data_x_a _audit_creation_method 'SHELXL-2016/4' _shelx_SHELXL_version_number '2016/4' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C14 H20 O3' _chemical_formula_weight 236.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.0333(5) _cell_length_b 13.7700(12) _cell_length_c 14.9912(13) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1245.45(18) _cell_formula_units_Z 4 _cell_measurement_temperature 250(2) _cell_measurement_reflns_used 9829 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 61.91 _exptl_crystal_description bar _exptl_crystal_colour colorless _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_F_000 512 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.060 _exptl_absorpt_coefficient_mu 0.701 _shelx_estimated_absorpt_T_min 0.884 _shelx_estimated_absorpt_T_max 0.959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6704 _exptl_absorpt_correction_T_max 0.7521 _exptl_absorpt_process_details 'SADABS-2012/1 (Bruker,2012)' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 250(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker Kappa APEX-Duo CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22857 _diffrn_reflns_av_unetI/netI 0.0079 _diffrn_reflns_av_R_equivalents 0.0215 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.360 _diffrn_reflns_theta_max 61.934 _diffrn_reflns_theta_full 61.934 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 1944 _reflns_number_gt 1940 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.683 _reflns_Friedel_fraction_max 0.999 _reflns_Friedel_fraction_full 0.999 _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 'Bruker APEX3' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2016/4 (Sheldrick, 2016)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ? _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^)+(0.0428P)^2^+0.1239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 785 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.09(3) _chemical_absolute_configuration ad _refine_ls_number_reflns 1944 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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_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 C1 C 0.3766(3) 0.53018(12) 0.21007(11) 0.0315(4) Uani 1 1 d . . . . . H1 H 0.244(3) 0.5381(13) 0.1716(13) 0.034(5) Uiso 1 1 d . . . . . O1 O 0.5315(2) 0.40944(9) 0.10525(8) 0.0402(3) Uani 1 1 d . . . . . H1O H 0.413(5) 0.405(2) 0.0696(17) 0.073(8) Uiso 1 1 d . . . . . O2 O 0.3315(2) 0.61457(9) 0.49675(8) 0.0397(3) Uani 1 1 d . . . . . H2O H 0.444(5) 0.6528(19) 0.5236(17) 0.077(8) Uiso 1 1 d . . . . . C2 C 0.5488(3) 0.60557(11) 0.18660(10) 0.0296(4) Uani 1 1 d . . . . . O3 O 0.6335(2) 0.71953(10) 0.57882(8) 0.0441(3) Uani 1 1 d . . . . . H4O H 0.754(4) 0.679(2) 0.5900(17) 0.069(8) Uiso 1 1 d . . . . . H3O H 0.691(5) 0.773(2) 0.5568(17) 0.075(8) Uiso 1 1 d . . . . . C3 C 0.5757(3) 0.63686(13) 0.09893(11) 0.0386(4) Uani 1 1 d . . . . . H3 H 0.480(4) 0.6106(16) 0.0516(14) 0.051(5) Uiso 1 1 d . . . . . C4 C 0.7420(3) 0.70083(13) 0.07534(12) 0.0434(4) Uani 1 1 d . . . . . H4 H 0.756(3) 0.7215(14) 0.0147(14) 0.045(5) Uiso 1 1 d . . . . . C6 C 0.8574(3) 0.70695(12) 0.22802(11) 0.0342(4) Uani 1 1 d . . . . . H6 H 0.951(3) 0.7310(14) 0.2753(13) 0.042(5) Uiso 1 1 d . . . . . C5 C 0.8834(3) 0.73561(13) 0.14042(12) 0.0422(4) Uani 1 1 d . . . . . H5 H 1.005(4) 0.7804(16) 0.1235(14) 0.054(6) Uiso 1 1 d . . . . . C8 C 0.6667(3) 0.61408(12) 0.34986(10) 0.0323(4) Uani 1 1 d . . . . . H8B H 0.612(4) 0.6701(14) 0.3825(12) 0.040(5) Uiso 1 1 d . . . . . H8A H 0.816(4) 0.5981(16) 0.3773(14) 0.050(5) Uiso 1 1 d . . . . . C7 C 0.6911(3) 0.64179(11) 0.25246(10) 0.0287(4) Uani 1 1 d . . . . . C9 C 0.5086(3) 0.52920(12) 0.36875(10) 0.0313(4) Uani 1 1 d . . . . . C10 C 0.3053(3) 0.53867(13) 0.30807(11) 0.0339(4) Uani 1 1 d . . . . . H10B H 0.194(3) 0.4851(14) 0.3240(12) 0.035(5) Uiso 1 1 d . . . . . H10A H 0.230(3) 0.6007(16) 0.3176(13) 0.043(5) Uiso 1 1 d . . . . . C11 C 0.6198(3) 0.43027(13) 0.35208(12) 0.0394(4) Uani 1 1 d . . . . . H11A H 0.758(4) 0.4230(15) 0.3887(14) 0.048(6) Uiso 1 1 d . . . . . H11B H 0.514(4) 0.3777(17) 0.3758(13) 0.050(6) Uiso 1 1 d . . . . . C12 C 0.6697(3) 0.40869(14) 0.25404(12) 0.0390(4) Uani 1 1 d . . . . . H12B H 0.793(3) 0.4502(14) 0.2314(13) 0.040(5) Uiso 1 1 d . . . . . H12A H 0.712(3) 0.3403(14) 0.2468(12) 0.038(5) Uiso 1 1 d . . . . . C13 C 0.4675(3) 0.42674(12) 0.19576(11) 0.0346(4) Uani 1 1 d . . . . . H13 H 0.351(4) 0.3825(15) 0.2130(12) 0.036(5) Uiso 1 1 d . . . . . C14 C 0.4432(3) 0.52827(13) 0.46743(12) 0.0386(4) Uani 1 1 d . . . . . H14A H 0.344(4) 0.4752(15) 0.4759(13) 0.044(5) Uiso 1 1 d . . . . . H14B H 0.583(4) 0.5156(14) 0.5068(14) 0.047(5) 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 C1 0.0256(8) 0.0337(8) 0.0351(8) -0.0012(7) -0.0054(7) 0.0010(7) O1 0.0410(7) 0.0418(7) 0.0378(6) -0.0102(5) -0.0091(6) 0.0031(5) O2 0.0380(7) 0.0454(7) 0.0356(6) -0.0015(5) 0.0100(5) 0.0031(5) C2 0.0297(8) 0.0281(8) 0.0310(8) -0.0011(6) -0.0024(6) 0.0028(6) O3 0.0475(8) 0.0423(7) 0.0426(7) 0.0026(6) 0.0011(6) 0.0029(6) C3 0.0481(10) 0.0371(9) 0.0306(8) -0.0008(7) -0.0074(8) 0.0008(8) C4 0.0615(12) 0.0402(9) 0.0284(9) 0.0042(7) 0.0027(8) -0.0050(9) C6 0.0345(9) 0.0352(8) 0.0330(8) -0.0033(7) 0.0002(8) -0.0049(7) C5 0.0496(11) 0.0388(9) 0.0383(9) 0.0017(7) 0.0079(8) -0.0091(8) C8 0.0303(9) 0.0398(9) 0.0269(8) -0.0009(7) 0.0007(7) -0.0022(8) C7 0.0283(8) 0.0295(7) 0.0284(8) -0.0020(6) 0.0010(7) 0.0029(6) C9 0.0316(8) 0.0329(8) 0.0294(8) 0.0009(7) 0.0016(7) 0.0024(7) C10 0.0257(8) 0.0349(8) 0.0412(9) 0.0003(7) 0.0019(7) -0.0006(7) C11 0.0455(10) 0.0368(9) 0.0360(9) 0.0019(7) -0.0039(9) 0.0102(8) C12 0.0437(10) 0.0352(9) 0.0382(9) -0.0050(7) -0.0062(8) 