3) 0.043(4) 0.031(2) -0.008(2) 0.028(2) -0.005(2) C28 0.034(3) 0.050(3) 0.029(2) 0.006(2) 0.020(2) 0.007(2) C29 0.025(2) 0.038(3) 0.027(2) 0.0061(19) 0.0141(19) 0.005(2) _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 P1 O4 1.471(3) . ? P1 O3 1.500(4) . ? P1 O1 1.592(3) . ? P1 O2 1.593(3) . ? O1 C3 1.413(5) . ? O2 C11 1.406(5) . ? O3 H3 0.8400 . ? O5 H1 0.98(7) . ? O5 H2 0.79(6) . ? C1 C2 1.510(6) . ? C1 C10 1.514(6) . ? C1 C9 1.553(6) . ? C1 C17 1.556(6) . ? C2 C3 1.377(6) . ? C2 C7 1.396(6) . ? C3 C4 1.389(6) . ? C4 C5 1.402(6) . ? C4 C18 1.484(6) . ? C5 C6 1.380(6) . ? C5 H5 0.9500 . ? C6 C7 1.387(6) . ? C6 H6 0.9500 . ? C7 C8 1.501(6) . ? C8 C9 1.531(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C15 1.379(6) . ? C10 C11 1.386(6) . ? C11 C12 1.399(6) . ? C12 C13 1.392(6) . ? C12 C24 1.477(6) . ? C13 C14 1.376(6) . ? C13 H13 0.9500 . ? C14 C15 1.383(6) . ? C14 H14 0.9500 . ? C15 C16 1.494(6) . ? C16 C17 1.527(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.380(7) . ? C18 C19 1.386(7) . ? C19 C20 1.393(7) . ? C19 H19 0.9500 . ? C20 C21 1.374(9) . ? C20 H20 0.9500 . ? C21 C22 1.373(9) . ? C21 H21 0.9500 . ? C22 C23 1.390(7) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.382(7) . ? C24 C29 1.392(6) . ? C25 C26 1.384(6) . ? C25 H25 0.9500 . ? C26 C27 1.377(7) . ? C26 H26 0.9500 . ? C27 C28 1.369(7) . ? C27 H27 0.9500 . ? C28 C29 1.381(6) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? 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 O4 P1 O3 119.6(2) . . ? O4 P1 O1 106.52(18) . . ? O3 P1 O1 107.63(18) . . ? O4 P1 O2 112.60(17) . . ? O3 P1 O2 104.0(2) . . ? O1 P1 O2 105.51(16) . . ? C3 O1 P1 119.4(3) . . ? C11 O2 P1 116.0(3) . . ? P1 O3 H3 109.5 . . ? H1 O5 H2 107(6) . . ? C2 C1 C10 124.2(4) . . ? C2 C1 C9 100.9(3) . . ? C10 C1 C9 111.1(4) . . ? C2 C1 C17 111.0(4) . . ? C10 C1 C17 99.8(3) . . ? C9 C1 C17 109.8(4) . . ? C3 C2 C7 119.2(4) . . ? C3 C2 C1 131.7(4) . . ? C7 C2 C1 109.0(4) . . ? C2 C3 C4 122.2(4) . . ? C2 C3 O1 117.9(4) . . ? C4 C3 O1 119.8(4) . . ? C3 C4 C5 117.0(4) . . ? C3 C4 C18 123.4(4) . . ? C5 C4 C18 119.6(4) . . ? C6 C5 C4 121.7(4) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 119.6(4) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 119.9(4) . . ? C6 C7 C8 128.9(4) . . ? C2 C7 C8 111.3(4) . . ? C7 C8 C9 102.1(3) . . ? C7 C8 H8A 111.3 . . ? C9 C8 H8A 111.3 . . ? C7 C8 H8B 111.3 . . ? C9 C8 H8B 111.3 . . ? H8A C8 H8B 109.2 . . ? C8 C9 C1 104.7(4) . . ? C8 C9 H9A 110.8 . . ? C1 C9 H9A 110.8 . . ? C8 C9 H9B 110.8 . . ? C1 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? C15 C10 C11 119.6(4) . . ? C15 C10 C1 110.4(4) . . ? C11 C10 C1 130.0(4) . . ? C10 C11 C12 121.1(4) . . ? C10 C11 O2 118.5(4) . . ? C12 C11 O2 120.3(4) . . ? C13 C12 C11 117.1(4) . . ? C13 C12 C24 119.8(4) . . ? C11 C12 C24 123.0(4) . . ? C14 C13 C12 122.3(4) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 119.2(4) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C10 C15 C14 120.4(4) . . ? C10 C15 C16 110.6(4) . . ? C14 C15 C16 129.0(4) . . ? C15 C16 C17 102.9(4) . . ? C15 C16 H16A 111.2 . . ? C17 C16 H16A 111.2 . . ? C15 C16 H16B 111.2 . . ? C17 C16 H16B 111.2 . . ? H16A C16 H16B 109.1 . . ? C16 C17 C1 104.9(4) . . ? C16 C17 H17A 110.8 . . ? C1 C17 H17A 110.8 . . ? C16 C17 H17B 110.8 . . ? C1 C17 H17B 110.8 . . ? H17A C17 H17B 108.8 . . ? C23 C18 C19 119.0(5) . . ? C23 C18 C4 121.2(5) . . ? C19 C18 C4 119.5(5) . . ? C18 C19 C20 120.3(5) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C21 C20 C19 120.1(6) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.0 . . ? C22 C21 C20 119.9(5) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 120.3(6) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C18 C23 C22 120.4(5) . . ? C18 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C25 C24 C29 118.7(4) . . ? C25 C24 C12 122.3(4) . . ? C29 C24 C12 119.0(4) . . ? C24 C25 C26 121.0(4) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C27 C26 C25 119.6(5) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C28 C27 C26 120.1(5) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 120.6(5) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C28 C29 C24 120.0(5) . . ? C28 C29 H29 120.0 . . ? C24 C29 H29 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 P1 O1 C3 -178.2(3) . . . . ? O3 P1 O1 C3 52.3(4) . . . . ? O2 P1 O1 C3 -58.3(3) . . . . ? O4 P1 O2 C11 50.0(3) . . . . ? O3 P1 O2 C11 -178.9(3) . . . . ? O1 P1 O2 C11 -65.8(3) . . . . ? C10 C1 C2 C3 -32.8(7) . . . . ? C9 C1 C2 C3 -157.8(5) . . . . ? C17 C1 C2 C3 85.9(6) . . . . ? C10 C1 C2 C7 151.3(4) . . . . ? C9 C1 C2 C7 26.3(4) . . . . ? C17 C1 C2 C7 -90.0(4) . . . . ? C7 C2 C3 C4 8.0(7) . . . . ? C1 C2 C3 C4 -167.6(4) . . . . ? C7 C2 C3 O1 -172.3(4) . . . . ? C1 C2 C3 O1 12.2(7) . . . . ? P1 O1 C3 C2 82.0(4) . . . . ? P1 O1 C3 C4 -98.2(4) . . . . ? C2 C3 C4 C5 -5.9(7) . . . . ? O1 C3 C4 C5 174.3(4) . . . . ? C2 C3 C4 C18 171.7(4) . . . . ? O1 C3 C4 C18 -8.0(7) . . . . ? C3 C4 C5 C6 0.2(7) . . . . ? C18 C4 C5 C6 -177.5(4) . . . . ? C4 C5 C6 C7 3.3(7) . . . . ? C5 C6 C7 C2 -1.2(7) . . . . ? C5 C6 C7 C8 179.4(4) . . . . ? C3 C2 C7 C6 -4.2(6) . . . . ? C1 C2 C7 C6 172.2(4) . . . . ? C3 C2 C7 C8 175.2(4) . . . . ? C1 C2 C7 C8 -8.3(5) . . . . ? C6 C7 C8 C9 165.5(5) . . . . ? C2 C7 C8 C9 -13.9(5) . . . . ? C7 C8 C9 C1 29.7(4) . . . . ? C2 C1 C9 C8 -34.2(4) . . . . ? C10 C1 C9 C8 -167.6(4) . . . . ? C17 C1 C9 C8 83.0(4) . . . . ? C2 C1 C10 C15 150.6(4) . . . . ? C9 C1 C10 C15 -89.0(5) . . . . ? C17 C1 C10 C15 26.8(5) . . . . ? C2 C1 C10 C11 -32.3(7) . . . . ? C9 C1 C10 C11 88.1(6) . . . . ? C17 C1 C10 C11 -156.1(5) . . . . ? C15 C10 C11 C12 6.0(7) . . . . ? C1 C10 C11 C12 -170.9(4) . . . . ? C15 C10 C11 O2 -171.6(4) . . . . ? C1 C10 C11 O2 11.5(7) . . . . ? P1 O2 C11 C10 85.1(4) . . . . ? P1 O2 C11 C12 -92.5(4) . . . . ? C10 C11 C12 C13 -1.9(7) . . . . ? O2 C11 C12 C13 175.7(4) . . . . ? C10 C11 C12 C24 -178.3(4) . . . . ? O2 C11 C12 C24 -0.7(6) . . . . ? C11 C12 C13 C14 -2.3(7) . . . . ? C24 C12 C13 C14 174.3(4) . . . . ? C12 C13 C14 C15 2.2(7) . . . . ? C11 C10 C15 C14 -6.1(7) . . . . ? C1 C10 C15 C14 171.4(4) . . . . ? C11 C10 C15 C16 172.7(4) . . . . ? C1 C10 C15 C16 -9.9(5) . . . . ? C13 C14 C15 C10 2.0(7) . . . . ? C13 C14 C15 C16 -176.4(4) . . . . ? C10 C15 C16 C17 -12.1(5) . . . . ? C14 C15 C16 C17 166.5(5) . . . . ? C15 C16 C17 C1 28.5(5) . . . . ? C2 C1 C17 C16 -165.7(4) . . . . ? C10 C1 C17 C16 -33.1(5) . . . . ? C9 C1 C17 C16 83.6(4) . . . . ? C3 C4 C18 C23 -43.6(7) . . . . ? C5 C4 C18 C23 134.0(5) . . . . ? C3 C4 C18 C19 142.1(5) . . . . ? C5 C4 C18 C19 -40.4(6) . . . . ? C23 C18 C19 C20 -1.1(7) . . . . ? C4 C18 C19 C20 173.4(4) . . . . ? C18 C19 C20 C21 0.5(7) . . . . ? C19 C20 C21 C22 0.4(8) . . . . ? C20 C21 C22 C23 -0.8(8) . . . . ? C19 C18 C23 C22 0.7(7) . . . . ? C4 C18 C23 C22 -173.6(4) . . . . ? C21 C22 C23 C18 0.2(8) . . . . ? C13 C12 C24 C25 132.3(5) . . . . ? C11 C12 C24 C25 -51.3(7) . . . . ? C13 C12 C24 C29 -45.6(6) . . . . ? C11 C12 C24 C29 130.7(5) . . . . ? C29 C24 C25 C26 -0.4(7) . . . . ? C12 C24 C25 C26 -178.4(5) . . . . ? C24 C25 C26 C27 0.6(8) . . . . ? C25 C26 C27 C28 0.3(8) . . . . ? C26 C27 C28 C29 -1.2(8) . . . . ? C27 C28 C29 C24 1.4(7) . . . . ? C25 C24 C29 C28 -0.6(7) . . . . ? C12 C24 C29 C28 177.5(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O3 H3 O5 0.84 1.65 2.438(5) 154.5 1_545 O5 H1 O4 0.98(7) 1.85(8) 2.783(5) 158(6) . O5 H2 O4 0.79(6) 1.95(6) 2.728(5) 173(7) 4_656 _refine_diff_density_max 0.276 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.076 _shelxl_version_number 2013-2 _shelx_res_file ; TITL _m130503b CELL 0.71075 25.33000 6.66400 16.09000 90.000 121.291 90.000 ZERR 4 0.00400 0.00080 0.00200 0.000 0.016 0.000 LATT -7 SYMM -X, +Y, -Z SFAC C H O P UNIT 116 100 20 4 L.S. 5 ACTA BOND $H FMAP 2 PLAN 5 LIST 4 SIZE 0.160 0.140 0.120 CONF HTAB EQIV $1 x, y-1, z HTAB O3 O5_$1 HTAB O5 O4 EQIV $2 -x+3/2, y+1/2, -z+1 HTAB O5 O4_$2 WPDB -2 SHEL 99999.000000 0.000000 TEMP -160.0 WGHT 0.058200 EXTI 0.006920 FVAR 0.42037 P1 4 0.782823 0.423231 0.692124 11.00000 0.02776 0.02969 = 0.02552 -0.00110 0.01437 -0.00366 O1 3 0.759389 0.535223 0.754487 11.00000 0.02757 0.03383 = 0.02561 0.00261 0.01581 -0.00064 O2 3 0.856167 0.415433 0.759938 11.00000 0.02466 0.02691 = 0.02629 -0.00123 0.01424 -0.00384 O3 3 0.763386 0.207710 0.682631 11.00000 0.03675 0.03457 = 0.03643 -0.00962 0.02281 -0.00905 AFIX 147 H3 2 0.769187 0.150373 0.641541 11.00000 -1.50000 AFIX 0 O4 3 0.762025 0.544808 0.604091 11.00000 0.03210 0.03963 = 0.02351 0.00196 0.01407 -0.00224 O5 3 0.774457 0.953902 0.583619 11.00000 0.04076 0.03582 = 0.02978 -0.00147 0.01889 0.00178 C1 1 0.880530 0.646955 0.939327 11.00000 0.02692 0.02401 = 0.02846 -0.00025 0.01668 -0.00257 C2 1 0.831537 0.497972 0.924874 11.00000 0.02778 0.02133 = 0.02625 -0.00262 0.01716 0.00045 C3 1 0.774196 0.455372 0.845441 11.00000 0.02989 0.02470 = 0.02472 -0.00116 0.01741 0.00128 C4 1 0.731243 0.338496 0.852424 11.00000 0.02667 0.03077 = 0.02771 -0.00283 0.01779 -0.00184 C5 1 0.750735 0.248813 0.942673 11.00000 0.03020 0.02309 = 0.03395 -0.00115 0.01933 -0.00330 AFIX 43 H5 2 0.722542 0.167609 0.949894 11.00000 -1.20000 AFIX 0 C6 1 0.809803 