data_7b' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_absolute_configuration syn _chemical_formula_moiety ? _chemical_formula_sum 'C21 H20 F N O4' _chemical_formula_weight 369.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.8117(6) _cell_length_b 5.5768(3) _cell_length_c 12.9121(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.001(2) _cell_angle_gamma 90.00 _cell_volume 898.90(8) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2802 _cell_measurement_theta_min 3.24 _cell_measurement_theta_max 27.55 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 0.101 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9511 _exptl_absorpt_correction_T_max 0.9950 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type Bruker _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13888 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 27.55 _reflns_number_total 4092 _reflns_number_gt 2802 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0313P)^2^+0.1074P] 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 none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.4(9) _refine_ls_number_reflns 4092 _refine_ls_number_parameters 247 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0455 _refine_ls_wR_factor_ref 0.0870 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 F1 F -0.31835(9) 0.4235(3) 0.85424(11) 0.0813(5) Uani 1 1 d . . . O1 O 0.27679(10) 0.6974(2) 0.68602(10) 0.0469(3) Uani 1 1 d . . . O2 O 0.41916(13) 0.5579(3) 0.62014(12) 0.0614(4) Uani 1 1 d . . . O3 O 0.38939(11) 0.2486(2) 0.72645(11) 0.0486(4) Uani 1 1 d . . . O4 O 0.35593(11) 0.5770(3) 0.95597(10) 0.0575(4) Uani 1 1 d . . . N1 N 0.10195(11) 0.5272(3) 0.83887(11) 0.0399(4) Uani 1 1 d . . . C1 C -0.19042(17) 0.6307(4) 0.78701(17) 0.0524(6) Uani 1 1 d . . . H1 H -0.2443 0.7288 0.7489 0.063 Uiso 1 1 calc R . . C2 C -0.21404(16) 0.4537(5) 0.84963(17) 0.0546(6) Uani 1 1 d . . . C3 C -0.13938(18) 0.3012(4) 0.90925(16) 0.0554(6) Uani 1 1 d . . . H3 H -0.1592 0.1828 0.9518 0.067 Uiso 1 1 calc R . . C4 C -0.03501(17) 0.3311(4) 0.90335(16) 0.0508(5) Uani 1 1 d . . . H4 H 0.0173 0.2303 0.9422 0.061 Uiso 1 1 calc R . . C5 C -0.00555(15) 0.5114(3) 0.83967(14) 0.0407(5) Uani 1 1 d . . . C6 C 0.13331(14) 0.6919(3) 0.78163(14) 0.0364(4) Uani 1 1 d . . . C7 C 0.06201(15) 0.8649(3) 0.71870(15) 0.0384(4) Uani 1 1 d . . . C8 C 0.09888(16) 1.0488(4) 0.66199(15) 0.0460(5) Uani 1 1 d . . . H8 H 0.1717 1.0620 0.6643 0.055 Uiso 1 1 calc R . . C9 C 0.02891(18) 1.2091(4) 0.60331(16) 0.0539(5) Uani 1 1 d . . . H9 H 0.0542 1.3306 0.5661 0.065 Uiso 1 1 calc R . . C10 C -0.08020(18) 1.1901(4) 0.59938(17) 0.0567(6) Uani 1 1 d . . . H10 H -0.1278 1.2968 0.5580 0.068 Uiso 1 1 calc R . . C11 C -0.11789(16) 1.0166(4) 0.65564(16) 0.0518(6) Uani 1 1 d . . . H11 H -0.1909 1.0085 0.6532 0.062 Uiso 1 1 calc R . . C12 C -0.04852(15) 0.8498(4) 0.71722(14) 0.0402(5) Uani 