0.0137(8) C13 0.0356(9) 0.0314(8) 0.0368(9) -0.0031(7) -0.0028(8) -0.0018(7) C14 0.0436(10) 0.0361(9) 0.0361(9) 0.0043(8) 0.0092(8) 0.0002(8) _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 C1 C2 1.510(2) . ? C1 C10 1.535(2) . ? C1 C13 1.541(2) . ? C1 H1 0.994(19) . ? O1 C13 1.431(2) . ? O1 H1O 0.89(3) . ? O2 C14 1.435(2) . ? O2 H2O 0.95(3) . ? C2 C3 1.393(2) . ? C2 C7 1.400(2) . ? O3 H4O 0.93(3) . ? O3 H3O 0.88(3) . ? C3 C4 1.381(3) . ? C3 H3 0.98(2) . ? C4 C5 1.382(3) . ? C4 H4 0.96(2) . ? C6 C5 1.380(2) . ? C6 C7 1.395(2) . ? C6 H6 0.96(2) . ? C5 H5 0.99(2) . ? C8 C7 1.516(2) . ? C8 C9 1.535(2) . ? C8 H8B 0.971(19) . ? C8 H8A 1.01(2) . ? C9 C14 1.531(2) . ? C9 C10 1.533(2) . ? C9 C11 1.539(2) . ? C10 H10B 1.028(19) . ? C10 H10A 0.98(2) . ? C11 C12 1.529(2) . ? C11 H11A 1.00(2) . ? C11 H11B 1.03(2) . ? C12 C13 1.521(3) . ? C12 H12B 1.00(2) . ? C12 H12A 0.98(2) . ? C13 H13 0.96(2) . ? C14 H14A 0.95(2) . ? C14 H14B 1.05(2) . ? 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 C2 C1 C10 111.31(13) . . ? C2 C1 C13 110.99(13) . . ? C10 C1 C13 107.65(14) . . ? C2 C1 H1 110.1(11) . . ? C10 C1 H1 108.8(11) . . ? C13 C1 H1 107.9(10) . . ? C13 O1 H1O 111.2(17) . . ? C14 O2 H2O 104.6(16) . . ? C3 C2 C7 118.93(15) . . ? C3 C2 C1 120.85(14) . . ? C7 C2 C1 120.15(14) . . ? H4O O3 H3O 105(2) . . ? C4 C3 C2 121.58(17) . . ? C4 C3 H3 118.4(12) . . ? C2 C3 H3 119.9(12) . . ? C3 C4 C5 119.26(17) . . ? C3 C4 H4 119.8(12) . . ? C5 C4 H4 121.0(12) . . ? C5 C6 C7 121.03(16) . . ? C5 C6 H6 122.3(12) . . ? C7 C6 H6 116.7(11) . . ? C6 C5 C4 120.18(17) . . ? C6 C5 H5 120.3(13) . . ? C4 C5 H5 119.5(13) . . ? C7 C8 C9 115.45(13) . . ? C7 C8 H8B 108.5(11) . . ? C9 C8 H8B 107.5(12) . . ? C7 C8 H8A 111.1(12) . . ? C9 C8 H8A 108.1(12) . . ? H8B C8 H8A 105.7(17) . . ? C6 C7 C2 119.01(14) . . ? C6 C7 C8 118.99(14) . . ? C2 C7 C8 121.99(14) . . ? C14 C9 C10 111.58(14) . . ? C14 C9 C8 110.17(14) . . ? C10 C9 C8 108.84(13) . . ? C14 C9 C11 105.18(13) . . ? C10 C9 C11 109.13(14) . . ? C8 C9 C11 111.92(14) . . ? C9 C10 C1 109.71(14) . . ? C9 C10 H10B 109.0(10) . . ? C1 C10 H10B 110.6(10) . . ? C9 C10 H10A 111.1(12) . . ? C1 C10 H10A 109.7(11) . . ? H10B C10 H10A 106.7(16) . . ? C12 C11 C9 114.45(14) . . ? C12 C11 H11A 110.1(12) . . ? C9 C11 H11A 111.2(12) . . ? C12 C11 H11B 108.5(11) . . ? C9 C11 H11B 107.3(12) . . ? H11A C11 H11B 104.7(16) . . ? C13 C12 C11 111.23(16) . . ? C13 C12 H12B 108.0(11) . . ? C11 C12 H12B 111.2(12) . . ? C13 C12 H12A 107.7(12) . . ? C11 C12 H12A 110.1(11) . . ? H12B C12 H12A 108.4(16) . . ? O1 C13 C12 107.51(15) . . ? O1 C13 C1 112.46(13) . . ? C12 C13 C1 110.88(14) . . ? O1 C13 H13 110.2(11) . . ? C12 C13 H13 109.0(11) . . ? C1 C13 H13 106.7(12) . . ? O2 C14 C9 114.21(14) . . ? O2 C14 H14A 107.5(13) . . ? C9 C14 H14A 107.3(12) . . ? O2 C14 H14B 110.1(11) . . ? C9 C14 H14B 109.8(11) . . ? H14A C14 H14B 107.7(16) . . ? 