0.275380 1.021307 11.00000 0.03422 0.02796 = 0.02724 0.00165 0.01647 -0.00122 AFIX 43 H6 2 0.822626 0.207517 1.080765 11.00000 -1.20000 AFIX 0 C7 1 0.850328 0.401740 1.013007 11.00000 0.02821 0.02513 = 0.02778 -0.00159 0.01646 0.00279 C8 1 0.915817 0.454284 1.088220 11.00000 0.02695 0.03452 = 0.02575 -0.00007 0.01425 0.00055 AFIX 23 H8A 2 0.940090 0.333051 1.122150 11.00000 -1.20000 H8B 2 0.917577 0.549805 1.136723 11.00000 -1.20000 AFIX 0 C9 1 0.938915 0.551014 1.026593 11.00000 0.02072 0.03089 = 0.02923 0.00003 0.01253 -0.00190 AFIX 23 H9A 2 0.956989 0.448886 1.003883 11.00000 -1.20000 H9B 2 0.970529 0.654451 1.064348 11.00000 -1.20000 AFIX 0 C10 1 0.892662 0.709732 0.860286 11.00000 0.02539 0.02400 = 0.02692 -0.00180 0.01412 -0.00077 C11 1 0.886775 0.601430 0.782350 11.00000 0.02293 0.02174 = 0.02572 0.00028 0.01123 -0.00247 C12 1 0.908596 0.677652 0.724699 11.00000 0.02385 0.02559 = 0.02794 0.00161 0.01435 0.00204 C13 1 0.934648 0.868644 0.747246 11.00000 0.02824 0.02780 = 0.02649 0.00351 0.01387 0.00087 AFIX 43 H13 2 0.951188 0.922034 0.710750 11.00000 -1.20000 AFIX 0 C14 1 0.937262 0.982705 0.820562 11.00000 0.03370 0.02191 = 0.03379 0.00293 0.01682 -0.00069 AFIX 43 H14 2 0.954015 1.114424 0.832849 11.00000 -1.20000 AFIX 0 C15 1 0.915197 0.903207 0.876142 11.00000 0.02260 0.02698 = 0.02872 -0.00228 0.01161 0.00084 C16 1 0.910031 1.000466 0.955286 11.00000 0.03891 0.02155 = 0.03217 -0.00330 0.01737 -0.00006 AFIX 23 H16A 2 0.891004 1.135155 0.935397 11.00000 -1.20000 H16B 2 0.951001 1.012917 1.015645 11.00000 -1.20000 AFIX 0 C17 1 0.868405 0.856124 0.969124 11.00000 0.03256 0.02775 = 0.03621 -0.00516 0.02000 -0.00283 AFIX 23 H17A 2 0.824459 0.894658 0.927190 11.00000 -1.20000 H17B 2 0.879198 0.855320 1.037739 11.00000 -1.20000 AFIX 0 C18 1 0.666462 0.311929 0.771272 11.00000 0.03180 0.04069 = 0.02513 -0.00605 0.01830 -0.00710 C19 1 0.638201 0.126462 0.756829 11.00000 0.04403 0.04804 = 0.02583 -0.00681 0.02222 -0.01542 AFIX 43 H19 2 0.661599 0.014276 0.794300 11.00000 -1.20000 AFIX 0 C20 1 0.575634 0.103802 0.687609 11.00000 0.04338 0.07087 = 0.03142 -0.02032 0.02320 -0.03003 AFIX 43 H20 2 0.556410 -0.023392 0.678373 11.00000 -1.20000 AFIX 0 C21 1 0.541707 0.265287 0.632684 11.00000 0.02432 0.08650 = 0.03946 -0.01066 0.01818 -0.01649 AFIX 43 H21 2 0.498982 0.250073 0.585806 11.00000 -1.20000 AFIX 0 C22 1 0.569680 0.448613 0.645694 11.00000 0.02543 0.07689 = 0.03299 0.00084 0.01202 0.00115 AFIX 43 H22 2 0.546333 0.559777 0.607116 11.00000 -1.20000 AFIX 0 C23 1 0.631980 0.472399 0.715017 11.00000 0.03344 0.04513 = 0.03831 -0.00330 0.01920 -0.00153 AFIX 43 H23 2 0.650948 0.599904 0.723737 11.00000 -1.20000 AFIX 0 C24 1 0.901793 0.569968 0.639438 11.00000 0.02337 0.03173 = 0.03230 0.00239 0.01750 -0.00266 C25 1 0.919685 0.372262 0.644274 11.00000 0.05343 0.02930 = 0.03570 0.00453 0.03078 0.00635 AFIX 43 H25 2 0.936007 0.300858 0.703764 11.00000 -1.20000 AFIX 0 C26 1 0.914175 0.276740 0.563718 11.00000 0.06162 0.03116 = 0.04427 -0.00165 0.03696 0.00021 AFIX 43 H26 2 0.926283 0.140445 0.567770 11.00000 -1.20000 AFIX 0 C27 1 0.891030 0.380607 0.477701 11.00000 0.05128 0.04343 = 0.03070 -0.00792 0.02815 -0.00487 AFIX 43 H27 2 0.886982 0.315735 0.422099 11.00000 -1.20000 AFIX 0 C28 1 0.873838 0.577240 0.472172 11.00000 0.03408 0.05048 = 0.02854 0.00635 0.01971 0.00684 AFIX 43 H28 2 0.858663 0.648814 0.412961 11.00000 -1.20000 AFIX 0 C29 1 0.878341 0.672582 0.551836 11.00000 0.02529 0.03769 = 0.02739 0.00612 0.01408 0.00498 AFIX 43 H29 2 0.865433 0.808172 0.546840 11.00000 -1.20000 AFIX 0 H1 2 0.759108 0.819162 0.585064 11.00000 0.07353 H2 2 0.761099 0.982111 0.528779 11.00000 0.05966 HKLF 4 REM _m130503b REM R1 = 0.0630 for 3636 Fo > 4sig(Fo) and 0.0814 for all 4627 data REM 326 parameters refined using 1 restraints END WGHT 0.0581 0.0000 REM Instructions for potential hydrogen bonds HTAB O3 O5_$1 HTAB O5 O4 HTAB O5 O4_$2 REM Highest difference peak 0.276, deepest hole -0.439, 1-sigma level 0.076 Q1 1 0.7501 1.0592 0.5834 11.00000 0.05 0.28 Q2 1 0.5842 0.4944 0.7863 11.00000 0.05 0.28 Q3 1 0.7734 0.7980 0.4703 11.00000 0.05 0.27 Q4 1 0.7745 0.4236 0.5856 11.00000 0.05 0.26 Q5 1 0.9199 0.9261 1.0505 11.00000 0.05 0.26 ; _shelx_res_checksum 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14.24 -10 -6 15 10.94 8.13 -10 6 15 19.43 10.78 -10 -6 15 10.97 12.42 -5 -5 16 16.87 14.44 5 -5 -16 42.34 18.27 -5 5 16 23.52 12.52 -5 -5 16 14.59 7.04 -20 -2 -7 40.97 21.81 20 -2 7 6.46 9.09 -20 2 -7 60.54 20.09 16 -4 8 11.29 12.51 -23 -5 0 25.98 15.67 -16 -4 -8 19.54 11.41 -16 -4 -8 8.76 11.08 -16 4 -8 24.67 12.65 23 -5 0 14.98 11.43 -23 5 0 31.84 22.34 -8 -8 8 11.36 10.80 8 -8 -8 11.13 11.09 8 -8 -8 12.03 7.80 19 -7 -4 13.33 5.10 19 -7 -4 13.42 6.98 -19 -7 4 -0.37 8.91 8 0 -20 8.85 8.08 -8 0 20 10.40 8.47 24 -4 -17 25.75 12.43 -24 -4 17 28.13 11.02 -20 -4 -5 -1.42 8.71 10 -8 1 22.32 23.85 20 -4 5 8.84 7.30 -10 -8 -1 50.95 25.63 -20 4 -5 11.14 11.82 -20 -4 -5 2.49 6.67 19 -3 7 30.06 15.12 -19 -3 -7 -10.51 8.39 -19 3 -7 14.13 16.61 31 -1 -16 10.95 7.61 -27 -1 19 106.96 26.47 32 -2 -12 11.51 8.25 -11 5 17 15.98 9.83 27 -1 -19 58.42 31.93 -11 -5 17 11.57 11.00 11 -5 -17 2.72 8.56 -27 -5 9 13.67 8.91 -32 2 9 1.84 5.13 27 -5 -9 22.57 9.86 -17 5 17 11.59 8.33 17 -5 -17 20.67 11.13 -17 -5 17 7.44 9.06 0 -8 -7 70.99 19.02 0 -8 -7 45.58 19.52 0 -8 7 45.73 25.94 -31 -3 10 34.70 16.97 31 -3 -10 42.06 24.68 4 2 16 10.79 8.44 -4 -2 -16 23.72 12.08 4 -2 16 1.00 5.27 4 -2 16 14.16 8.48 -4 2 -16 7.35 6.29 28 -4 -14 15.04 9.34 4 -8 -8 25.32 13.99 -4 -8 8 32.20 21.52 13 -3 11 31.43 12.26 4 -8 -8 36.75 16.46 -13 -3 -11 10.80 14.73 -13 3 -11 13.45 11.39 -22 2 20 29.46 14.34 -1 5 15 71.30 27.30 -1 -5 15 70.08 20.56 1 -5 -15 66.03 30.69 22 -2 -20 26.88 18.03 -22 -2 20 36.74 14.28 -1 -5 15 67.50 20.24 31 -3 -11 140.10 51.93 27 -5 -8 11.64 7.47 -27 -5 8 3.21 5.43 27 -5 -8 10.41 8.92 -31 -3 11 50.45 39.17 0 -6 13 34.97 12.85 0 -6 -13 16.99 10.46 0 -6 13 7.73 5.58 -26 -4 16 2.41 6.81 26 -4 -16 5.54 7.43 -19 -7 9 15.27 10.76 19 -7 -9 7.27 5.47 27 -5 -10 13.07 11.00 -27 -5 10 10.54 9.61 -32 0 6 19.19 10.57 16 0 -21 4.94 4.72 -16 0 21 0.34 7.92 -1 -7 11 6.68 4.84 1 -7 -11 11.03 6.80 -1 -7 11 5.05 6.35 1 -7 -11 14.53 8.42 -17 -7 11 34.27 14.76 17 -7 -11 27.77 12.98 -8 4 18 34.38 13.06 8 -4 -18 39.08 20.18 -5 3 -15 108.67 25.99 5 -3 15 101.00 25.48 -8 -4 18 40.53 16.90 -5 -3 -15 61.87 45.69 5 3 15 95.68 27.96 5 -3 15 100.29 26.08 24 -6 -8 7.31 4.80 31 -3 -9 6.50 5.92 24 -6 -8 16.43 10.63 -31 -3 9 19.34 10.77 -24 -6 8 18.76 16.83 15 -7 2 42.25 13.97 -5 -7 12 14.16 8.20 -29 -1 18 19.24 14.13 8 -8 3 8.12 7.68 -5 1 -16 19.45 12.29 29 -1 -18 22.76 15.56 5 -1 16 10.76 7.51 5 -7 -12 9.52 7.55 -5 -7 12 6.16 8.63 5 -1 16 12.01 7.79 -15 -7 -2 46.33 21.45 -8 -8 -3 7.97 9.77 15 -7 2 24.84 12.15 -5 -1 -16 32.50 13.16 5 1 16 5.31 13.07 -16 -6 15 10.41 6.03 -16 -6 15 9.08 9.65 16 -6 -15 7.85 9.98 -22 -6 2 22.75 9.22 22 -6 -2 14.48 10.57 25 -5 -14 18.89 11.69 -12 -8 1 22.13 8.30 12 -8 -1 0.54 7.54 -25 -5 14 59.44 20.14 12 -8 -1 3.87 5.93 14 -6 6 5.92 4.93 24 -6 -7 25.46 9.61 -24 -6 7 41.97 14.06 -14 -6 -6 5.47 7.51 -14 6 -6 11.15 6.41 -14 -6 -6 12.09 8.89 24 -6 -7 28.10 16.95 0 0 -18 166.13 36.76 0 0 18 121.08 49.10 10 -8 -8 18.48 15.67 10 -8 -8 39.74 16.75 -10 -8 8 47.66 18.07 0 -4 16 13.38 7.72 12 -8 -7 7.66 5.61 -24 -6 9 36.45 12.74 12 -8 -7 31.31 15.49 -12 -8 7 60.27 32.24 24 -6 -9 30.18 15.09 0 4 16 42.97 15.26 0 -4 16 22.31 7.48 0 -4 -16 36.67 14.70 23 -3 -19 11.69 6.90 -23 -3 19 1.62 6.82 15 -7 -12 15.16 8.32 -15 -7 12 8.07 8.15 -15 -7 12 2.76 6.24 31 -3 -12 16.83 9.71 26 -4 -1 13.73 9.28 -26 -4 1 6.85 4.15 -26 4 1 5.23 4.57 -26 -4 1 5.84 5.18 32 -2 -13 51.36 25.30 -28 -2 18 14.97 6.47 27 -5 -7 18.71 11.47 -27 -5 7 8.98 6.02 26 -2 -19 21.83 7.20 -8 -6 15 12.82 10.81 -8 -6 15 13.02 11.60 27 -5 -7 4.26 5.02 28 -2 -18 23.69 11.07 -26 -2 19 14.94 11.18 -8 6 15 10.06 11.06 8 -6 -15 14.24 10.93 -15 1 -11 38.52 16.17 15 1 11 34.92 13.37 -15 -1 -11 43.11 16.71 15 -1 11 31.01 13.16 17 -7 0 13.56 11.09 -17 -7 0 33.71 14.37 33 -1 -11 7.08 5.97 17 -7 0 24.42 13.87 32 -2 -8 -0.56 3.27 -20 0 21 30.50 19.60 -9 -5 -11 11.26 5.94 -9 5 -11 10.84 10.24 -9 -5 -11 10.46 11.42 -10 -2 20 12.34 14.53 10 -2 -20 10.34 7.19 9 -5 11 22.22 10.83 -10 2 20 17.76 13.39 -29 -1 1 4.38 7.76 -29 1 1 3.54 8.11 19 -7 -3 19.68 6.55 -27 -5 11 22.99 10.38 -7 -5 -12 5.51 4.24 -7 -5 -12 12.50 7.21 19 -7 -3 13.87 7.19 7 -5 12 4.35 4.61 -19 -7 3 12.27 8.93 27 -5 -11 20.59 9.16 16 2 10 22.45 7.56 -16 -2 -10 72.78 21.38 20 -6 -14 29.10 19.89 -16 2 -10 57.45 20.64 16 -2 10 80.74 26.22 -20 -6 14 40.45 16.58 -20 -6 14 35.60 19.74 14 0 -21 38.06 13.57 -14 0 21 21.39 12.96 -22 -4 18 6.65 6.29 22 -4 -18 2.43 7.92 -28 0 19 15.22 9.52 -17 1 21 13.94 11.78 -17 -1 21 22.14 12.64 17 -1 -21 5.16 5.44 17 -5 6 2.00 9.26 33 -1 -12 4.88 3.70 -17 -5 -6 11.88 7.33 -17 -5 -6 19.53 11.48 -25 1 20 18.13 11.15 -31 -3 8 25.47 14.15 31 -3 -8 19.09 9.00 25 -1 -20 14.35 8.28 -25 -1 20 27.03 17.70 -28 -4 4 23.33 7.83 28 -4 -4 12.79 7.78 -24 -6 6 19.24 10.95 24 -6 -6 34.15 14.38 24 -6 -6 3.02 6.21 -9 5 17 19.76 8.34 -13 -7 -4 59.82 18.02 -9 -5 17 18.55 10.30 13 -7 4 25.43 12.11 -24 -6 10 22.83 15.07 -29 -3 16 6.15 4.66 25 -3 2 75.31 