1 1 d . . . C13 C -0.08296(15) 0.6649(4) 0.78008(15) 0.0419(5) Uani 1 1 d . . . C14 C 0.38953(17) 0.6531(4) 0.70778(17) 0.0488(5) Uani 1 1 d . . . H14 H 0.4307 0.7977 0.7335 0.059 Uiso 1 1 calc R . . C15 C 0.40714(15) 0.4588(4) 0.79092(15) 0.0427(5) Uani 1 1 d . . . H15 H 0.4789 0.4638 0.8377 0.051 Uiso 1 1 calc R . . C16 C 0.31814(14) 0.4977(3) 0.85054(14) 0.0405(5) Uani 1 1 d . . . H16 H 0.2744 0.3529 0.8484 0.049 Uiso 1 1 calc R . . C17 C 0.25242(14) 0.7024(4) 0.78938(14) 0.0391(4) Uani 1 1 d . . . H17 H 0.2794 0.8537 0.8239 0.047 Uiso 1 1 calc R . . C18 C 0.41679(17) 0.2991(4) 0.62735(16) 0.0460(5) Uani 1 1 d . . . C19 C 0.52689(16) 0.2071(4) 0.62591(17) 0.0567(6) Uani 1 1 d . . . H19A H 0.5782 0.2751 0.6843 0.085 Uiso 1 1 calc R . . H19B H 0.5448 0.2519 0.5603 0.085 Uiso 1 1 calc R . . H19C H 0.5279 0.0355 0.6322 0.085 Uiso 1 1 calc R . . C20 C 0.33182(18) 0.1990(5) 0.53951(17) 0.0654(6) Uani 1 1 d . . . H20A H 0.3241 0.0304 0.5508 0.098 Uiso 1 1 calc R . . H20B H 0.3516 0.2235 0.4729 0.098 Uiso 1 1 calc R . . H20C H 0.2651 0.2786 0.5383 0.098 Uiso 1 1 calc R . . C21 C 0.3887(3) 0.3872(7) 1.0281(2) 0.0987(11) Uani 1 1 d . . . H21A H 0.3322 0.2712 1.0206 0.148 Uiso 1 1 calc R . . H21B H 0.4049 0.4487 1.0994 0.148 Uiso 1 1 calc R . . H21C H 0.4514 0.3127 1.0135 0.148 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0470(7) 0.1154(12) 0.0879(9) -0.0051(10) 0.0282(6) -0.0181(8) O1 0.0541(9) 0.0436(8) 0.0499(8) 0.0091(7) 0.0262(6) 0.0067(7) O2 0.0883(11) 0.0403(8) 0.0738(10) 0.0106(8) 0.0567(9) 0.0061(8) O3 0.0679(10) 0.0347(8) 0.0521(8) 0.0040(7) 0.0322(7) 0.0020(7) O4 0.0607(9) 0.0694(10) 0.0419(8) -0.0007(8) 0.0103(7) 0.0142(8) N1 0.0403(9) 0.0420(10) 0.0393(8) -0.0004(8) 0.0127(7) -0.0015(8) C1 0.0401(12) 0.0673(16) 0.0495(12) -0.0079(12) 0.0095(10) 0.0015(10) C2 0.0406(12) 0.0762(16) 0.0519(13) -0.0127(14) 0.0203(10) -0.0141(13) C3 0.0561(14) 0.0659(16) 0.0483(12) -0.0016(12) 0.0200(11) -0.0152(12) C4 0.0522(13) 0.0564(14) 0.0459(12) 0.0035(11) 0.0155(10) -0.0045(11) C5 0.0430(11) 0.0461(13) 0.0345(9) -0.0053(10) 0.0121(8) -0.0046(10) C6 0.0432(11) 0.0334(10) 0.0343(9) -0.0051(9) 0.0121(8) -0.0004(9) C7 0.0466(11) 0.0347(10) 0.0352(10) -0.0052(9) 0.0118(8) 0.0008(9) C8 0.0533(12) 0.0404(11) 0.0462(11) -0.0013(11) 0.0154(9) 0.0015(10) C9 0.0686(15) 0.0427(12) 0.0514(12) 0.0061(11) 0.0153(10) 0.0077(11) C10 0.0649(16) 0.0496(13) 0.0508(12) 0.0042(12) 0.0029(11) 0.0173(12) C11 0.0461(12) 0.0561(15) 0.0500(12) -0.0040(11) 0.0045(9) 0.0098(11) C12 0.0410(11) 0.0438(11) 0.0348(10) -0.0083(9) 0.0060(8) 0.0017(9) C13 0.0420(11) 0.0464(12) 0.0385(10) -0.0094(10) 0.0117(8) -0.0028(10) C14 0.0556(14) 0.0365(12) 0.0643(14) 0.0010(10) 0.0345(11) 0.0002(10) C15 0.0438(11) 0.0351(10) 0.0538(12) -0.0018(10) 0.0209(9) 0.0006(9) C16 0.0414(11) 0.0405(12) 0.0420(10) 0.0001(9) 0.0146(8) -0.0003(8) C17 0.0428(11) 0.0359(10) 