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 C10 C1 C2 C3 -155.17(15) . . . . ? C13 C1 C2 C3 84.95(18) . . . . ? C10 C1 C2 C7 27.8(2) . . . . ? C13 C1 C2 C7 -92.08(17) . . . . ? C7 C2 C3 C4 1.5(3) . . . . ? C1 C2 C3 C4 -175.60(16) . . . . ? C2 C3 C4 C5 -0.8(3) . . . . ? C7 C6 C5 C4 0.8(3) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C5 C6 C7 C2 -0.2(2) . . . . ? C5 C6 C7 C8 -178.83(16) . . . . ? C3 C2 C7 C6 -0.9(2) . . . . ? C1 C2 C7 C6 176.15(15) . . . . ? C3 C2 C7 C8 177.66(15) . . . . ? C1 C2 C7 C8 -5.3(2) . . . . ? C9 C8 C7 C6 -169.62(14) . . . . ? C9 C8 C7 C2 11.8(2) . . . . ? C7 C8 C9 C14 -162.72(14) . . . . ? C7 C8 C9 C10 -40.08(19) . . . . ? C7 C8 C9 C11 80.62(18) . . . . ? C14 C9 C10 C1 -175.00(13) . . . . ? C8 C9 C10 C1 63.21(18) . . . . ? C11 C9 C10 C1 -59.20(18) . . . . ? C2 C1 C10 C9 -57.11(18) . . . . ? C13 C1 C10 C9 64.73(17) . . . . ? C14 C9 C11 C12 171.64(16) . . . . ? C10 C9 C11 C12 51.8(2) . . . . ? C8 C9 C11 C12 -68.7(2) . . . . ? C9 C11 C12 C13 -49.5(2) . . . . ? C11 C12 C13 O1 177.25(14) . . . . ? C11 C12 C13 C1 54.0(2) . . . . ? C2 C1 C13 O1 -60.17(17) . . . . ? C10 C1 C13 O1 177.78(14) . . . . ? C2 C1 C13 C12 60.22(18) . . . . ? C10 C1 C13 C12 -61.82(18) . . . . ? C10 C9 C14 O2 -60.7(2) . . . . ? C8 C9 C14 O2 60.3(2) . . . . ? C11 C9 C14 O2 -178.89(15) . . . . ? _refine_diff_density_max 0.092 _refine_diff_density_min -0.153 _refine_diff_density_rms 0.038 _shelx_res_file ; TITL x_a.res in P2(1)2(1)2(1) x_a.res created by SHELXL-2016/4 at 18:19:32 on 24-Mar-2019 REM Old TITL x in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1) REM R1 0.113, Rweak 0.020, Alpha 0.001, Orientation as input REM Flack x = 0.162 ( 0.025 ) from Parsons' quotients REM Formula found by SHELXT: C14 O3 CELL 1.54178 6.0333 13.7700 14.9912 90.000 90.000 90.000 ZERR 4.000 0.0005 0.0012 0.0013 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H O UNIT 56 80 12 TEMP -23.000 OMIT 0 3 14 L.S. 10 BOND $H CONF HTAB SIZE 0.06 0.08 0.18 ACTA LIST 6 FMAP 2 PLAN 20 WGHT 0.042800 0.123900 FVAR 0.99354 C1 1 0.376612 0.530179 0.210073 11.00000 0.02561 0.03373 = 0.03506 -0.00121 -0.00541 0.00101 H1 2 0.243806 0.538117 0.171558 11.00000 0.03429 O1 3 0.531522 0.409440 0.105255 11.00000 0.04105 0.04177 = 0.03777 -0.01022 -0.00914 0.00311 H1O 2 0.412955 0.405317 0.069623 11.00000 0.07332 O2 3 0.331534 0.614565 0.496754 11.00000 0.03804 0.04542 = 0.03560 -0.00153 0.00997 0.00306 H2O 2 0.444461 0.652833 0.523649 11.00000 0.07677 C2 1 0.548812 0.605573 0.186595 11.00000 0.02970 0.02808 = 0.03101 -0.00106 -0.00237 0.00277 O3 3 0.633528 0.719527 0.578816 11.00000 0.04746 0.04230 = 0.04261 0.00262 0.00112 0.00292 H4O 2 0.754488 0.679341 0.589973 11.00000 0.06906 H3O 2 0.691347 0.772968 0.556838 11.00000 0.07510 C3 1 0.575723 0.636861 0.098929 11.00000 0.04810 0.03713 = 0.03065 -0.00076 -0.00735 0.00076 