data_global _audit_creation_method 'APEX3 v2018.1-0' _publ_requested_journal ? _publ_contact_author_name ? _publ_contact_author_address ; ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_jar127b _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C15 H18 O4' _chemical_formula_sum 'C15 H18 O4' _chemical_formula_iupac ? _chemical_formula_weight 262.29 _chemical_absolute_configuration ad _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 9.5399(2) _cell_length_b 9.9824(2) _cell_length_c 13.6680(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1301.62(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9879 _cell_measurement_theta_min 5.4877 _cell_measurement_theta_max 72.1174 _cell_measurement_temperature 100.(2) _exptl_crystal_description plate _exptl_crystal_colour 'clear light colourless' _exptl_crystal_size_max 0.400 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.060 _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 560 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_process_details ; SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction ; _exptl_absorpt_correction_T_min 0.68 _exptl_absorpt_correction_T_max 0.95 _exptl_special_details ; ; _diffrn_ambient_temperature 100.(2) _diffrn_source 'Ius Diamond' _diffrn_source_type Microfocus _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_monochromator 'Helixos MX multilayer Optic' _diffrn_measurement_device_type 'Bruker D8 QUEST PHOTON II' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 7.3910 _diffrn_reflns_number 13898 _diffrn_reflns_av_R_equivalents 0.0386 _diffrn_reflns_av_unetI/netI 0.0281 _diffrn_reflns_theta_min 5.49 _diffrn_reflns_theta_max 72.33 _diffrn_reflns_theta_full 72.33 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _refine_special_details ; ; _reflns_number_total 2554 _reflns_number_gt 2533 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_gt 0.0804 _refine_ls_wR_factor_ref 0.0808 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_number_reflns 2554 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0484P)^2^+0.2619P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.249 _refine_diff_density_min -0.300 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 1059 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.06(4) 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' _computing_data_collection 'Bruker Instrument Service vV6.2.9' _computing_cell_refinement 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_data_reduction 'SAINT V8.38A (Bruker AXS Inc., 2017)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group O O1 0.29879(13) 0.33887(12) 0.48818(11) 0.0208(3) Uani d . . . 