30.47 -2 -8 8 25.56 16.04 2 -8 -8 12.27 8.54 -19 -1 21 -0.38 7.44 -11 -5 -10 54.16 30.42 11 -5 10 39.50 20.90 26 -2 2 -3.50 7.91 15 -3 10 17.90 12.08 21 -1 7 21.26 9.81 -15 -1 21 42.12 19.50 -15 1 21 30.10 14.01 23 -3 4 21.94 9.74 -5 -5 -13 9.03 6.79 5 -5 13 25.79 12.42 -18 -6 -3 29.70 11.82 18 -6 3 7.74 6.53 10 0 14 9.74 9.28 33 -1 -9 -1.29 3.29 24 -2 4 26.95 13.36 10 0 14 10.66 9.97 -19 -7 10 38.45 14.47 -20 -6 -1 28.79 16.66 -22 -6 13 5.66 5.38 20 -6 1 14.48 8.88 29 -3 -3 49.94 22.35 7 -7 8 49.71 24.35 -7 -7 -8 59.65 18.70 -5 -7 -9 56.37 22.54 5 -7 9 30.78 16.52 -25 -5 2 21.15 12.99 3 -3 16 7.46 8.02 25 -5 -2 16.25 9.41 3 3 16 14.94 9.58 27 -5 -6 -0.80 5.64 -27 -5 6 7.98 6.62 30 -2 -3 44.80 17.77 8 0 15 3.52 4.01 8 0 15 7.09 9.77 12 0 13 20.66 7.87 2 2 17 14.51 10.37 12 0 13 27.09 13.61 2 -2 17 16.19 10.75 -3 3 18 17.85 10.45 -17 3 20 8.50 6.41 3 1 17 10.79 8.48 3 -1 17 8.05 6.65 -27 -5 12 7.14 7.14 -18 -4 -7 -6.54 6.94 -15 3 20 71.69 18.98 -3 -1 19 43.69 16.93 -3 1 19 21.56 8.19 -7 3 19 16.54 12.52 -24 -6 5 61.37 19.42 -7 -1 20 19.78 8.68 -7 1 20 8.94 9.27 -16 4 19 12.22 5.20 -8 -6 -10 -1.67 5.88 -9 -7 -7 87.75 23.09 -21 1 21 17.65 9.56 -6 -6 -11 7.19 4.43 -14 4 19 19.10 15.73 -19 3 20 16.64 10.84 -13 1 21 6.73 9.13 -6 6 15 12.92 7.73 ; _shelx_hkl_checksum 98983 _database_code_depnum_ccdc_archive 'CCDC 960976' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H83 O7 P' _chemical_formula_sum 'C56 H83 O7 P' _chemical_formula_weight 899.19 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.7790(13) _cell_length_b 17.451(2) _cell_length_c 13.8490(16) _cell_angle_alpha 90 _cell_angle_beta 110.544(4) _cell_angle_gamma 90 _cell_volume 2665.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11336 _cell_measurement_theta_min 1.60 _cell_measurement_theta_max 33.10 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.120 _exptl_crystal_F_000 980 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.240 _exptl_crystal_size_min 0.180 _exptl_absorpt_coefficient_mu 0.100 _shelx_estimated_absorpt_T_min 0.974 _shelx_estimated_absorpt_T_max 0.982 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.982 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Rigaku Saturn724 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.222 _diffrn_reflns_number 45085 _diffrn_reflns_av_unetI/netI 0.0825 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.570 _diffrn_reflns_theta_max 33.146 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 20147 _reflns_number_gt 16973 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.930 _reflns_Friedel_fraction_max 0.983 _reflns_Friedel_fraction_full 1.000 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _refine_special_details ; ENTER TEXT OF LETTER ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0352P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 5884 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.02(4) _chemical_absolute_configuration ? _refine_ls_number_reflns 20147 _refine_ls_number_parameters 619 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P1 P 0.30509(4) 0.72170(3) 0.22927(3) 0.01671(10) Uani 1 1 d . . . . . O1 O 0.32816(11) 0.78977(7) 0.16237(9) 0.0160(2) Uani 1 1 d . . . . . O2 O 0.37982(11) 0.64951(7) 0.21133(10) 0.0170(3) Uani 1 1 d . . . . . O3 O 0.34341(12) 0.74759(8) 0.33678(10) 0.0231(3) Uani 1 1 d . . . . . O4 O 0.17296(12) 0.69686(8) 0.17604(10) 0.0228(3) Uani 1 1 d . . . . . H4 H 0.143(2) 0.6704(14) 0.2171(19) 0.034 Uiso 1 1 d . U . . . O5 O 0.07356(16) 0.62208(10) 0.28295(14) 0.0368(4) Uani 1 1 d D . . . . H5 H 0.069(3) 0.6483(17) 0.341(2) 0.055 Uiso 1 1 d . U . . . O6 O 0.07145(14) 0.69543(10) 0.45667(12) 0.0317(4) Uani 1 1 d . . . . . H6 H 0.108(3) 0.7362(17) 0.452(2) 0.047 Uiso 1 1 d . U . . . O7 O 0.19361(15) 0.81606(9) 0.42422(13) 0.0341(4) Uani 1 1 d . . . . . H7 H 0.244(3) 0.7921(17) 0.399(2) 0.051 Uiso 1 1 d . U . . . C1 C 0.52631(15) 0.72482(11) 0.08991(13) 0.0165(3) Uani 1 1 d . . . . . C2 C 0.39726(16) 0.74799(10) 0.02695(13) 0.0156(3) Uani 1 1 d . . . . . C3 C 0.30852(16) 0.78235(10) 0.05696(13) 0.0146(3) Uani 1 1 d . . . . . C4 C 0.20354(16) 0.81342(10) -0.01545(14) 0.0161(3) Uani 1 1 d . . . . . C5 C 0.18714(17) 0.80339(11) -0.11966(14) 0.0195(4) Uani 1 1 d . . . . . H5A H 0.1174 0.8249 -0.1703 0.023 Uiso 1 1 calc R U . . . C6 C 0.26938(18) 0.76305(12) -0.15159(14) 0.0214(4) Uani 1 1 d . . . . . H6A H 0.2538 0.7543 -0.2228 0.026 Uiso 1 1 calc R U . . . C7 C 0.37483(17) 0.73570(10) -0.07751(14) 0.0183(4) Uani 1 1 d . . . . . C8 C 0.47783(19) 0.69126(12) -0.09254(15) 0.0235(4) Uani 1 1 d . . . . . H8A H 0.5294 0.7248 -0.1176 0.028 Uiso 1 1 calc R U . . . H8B H 0.4472 0.6482 -0.1414 0.028 Uiso 1 1 calc R U . . . C9 C 0.54730(18) 0.66201(11) 0.01790(15) 0.0220(4) Uani 1 1 d . . . . . H9A H 0.6348 0.6562 0.0297 0.026 Uiso 1 1 calc R U . . . H9B H 0.5148 0.6120 0.0299 0.026 Uiso 1 1 calc R U . . . C10 C 0.56759(16) 0.69619(10) 0.20043(13) 0.0156(3) Uani 1 1 d . . . . . C11 C 0.50709(16) 0.65450(10) 0.25315(13) 0.0160(3) Uani 1 1 d . . . . . C12 C 0.57094(17) 0.61711(10) 0.34628(14) 0.0170(3) Uani 1 1 d . . . . . C13 C 0.69627(17) 0.62933(11) 0.38866(14) 0.0206(4) Uani 1 1 d . . . . . H13 H 0.7416 0.6039 0.4509 0.025 Uiso 1 1 calc R U . . . C14 C 0.75674(17) 0.67757(11) 0.34263(15) 0.0222(4) Uani 1 1 d . . . . . H14 H 0.8410 0.6874 0.3749 0.027 Uiso 1 1 calc R U . . . C15 C 0.69158(16) 0.71088(11) 0.24889(14) 0.0189(4) Uani 1 1 d . . . . . C16 C 0.73595(17) 0.76449(12) 0.18419(16) 0.0240(4) Uani 1 1 d . . . . . H16A H 0.7885 0.7374 0.1531 0.029 Uiso 1 1 calc R U . . . H16B H 0.7813 0.8081 0.2257 0.029 Uiso 1 1 calc R U . . . C17 C 0.61732(17) 0.79165(11) 0.10063(15) 0.0205(4) Uani 1 1 d . . . . . H17A H 0.6297 0.8010 0.0345 0.025 Uiso 1 1 calc R U . . . H17B H 0.5876 0.8394 0.1222 0.025 Uiso 1 1 calc R U . . . C18 C 0.11710(16) 0.86169(10) 0.01635(13) 0.0164(3) Uani 1 1 d . . . . . C19 C 0.15648(17) 0.93457(11) 0.06085(14) 0.0192(4) Uani 1 1 d . . . . . C20 C 0.07558(19) 0.97967(11) 0.08822(15) 0.0221(4) Uani 1 1 d . . . . . H20 H 0.1021 1.0281 0.1191 0.027 Uiso 1 1 calc R U . . . C21 C -0.04306(18) 0.95673(11) 0.07219(15) 0.0219(4) Uani 1 1 d . . . . . C22 C -0.08064(18) 0.88566(12) 0.02688(15) 0.0225(4) Uani 1 1 d . . . . . H22 H -0.1614 0.8693 0.0148 0.027 Uiso 1 1 calc R U . . . C23 C -0.00205(17) 0.83736(11) -0.00150(14) 0.0186(4) Uani 1 1 d . . . . . C24 C 0.28288(19) 0.96361(11) 0.07320(17) 0.0257(4) Uani 1 1 d . . . . . H24 H 0.3399 0.9193 0.0957 0.031 Uiso 1 1 calc R U . . . C25 C 0.3306(2) 1.02743(12) 0.15340(18) 0.0302(5) Uani 1 1 d . . . . . H25A H 0.3244 1.0111 0.2191 0.045 Uiso 1 1 calc R U . . . H25B H 0.2824 1.0739 0.1293 0.045 Uiso 1 1 calc R U . . . H25C H 0.4156 1.0380 0.1631 0.045 Uiso 1 1 calc R U . . . C26 C 0.2853(3) 0.99072(15) -0.0314(2) 0.0403(6) Uani 1 1 d . . . . . H26A H 0.2355 1.0369 -0.0529 0.060 Uiso 1 1 calc R U . . . H26B H 0.2531 0.9503 -0.0828 0.060 Uiso 1 1 calc R U . . . H26C H 0.3690 1.0023 -0.0252 0.060 Uiso 1 1 calc R U . . . C27 C -0.1259(2) 1.01213(12) 0.10243(17) 0.0276(4) Uani 1 1 d . . . . . H27 H -0.0743 1.0382 0.1673 0.033 Uiso 1 1 calc R U . . . C28 C -0.2294(3) 0.97562(15) 0.1248(2) 0.0460(7) Uani 1 1 d . . . . . H28A H -0.1983 0.9350 0.1761 0.069 Uiso 1 1 calc R U . . . H28B H -0.2866 0.9537 0.0612 0.069 Uiso 1 1 calc R U . . . H28C H -0.2707 1.0144 0.1516 0.069 Uiso 1 1 calc R U . . . C29 C -0.1729(3) 1.07463(15) 0.0209(2) 0.0492(7) Uani 1 1 d . . . . . H29A H -0.2143 1.1142 0.0465 0.074 Uiso 1 1 calc R U . . . H29B H -0.2299 1.0522 -0.0424 0.074 Uiso 1 1 calc R U . . . H29C H -0.1047 1.0976 0.0064 0.074 Uiso 1 1 calc R U . . . C30 C -0.04681(17) 0.76057(12) -0.05280(15) 0.0230(4) Uani 1 1 d . . . . . H30 H 0.0258 0.7308 -0.0525 0.028 Uiso 1 1 calc R U . . . C31 C -0.11170(19) 0.71311(13) 0.00515(17) 0.0289(5) Uani 1 1 d . . . . . H31A H -0.1901 0.7367 -0.0033 0.043 Uiso 1 1 calc R U . . . H31B H -0.0619 0.7114 0.0786 0.043 Uiso 1 1 calc R U . . . H31C H -0.1246 0.6609 -0.0227 0.043 Uiso 1 1 calc R U . . . C32 C -0.1297(2) 0.77047(15) -0.16570(18) 0.0360(5) Uani 1 1 d . . . . . H32A H -0.0871 0.7998 -0.2028 0.054 Uiso 1 1 calc R U . . . H32B H -0.2034 0.7979 -0.1685 0.054 Uiso 1 1 calc R U . . . H32C H -0.1515 0.7200 -0.1979 0.054 Uiso 1 1 calc R U . . . C33 C 0.51329(16) 0.56090(11) 0.39667(14) 0.0178(3) Uani 1 1 d . . . . . C34 C 0.49184(17) 0.57933(11) 0.48729(14) 0.0183(4) Uani 1 1 d . . . . . C35 C 0.45001(18) 0.52197(11) 0.53711(15) 0.0218(4) Uani 1 1 d . . . . . H35 H 0.4347 0.5345 0.5982 0.026 Uiso 1 1 calc R U . . . C36 C 0.43020(18) 0.44746(12) 0.50037(15) 0.0235(4) Uani 1 1 d . . . . . C37 C 0.45173(19) 0.43054(12) 0.41008(16) 0.0250(4) Uani 1 1 d . . . . . H37 H 0.4378 0.3798 0.3838 0.030 Uiso 1 1 calc R U . . . C38 C 0.49275(18) 0.48498(11) 0.35687(14) 0.0209(4) Uani 1 1 d . . . . . C39 C 0.51495(18) 0.66000(11) 0.53262(14) 0.0208(4) Uani 1 1 d . . . . . H39 H 0.5186 0.6954 0.4770 0.025 Uiso 1 1 calc R U . . . C40 C 0.4131(2) 0.68833(13) 0.56853(16) 0.0292(5) Uani 1 1 d . . . . . H40A H 0.4179 0.6616 0.6321 0.044 Uiso 1 1 calc R U . . . H40B H 0.3345 0.6779 0.5149 0.044 Uiso 1 1 calc R U . . . H40C H 0.4219 0.7436 0.5816 0.044 Uiso 1 1 calc R U . . . C41 