H3 2 0.480468 0.610556 0.051637 11.00000 0.05050 C4 1 0.742021 0.700831 0.075341 11.00000 0.06153 0.04015 = 0.02840 0.00419 0.00274 -0.00502 H4 2 0.755825 0.721521 0.014672 11.00000 0.04522 C6 1 0.857428 0.706954 0.228020 11.00000 0.03452 0.03521 = 0.03298 -0.00325 0.00025 -0.00487 H6 2 0.950814 0.731002 0.275252 11.00000 0.04222 C5 1 0.883401 0.735614 0.140419 11.00000 0.04964 0.03880 = 0.03828 0.00175 0.00789 -0.00913 H5 2 1.005448 0.780436 0.123487 11.00000 0.05407 C8 1 0.666669 0.614085 0.349856 11.00000 0.03029 0.03977 = 0.02694 -0.00091 0.00073 -0.00224 H8B 2 0.611994 0.670103 0.382455 11.00000 0.04005 H8A 2 0.815694 0.598078 0.377281 11.00000 0.05002 C7 1 0.691108 0.641787 0.252456 11.00000 0.02825 0.02949 = 0.02835 -0.00199 0.00096 0.00286 C9 1 0.508602 0.529202 0.368748 11.00000 0.03160 0.03288 = 0.02939 0.00087 0.00161 0.00240 C10 1 0.305308 0.538670 0.308071 11.00000 0.02574 0.03488 = 0.04121 0.00031 0.00185 -0.00060 H10B 2 0.193660 0.485058 0.324027 11.00000 0.03550 H10A 2 0.229633 0.600740 0.317632 11.00000 0.04348 C11 1 0.619772 0.430272 0.352075 11.00000 0.04554 0.03681 = 0.03599 0.00186 -0.00393 0.01017 H11A 2 0.758106 0.422997 0.388745 11.00000 0.04846 H11B 2 0.514265 0.377653 0.375835 11.00000 0.05018 C12 1 0.669710 0.408690 0.254043 11.00000 0.04365 0.03518 = 0.03822 -0.00504 -0.00624 0.01370 H12B 2 0.793060 0.450167 0.231423 11.00000 0.03984 H12A 2 0.712463 0.340345 0.246836 11.00000 0.03813 C13 1 0.467469 0.426742 0.195760 11.00000 0.03559 0.03138 = 0.03684 -0.00305 -0.00283 -0.00183 H13 2 0.351207 0.382463 0.213034 11.00000 0.03598 C14 1 0.443173 0.528275 0.467431 11.00000 0.04364 0.03607 = 0.03606 0.00431 0.00917 0.00020 H14A 2 0.344162 0.475197 0.475923 11.00000 0.04374 H14B 2 0.583161 0.515645 0.506812 11.00000 0.04728 HKLF 4 REM x_a.res in P2(1)2(1)2(1) REM R1 = 0.0248 for 1940 Fo > 4sig(Fo) and 0.0249 for all 1944 data REM 234 parameters refined using 0 restraints END WGHT 0.0428 0.1239 REM Instructions for potential hydrogen bonds EQIV $1 -x+1/2, -y+1, z-1/ HTAB O1 O2_$1 HTAB O2 O3 EQIV $2 -x+3/2, -y+1, z+1/ HTAB O3 O1_$2 EQIV $3 x+1/2, -y+3/2, -z+ HTAB O3 O2_$3 REM Highest difference peak 0.092, deepest hole -0.153, 1-sigma level 0.038 Q1 1 0.9858 0.4619 0.1597 11.00000 0.05 0.09 Q2 1 0.4682 0.5080 0.6003 11.00000 0.05 0.09 Q3 1 0.8851 0.4949 0.1821 11.00000 0.05 0.09 Q4 1 -0.0406 0.5367 0.1526 11.00000 0.05 0.09 Q5 1 0.9983 0.4830 0.2449 11.00000 0.05 0.09 Q6 1 0.3424 0.6417 0.0751 11.00000 0.05 0.09 Q7 1 0.3801 0.3750 0.5617 11.00000 0.05 0.08 Q8 1 0.0265 0.4447 0.3810 11.00000 0.05 0.08 Q9 1 0.1915 0.3729 0.4415 11.00000 0.05 0.08 Q10 1 0.4449 0.7024 0.3442 11.00000 0.05 0.08 Q11 1 0.9497 0.5191 0.2917 11.00000 0.05 0.08 Q12 1 0.5573 0.7665 0.3440 11.00000 0.05 0.08 Q13 1 -0.0148 0.4391 0.2989 11.00000 0.05 0.08 Q14 1 0.6631 0.6330 0.3019 11.00000 0.05 0.08 Q15 1 0.8444 0.4563 