1 . . H H17 0.219814 0.305521 0.500218 0.031 Uiso calc U . R 1 . . O O2 0.40968(13) 0.86729(12) 0.54180(9) 0.0156(3) Uani d . . . 1 . . O O3 0.26663(12) 0.69196(11) 0.56216(8) 0.0123(3) Uani d . . . 1 . . O O4 0.57188(12) 0.30966(12) 0.48429(10) 0.0170(3) Uani d . . . 1 . . H H18 0.485317 0.294276 0.484039 0.026 Uiso calc U . R 1 . . C C1 0.77210(18) 0.4762(2) 0.73855(14) 0.0201(4) Uani d . . . 1 . . H H11 0.821244 0.544569 0.776866 0.03 Uiso calc U . R 1 . . H H1 0.827843 0.453403 0.680665 0.03 Uiso calc U . R 1 . . H H10 0.758697 0.395835 0.778707 0.03 Uiso calc U . R 1 . . C C2 0.63024(17) 0.52990(17) 0.70665(13) 0.0137(4) Uani d . . . 1 . . C C3 0.63671(17) 0.66186(16) 0.64145(13) 0.0128(3) Uani d . . . 1 . . H H7 0.633005 0.744013 0.681943 0.015 Uiso calc U . R 1 . . H H6 0.721486 0.663891 0.59971 0.015 Uiso calc U . R 1 . . C C4 0.50285(17) 0.64353(15) 0.58082(12) 0.0098(3) Uani d . . . 1 . . C C5 0.54045(16) 0.55971(16) 0.48806(12) 0.0109(3) Uani d . . . 1 . . H H4 0.615905 0.605416 0.449786 0.013 Uiso calc U . R 1 . . C C6 0.41204(17) 0.53522(17) 0.42322(12) 0.0130(3) Uani d . . . 1 . . H H3 0.385373 0.62048 0.391234 0.016 Uiso calc U . R 1 . . H H2 0.437469 0.470729 0.371132 0.016 Uiso calc U . R 1 . . C C7 0.28597(17) 0.48106(17) 0.47927(12) 0.0137(3) Uani d . . . 1 . . H H16 0.198586 0.502367 0.441973 0.016 Uiso calc U . R 1 . . C C8 0.27660(17) 0.54493(16) 0.58122(12) 0.0118(3) Uani d . . . 1 . . C C9 0.41386(16) 0.53912(15) 0.63970(12) 0.0103(3) Uani d . . . 1 . . C C10 0.39631(17) 0.75018(16) 0.55975(11) 0.0109(3) Uani d . . . 1 . . C C11 0.59883(16) 0.43045(16) 0.53706(13) 0.0127(3) Uani d . . . 1 . . H H12 0.702783 0.440656 0.542797 0.015 Uiso calc U . R 1 . . C C12 0.53707(17) 0.43655(16) 0.64073(13) 0.0122(3) Uani d . . . 1 . . H H5 0.513944 0.347547 0.670175 0.015 Uiso calc U . R 1 . . C C13 0.52827(19) 0.56716(18) 0.78650(13) 0.0162(4) Uani d . . . 1 . . H H8 0.550562 0.580968 0.853488 0.019 Uiso calc U . R 1 . . C C14 0.40201(18) 0.57721(17) 0.74661(12) 0.0138(3) Uani d . . . 1 . . H H9 0.31867 0.603683 0.779377 0.017 Uiso calc U . R 1 . . C C15 0.14369(17) 0.50393(18) 0.63357(14) 0.0177(4) Uani d . . . 