0.0420(10) -0.0041(10) 0.0170(8) -0.0014(9) C18 0.0562(13) 0.0400(13) 0.0486(12) 0.0050(10) 0.0262(10) 0.0025(9) C19 0.0572(14) 0.0572(13) 0.0628(14) -0.0005(12) 0.0284(11) 0.0036(12) C20 0.0673(15) 0.0751(16) 0.0552(13) 0.0104(14) 0.0164(11) -0.0061(14) C21 0.122(2) 0.116(3) 0.0568(16) 0.0259(18) 0.0177(15) 0.051(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 F1 C2 1.361(2) . ? O1 C14 1.429(2) . ? O1 C17 1.438(2) . ? O2 C14 1.378(2) . ? O2 C18 1.447(2) . ? O3 C15 1.426(2) . ? O3 C18 1.429(2) . ? O4 C16 1.409(2) . ? O4 C21 1.410(3) . ? N1 C6 1.298(2) . ? N1 C5 1.382(2) . ? C1 C2 1.353(3) . ? C1 C13 1.413(3) . ? C1 H1 0.9300 . ? C2 C3 1.378(3) . ? C3 C4 1.366(3) . ? C3 H3 0.9300 . ? C4 C5 1.403(3) . ? C4 H4 0.9300 . ? C5 C13 1.402(3) . ? C6 C7 1.446(3) . ? C6 C17 1.508(2) . ? C7 C8 1.402(3) . ? C7 C12 1.414(3) . ? C8 C9 1.368(3) . ? C8 H8 0.9300 . ? C9 C10 1.391(3) . ? C9 H9 0.9300 . ? C10 C11 1.362(3) . ? C10 H10 0.9300 . ? C11 C12 1.403(3) . ? C11 H11 0.9300 . ? C12 C13 1.441(3) . ? C14 C15 1.506(3) . ? C14 H14 0.9800 . ? C15 C16 1.528(2) . ? C15 H15 0.9800 . ? C16 C17 1.529(3) . ? C16 H16 0.9800 . ? C17 H17 0.9800 . ? C18 C20 1.493(3) . ? C18 C19 1.505(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? 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 C14 O1 C17 104.00(14) . . ? C14 O2 C18 108.53(15) . . ? C15 O3 C18 108.76(14) . . ? C16 O4 C21 112.9(2) . . ? C6 N1 C5 119.08(16) . . ? C2 C1 C13 119.2(2) . . ? C2 C1 H1 120.4 . . ? C13 C1 H1 120.4 . . ? C1 C2 F1 118.0(2) . . ? C1 C2 C3 124.31(18) . . ? F1 C2 C3 117.7(2) . . ? C4 C3 C2 117.3(2) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C5 121.0(2) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? N1 C5 C13 122.67(17) . . ? N1 C5 C4 116.74(18) . . ? C13 C5 C4 120.59(17) . . ? N1 C6 C7 123.68(17) . . ? N1 C6 C17 115.34(16) . . ? C7 C6 C17 120.89(17) . . ? C8 C7 C12 119.37(17) . . ? C8 C7 C6 122.46(17) . . ? C12 C7 C6 118.15(17) . . ? C9 C8 C7 120.75(19) . . ? C9 C8 H8 119.6 . . ? C7 C8 H8 119.6 . . ? C8 C9 C10 119.9(2) . . ? C8 C9 H9 120.1 . . ? C10 C9 H9 120.1 . . ? C11 C10 C9 120.6(2) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 121.19(19) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 118.20(18) . . ? C11 C12 C13 123.93(17) . . ? C7 C12 C13 117.87(17) . . ? C5 C13 C1 117.52(19) . . ? C5 C13 C12 118.53(17) . . ? C1 C13 C12 123.94(19) . . ? O2 C14 O1 110.97(18) . . ? O2 C14 C15 106.45(16) . . ? O1 C14 C15 104.30(15) . . ? O2 C14 H14 111.6 . . ? O1 C14 H14 111.6 . . ? C15 C14 H14 111.6 . . ? O3 C15 C14 101.35(15) . . ? O3 C15 C16 111.84(15) . . ? C14 C15 C16 104.34(15) . . ? O3 C15 H15 112.8 . . ? C14 C15 H15 112.8 . . ? C16 C15 H15 112.8 . . ? O4 C16 C15 113.46(15) . . ? O4 C16 C17 107.12(15) . . ? C15 C16 C17 103.46(14) . . ? O4 C16 H16 110.8 . . ? C15 C16 H16 110.8 . . ? C17 C16 H16 110.8 . . ? O1 C17 C6 111.44(14) . . ? O1 