0.3726 11.00000 0.05 0.07 Q16 1 0.8680 0.5552 0.3516 11.00000 0.05 0.07 Q17 1 0.1175 0.3822 0.3461 11.00000 0.05 0.07 Q18 1 0.1715 0.4750 0.4350 11.00000 0.05 0.07 Q19 1 0.8669 0.5382 0.2361 11.00000 0.05 0.07 Q20 1 0.6363 0.4348 0.5055 11.00000 0.05 0.07 ; _shelx_res_checksum 5471 _shelx_hkl_file ; -1 0 0 1.50 0.30 -2 0 0 23.60 1.00 2 0 0 24.00 0.80 -2 0 0 26.10 0.80 -2 0 0 24.10 1.10 2 0 0 25.70 0.80 2 0 0 25.50 0.90 3 0 0 0.30 0.30 -3 0 0 0.10 0.20 3 0 0 0.40 0.20 -4 0 0 240.38 5.50 4 0 0 237.08 5.90 -4 0 0 236.38 5.60 -4 0 0 232.38 5.50 4 0 0 244.48 6.00 4 0 0 240.88 6.10 -4 0 0 239.98 5.40 4 0 0 230.78 6.20 5 0 0 4.90 0.30 -6 0 0 259.97 6.30 -6 0 0 272.07 6.30 -6 0 0 268.77 6.00 6 0 0 253.27 6.00 0 -1 0 1.90 0.10 1 -1 0 422.36 9.00 -1 1 0 391.76 9.10 -1 -1 0 419.56 9.80 -1 1 0 417.76 9.10 -1 1 0 422.26 10.10 1 -1 0 408.56 9.30 -1 -1 0 408.06 9.20 1 1 0 417.06 9.30 2 1 0 40.20 1.30 2 1 0 44.60 1.30 2 -1 0 40.50 1.10 -2 -1 0 40.70 1.20 -2 -1 0 41.50 1.50 -2 1 0 42.00 1.40 -2 1 0 43.50 1.30 -2 -1 0 46.10 1.40 -2 1 0 41.90 1.60 2 1 0 41.50 1.30 -3 1 0 104.29 2.90 -3 1 0 107.69 3.60 3 1 0 109.29 2.90 -3 -1 0 112.39 3.50 -3 1 0 102.59 2.90 3 -1 0 110.89 3.00 3 -1 0 109.59 3.00 3 -1 0 105.99 2.80 -3 -1 0 107.99 3.20 3 1 0 106.19 3.00 3 -1 0 105.09 2.80 -4 1 0 15.00 0.60 4 1 0 17.10 1.10 -4 1 0 14.30 0.70 4 1 0 15.60 0.90 4 1 0 14.80 0.90 -4 -1 0 15.20 0.60 -4 -1 0 15.10 0.70 4 -1 0 14.10 0.90 4 -1 0 14.60 1.00 -4 -1 0 14.10 0.70 -4 1 0 14.80 0.60 -4 1 0 14.60 0.70 -4 1 0 15.30 0.60 5 1 0 7.30 0.40 -5 1 0 7.70 0.60 -5 -1 0 8.00 0.60 -5 1 0 7.90 0.50 -5 1 0 7.70 0.60 -5 -1 0 7.60 0.50 5 -1 0 7.80 0.50 5 -1 0 7.80 0.80 -5 -1 0 8.20 0.60 -5 1 0 8.20 0.60 5 1 0 8.00 0.90 5 1 0 7.70 0.90 -6 -1 0 46.90 1.40 -6 1 0 47.40 1.40 -6 -1 0 46.70 1.50 -6 1 0 47.10 1.60 -6 1 0 48.40 1.50 6 -1 0 44.70 1.30 6 1 0 45.70 1.30 0 2 0 2054.79 49.80 -1 2 0 572.44 12.80 1 -2 0 589.04 12.60 -1 2 0 593.24 13.40 -1 2 0 585.84 13.90 1 2 0 552.74 12.70 1 2 0 586.84 12.90 -1 -2 0 584.94 13.00 1 -2 0 563.94 13.00 -1 2 0 560.24 12.60 -1 -2 0 560.94 22.70 -1 -2 0 574.54 12.90 -1 -2 0 589.44 13.50 1 -2 0 578.44 12.60 -2 -2 0 1272.77 29.90 -2 2 0 1230.68 28.20 2 -2 0 1262.67 28.00 -2 2 0 1329.27 29.70 2 2 0 1265.37 28.30 -2 2 0 1305.97 39.60 -2 -2 0 1287.47 30.70 -2 -2 0 1266.97 28.20 2 -2 0 1301.17 28.10 2 -2 0 1290.67 28.90 2 2 0 1244.68 28.10 3 -2 0 830.12 19.50 -3 2 0 834.52 19.10 -3 -2 0 849.22 19.30 3 -2 0 888.51 19.00 3 2 0 895.31 19.00 3 -2 0 873.01 19.20 -3 2 0 860.21 19.60 -3 2 0 853.91 19.10 3 -2 0 868.71 19.20 3 2 0 866.01 19.20 -3 -2 0 831.52 19.80 4 2 0 274.67 7.10 -4 -2 0 273.37 6.40 -4 -2 0 284.87 6.60 4 2 0 272.67 6.90 -4 -2 0 275.27 6.30 -4 2 0 277.37 6.20 4 -2 0 277.37 7.00 4 -2 0 286.17 6.30 4 2 0 274.87 6.20 -4 2 0 278.57 6.50 -4 2 0 269.67 6.50 -4 2 0 289.37 6.40 -4 2 0 283.27 6.30 5 2 0 33.50 1.90 -5 2 0 33.60 1.20 -5 