1 . . H H15 0.130519 0.560521 0.691434 0.027 Uiso calc U . R 1 . . H H13 0.150898 0.409985 0.65376 0.027 Uiso calc U . R 1 . . H H14 0.063518 0.514726 0.589436 0.027 Uiso calc U . R 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 O1 0.0102(6) 0.0088(6) 0.0435(8) -0.0027(5) 0.0019(6) -0.0049(5) O2 0.0195(6) 0.0080(5) 0.0195(6) 0.0010(5) -0.0017(5) 0.0001(4) O3 0.0099(5) 0.0092(6) 0.0179(6) 0.0026(4) -0.0005(4) 0.0005(4) O4 0.0102(6) 0.0098(5) 0.0311(7) 0.0017(5) -0.0002(5) -0.0066(5) C1 0.0114(8) 0.0253(10) 0.0237(8) 0.0018(7) -0.0036(7) 0.0066(7) C2 0.0101(7) 0.0136(8) 0.0176(8) -0.0002(6) -0.0022(6) 0.0032(6) C3 0.0109(7) 0.0114(7) 0.0162(7) -0.0026(6) -0.0014(6) 0.0019(6) C4 0.0086(7) 0.0068(7) 0.0139(7) -0.0015(6) 0.0014(6) 0.0010(6) C5 0.0081(7) 0.0097(7) 0.0151(8) -0.0010(6) 0.0025(6) -0.0017(6) C6 0.0109(8) 0.0118(7) 0.0164(7) 0.0002(6) -0.0011(7) -0.0033(6) C7 0.0089(7) 0.0104(7) 0.0217(8) -0.0009(6) -0.0021(6) -0.0023(6) C8 0.0084(7) 0.0081(7) 0.0190(8) 0.0012(6) -0.0002(6) 0.0024(6) C9 0.0078(7) 0.0078(7) 0.0153(7) 0.0006(6) 0.0010(6) 0.0022(6) C10 0.0112(8) 0.0107(7) 0.0107(7) 0.0015(6) 0.0006(6) -0.0007(6) C11 0.0079(7) 0.0097(7) 0.0204(8) 0.0005(6) 0.0012(6) -0.0020(7) C12 0.0083(7) 0.0087(7) 0.0196(8) 0.0011(6) 0.0007(6) 0.0038(6) C13 0.0183(8) 0.0156(8) 0.0148(7) 0.0001(7) 0.0008(7) 0.0044(7) C14 0.0136(8) 0.0138(7) 0.0141(7) 0.0006(6) 0.0041(7) 0.0032(6) C15 0.0092(7) 0.0207(9) 0.0231(9) -0.0005(7) 0.0023(7) 0.0039(7) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag O1 C7 . 1.430(2) ? O1 H17 . 0.84 ? O2 C10 . 1.201(2) ? O3 C10 . 1.367(2) ? O3 C8 . 1.4937(19) ? O4 C11 . 1.4284(19) ? O4 H18 . 0.84 ? C1 C2 . 1.520(2) ? C1 H11 . 0.98 ? C1 H1 . 0.98 ? C1 H10 . 0.98 ? C2 C13 . 1.509(2) ? C2 C12 . 1.572(2) ? C2 C3 . 1.592(2) ? C3 C4 . 1.533(2) ? C3 H7 . 0.99 ? C3 H6 . 0.99 ? C4 C10 . 1.500(2) ? C4 C5 . 1.561(2) ? C4 C9 . 1.567(2) ? C5 C6 . 1.532(2) ? C5 C11 . 1.557(2) ? C5 H4 . 1.0 ? C6 C7 . 1.525(2) ? C6 H3 . 0.99 ? C6 H2 . 0.99 ? C7 C8 . 1.535(2) ? C7 H16 . 1.0 ? C8 C15 . 1.512(2) ? C8 C9 . 1.535(2) ? C9 C14 . 1.514(2) ? C9 C12 . 1.559(2) ? C11 C12 . 1.536(2) ? C11 H12 . 1.0 ? C12 H5 . 1.0 ? C13 C14 . 1.326(3) ? C13 H8 . 0.95 ? C14 H9 . 0.95 ? C15 H15 . 0.98 ? C15 H13 . 0.98 ? C15 H14 . 0.98 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C7 O1 H17 . . 109.5 ? C10 O3 C8 . . 111.36(12) ? C11 O4 H18 . . 109.5 ? C2 C1 H11 . . 109.5 ? C2 C1 H1 . . 109.5 ? H11 C1 H1 . . 109.5 ? C2 C1 H10 . . 109.5 ? H11 C1 H10 . . 109.5 ? H1 C1 H10 . . 109.5 ? C13 C2 C1 . . 116.98(15) ? C13 C2 C12 . . 101.32(13) ? C1 C2 C12 . . 117.31(15) ? C13 C2 C3 . . 103.06(13) ? C1 C2 C3 . . 114.73(14) ? C12 C2 C3 . . 101.05(13) ? C4 C3 C2 . . 99.88(12) ? C4 C3 H7 . . 111.8 ? C2 C3 H7 . . 111.8 ? C4 C3 H6 . . 111.8 ? C2 C3 H6 . . 111.8 ? H7 C3 H6 . . 109.5 ? C10 C4 C3 . . 