C 0.6373(2) 0.66531(13) 0.62210(17) 0.0315(5) Uani 1 1 d . . . . . H41A H 0.7026 0.6492 0.5980 0.047 Uiso 1 1 calc R U . . . H41B H 0.6360 0.6318 0.6785 0.047 Uiso 1 1 calc R U . . . H41C H 0.6513 0.7183 0.6468 0.047 Uiso 1 1 calc R U . . . C42 C 0.3862(2) 0.38343(13) 0.55408(17) 0.0295(5) Uani 1 1 d . . . . . H42 H 0.4316 0.3361 0.5490 0.035 Uiso 1 1 calc R U . . . C43 C 0.2530(3) 0.36685(19) 0.4982(2) 0.0555(8) Uani 1 1 d . . . . . H43A H 0.2386 0.3572 0.4251 0.083 Uiso 1 1 calc R U . . . H43B H 0.2048 0.4110 0.5046 0.083 Uiso 1 1 calc R U . . . H43C H 0.2294 0.3216 0.5286 0.083 Uiso 1 1 calc R U . . . C44 C 0.4130(3) 0.39792(17) 0.6675(2) 0.0517(8) Uani 1 1 d . . . . . H44A H 0.3954 0.3515 0.6996 0.078 Uiso 1 1 calc R U . . . H44B H 0.3622 0.4401 0.6757 0.078 Uiso 1 1 calc R U . . . H44C H 0.4986 0.4115 0.7007 0.078 Uiso 1 1 calc R U . . . C45 C 0.5254(2) 0.46129(12) 0.26405(16) 0.0286(5) Uani 1 1 d . . . . . H45 H 0.5233 0.5084 0.2223 0.034 Uiso 1 1 calc R U . . . C46 C 0.4366(3) 0.40330(15) 0.19397(19) 0.0413(6) Uani 1 1 d . . . . . H46A H 0.3541 0.4242 0.1719 0.062 Uiso 1 1 calc R U . . . H46B H 0.4399 0.3554 0.2319 0.062 Uiso 1 1 calc R U . . . H46C H 0.4588 0.3932 0.1333 0.062 Uiso 1 1 calc R U . . . C47 C 0.6547(2) 0.42972(15) 0.2998(2) 0.0397(6) Uani 1 1 d . . . . . H47A H 0.6616 0.3865 0.3467 0.060 Uiso 1 1 calc R U . . . H47B H 0.7118 0.4701 0.3357 0.060 Uiso 1 1 calc R U . . . H47C H 0.6736 0.4123 0.2398 0.060 Uiso 1 1 calc R U . . . C48 C -0.0156(3) 0.5044(2) 0.3157(3) 0.0403(9) Uani 0.839(4) 1 d D . P A 1 H48A H -0.0337 0.5293 0.3720 0.061 Uiso 0.839(4) 1 calc R U P A 1 H48B H -0.0027 0.4495 0.3301 0.061 Uiso 0.839(4) 1 calc R U P A 1 H48C H -0.0838 0.5117 0.2509 0.061 Uiso 0.839(4) 1 calc R U P A 1 C49 C 0.0974(3) 0.53930(15) 0.3064(2) 0.0305(6) Uani 0.839(4) 1 d D . P A 1 H49 H 0.1667 0.5331 0.3729 0.037 Uiso 0.839(4) 1 calc R U P A 1 C50 C 0.1304(4) 0.50584(19) 0.2202(3) 0.0481(9) Uani 0.839(4) 1 d D . P A 1 H50A H 0.0635 0.5137 0.1547 0.072 Uiso 0.839(4) 1 calc R U P A 1 H50B H 0.1458 0.4508 0.2320 0.072 Uiso 0.839(4) 1 calc R U P A 1 H50C H 0.2036 0.5311 0.2174 0.072 Uiso 0.839(4) 1 calc R U P A 1 C48' C -0.0508(18) 0.5156(11) 0.2873(16) 0.0403(9) Uani 0.161(4) 1 d D . P A 2 H48D H -0.0086 0.5058 0.3609 0.061 Uiso 0.161(4) 1 calc R U P A 2 H48E H -0.0861 0.4678 0.2526 0.061 Uiso 0.161(4) 1 calc R U P A 2 H48F H -0.1153 0.5533 0.2786 0.061 Uiso 0.161(4) 1 calc R U P A 2 C49' C 0.0402(11) 0.5472(6) 0.2396(11) 0.0305(6) Uani 0.161(4) 1 d D . P A 2 H49' H 0.0032 0.5496 0.1627 0.037 Uiso 0.161(4) 1 calc R U P A 2 C50' C 0.1658(16) 0.5055(8) 0.2747(16) 0.0481(9) Uani 0.161(4) 1 d D . P A 2 H50D H 0.2170 0.5287 0.2400 0.072 Uiso 0.161(4) 1 calc R U P A 2 H50E H 0.1537 0.4511 0.2566 0.072 Uiso 0.161(4) 1 calc R U P A 2 H50F H 0.2055 0.5108 0.3496 0.072 Uiso 0.161(4) 1 calc R U P A 2 C51 C 0.1058(5) 0.6007(2) 0.5862(3) 0.0856(14) Uani 1 1 d . . . . . H51A H 0.1642 0.5765 0.5599 0.128 Uiso 1 1 calc R U . . . H51B H 0.0252 0.5787 0.5512 0.128 Uiso 1 1 calc R U . . . H51C H 0.1303 0.5916 0.6605 0.128 Uiso 1 1 calc R U . . . C52 C 0.1021(2) 0.68463(16) 0.56625(17) 0.0366(5) Uani 1 1 d . . . . . H52 H 0.1848 0.7063 0.6025 0.044 Uiso 1 1 calc R U . . . C53 C 0.0127(2) 0.7268(2) 0.6031(2) 0.0628(9) Uani 1 1 d . . . . . H53A H -0.0694 0.7079 0.5656 0.094 Uiso 1 1 calc R U . . . H53B H 0.0166 0.7818 0.5903 0.094 Uiso 1 1 calc R U . . . H53C H 0.0329 0.7179 0.6771 0.094 Uiso 1 1 calc R U . . . C54 C 0.0297(3) 0.9023(2) 0.3977(3) 0.0649(9) Uani 1 1 d . . . . . H54A H 0.0613 0.9178 0.4703 0.097 Uiso 1 1 calc R U . . . H54B H -0.0239 0.8580 0.3896 0.097 Uiso 1 1 calc R U . . . H54C H -0.0158 0.9449 0.3556 0.097 Uiso 1 1 calc R U . . . C55 C 0.1350(2) 0.88091(14) 0.36298(19) 0.0354(5) Uani 1 1 d . . . . . H55 H 0.1026 0.8658 0.2886 0.043 Uiso 1 1 calc R U . . . C56 C 0.2231(3) 0.94522(17) 0.3775(2) 0.0532(7) Uani 1 1 d . . . . . H56A H 0.2862 0.9302 0.3502 0.080 Uiso 1 1 calc R U . . . H56B H 0.2604 0.9569 0.4511 0.080 Uiso 1 1 calc R U . . . H56C H 0.1806 0.9906 0.3406 0.080 Uiso 1 1 calc R U . . . 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 P1 0.0154(2) 0.0205(2) 0.0151(2) 0.00223(18) 0.00643(16) 0.00153(18) O1 0.0187(6) 0.0167(6) 0.0130(6) -0.0002(5) 0.0063(5) 0.0015(5) O2 0.0159(6) 0.0167(7) 0.0191(6) 0.0017(5) 0.0070(5) -0.0007(5) O3 0.0241(7) 0.0295(8) 0.0155(6) 0.0014(5) 0.0068(5) 0.0053(6) O4 0.0170(6) 0.0304(8) 0.0216(7) 0.0050(6) 0.0075(5) -0.0004(6) O5 0.0497(11) 0.0327(9) 0.0399(10) -0.0082(7) 0.0306(9) -0.0118(8) O6 0.0297(8) 0.0429(10) 0.0233(7) -0.0025(7) 0.0104(6) -0.0048(7) O7 0.0366(9) 0.0334(9) 0.0376(9) 0.0016(7) 0.0195(8) 0.0053(7) C1 0.0162(7) 0.0161(8) 0.0192(8) 0.0010(7) 0.0088(6) 0.0013(7) C2 0.0183(8) 0.0126(8) 0.0173(8) 0.0007(6) 0.0078(6) -0.0028(6) C3 0.0172(8) 0.0131(8) 0.0148(7) -0.0002(6) 0.0071(6) -0.0026(6) C4 0.0170(8) 0.0147(8) 0.0171(8) 0.0004(6) 0.0066(6) -0.0029(7) C5 0.0194(9) 0.0215(10) 0.0164(8) 0.0017(7) 0.0046(7) -0.0007(7) C6 0.0257(9) 0.0253(10) 0.0140(8) -0.0013(7) 0.0080(7) -0.0030(8) C7 0.0222(9) 0.0179(9) 0.0178(8) -0.0013(7) 0.0107(7) -0.0029(7) C8 0.0282(10) 0.0255(10) 0.0207(9) -0.0030(8) 0.0136(8) 0.0032(8) C9 0.0229(9) 0.0210(10) 0.0252(9) -0.0021(7) 0.0120(8) 0.0031(8) C10 0.0166(8) 0.0134(8) 0.0177(8) -0.0004(6) 0.0072(6) 0.0011(6) C11 0.0144(8) 0.0153(8) 0.0184(8) -0.0021(6) 0.0060(6) 0.0004(6) C12 0.0189(8) 0.0144(9) 0.0182(8) 0.0008(6) 0.0070(7) 0.0012(7) C13 0.0191(9) 0.0224(10) 0.0186(9) 0.0027(7) 0.0043(7) 0.0016(7) C14 0.0165(8) 0.0248(10) 0.0240(9) 0.0010(8) 0.0056(7) 0.0003(8) C15 0.0166(8) 0.0190(10) 0.0227(8) 0.0008(7) 0.0091(7) -0.0003(7) C16 0.0177(9) 0.0292(11) 0.0259(10) 0.0033(8) 0.0085(7) -0.0023(8) C17 0.0211(9) 0.0197(9) 0.0232(9) 0.0030(7) 0.0108(7) -0.0012(7) C18 0.0183(8) 0.0155(9) 0.0148(8) 0.0018(6) 0.0052(6) 0.0023(7) C19 0.0202(8) 0.0175(9) 0.0185(8) 0.0030(7) 0.0049(7) 0.0002(7) C20 0.0276(10) 0.0150(9) 0.0233(9) 0.0005(7) 0.0084(8) 0.0018(8) C21 0.0252(10) 0.0199(9) 0.0226(9) 0.0028(7) 0.0109(8) 0.0044(8) C22 0.0179(9) 0.0242(10) 0.0249(10) 0.0006(8) 0.0068(7) 0.0024(7) C23 0.0183(8) 0.0187(9) 0.0181(8) 0.0002(7) 0.0053(7) 0.0011(7) C24 0.0237(10) 0.0174(10) 0.0350(11) -0.0030(8) 0.0091(8) -0.0024(8) C25 0.0283(11) 0.0220(11) 0.0345(12) -0.0023(9) 0.0035(9) -0.0032(8) C26 0.0531(16) 0.0313(13) 0.0464(15) -0.0085(11) 0.0298(13) -0.0186(12) C27 0.0312(11) 0.0230(11) 0.0322(11) -0.0022(8) 0.0157(9) 0.0030(9) C28 0.0577(17) 0.0300(13) 0.0686(19) -0.0004(12) 0.0448(16) 0.0035(12) C29 0.0590(18) 0.0379(15) 0.0614(18) 0.0161(13) 0.0346(15) 0.0252(13) C30 0.0173(8) 0.0239(10) 0.0276(10) -0.0077(8) 0.0074(7) -0.0029(8) C31 0.0237(10) 0.0249(11) 0.0404(12) -0.0064(9) 0.0140(9) -0.0058(9) C32 0.0256(11) 0.0472(15) 0.0316(12) -0.0135(10) 0.0054(9) -0.0052(10) C33 0.0162(8) 0.0185(9) 0.0175(8) 0.0029(7) 0.0041(6) 0.0012(7) C34 0.0174(8) 0.0185(9) 0.0171(8) 0.0017(7) 0.0035(7) 0.0006(7) C35 0.0234(9) 0.0246(10) 0.0181(9) 0.0030(7) 0.0082(7) 0.0011(8) C36 0.0243(10) 0.0218(10) 0.0237(9) 0.0046(8) 0.0077(8) -0.0011(8) C37 0.0297(10) 0.0187(10) 0.0261(10) 0.0008(8) 0.0090(8) 0.0002(8) C38 0.0239(9) 0.0180(9) 0.0200(9) 0.0016(7) 0.0068(7) -0.0001(8) C39 0.0248(9) 0.0192(9) 0.0173(8) 0.0013(7) 0.0060(7) -0.0001(8) C40 0.0377(12) 0.0266(11) 0.0256(10) -0.0007(9) 0.0141(9) 0.0046(9) C41 0.0349(12) 0.0264(11) 0.0255(10) -0.0019(9) 0.0009(9) -0.0031(9) C42 0.0360(12) 0.0236(11) 0.0310(11) 0.0049(8) 0.0145(9) -0.0037(9) C43 0.0466(16) 0.0619(19) 0.0502(17) 0.0230(14) 0.0071(13) -0.0245(14) C44 0.076(2) 0.0457(16) 0.0330(13) 0.0106(11) 0.0190(14) -0.0248(15) C45 0.0447(13) 0.0207(10) 0.0236(10) -0.0006(8) 0.0160(9) -0.0011(9) C46 0.0554(16) 0.0367(14) 0.0319(13) -0.0137(10) 0.0153(12) -0.0056(12) C47 0.0457(14) 0.0413(15) 0.0411(14) -0.0089(11) 0.0265(12) 0.0002(12) C48 0.044(2) 0.0407(18) 0.039(2) 0.0002(14) 0.0178(16) -0.0138(16) C49 0.0367(15) 0.0284(14) 0.0275(13) 0.0015(10) 0.0126(11) -0.0077(11) C50 0.067(3) 0.0340(16) 0.054(2) 0.0014(17) 0.035(2) 0.0024(16) C48' 0.044(2) 0.0407(18) 0.039(2) 0.0002(14) 0.0178(16) -0.0138(16) C49' 0.0367(15) 0.0284(14) 0.0275(13) 0.0015(10) 0.0126(11) -0.0077(11) C50' 0.067(3) 0.0340(16) 0.054(2) 0.0014(17) 0.035(2) 0.0024(16) C51 0.153(4) 0.063(2) 0.0400(18) 0.0108(16) 0.033(2) -0.012(2) C52 0.0304(12) 0.0564(16) 0.0230(10) -0.0042(10) 0.0092(9) -0.0051(11) C53 0.0316(13) 0.124(3) 0.0325(13) -0.0207(17) 0.0108(10) 0.0005(17) C54 0.0489(18) 0.060(2) 0.091(3) 0.0013(18) 0.0311(18) 0.0183(16) C55 0.0349(12) 0.0369(14) 0.0309(12) -0.0010(10) 0.0071(10) 0.0074(10) C56 0.0511(17) 0.0486(17) 0.0528(17) 0.0128(14) 0.0096(14) -0.0050(14) _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 P1 O3 1.4674(14) . ? P1 O4 1.5325(14) . ? P1 O1 1.5875(13) . ? P1 O2 1.6053(13) . ? O1 C3 1.401(2) . ? O2 C11 1.407(2) . ? O4 H4 0.89(3) . ? O5 C49' 1.434(10) . ? O5 C49 1.486(3) . ? O5 H5 0.94(3) . ? O6 C52 1.444(3) . ? O6 H6 0.85(3) . ? O7 C55 1.437(3) . ? O7 H7 0.89(3) . ? C1 C2 1.518(2) . ? C1 C10 1.519(2) . ? C1 C17 1.555(3) . ? C1 C9 1.559(3) . ? C2 C3 1.389(2) . ? C2 C7 1.393(2) . ? C3 C4 1.399(2) . ? C4 C5 1.398(2) . ? C4 C18 1.502(3) . ? C5 C6 1.389(3) . ? C5 H5A 0.9500 . ? C6 C7 1.389(3) . ? C6 H6A 0.9500 . ? C7 C8 1.515(3) . ? C8 C9 1.546(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.391(2) . ? C10 C15 1.400(2) . ? C11 C12 1.405(3) . ? C12 C13 1.400(3) . ? C12 C33 1.498(3) . ? C13 C14 1.393(3) . ? C13 H13 0.9500 . ? C14 C15 1.383(3) . ? C14 H14 0.9500 . ? C15 C16 1.510(3) . ? C16 C17 1.543(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C23 1.403(3) . ? C18 C19 1.418(3) . ? C19 C20 1.387(3) . ? C19 C24 1.525(3) . ? C20 C21 1.394(3) . ? C20 H20 0.9500 . ? C21 C22 1.390(3) . ? C21 C27 1.532(3) . ? C22 C23 1.406(3) . ? C22 H22 0.9500 . ? C23 C30 1.522(3) . ? C24 C26 1.533(3) . ? C24 C25 1.534(3) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.501(3) . ? C27 C29 1.527(3) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.531(3) . ? C30 C32 1.535(3) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.402(3) . ? C33 C38 1.423(3) . ? C34 C35 1.400(3) . ? C34 C39 1.526(3) . ? C35 C36 1.386(3) . ? C35 H35 0.9500 . ? C36 C37 1.392(3) . ? C36 C42 1.530(3) . ? C37 C38 1.389(3) . ? C37 H37 0.9500 . ? C38 C45 1.523(3) . ? C39 C40 1.533(3) . ? C39 C41 1.539(3) . ? C39 H39 1.0000 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C44 1.511(3) . ? C42 C43 1.514(4) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C47 1.529(3) . ? C45 C46 1.533(3) . ? C45 H45 1.0000 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.510(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.497(4) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C48' C49' 1.544(12) . ? C48' H48D 0.9800 . ? C48' H48E 0.9800 . ? C48' H48F 0.9800 . ? C49' C50' 1.565(12) . ? C49' H49' 1.0000 . ? C50' H50D 0.9800 . ? C50' H50E 0.9800 . ? C50' H50F 0.9800 . ? C51 C52 1.488(4) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.513(4) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 C55 1.525(4) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.494(4) . ? C55 H55 1.0000 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 P1 O4 118.29(8) . . ? O3 P1 O1 107.88(8) . . ? O4 P1 O1 106.49(7) . . ? O3 P1 O2 114.12(8) . . ? O4 P1 O2 102.89(8) . . ? O1 P1 O2 106.35(6) . . ? C3 O1 P1 122.63(11) . . ? C11 O2 P1 116.77(11) . . ? P1 O4 H4 113.4(16) . . ? C49' O5 H5 135.2(19) . . ? C49 O5 H5 110.3(18) . . ? C52 O6 H6 104(2) . . ? C55 O7 H7 112.7(18) . . ? C2 C1 C10 124.64(14) . . ? C2 C1 C17 111.89(15) . . ? C10 C1 C17 100.62(14) . . ? C2 C1 C9 99.87(14) . . ? C10 C1 C9 110.29(15) . . ? C17 C1 C9 109.25(14) . . ? C3 C2 C7 119.26(16) . . ? C3 C2 C1 130.55(16) . . ? C7 C2 C1 110.02(15) . . ? C2 C3 C4 121.42(16) . . ? C2 C3 O1 119.01(15) . . ? C4 C3 O1 119.47(15) . . ? C5 C4 C3 117.28(16) . . ? C5 C4 C18 120.70(16) . . ? C3 C4 C18 121.79(16) . . ? C6 C5 C4 122.19(17) . . ? C6 C5 H5A 118.9 . . ? C4 C5 H5A 118.9 . . ? C7 C6 C5 118.80(17) . . ? C7 C6 H6A 120.6 . . ? C5 C6 H6A 120.6 . . ? C6 C7 C2 120.58(17) . . ? C6 C7 C8 128.78(17) . . ? C2 C7 C8 110.64(16) . . ? C7 C8 C9 101.80(14) . . ? C7 C8 H8A 111.4 . . ? C9 C8 H8A 111.4 . . ? C7 C8 H8B 111.4 . . ? C9 C8 H8B 111.4 . . ? H8A C8 H8B 109.3 . . ? C8 C9 C1 104.65(15) . . ? C8 C9 H9A 110.8 . . ? C1 C9 H9A 110.8 . . ? C8 C9 H9B 110.8 . . ? C1 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? C11 C10 C15 118.97(16) . . ? C11 C10 C1 131.24(16) . . ? C15 C10 C1 109.51(15) . . ? C10 C11 C12 121.13(16) . . ? C10 C11 O2 118.96(15) . . ? C12 C11 O2 119.92(15) . . ? C13 C12 C11 117.38(17) . . ? C13 C12 C33 119.22(16) . . ? C11 C12 C33 123.21(16) . . ? C14 C13 C12 122.23(17) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C15 C14 C13 118.62(17) . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C14 C15 C10 120.98(17) . . ? C14 C15 C16 128.59(17) . . ? C10 C15 C16 110.42(16) . . ? C15 C16 C17 102.97(15) . . ? C15 C16 H16A 111.2 . . ? C17 C16 H16A 111.2 . . ? C15 C16 H16B 111.2 . . ? C17 C16 H16B 111.2 . . ? H16A C16 H16B 109.1 . . ? C16 C17 C1 104.69(15) . . ? C16 C17 H17A 110.8 . . ? C1 C17 H17A 110.8 . . ? C16 C17 H17B 110.8 . . ? C1 C17 H17B 110.8 . . ? H17A C17 H17B 108.9 . . ? C23 C18 C19 120.15(17) . . ? C23 C18 C4 121.20(16) . . ? C19 C18 C4 118.59(16) . . ? C20 C19 C18 118.44(17) . . ? C20 C19 C24 121.21(17) . . ? C18 C19 C24 120.29(17) . . ? C19 C20 C21 122.66(18) . . ? C19 C20 H20 118.7 . . ? C21 C20 H20 118.7 . . ? C22 C21 C20 118.07(18) . . ? C22 C21 C27 123.63(18) . . ? C20 C21 C27 118.28(18) . . ? C21 C22 C23 121.62(18) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C18 C23 C22 119.04(17) . . ? C18 C23 C30 120.67(16) . . ? C22 C23 C30 120.28(17) . . ? C19 C24 C26 109.75(18) . . ? C19 C24 C25 114.72(18) . . ? C26 C24 C25 109.65(18) . . ? C19 C24 H24 107.5 . . ? C26 C24 H24 107.5 . . ? C25 C24 H24 107.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C29 110.2(2) . . ? C28 C27 C21 115.43(18) . . ? C29 C27 C21 110.44(18) . . ? C28 C27 H27 106.8 . . ? C29 C27 H27 106.8 . . ? C21 C27 H27 106.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C23 C30 C31 112.73(16) . . ? C23 C30 C32 111.64(18) . . ? C31 C30 C32 109.80(17) . . ? C23 C30 H30 107.5 . . ? C31 C30 H30 107.5 . . ? C32 C30 H30 107.5 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C38 120.06(17) . . ? C34 C33 C12 121.37(17) . . ? C38 C33 C12 118.21(16) . . ? C35 C34 C33 118.84(17) . . ? C35 C34 C39 119.98(17) . . ? C33 C34 C39 121.18(17) . . ? C36 C35 C34 122.21(18) . . ? C36 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? C35 C36 C37 117.94(18) . . ? C35 C36 C42 123.29(18) . . ? C37 C36 C42 118.77(19) . . ? C38 C37 C36 122.58(19) . . ? C38 C37 H37 118.7 . . ? C36 C37 H37 118.7 . . ? C37 C38 C33 118.36(17) . . ? C37 C38 C45 120.02(18) . . ? C33 C38 C45 121.38(17) . . ? C34 C39 C40 112.58(17) . . ? C34 C39 C41 111.61(16) . . ? C40 C39 C41 109.75(17) . . ? C34 C39 H39 107.6 . . ? C40 C39 H39 107.6 . . ? C41 C39 H39 107.6 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C44 C42 C43 111.4(2) . . ? C44 C42 C36 113.61(19) . . ? C43 C42 C36 110.97(19) . . ? C44 C42 H42 106.8 . . ? C43 C42 H42 106.8 . . ? C36 C42 H42 106.8 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C38 C45 C47 110.03(18) . . ? C38 C45 C46 113.26(19) . . ? C47 C45 C46 110.39(19) . . ? C38 C45 H45 107.6 . . ? C47 C45 H45 107.6 . . ? C46 C45 H45 107.6 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 H48A 109.5 . . ? C49 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C49 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? O5 C49 C50 106.7(2) . . ? O5 C49 C48 107.8(2) . . ? C50 C49 C48 113.2(3) . . ? O5 C49 H49 109.7 . . ? C50 C49 H49 109.7 . . ? C48 C49 H49 109.7 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49' C48' H48D 109.5 . . ? C49' C48' H48E 109.5 . . ? H48D C48' H48E 109.5 . . ? C49' C48' H48F 109.5 . . ? H48D C48' H48F 109.5 . . ? H48E C48' H48F 109.5 . . ? O5 C49' C48' 106.0(9) . . ? O5 C49' C50' 101.7(8) . . ? C48' C49' C50' 115.1(14) . . ? O5 C49' H49' 111.2 . . ? C48' C49' H49' 111.2 . . ? C50' C49' H49' 111.2 . . ? C49' C50' H50D 109.5 . . ? C49' C50' H50E 109.5 . . ? H50D C50' H50E 109.5 . . ? C49' C50' H50F 109.5 . . ? H50D C50' H50F 109.5 . . ? H50E C50' H50F 109.5 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O6 C52 C51 107.7(2) . . ? O6 C52 C53 110.1(2) . . ? C51 C52 C53 113.2(3) . . ? O6 C52 H52 108.6 . . ? C51 C52 H52 108.6 . . ? C53 C52 H52 108.6 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C55 C54 H54A 109.5 . . ? C55 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C55 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O7 C55 C56 110.2(2) . . ? O7 C55 C54 106.4(2) . . ? C56 C55 C54 112.2(2) . . ? O7 C55 H55 109.4 . . ? C56 C55 H55 109.4 . . ? C54 C55 H55 109.4 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 P1 O1 C3 175.81(13) . . . . ? O4 P1 O1 C3 -56.24(14) . . . . ? O2 P1 O1 C3 52.99(14) . . . . ? O3 P1 O2 C11 -49.92(14) . . . . ? O4 P1 O2 C11 -179.36(12) . . . . ? O1 P1 O2 C11 68.89(13) . . . . ? C10 C1 C2 C3 33.6(3) . . . . ? C17 C1 C2 C3 -87.7(2) . . . . ? C9 C1 C2 C3 156.85(18) . . . . ? C10 C1 C2 C7 -151.35(17) . . . . ? C17 C1 C2 C7 87.38(18) . . . . ? C9 C1 C2 C7 -28.12(19) . . . . ? C7 C2 C3 C4 -8.0(3) . . . . ? C1 C2 C3 C4 166.63(18) . . . . ? C7 C2 C3 O1 175.63(16) . . . . ? C1 C2 C3 O1 -9.7(3) . . . . ? P1 O1 C3 C2 -81.48(18) . . . . ? P1 O1 C3 C4 102.10(17) . . . . ? C2 C3 C4 C5 4.7(3) . . . . ? O1 C3 C4 C5 -178.96(15) . . . . ? C2 C3 C4 C18 -169.88(16) . . . . ? O1 C3 C4 C18 6.4(3) . . . . ? C3 C4 C5 C6 1.3(3) . . . . ? C18 C4 C5 C6 175.96(17) . . . . ? C4 C5 C6 C7 -3.9(3) . . . . ? C5 C6 C7 C2 0.5(3) . . . . ? C5 C6 C7 C8 -179.43(19) . . . . ? C3 C2 C7 C6 5.3(3) . . . . ? C1 C2 C7 C6 -170.35(17) . . . . ? C3 C2 C7 C8 -174.74(16) . . . . ? C1 C2 C7 C8 9.6(2) . . . . ? C6 C7 C8 C9 -166.42(19) . . . . ? C2 C7 C8 C9 13.7(2) . . . . ? C7 C8 C9 C1 -30.72(19) . . . . ? C2 C1 C9 C8 35.59(18) . . . . ? C10 C1 C9 C8 168.39(15) . . . . ? C17 C1 C9 C8 -81.90(18) . . . . ? C2 C1 C10 C11 31.4(3) . . . . ? C17 C1 C10 C11 157.59(19) . . . . ? C9 C1 C10 C11 -87.1(2) . . . . ? C2 C1 C10 C15 -154.93(18) . . . . ? C17 C1 C10 C15 -28.72(18) . . . . ? C9 C1 C10 C15 86.54(18) . . . . ? C15 C10 C11 C12 -10.0(3) . . . . ? C1 C10 C11 C12 163.16(18) . . . . ? C15 C10 C11 O2 170.54(15) . . . . ? C1 C10 C11 O2 -16.3(3) . . . . ? P1 O2 C11 C10 -79.86(18) . . . . ? P1 O2 C11 