2 0 32.40 1.00 -5 2 0 33.80 1.60 5 -2 0 32.20 1.10 5 2 0 34.60 1.60 5 2 0 32.00 1.00 -5 2 0 34.80 1.20 -5 -2 0 34.50 1.10 -5 -2 0 33.70 1.20 6 2 0 30.90 1.00 -6 2 0 31.80 1.20 -6 2 0 32.00 1.20 -6 -2 0 30.80 1.00 6 -2 0 30.00 1.00 6 -2 0 30.00 1.10 -6 2 0 31.10 1.00 -6 -2 0 29.50 1.20 0 3 0 -0.20 0.30 0 -3 0 0.10 0.10 0 -3 0 0.20 0.20 0 3 0 0.20 0.30 -1 3 0 6937.11 157.48 -1 3 0 6675.13 155.18 -1 -3 0 7240.58 180.08 1 -3 0 6872.11 161.98 -1 -3 0 7537.55 170.08 1 3 0 7384.06 193.88 1 3 0 7105.39 156.48 1 -3 0 7034.00 171.88 -1 -3 0 7275.97 171.78 1 -3 0 7219.48 173.18 -1 -3 0 7331.57 172.38 -1 3 0 7075.29 175.58 -2 -3 0 561.14 12.60 2 -3 0 578.94 12.70 2 -3 0 572.84 12.70 2 3 0 562.44 12.90 2 3 0 566.74 12.70 2 3 0 564.14 13.10 -2 3 0 584.14 12.80 -2 -3 0 579.44 12.60 -2 3 0 568.34 12.70 2 -3 0 556.34 12.70 2 -3 0 582.34 12.60 -2 -3 0 552.64 12.70 2 3 0 581.24 12.90 -2 -3 0 569.64 13.10 3 3 0 215.78 5.00 -3 -3 0 224.98 6.20 3 -3 0 225.58 5.60 -3 -3 0 227.88 5.40 3 -3 0 231.58 5.50 -3 3 0 227.58 5.60 3 3 0 220.08 5.60 -3 -3 0 222.88 5.70 3 3 0 224.48 5.50 -3 3 0 225.68 5.60 3 -3 0 225.28 5.10 -4 3 0 197.98 4.50 -4 3 0 190.28 4.70 -4 -3 0 190.68 4.50 4 -3 0 196.28 4.60 -4 3 0 194.38 4.70 -4 -3 0 191.28 4.50 -4 -3 0 192.38 4.60 4 -3 0 196.08 5.30 -4 3 0 198.18 4.70 -4 -3 0 195.98 4.70 4 -3 0 193.98 5.20 4 3 0 201.48 4.40 4 3 0 195.88 5.40 4 3 0 194.98 5.10 -4 3 0 199.68 4.60 -5 3 0 -0.10 0.20 -5 3 0 0.30 0.30 -5 3 0 -0.30 0.20 -5 -3 0 0.10 0.20 5 -3 0 0.30 0.20 5 3 0 0.00 0.10 -5 -3 0 0.80 0.30 5 3 0 0.00 0.30 -6 3 0 14.60 0.80 6 -3 0 15.00 0.70 -6 -3 0 13.80 0.60 -6 3 0 13.70 0.70 6 3 0 14.20 0.60 6 3 0 14.40 0.50 6 -3 0 13.30 0.60 -6 -3 0 13.30 0.80 0 4 0 817.72 18.50 0 -4 0 830.22 18.60 0 -4 0 848.52 19.10 0 4 0 841.02 18.90 1 4 0 142.69 3.80 -1 -4 0 140.49 3.80 -1 -4 0 146.09 3.40 1 -4 0 148.29 3.50 -1 4 0 152.28 3.70 1 -4 0 148.39 3.40 1 -4 0 142.59 3.50 1 4 0 148.69 4.10 -1 -4 0 145.49 3.50 -1 4 0 159.48 4.10 -1 4 0 151.08 3.70 2 4 0 0.40 0.40 -2 4 0 0.20 0.20 2 -4 0 0.30 0.20 2 -4 0 0.40 0.30 -2 4 0 0.30 0.20 2 4 0 0.40 0.40 2 4 0 0.70 0.40 2 4 0 0.80 0.30 -2 4 0 0.30 0.30 -3 4 0 44.20 1.70 3 -4 0 43.70 1.30 3 -4 0 46.10 1.60 3 4 0 40.00 2.50 -3 4 0 45.50 1.70 -3 -4 0 46.30 1.50 -3 4 0 44.50 2.00 3 4 0 43.20 1.70 -3 -4 0 43.20 1.70 -3 -4 0 46.30 2.10 3 4 0 45.20 2.30 3 -4 0 43.00 1.70 3 4 0 43.00 1.10 -4 4 0 40.00 1.40 4 -4 0 39.10 1.30 -4 4 0 38.40 1.20 -4 -4 0 38.90 1.10 4 4 0 38.90 1.60 -4 4 0 38.50 1.30 -4 -4 0 39.30 1.10 -4 -4 0 39.40 1.30 4 4 0 39.30 1.10 -4 4 0 37.00 1.20 -4 -4 0 39.20 1.40 4 -4 0 37.00 1.60 -5 -4 0 0.80 0.30 5 4 0 0.60 0.40 5 -4 0 0.80 0.30 5 -4 0 1.00 0.30 -5 -4 0 0.60 0.30 -5 4 0 0.50 0.20 -5 4 0 1.20 0.30 5 -4 0 0.80 0.40 5 4 0 0.80 0.20 -5 -4 0 0.70 0.20 -5 4 0 0.30 0.30 6 4 0 34.70 1.10 -6 4 0 36.60 1.20 6 -4 0 36.30 1.10 -6 -4 0 36.80 1.10 6 4 0 34.40 1.00 -6 4 0 35.70 1.30 