C17 C16 104.80(14) . . ? C6 C17 C16 115.91(16) . . ? O1 C17 H17 108.1 . . ? C6 C17 H17 108.1 . . ? C16 C17 H17 108.1 . . ? O3 C18 O2 105.50(15) . . ? O3 C18 C20 108.82(17) . . ? O2 C18 C20 110.3(2) . . ? O3 C18 C19 111.32(16) . . ? O2 C18 C19 107.82(18) . . ? C20 C18 C19 112.85(19) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 C21 H21A 109.5 . . ? O4 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O4 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 C13 C1 C2 F1 -179.53(18) . . . . ? C13 C1 C2 C3 0.5(3) . . . . ? C1 C2 C3 C4 -0.6(3) . . . . ? F1 C2 C3 C4 179.35(19) . . . . ? C2 C3 C4 C5 0.5(3) . . . . ? C6 N1 C5 C13 0.7(3) . . . . ? C6 N1 C5 C4 -179.63(17) . . . . ? C3 C4 C5 N1 -179.96(18) . . . . ? C3 C4 C5 C13 -0.3(3) . . . . ? C5 N1 C6 C7 0.9(2) . . . . ? C5 N1 C6 C17 177.46(16) . . . . ? N1 C6 C7 C8 176.57(17) . . . . ? C17 C6 C7 C8 0.2(3) . . . . ? N1 C6 C7 C12 -1.7(3) . . . . ? C17 C6 C7 C12 -178.13(17) . . . . ? C12 C7 C8 C9 -1.7(3) . . . . ? C6 C7 C8 C9 180.00(17) . . . . ? C7 C8 C9 C10 -0.1(3) . . . . ? C8 C9 C10 C11 1.6(3) . . . . ? C9 C10 C11 C12 -1.3(3) . . . . ? C10 C11 C12 C7 -0.6(3) . . . . ? C10 C11 C12 C13 178.79(19) . . . . ? C8 C7 C12 C11 2.0(3) . . . . ? C6 C7 C12 C11 -179.60(16) . . . . ? C8 C7 C12 C13 -177.36(16) . . . . ? C6 C7 C12 C13 1.0(2) . . . . ? N1 C5 C13 C1 179.75(17) . . . . ? C4 C5 C13 C1 0.1(3) . . . . ? N1 C5 C13 C12 -1.3(3) . . . . ? C4 C5 C13 C12 179.01(18) . . . . ? C2 C1 C13 C5 -0.2(3) . . . . ? C2 C1 C13 C12 -179.04(19) . . . . ? C11 C12 C13 C5 -178.96(17) . . . . ? C7 C12 C13 C5 0.4(3) . . . . ? C11 C12 C13 C1 -0.1(3) . . . . ? C7 C12 C13 C1 179.27(18) . . . . ? C18 O2 C14 O1 -92.3(2) . . . . ? C18 O2 C14 C15 20.5(2) . . . . ? C17 O1 C14 O2 158.09(16) . . . . ? C17 O1 C14 C15 43.85(19) . . . . ? C18 O3 C15 C14 28.52(18) . . . . ? C18 O3 C15 C16 139.16(16) . . . . ? O2 C14 C15 O3 -29.99(19) . . . . ? O1 C14 C15 O3 87.42(16) . . . . ? O2 C14 C15 C16 -146.27(17) . . . . ? O1 C14 C15 C16 -28.87(19) . . . . ? C21 O4 C16 C15 -85.0(2) . . . . ? C21 O4 C16 C17 161.52(19) . . . . ? O3 C15 C16 O4 139.61(16) . . . . ? C14 C15 C16 O4 -111.65(19) . . . . ? O3 C15 C16 C17 -104.68(16) . . . . ? C14 C15 C16 C17 4.06(19) . . . . ? C14 O1 C17 C6 -167.20(16) . . . . ? C14 O1 C17 C16 -41.10(18) . . . . ? N1 C6 C17 O1 127.99(17) . . . . ? C7 C6 C17 O1 -55.3(2) . . . . ? N1 C6 C17 C16 8.3(2) . . . . ? C7 C6 C17 C16 -175.05(15) . . . . ? O4 C16 C17 O1 142.03(14) . . . . ? C15 C16 C17 O1 21.90(18) . . . . ? O4 C16 C17 C6 -94.69(18) . . . . ? C15 C16 C17 C6 145.18(16) . . . . ? C15 O3 C18 O2 -17.3(2) . . . . ? C15 O3 C18 C20 -135.63(19) . . . . ? C15 O3 C18 C19 99.38(19) . . . . ? C14 O2 C18 O3 -2.8(2) . . . . ? C14 O2 C18 C20 114.54(19) . . . . ? C14 O2 C18 C19 -121.85(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.144 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.038