C12 100.70(17) . . . . ? C10 C11 C12 C13 5.8(3) . . . . ? O2 C11 C12 C13 -174.75(16) . . . . ? C10 C11 C12 C33 -169.18(17) . . . . ? O2 C11 C12 C33 10.2(3) . . . . ? C11 C12 C13 C14 1.2(3) . . . . ? C33 C12 C13 C14 176.41(18) . . . . ? C12 C13 C14 C15 -3.8(3) . . . . ? C13 C14 C15 C10 -0.5(3) . . . . ? C13 C14 C15 C16 -179.88(19) . . . . ? C11 C10 C15 C14 7.3(3) . . . . ? C1 C10 C15 C14 -167.27(18) . . . . ? C11 C10 C15 C16 -173.23(17) . . . . ? C1 C10 C15 C16 12.2(2) . . . . ? C14 C15 C16 C17 -170.5(2) . . . . ? C10 C15 C16 C17 10.1(2) . . . . ? C15 C16 C17 C1 -27.61(19) . . . . ? C2 C1 C17 C16 168.23(15) . . . . ? C10 C1 C17 C16 33.92(17) . . . . ? C9 C1 C17 C16 -82.14(18) . . . . ? C5 C4 C18 C23 70.0(2) . . . . ? C3 C4 C18 C23 -115.6(2) . . . . ? C5 C4 C18 C19 -107.1(2) . . . . ? C3 C4 C18 C19 67.3(2) . . . . ? C23 C18 C19 C20 1.6(3) . . . . ? C4 C18 C19 C20 178.72(17) . . . . ? C23 C18 C19 C24 -175.56(17) . . . . ? C4 C18 C19 C24 1.6(2) . . . . ? C18 C19 C20 C21 -1.1(3) . . . . ? C24 C19 C20 C21 176.04(18) . . . . ? C19 C20 C21 C22 0.0(3) . . . . ? C19 C20 C21 C27 -178.19(18) . . . . ? C20 C21 C22 C23 0.6(3) . . . . ? C27 C21 C22 C23 178.68(19) . . . . ? C19 C18 C23 C22 -1.0(3) . . . . ? C4 C18 C23 C22 -178.09(17) . . . . ? C19 C18 C23 C30 177.74(17) . . . . ? C4 C18 C23 C30 0.7(3) . . . . ? C21 C22 C23 C18 -0.1(3) . . . . ? C21 C22 C23 C30 -178.84(18) . . . . ? C20 C19 C24 C26 -100.8(2) . . . . ? C18 C19 C24 C26 76.3(2) . . . . ? C20 C19 C24 C25 23.2(3) . . . . ? C18 C19 C24 C25 -159.74(17) . . . . ? C22 C21 C27 C28 25.9(3) . . . . ? C20 C21 C27 C28 -156.0(2) . . . . ? C22 C21 C27 C29 -99.9(2) . . . . ? C20 C21 C27 C29 78.2(3) . . . . ? C18 C23 C30 C31 131.61(19) . . . . ? C22 C23 C30 C31 -49.6(2) . . . . ? C18 C23 C30 C32 -104.2(2) . . . . ? C22 C23 C30 C32 74.5(2) . . . . ? C13 C12 C33 C34 76.8(2) . . . . ? C11 C12 C33 C34 -108.2(2) . . . . ? C13 C12 C33 C38 -96.3(2) . . . . ? C11 C12 C33 C38 78.6(2) . . . . ? C38 C33 C34 C35 -0.1(3) . . . . ? C12 C33 C34 C35 -173.12(17) . . . . ? C38 C33 C34 C39 179.05(17) . . . . ? C12 C33 C34 C39 6.0(3) . . . . ? C33 C34 C35 C36 0.6(3) . . . . ? C39 C34 C35 C36 -178.54(18) . . . . ? C34 C35 C36 C37 -0.8(3) . . . . ? C34 C35 C36 C42 179.13(19) . . . . ? C35 C36 C37 C38 0.5(3) . . . . ? C42 C36 C37 C38 -179.42(19) . . . . ? C36 C37 C38 C33 0.0(3) . . . . ? C36 C37 C38 C45 174.48(19) . . . . ? C34 C33 C38 C37 -0.2(3) . . . . ? C12 C33 C38 C37 173.06(18) . . . . ? C34 C33 C38 C45 -174.62(18) . . . . ? C12 C33 C38 C45 -1.4(3) . . . . ? C35 C34 C39 C40 -44.3(2) . . . . ? C33 C34 C39 C40 136.52(18) . . . . ? C35 C34 C39 C41 79.6(2) . . . . ? C33 C34 C39 C41 -99.6(2) . . . . ? C35 C36 C42 C44 -23.0(3) . . . . ? C37 C36 C42 C44 157.0(2) . . . . ? C35 C36 C42 C43 103.4(3) . . . . ? C37 C36 C42 C43 -76.6(3) . . . . ? C37 C38 C45 C47 -83.1(2) . . . . ? C33 C38 C45 C47 91.2(2) . . . . ? C37 C38 C45 C46 40.9(3) . . . . ? C33 C38 C45 C46 -144.7(2) . . . . ? C49' O5 C49 C50 53.0(8) . . . . ? C49' O5 C49 C48 -68.8(8) . . . . ? C49 O5 C49' C48' 78.6(13) . . . . ? C49 O5 C49' C50' -42.0(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O7 H7 O3 0.89(3) 1.85(3) 2.740(2) 175(3) . O6 H6 O7 0.85(3) 1.84(3) 2.675(2) 170(3) . O5 H5 O6 0.94(3) 1.79(3) 2.733(2) 176(3) . O4 H4 O5 0.89(3) 1.66(3) 2.546(2) 174(2) . _refine_diff_density_max 0.431 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.048 _shelxl_version_number 2013-2 _shelx_res_file ; TITL _m130510b CELL 0.71075 11.77900 17.45100 13.84900 90.000 110.544 90.000 ZERR 2 0.00130 0.00200 0.00160 0.000 0.004 0.000 LATT -1 SYMM -X, .50+Y, -Z SFAC C H O P UNIT 112 166 14 2 L.S. 5 ACTA BOND $H FMAP 2 PLAN 5 LIST 4 HTAB O7 O3 HTAB O6 O7 HTAB O5 O6 HTAB O4 O5 SIZE 0.260 0.240 0.180 CONF HTAB WPDB -2 SHEL 99999.000000 0.000000 dfix 1.54 .01 c48 c49 c49 c50 c48' c49' c49' c50' dfix 1.45 .01 o5 c49 o5 c49' dfix 2.52 .01 c48 c50 sadi .01 o5 c48 o5 c50 o5 c48' o5 c50' eadp c48 c48' eadp c50 c50' eadp c49 c49' TEMP -160.0 WGHT 0.035200 FVAR 1.92915 0.83875 P1 4 0.305093 0.721696 0.229266 11.00000 0.01540 0.02047 = 0.01512 0.00223 0.00643 0.00153 O1 3 0.328155 0.789770 0.162365 11.00000 0.01873 0.01672 = 0.01298 -0.00024 0.00626 0.00154 O2 3 0.379821 0.649507 0.211325 11.00000 0.01586 0.01671 = 0.01908 0.00170 0.00699 -0.00070 O3 3 0.343410 0.747591 0.336776 11.00000 0.02407 0.02949 = 0.01555 0.00144 0.00677 0.00530 O4 3 0.172957 0.696858 0.176041 11.00000 0.01702 0.03037 = 0.02158 0.00498 0.00746 -0.00040 H4 2 0.143379 0.670396 0.217139 11.00000 -1.50000 O5 3 0.073559 0.622079 0.282949 11.00000 0.04970 0.03272 = 0.03993 -0.00816 0.03058 -0.01176 H5 2 0.069201 0.648252 0.341192 11.00000 -1.50000 O6 3 0.071449 0.695435 0.456670 11.00000 0.02970 0.04286 = 0.02327 -0.00247 0.01039 -0.00476 H6 2 0.107961 0.736187 0.452014 11.00000 -1.50000 O7 3 0.193608 0.816057 0.424222 11.00000 0.03662 0.03341 = 0.03757 0.00156 0.01950 0.00527 H7 2 0.243592 0.792138 0.398993 11.00000 -1.50000 C1 1 0.526314 0.724824 0.089909 11.00000 0.01625 0.01612 = 0.01915 0.00103 0.00884 0.00130 C2 1 0.397257 0.747991 0.026945 11.00000 0.01828 0.01261 = 0.01726 0.00073 0.00782 -0.00282 C3 1 0.308516 0.782351 0.056959 11.00000 0.01720 0.01311 = 0.01479 -0.00021 0.00712 -0.00261 C4 1 0.203535 0.813419 -0.015451 11.00000 0.01699 0.01469 = 0.01712 0.00043 0.00664 -0.00293 C5 1 0.187136 0.803390 -0.119655 11.00000 0.01935 0.02150 = 0.01641 0.00166 0.00464 -0.00072 AFIX 43 H5A 2 0.117434 0.824871 -0.170310 11.00000 -1.20000 AFIX 0 C6 1 0.269383 0.763054 -0.151588 11.00000 0.02569 0.02530 = 0.01398 -0.00132 0.00803 -0.00301 AFIX 43 H6A 2 0.253772 0.754342 -0.222809 11.00000 -1.20000 AFIX 0 C7 1 0.374830 0.735699 -0.077512 11.00000 0.02215 0.01790 = 0.01785 -0.00128 0.01073 -0.00294 C8 1 0.477828 0.691255 -0.092539 11.00000 0.02823 0.02552 = 0.02069 -0.00303 0.01358 0.00320 AFIX 23 H8A 2 0.529404 0.724799 -0.117594 11.00000 -1.20000 H8B 2 0.447219 0.648236 -0.141391 11.00000 -1.20000 AFIX 0 C9 1 0.547298 0.662006 0.017900 11.00000 0.02286 0.02095 = 0.02516 -0.00210 0.01204 0.00311 AFIX 23 H9A 2 0.634760 0.656242 0.029682 11.00000 -1.20000 H9B 2 0.514840 0.611990 0.029888 11.00000 -1.20000 AFIX 0 C10 1 0.567589 0.696190 0.200430 11.00000 0.01665 0.01345 = 0.01769 -0.00043 0.00723 0.00109 C11 1 0.507089 0.654500 0.253153 11.00000 0.01438 0.01527 = 0.01845 -0.00207 0.00603 0.00042 C12 1 0.570935 0.617106 0.346281 11.00000 0.01891 0.01442 = 0.01817 0.00081 0.00702 0.00119 C13 1 0.696269 0.629335 0.388664 11.00000 0.01912 0.02239 = 0.01857 0.00266 0.00429 0.00165 AFIX 43 H13 2 0.741588 0.603878 0.450912 11.00000 -1.20000 AFIX 0 C14 1 0.756742 0.677571 0.342626 11.00000 0.01654 0.02484 = 0.02400 0.00102 0.00556 0.00032 AFIX 43 H14 2 0.840983 0.687376 0.374947 11.00000 -1.20000 AFIX 0 C15 1 0.691581 0.710883 0.248893 11.00000 0.01661 0.01897 = 0.02273 0.00078 0.00908 -0.00029 C16 1 0.735947 0.764491 0.184193 11.00000 0.01768 0.02920 = 0.02589 0.00328 0.00847 -0.00227 AFIX 23 H16A 2 0.788546 0.737355 0.153137 11.00000 -1.20000 H16B 2 0.781316 0.808134 0.225666 11.00000 -1.20000 AFIX 0 C17 1 0.617322 0.791652 0.100631 11.00000 0.02107 0.01969 = 0.02322 0.00301 0.01084 -0.00121 AFIX 23 H17A 2 0.629732 0.800967 0.034515 11.00000 -1.20000 H17B 2 0.587605 0.839421 0.122205 11.00000 -1.20000 AFIX 0 C18 1 0.117100 0.861689 0.016345 11.00000 0.01828 0.01553 = 0.01481 0.00178 0.00523 0.00226 C19 1 0.156476 0.934572 0.060848 11.00000 0.02016 0.01749 = 0.01849 0.00300 0.00488 0.00020 C20 1 0.075576 0.979670 0.088222 11.00000 0.02760 0.01497 = 0.02329 0.00052 0.00840 0.00182 AFIX 43 H20 2 0.102072 1.028142 0.119143 11.00000 -1.20000 AFIX 0 C21 1 -0.043059 0.956728 0.072186 11.00000 0.02517 0.01992 = 0.02261 0.00283 0.01086 0.00439 C22 1 -0.080636 0.885659 0.026881 11.00000 0.01794 0.02417 = 0.02487 0.00060 0.00681 0.00237 AFIX 43 H22 2 -0.161398 0.869324 0.014802 11.00000 -1.20000 AFIX 0 C23 1 -0.002049 0.837363 -0.001499 11.00000 0.01826 0.01868 = 0.01805 0.00025 0.00529 0.00105 C24 1 0.282885 0.963611 0.073199 11.00000 0.02368 0.01743 = 0.03501 -0.00302 0.00911 -0.00237 AFIX 13 H24 2 0.339905 0.919275 0.095741 11.00000 -1.20000 AFIX 0 C25 1 0.330632 1.027434 0.153396 11.00000 0.02826 0.02198 = 0.03450 -0.00226 0.00351 -0.00321 AFIX 137 H25A 2 0.324401 1.011126 0.219068 11.00000 -1.50000 H25B 2 0.282368 1.073949 0.129284 11.00000 -1.50000 H25C 2 0.415641 1.038010 0.163083 11.00000 -1.50000 AFIX 0 C26 1 0.285329 0.990718 -0.031371 11.00000 0.05306 0.03131 = 0.04637 -0.00851 0.02976 -0.01862 AFIX 137 H26A 2 0.235483 1.036904 -0.052905 11.00000 -1.50000 H26B 2 0.253079 0.950258 -0.082811 11.00000 -1.50000 H26C 2 0.368986 1.002316 -0.025230 11.00000 -1.50000 AFIX 0 C27 1 -0.125867 1.012133 0.102428 11.00000 0.03118 0.02302 = 0.03220 -0.00222 0.01574 0.00303 AFIX 13 H27 2 -0.074326 1.038166 0.167337 11.00000 -1.20000 AFIX 0 C28 1 -0.229362 0.975622 0.124758 11.00000 0.05773 0.02996 = 0.06855 -0.00043 0.04483 0.00350 AFIX 137 H28A 2 -0.198289 0.934953 0.176089 11.00000 -1.50000 H28B 2 -0.286641 0.953697 0.061153 11.00000 -1.50000 H28C 2 -0.270738 1.014375 0.151613 11.00000 -1.50000 AFIX 0 C29 1 -0.172920 1.074633 0.020908 11.00000 0.05901 0.03787 = 0.06145 0.01611 0.03464 0.02517 AFIX 137 H29A 2 -0.214281 1.114187 0.046484 11.00000 -1.50000 H29B 2 -0.229950 1.052198 -0.042431 11.00000 -1.50000 H29C 2 -0.104723 1.097620 0.006358 11.00000 -1.50000 AFIX 0 C30 1 -0.046807 0.760568 -0.052805 11.00000 0.01726 0.02390 = 0.02756 -0.00765 0.00745 -0.00291 AFIX 13 H30 2 0.025833 0.730769 -0.052498 11.00000 -1.20000 AFIX 0 C31 1 -0.111698 0.713111 0.005152 11.00000 0.02372 0.02493 = 0.04041 -0.00641 0.01402 -0.00583 AFIX 137 H31A 2 -0.190122 0.736686 -0.003298 11.00000 -1.50000 H31B 2 -0.061865 0.711353 0.078569 11.00000 -1.50000 H31C 2 -0.124635 0.660923 -0.022724 11.00000 -1.50000 AFIX 0 C32 1 -0.129689 0.770469 -0.165704 11.00000 0.02556 0.04721 = 0.03157 -0.01348 0.00538 -0.00521 AFIX 137 H32A 2 -0.087057 0.799849 -0.202819 11.00000 -1.50000 H32B 2 -0.203382 0.797900 -0.168518 11.00000 -1.50000 H32C 2 -0.151544 0.719979 -0.197853 11.00000 -1.50000 AFIX 0 C33 1 0.513288 0.560901 0.396669 11.00000 0.01619 0.01846 = 0.01746 0.00289 0.00411 0.00123 C34 1 0.491838 0.579335 0.487292 11.00000 0.01738 0.01850 = 0.01706 0.00173 0.00348 0.00058 C35 1 0.450014 0.521969 0.537112 11.00000 0.02338 0.02458 = 0.01813 0.00295 0.00822 0.00113 AFIX 43 H35 2 0.434695 0.534534 0.598160 11.00000 -1.20000 AFIX 0 C36 1 0.430201 0.447460 0.500372 11.00000 0.02426 0.02176 = 0.02374 0.00465 0.00767 -0.00109 C37 1 0.451730 0.430543 0.410077 11.00000 0.02966 0.01873 = 0.02613 0.00081 0.00903 0.00022 AFIX 43 H37 2 0.437814 0.379766 0.383817 11.00000 -1.20000 AFIX 0 C38 1 0.492748 0.484977 0.356875 11.00000 0.02393 0.01803 = 0.01998 0.00156 0.00682 -0.00007 C39 1 0.514954 0.660000 0.532621 11.00000 0.02479 0.01921 = 0.01727 0.00133 0.00598 -0.00013 AFIX 13 H39 2 0.518642 0.695352 0.476969 11.00000 -1.20000 AFIX 0 C40 1 0.413116 0.688326 0.568529 11.00000 0.03770 0.02660 = 0.02564 -0.00073 0.01412 0.00457 AFIX 137 H40A 2 0.417860 0.661601 0.632067 11.00000 -1.50000 H40B 2 0.334464 0.677898 0.514872 11.00000 -1.50000 H40C 2 0.421909 0.743588 0.581607 11.00000 -1.50000 AFIX 0 C41 1 0.637329 0.665313 0.622103 11.00000 0.03486 0.02638 = 0.02547 -0.00188 0.00092 -0.00307 AFIX 137 H41A 2 0.702561 0.649226 0.598014 11.00000 -1.50000 H41B 2 0.636026 0.631774 0.678462 11.00000 -1.50000 H41C 2 0.651327 0.718320 0.646815 11.00000 -1.50000 AFIX 0 C42 1 0.386216 0.383430 0.554076 11.00000 0.03600 0.02360 = 0.03098 0.00487 0.01451 -0.00366 AFIX 13 H42 2 0.431568 0.336056 0.549021 11.00000 -1.20000 AFIX 0 C43 1 0.253022 0.366852 0.498178 11.00000 0.04656 0.06191 = 0.05023 0.02298 0.00712 -0.02449 AFIX 137 H43A 2 0.238640 0.357228 0.425116 11.00000 -1.50000 H43B 2 0.204761 0.411000 0.504637 11.00000 -1.50000 H43C 2 0.229445 0.321597 0.528596 11.00000 -1.50000 AFIX 0 C44 1 0.412979 0.397920 0.667513 11.00000 0.07637 0.04569 = 0.03296 0.01056 0.01901 -0.02479 AFIX 137 H44A 2 0.395431 0.351532 0.699631 11.00000 -1.50000 H44B 2 0.362212 0.440109 0.675737 11.00000 -1.50000 H44C 2 0.498649 0.411516 0.700734 11.00000 -1.50000 AFIX 0 C45 1 0.525433 0.461292 0.264054 11.00000 0.04472 0.02066 = 0.02355 -0.00063 0.01604 -0.00110 AFIX 13 H45 2 0.523312 0.508361 0.222273 11.00000 -1.20000 AFIX 0 C46 1 0.436554 0.403296 0.193965 11.00000 0.05537 0.03668 = 0.03195 -0.01373 0.01532 -0.00558 AFIX 137 H46A 2 0.354142 0.424183 0.171941 11.00000 -1.50000 H46B 2 0.439930 0.355425 0.231873 11.00000 -1.50000 H46C 2 0.458763 0.393197 0.133269 11.00000 -1.50000 AFIX 0 C47 1 0.654724 0.429716 0.299803 11.00000 0.04569 0.04129 = 0.04110 -0.00895 0.02652 0.00023 AFIX 137 H47A 2 0.661625 0.386510 0.346732 11.00000 -1.50000 H47B 2 0.711801 0.470053 0.335744 11.00000 -1.50000 H47C 2 0.673595 0.412349 0.239841 11.00000 -1.50000 PART 1 AFIX 0 C48 1 -0.015615 0.504400 0.315651 21.00000 0.04397 0.04070 = 0.03896 0.00021 0.01781 -0.01380 AFIX 137 H48A 2 -0.033694 0.529336 0.372003 21.00000 -1.50000 H48B 2 -0.002696 0.449478 0.330092 21.00000 -1.50000 H48C 2 -0.083812 0.511742 0.250892 21.00000 -1.50000 AFIX 0 C49 1 0.097446 0.539300 0.306353 21.00000 0.03668 0.02843 = 0.02746 0.00149 0.01263 -0.00768 AFIX 13 H49 2 0.166749 0.533126 0.372939 21.00000 -1.20000 AFIX 0 C50 1 0.130435 0.505844 0.220184 21.00000 0.06741 0.03400 = 0.05418 0.00142 0.03528 0.00235 AFIX 137 H50A 2 0.063550 0.513744 0.154716 21.00000 -1.50000 H50B 2 0.145766 0.450827 0.231983 21.00000 -1.50000 H50C 2 0.203583 0.531063 0.217449 21.00000 -1.50000 PART 2 AFIX 0 C48' 1 -0.050772 0.515629 0.287292 -21.00000 0.04397 0.04070 = 0.03896 0.00021 0.01781 -0.01380 AFIX 137 H48D 2 -0.008618 0.505779 0.360916 -21.00000 -1.50000 H48E 2 -0.086092 0.467789 0.252620 -21.00000 -1.50000 H48F 2 -0.115336 0.553283 0.278606 -21.00000 -1.50000 AFIX 0 C49' 1 0.040209 0.547204 0.239591 -21.00000 0.03668 0.02843 = 0.02746 0.00149 0.01263 -0.00768 AFIX 13 H49' 2 0.003199 0.549554 0.162694 -21.00000 -1.20000 AFIX 0 C50' 1 0.165829 0.505543 0.274738 -21.00000 0.06741 0.03400 = 0.05418 0.00142 0.03528 0.00235 AFIX 137 H50D 2 0.217008 0.528668 0.240046 -21.00000 -1.50000 H50E 2 0.153670 0.451115 0.256619 -21.00000 -1.50000 H50F 2 0.205466 0.510758 0.349559 -21.00000 -1.50000 PART 0 AFIX 0 C51 1 0.105776 0.600703 0.586156 11.00000 0.15264 0.06308 = 0.04003 0.01077 0.03254 -0.01196 AFIX 137 H51A 2 0.164226 0.576520 0.559879 11.00000 -1.50000 H51B 2 0.025153 0.578749 0.551183 11.00000 -1.50000 H51C 2 0.130340 0.591573 0.660513 11.00000 -1.50000 AFIX 0 C52 1 0.102143 0.684635 0.566253 11.00000 0.03036 0.05638 = 0.02304 -0.00423 0.00922 -0.00513 AFIX 13 H52 2 0.184842 0.706257 0.602489 11.00000 -1.20000 AFIX 0 C53 1 0.012670 0.726754 0.603053 11.00000 0.03162 0.12393 = 0.03253 -0.02074 0.01085 0.00051 AFIX 137 H53A 2 -0.069428 0.707899 0.565601 11.00000 -1.50000 H53B 2 0.016552 0.781763 0.590317 11.00000 -1.50000 H53C 2 0.032913 0.717890 0.677086 11.00000 -1.50000 AFIX 0 C54 1 0.029748 0.902318 0.397714 11.00000 0.04895 0.05999 = 0.09092 0.00133 0.03110 0.01831 AFIX 137 H54A 2 0.061342 0.917822 0.470331 11.00000 -1.50000 H54B 2 -0.023930 0.858006 0.389565 11.00000 -1.50000 H54C 2 -0.015790 0.944882 0.355566 11.00000 -1.50000 AFIX 0 C55 1 0.134982 0.880911 0.362978 11.00000 0.03493 0.03691 = 0.03091 -0.00103 0.00711 0.00737 AFIX 13 H55 2 0.102642 0.865849 0.288593 11.00000 -1.20000 AFIX 0 C56 1 0.223139 0.945215 0.377466 11.00000 0.05109 0.04864 = 0.05285 0.01276 0.00963 -0.00499 AFIX 137 H56A 2 0.286221 0.930244 0.350170 11.00000 -1.50000 H56B 2 0.260439 0.956944 0.451101 11.00000 -1.50000 H56C 2 0.180591 0.990642 0.340631 11.00000 -1.50000 AFIX 0 HKLF 4 REM _m130510b REM R1 = 0.0524 for 16973 Fo > 4sig(Fo) and 0.0624 for all 20147 data REM 619 parameters refined using 14 restraints END WGHT 0.0352 0.0000 REM Instructions for potential hydrogen bonds HTAB O4 O5 HTAB O5 O6 HTAB O6 O7 HTAB O7 O3 REM Highest difference peak 0.431, deepest hole -0.382, 1-sigma level 0.048 Q1 1 0.3206 0.7503 0.1787 11.00000 0.05 0.26 Q2 1 0.5268 0.7062 0.1414 11.00000 0.05 0.25 Q3 1 0.4980 0.5546 0.5313 11.00000 0.05 0.23 Q4 1 0.6354 0.6143 0.3619 11.00000 0.05 0.23 Q5 1 0.3744 0.7217 0.2974 11.00000 0.05 0.23 ; _shelx_res_checksum 72771 _shelx_hkl_file ; 0 1 0 1.43 1.41 0 0 1 4267.17 116.00 0 0 -1 4250.35 116.00 0 0 -1 2868.16 23.29 0 0 -1 4044.89 108.52 0 0 1 3448.10 94.59 -1 0 013286.48 85.85 1 0 012433.95 75.31 1 0 012766.05 79.17 1 0 012064.77 77.62 -1 0 012483.76 77.73 -1 0 012123.13 74.93 0 -1 -153036.65 282.35 0 -1 155060.22 291.03 0 1 151480.46 272.24 0 1 -154095.73 285.17 0 1 151739.31 271.76 0 -1 152910.42 278.48 0 1 155552.83 295.09 0 -1 -153024.91 280.13 0 -1 154443.33 285.18 0 -1 -150587.43 268.18 1 0 -131478.20 174.86 -1 0 132963.33 178.62 1 0 -132621.87 181.51 -1 0 133091.45 181.79 1 0 -135949.11 191.95 -1 0 134105.86 181.53 -1 -1 025633.80 147.92 1 1 024099.29 140.71 -1 -1 023073.75 136.02 1 -1 022800.58 121.09 -1 -1 025395.34 143.38 1 1 025843.75 145.54 -1 1 021666.84 127.80 1 -1 020841.90 123.60 1 1 023038.51 134.21 1 -1 022757.98 134.77 -1 1 022734.95 135.05 1 1 -113903.10 81.75 -1 -1 114961.14 86.48 1 1 -117472.92 106.77 -1 1 115072.90 83.81 -1 1 112952.68 87.19 1 1 -114575.29 86.17 1 -1 -114451.40 89.55 -1 -1 115445.76 91.16 -1 -1 115340.67 96.28 1 -1 -113987.09 91.32 -1 1 113992.98 92.12 1 -1 -114138.62 78.76 0 -2 023627.46 134.86 0 2 023760.93 132.61 0 -2 023410.13 140.74 0 2 023973.58 143.34 0 2 119717.29 113.13 0 2 120821.04 126.59 0 -2 -120934.18 135.73 0 -2 120771.79 122.57 -1 0 -1 1407.93 71.40 1 0 1 1405.99 70.80 -1 0 -1 1395.45 72.97 1 0 1 1365.75 70.02 1 0 1 1459.30 72.72 0 -2 -120329.63 117.01 0 2 -122042.80 128.60 0 -2 121497.62 124.41 0 2 121432.37 136.98 0 2 -121136.64 127.98 0 -2 120972.80 129.66 0 -2 -120768.35 127.28 -1 0 -1 1357.27 68.10 0 2 -123317.20 135.86 1 -2 011731.23 67.15 -1 -2 012847.45 80.83 -1 -2 011700.15 85.48 -1 2 011198.14 56.62 1 -2 012077.26 82.63 -1 2 012175.08 89.93 1 -2 012222.90 89.14 -1 -2 012507.38 89.25 1 2 011688.89 86.29 1 2 011563.67 73.37 1 2 011370.79 83.57 -1 0 2 4958.31 137.07 -1 0 2 5444.32 41.67 -1 0 2 5762.83 115.07 1 0 -2 5771.37 118.98 1 0 -2 6100.80 124.64 1 0 -2 5689.88 113.91 1 -1 112282.61 83.16 1 -1 111633.96 89.69 1 1 112218.38 88.49 1 1 112527.99 91.30 -1 1 -112345.61 82.72 1 -1 112249.36 83.27 -1 1 -113052.60 89.12 -1 -1 -112374.60 88.97 -1 -1 -112901.57 95.31 1 1 113506.23 98.98 -1 -1 -113311.00 98.25 -1 1 -112767.23 98.42 1 2 -121202.86 127.72 -1 2 121605.89 117.41 1 -2 -121025.49 123.75 1 2 -123525.57 143.21 -1 -2 121616.58 136.37 -1 2 122011.64 131.81 -1 -2 121327.48 125.93 1 -2 -121713.54 117.90 1 2 -121445.08 118.76 -1 2 121533.41 139.65 1 -2 -122169.08 144.59 -1 -2 123690.31 131.40 0 0 -221986.84 144.38 0 0 -221939.15 124.94 0 0 222711.25 146.99 0 0 224224.70 154.41 0 0 222444.63 128.80 0 0 -218629.31 123.67 1 1 -2 3350.67 89.98 1 1 -2 3534.44 98.90 1 -1 -2 4027.38 112.38 -1 -1 2 4423.03 122.51 -1 1 2 3390.99 95.09 -1 1 2 3769.90 105.76 -1 1 2 3296.79 94.41 -1 -1 2 3428.91 97.21 1 1 -2 3603.29 104.45 1 -1 -2 3498.28 97.58 1 -1 -2 3579.17 100.59 0 1 -2 8046.54 158.12 0 -1 -2 8282.55 166.73 0 1 2 8845.53 177.87 0 -1 2 7928.25 155.01 0 1 -2 8929.93 180.80 0 -1 -2 8683.34 176.92 0 -1 -2 8393.52 170.84 0 1 2 8210.17 168.70 0 1 2 8565.16 173.50 0 -1 2 9187.61 185.89 0 -1 2 8431.81 170.39 0 1 -2 7887.63 161.12 2 0 -1 3017.10 86.27 2 0 -1 3288.28 91.69 -2 0 1 3033.72 85.41 -2 0 1 3124.74 89.81 2 0 -1 3437.77 97.91 -2 0 1 2980.85 84.72 0 3 0 15.59 9.28 0 -3 0 -0.33 12.16 0 3 0 2.85 5.85 0 -3 0 -0.46 2.40 0 -3 0 7.11 9.42 1 2 129774.63 186.62 1 -2 130231.37 182.66 -1 -2 -131044.62 196.77 -1 2 -130255.86 187.79 -1 2 -130355.54 182.40 -1 -2 -134258.94 209.35 -1 2 -130645.97 174.46 1 2 135210.75 218.07 1 -2 130801.70 176.84 1 -2 130879.89 198.30 1 2 131158.29 190.56 -1 -2 -130761.69 185.80 -2 1 1 3411.78 97.74 -2 1 1 3549.49 102.68 2 1 -1 3488.22 98.60 2 -1 -1 3222.33 92.67 2 1 -1 3657.56 103.24 2 -1 -1 3188.41 92.39 2 1 -1 3447.96 97.88 -2 -1 1 3362.65 95.69 -2 -1 1 3483.60 98.92 -2 1 1 3638.61 99.34 -2 -1 1 3064.85 88.70 2 -1 -1 3826.54 103.95 2 0 0 7790.91 160.29 -2 0 0 7592.48 154.34 -2 0 0 8433.73 173.86 2 0 0 7969.71 160.58 2 0 0 8769.95 178.33 -2 0 0 7756.69 158.04 -1 -2 2 2138.07 84.66 1 2 -2 2229.36 93.10 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2342.24 134.06 0 -14 -4 2785.55 174.26 2 -2 10 2258.97 135.83 0 14 -4 2828.70 177.43 0 14 4 2790.55 180.08 2 -2 10 2333.06 159.85 0 -15 0 34.44 31.54 -6 -4 -6 1705.01 143.26 -6 -4 -6 1576.09 117.69 -6 4 -6 1488.53 104.19 7 10 -6 160.78 56.30 -7 -10 6 122.60 40.38 -6 4 -6 1495.18 118.43 -7 10 6 142.50 47.63 -7 -10 6 144.85 39.06 6 4 6 1674.75 300.55 -7 10 6 158.93 43.00 6 -4 6 1392.34 98.31 2 -8 -10 1943.93 176.29 -2 8 10 1901.48 145.80 2 8 -10 1963.29 143.69 -2 8 10 1813.26 123.91 -2 -8 10 1854.31 123.12 -4 -8 10 2102.33 68.25 -4 8 10 1724.02 116.86 4 -8 -10 1779.22 118.23 4 8 -10 1852.95 134.44 -4 8 10 1522.13 109.04 -5 13 3 1818.88 120.45 -5 -13 3 1865.77 146.70 -5 13 3 1917.84 138.92 5 13 -3 1820.35 127.75 3 -4 9 701.42 39.18 -3 -4 -9 897.54 216.63 3 4 9 732.58 81.33 3 4 9 719.57 159.80 -3 4 -9 763.46 61.85 3 -4 9 701.11 141.22 -8 -2 10 2559.59 160.86 -8 2 10 2218.73 136.08 -8 -2 10 2353.08 165.74 -8 2 10 2237.75 144.16 8 -2 -10 2382.21 143.73 8 2 -10 2094.19 52.83 -10 2 3 759.51 38.45 10 0 -6 320.74 78.64 10 2 -3 899.18 59.45 -10 -2 3 1126.37 255.50 -10 -2 3 871.52 65.16 10 -2 -3 891.30 73.45 -10 2 3 929.87 273.86 -10 0 6 285.13 80.67 -10 0 6 338.34 101.86 5 13 -1 1781.54 129.88 -5 13 1 1768.44 117.65 -5 13 1 1975.32 143.56 -5 -13 1 1954.53 137.18 5 9 5 226.20 78.57 5 9 5 222.99 90.88 -5 -9 -5 248.20 83.89 -5 9 -5 217.41 69.41 -5 9 -5 171.52 54.98 5 -9 5 266.42 65.22 -2 -13 6 1266.76 72.65 -2 13 6 1237.81 57.41 2 13 -6 1067.59 52.48 2 -13 -6 1160.87 57.49 -2 -13 6 1158.58 43.05 -2 13 6 1236.89 82.59 -6 4 11 1267.24 62.66 -1 -8 -9 2495.46 165.34 -6 -4 11 1257.20 67.41 -6 4 11 1322.99 100.60 1 8 9 2449.81 156.32 6 4 -11 1360.96 104.66 1 -8 9 2504.55 142.70 1 8 9 2532.99 162.65 6 -4 -11 1274.52 64.45 -1 8 -9 2438.27 154.17 1 -8 9 2313.18 150.19 7 0 -1111922.15 112.61 -8 -9 5 1137.09 80.40 -7 0 1113983.44 191.53 -8 9 5 1051.26 74.97 7 0 -1112428.31 213.78 -8 9 5 1011.09 66.98 8 9 -5 993.88 59.71 -8 -9 5 1036.86 53.26 0 15 1 503.63 190.79 -10 -1 6 3966.73 190.56 10 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139.93 -9 -6 1 1654.83 147.44 -6 -12 4 2287.79 169.94 -8 6 -2 3254.71 136.93 8 -6 2 3817.21 181.01 8 6 2 3528.72 176.70 -8 -6 -2 3121.18 153.95 -8 6 -2 3285.66 167.98 -8 -6 -2 3585.86 177.27 1 -11 -8 512.05 82.38 -1 11 8 500.44 34.95 -1 11 8 686.16 170.02 1 11 -8 547.09 23.99 -1 -11 8 608.34 79.55 1 11 -8 606.09 50.04 -1 -15 0 510.96 143.53 -1 15 0 571.63 162.14 1 -15 0 580.08 97.52 1 15 0 602.02 52.87 0 9 -9 747.91 195.21 1 -13 -6 1444.15 100.73 0 9 9 696.78 46.14 0 -9 -9 786.67 184.72 0 -9 9 903.59 101.76 7 -1 -11 590.60 104.44 -7 1 11 766.77 208.19 7 1 -11 777.26 179.28 -1 -13 6 1471.87 108.45 7 1 -11 606.91 29.09 -10 0 2 1902.55 135.95 -10 0 2 2200.68 137.52 10 0 -2 2240.63 148.50 0 -9 9 742.98 21.39 9 7 -3 919.99 56.26 0 9 9 860.55 232.87 -7 -1 11 666.53 156.95 -9 -7 3 1002.35 70.40 -9 -7 3 946.35 52.73 1 13 -6 1483.51 98.39 -9 7 3 1001.37 69.31 9 -7 -3 1005.16 215.71 -1 13 6 1483.97 124.41 -1 13 6 1442.08 93.39 -1 -13 6 1377.87 86.38 9 -5 0 658.62 143.13 1 -15 -1 1094.77 55.81 -9 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5154.73 226.07 8 8 -7 858.41 47.49 7 -3 5 5658.75 242.73 -7 3 -5 5356.57 229.97 -7 -3 -5 5713.93 393.58 -7 -3 -5 5329.63 234.70 -8 -8 7 792.50 122.05 -8 8 7 1015.86 63.25 -9 -1 9 5112.78 218.02 -9 1 9 4572.16 192.28 9 -1 -9 4716.07 198.46 -4 6 11 2095.87 75.19 4 -6 -11 1999.77 134.11 -4 -6 11 2089.93 85.20 -9 1 9 4400.51 198.44 -9 -1 9 4207.89 195.96 -4 6 11 2112.58 138.13 4 6 -11 2284.22 151.65 9 1 -9 4763.82 200.65 -8 7 8 3369.51 135.05 3 14 -4 1427.90 102.30 3 -14 -4 1241.36 54.93 7 6 4 1193.30 77.71 -3 14 4 1169.48 70.58 -3 -14 4 1328.07 99.74 -3 14 4 1311.38 109.12 -8 -7 8 3526.21 162.42 -7 6 -4 1262.72 66.59 8 7 -8 3356.77 143.91 -7 -6 -4 1447.24 108.08 -7 -6 -4 1271.88 83.59 -8 7 8 3346.84 164.87 -7 6 -4 1309.31 88.82 -8 7 8 3493.69 165.07 -3 0 12 63.72 30.91 3 0 -12 170.66 64.76 -8 -7 8 3591.29 203.34 7 -6 4 1506.19 107.55 -3 0 12 104.69 25.79 -2 10 9 800.83 57.88 -3 -13 6 365.14 17.35 -3 13 6 591.72 144.39 2 10 -9 797.49 52.93 -9 7 5 1002.96 69.01 -3 13 6 410.28 90.78 -3 -13 6 420.88 116.89 -9 -7 5 1021.84 63.16 2 -10 -9 1039.42 185.82 9 7 -5 1140.42 65.19 -9 -7 5 1147.67 63.51 3 13 -6 399.02 115.52 -9 7 5 1128.83 74.92 -2 10 9 828.26 48.96 -2 -10 9 815.45 45.62 3 -13 -6 403.43 28.92 -10 2 6 6916.20 276.68 -10 -3 5 3630.18 172.26 -10 -2 6 7091.87 303.43 -10 2 6 7368.77 313.60 10 -3 -5 3552.63 166.46 -10 -2 6 6750.90 281.34 10 3 -5 3782.20 169.62 -10 3 5 3883.45 183.78 -10 -3 5 3542.36 180.66 -10 3 5 3494.38 146.15 10 2 -6 6615.05 280.69 10 -2 -6 6801.82 284.64 7 11 -2 2365.92 159.67 -7 11 2 2146.76 138.42 2 3 10 989.70 65.70 2 -3 10 1027.56 48.32 -7 11 2 2412.41 164.90 -7 -11 2 2233.66 133.79 -2 3 -10 987.28 64.24 -7 -11 2 2253.55 149.51 -2 -3 -10 1204.05 250.09 2 3 10 1093.10 165.07 2 -3 10 1145.29 143.38 0 7 10 857.54 178.58 0 -7 -10 705.53 127.14 -4 -1 12 1227.47 73.36 0 7 -10 609.86 72.76 -1 -5 11 141.75 50.48 -1 5 11 101.55 29.89 -1 5 11 88.70 55.88 1 -5 -11 88.27 34.10 1 5 -11 138.05 50.80 0 7 10 611.71 48.74 0 -7 10 801.78 182.73 -4 1 12 1161.80 50.01 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2753.16 180.55 -7 11 4 1126.70 75.13 -1 15 -1 100.65 28.23 -8 -3 10 726.55 70.65 2 -9 8 2385.00 151.79 -7 11 4 1246.03 68.30 2 9 8 2558.56 181.35 -1 -15 -1 70.31 27.11 -7 2 11 3019.66 187.53 7 2 -11 2783.12 157.13 8 3 -10 662.90 32.07 -8 -3 10 805.16 205.90 -7 -11 4 1367.56 89.78 4 -12 -7 552.69 29.71 4 12 -7 532.72 37.27 -4 12 7 714.33 200.40 -4 12 7 592.92 37.30 -4 -12 7 754.41 183.72 -4 -12 7 519.19 23.15 -8 -9 1 4765.89 207.06 8 -9 -1 4720.90 209.72 -8 9 1 4554.15 204.17 8 9 -1 5044.44 226.14 -8 -9 1 5086.95 230.52 2 14 3 818.30 62.12 -2 14 -3 679.48 36.70 2 -14 3 725.31 140.97 -2 14 -3 703.50 49.01 2 14 3 696.57 18.49 -2 -14 -3 707.44 120.40 -4 14 2 1407.43 95.79 4 14 -2 1214.83 77.34 4 -14 -2 1325.29 82.15 -4 -14 2 1321.19 105.86 -4 14 2 1306.70 77.71 -10 2 2 3295.48 143.67 5 13 0 625.86 20.41 -5 13 0 690.82 179.67 5 13 0 671.59 179.81 -5 13 0 675.43 43.23 5 -13 0 603.37 19.28 -5 -13 0 651.62 177.67 10 -2 -2 3644.99 169.59 -10 -2 2 3518.35 164.77 10 2 -2 3565.20 169.63 -10 -2 2 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984.26 83.97 -8 4 11 989.41 69.53 -8 4 11 916.78 106.90 -9 9 2 1904.03 81.25 9 -9 -2 1854.48 115.03 9 9 -2 1807.91 112.73 -9 -9 2 1964.30 131.72 -9 -9 2 1757.79 111.60 -9 6 9 143.11 56.08 -9 -6 9 174.63 60.34 9 6 -9 184.05 72.71 -9 6 9 249.39 51.75 -9 6 9 227.81 53.07 -9 -6 9 184.86 46.28 -3 4 -10 3689.31 202.29 3 4 10 3537.78 202.92 -3 -4 -10 3720.21 206.48 3 4 10 3570.15 190.11 3 -4 10 3845.70 209.07 3 -4 10 3725.79 188.86 -2 -9 -9 3972.58 226.06 -8 -11 2 709.37 86.20 -8 -11 2 827.34 62.57 -8 11 2 755.65 59.40 8 11 -2 764.69 194.52 -2 9 -9 4082.15 218.16 2 9 9 3774.51 200.71 2 -9 9 4145.70 221.68 2 9 9 3996.48 218.93 2 -9 9 3971.11 194.24 -8 11 2 763.63 63.45 0 2 12 924.24 64.56 0 -2 12 760.57 30.41 0 2 12 835.99 160.68 0 2 -12 939.87 69.39 0 -2 12 1111.77 262.75 0 -2 -12 862.86 62.21 -2 -16 1 1470.11 94.61 2 -16 -1 1332.81 76.51 -2 16 1 1397.83 96.87 2 16 -1 1333.87 92.69 -4 15 0 1506.07 84.90 4 15 0 1502.65 100.03 -4 15 0 1508.70 99.77 -4 -15 0 1678.57 105.69 4 -15 0 1630.31 81.13 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