6 -4 0 34.90 1.10 -6 -4 0 33.70 1.20 0 5 0 0.50 0.30 0 -5 0 0.40 0.20 0 -5 0 0.30 0.20 0 5 0 0.80 0.40 0 -5 0 0.40 0.20 0 5 0 0.20 0.30 -1 -5 0 38.10 1.20 1 -5 0 38.40 1.20 -1 -5 0 38.60 1.20 -1 5 0 43.00 1.50 -1 -5 0 35.60 1.20 -1 -5 0 39.40 1.50 -1 5 0 38.60 1.40 1 -5 0 38.10 1.30 -1 5 0 42.70 1.50 1 -5 0 40.80 1.20 -1 5 0 33.40 1.20 2 -5 0 1659.53 36.40 2 -5 0 1687.93 37.20 -2 5 0 1692.33 49.40 2 5 0 1705.03 37.10 2 5 0 1729.73 37.20 -2 -5 0 1627.54 37.90 -2 -5 0 1717.03 38.30 2 5 0 1679.63 37.70 -2 -5 0 1623.84 51.59 2 -5 0 1703.43 38.20 2 5 0 1705.73 36.80 -2 -5 0 1682.83 40.40 2 -5 0 1702.53 38.20 2 5 0 1665.23 37.60 -2 5 0 1646.64 36.70 3 5 0 193.78 5.10 3 5 0 209.58 5.50 -3 -5 0 195.08 4.90 3 -5 0 193.78 5.00 3 -5 0 192.58 5.10 3 -5 0 197.48 5.00 -3 5 0 193.28 5.20 3 5 0 217.48 6.20 3 -5 0 184.58 4.70 3 5 0 210.38 5.50 3 5 0 187.38 4.50 -3 -5 0 186.18 5.70 4 5 0 4.60 0.40 -4 5 0 3.80 0.40 4 5 0 3.60 0.60 -4 -5 0 3.20 0.50 4 -5 0 3.60 0.60 -4 5 0 4.30 0.40 4 -5 0 4.70 0.50 -4 5 0 3.30 0.30 -4 -5 0 3.90 0.30 -4 -5 0 4.50 0.30 4 -5 0 4.00 0.60 -5 -5 0 58.39 1.60 5 5 0 57.59 1.70 -5 5 0 58.29 1.90 -5 -5 0 58.79 1.90 5 5 0 59.59 1.50 -5 -5 0 58.19 2.00 5 5 0 59.39 2.30 5 -5 0 57.99 1.80 -5 5 0 61.09 1.80 5 -5 0 59.89 2.30 -5 -5 0 55.79 1.60 5 -5 0 58.39 1.70 -5 5 0 63.09 1.70 -6 -5 0 1.40 0.20 6 5 0 1.10 0.20 6 -5 0 1.60 0.30 -6 5 0 1.00 0.30 6 5 0 1.10 0.20 -6 5 0 0.80 0.20 6 -5 0 1.20 0.30 0 6 0 3005.20 69.89 0 6 0 2970.80 67.39 0 -6 0 2962.00 66.19 0 -6 0 2949.21 65.89 0 6 0 2845.62 66.19 0 -6 0 3043.60 66.39 1 6 0 3.70 0.70 -1 -6 0 3.10 0.40 -1 6 0 2.90 0.40 1 6 0 2.80 0.60 1 -6 0 3.10 0.40 -1 -6 0 3.50 0.60 -1 -6 0 3.00 0.40 1 -6 0 3.50 0.40 1 6 0 3.30 0.70 -1 6 0 3.40 0.60 1 -6 0 3.50 0.40 -1 6 0 3.50 0.40 -1 6 0 3.50 0.60 -1 -6 0 3.40 0.40 2 -6 0 178.58 4.50 -2 -6 0 171.98 4.30 -2 -6 0 191.28 4.40 -2 -6 0 171.88 5.00 2 6 0 171.88 5.00 2 -6 0 178.08 4.50 2 6 0 170.48 4.50 -2 6 0 173.48 4.50 2 -6 0 172.68 4.50 2 6 0 168.68 4.10 2 6 0 170.08 4.90 2 6 0 166.88 5.50 -2 -6 0 194.58 4.40 2 -6 0 175.68 4.30 -2 6 0 181.18 4.70 3 -6 0 223.38 5.30 3 6 0 235.88 5.30 3 -6 0 230.18 5.70 3 -6 0 223.68 5.40 3 6 0 218.98 6.90 3 6 0 222.48 5.00 -3 6 0 217.48 5.10 -3 -6 0 229.98 5.40 3 6 0 230.48 6.30 -3 6 0 212.28 5.80 3 -6 0 223.08 5.80 3 -6 0 228.78 5.70 -3 -6 0 231.68 5.60 -3 6 0 219.78 5.10 3 6 0 226.58 5.20 3 6 0 235.18 5.90 -3 -6 0 227.18 5.10 -3 6 0 212.68 5.90 -3 6 0 221.58 5.20 -3 6 0 215.48 5.30 3 6 0 223.28 6.30 4 -6 0 21.80 1.00 -4 6 0 20.90 0.80 -4 6 0 19.60 0.90 4 6 0 24.00 0.90 4 -6 0 21.90 1.30 4 6 0 22.40 0.70 -4 6 0 21.10 0.80 -4 -6 0 21.40 0.80 -4 6 0 20.90 0.90 4 -6 0 21.20 1.10 -4 -6 0 20.40 0.80 4 -6 0 21.30 1.30 4 -6 0 24.40 0.90 -4 -6 0 21.30 1.00 4 6 0 21.20 1.20 -5 -6 0 2.50 0.30 -5 -6 0 2.70 0.50 5 -6 0 2.10 0.60 5 6 0 2.20 0.30 5 6 0 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