125.70(14) ? C10 C4 C5 . . 112.36(14) ? C3 C4 C5 . . 108.16(13) ? C10 C4 C9 . . 101.75(12) ? C3 C4 C9 . . 104.65(13) ? C5 C4 C9 . . 100.67(12) ? C6 C5 C11 . . 113.75(13) ? C6 C5 C4 . . 111.82(13) ? C11 C5 C4 . . 100.20(13) ? C6 C5 H4 . . 110.2 ? C11 C5 H4 . . 110.2 ? C4 C5 H4 . . 110.2 ? C7 C6 C5 . . 113.37(14) ? C7 C6 H3 . . 108.9 ? C5 C6 H3 . . 108.9 ? C7 C6 H2 . . 108.9 ? C5 C6 H2 . . 108.9 ? H3 C6 H2 . . 107.7 ? O1 C7 C6 . . 109.10(13) ? O1 C7 C8 . . 109.88(14) ? C6 C7 C8 . . 110.77(13) ? O1 C7 H16 . . 109.0 ? C6 C7 H16 . . 109.0 ? C8 C7 H16 . . 109.0 ? O3 C8 C15 . . 107.16(13) ? O3 C8 C7 . . 104.69(12) ? C15 C8 C7 . . 111.46(14) ? O3 C8 C9 . . 100.50(12) ? C15 C8 C9 . . 117.29(13) ? C7 C8 C9 . . 114.04(13) ? C14 C9 C8 . . 115.43(13) ? C14 C9 C12 . . 102.27(13) ? C8 C9 C12 . . 132.27(14) ? C14 C9 C4 . . 111.66(13) ? C8 C9 C4 . . 99.76(12) ? C12 C9 C4 . . 91.89(12) ? O2 C10 O3 . . 120.98(15) ? O2 C10 C4 . . 131.15(15) ? O3 C10 C4 . . 107.87(13) ? O4 C11 C12 . . 115.49(13) ? O4 C11 C5 . . 114.71(14) ? C12 C11 C5 . . 103.11(13) ? O4 C11 H12 . . 107.7 ? C12 C11 H12 . . 107.7 ? C5 C11 H12 . . 107.7 ? C11 C12 C9 . . 107.88(13) ? C11 C12 C2 . . 109.60(13) ? C9 C12 C2 . . 92.42(12) ? C11 C12 H5 . . 114.9 ? C9 C12 H5 . . 114.9 ? C2 C12 H5 . . 114.9 ? C14 C13 C2 . . 107.87(16) ? C14 C13 H8 . . 126.1 ? C2 C13 H8 . . 126.1 ? C13 C14 C9 . . 108.06(15) ? C13 C14 H9 . . 126.0 ? C9 C14 H9 . . 126.0 ? C8 C15 H15 . . 109.5 ? C8 C15 H13 . . 109.5 ? H15 C15 H13 . . 109.5 ? C8 C15 H14 . . 109.5 ? H15 C15 H14 . . 109.5 ? H13 C15 H14 . . 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag C13 C2 C3 C4 . . . . -80.69(15) ? C1 C2 C3 C4 . . . . 151.03(15) ? C12 C2 C3 C4 . . . . 23.82(15) ? C2 C3 C4 C10 . . . . 135.29(16) ? C2 C3 C4 C5 . . . . -87.95(14) ? C2 C3 C4 C9 . . . . 18.74(15) ? C10 C4 C5 C6 . . . . -37.49(18) ? C3 C4 C5 C6 . . . . 179.49(13) ? C9 C4 C5 C6 . . . . 70.06(15) ? C10 C4 C5 C11 . . . . -158.35(13) ? C3 C4 C5 C11 . . . . 58.63(15) ? C9 C4 C5 C11 . . . . -50.80(14) ? C11 C5 C6 C7 . . . . 62.53(18) ? C4 C5 C6 C7 . . . . -50.10(18) ? C5 C6 C7 O1 . . . . -84.10(16) ? C5 C6 C7 C8 . . . . 36.97(18) ? C10 O3 C8 C15 . . . . 150.91(13) ? C10 O3 C8 C7 . . . . -90.61(14) ? C10 O3 C8 C9 . . . . 27.87(15) ? O1 C7 C8 O3 . . . . 178.88(11) ? C6 C7 C8 O3 . . . . 58.27(16) ? O1 C7 C8 C15 . . . . -65.60(16) ? C6 C7 C8 C15 . . . . 173.78(14) ? O1 C7 C8 C9 . . . . 70.03(17) ? C6 C7 C8 C9 . . . . -50.59(17) ? O3 C8 C9 C14 . . . . 79.52(15) ? C15 C8 C9 C14 . . . . -36.1(2) ? C7 C8 C9 C14 . . . . -169.07(13) ? O3 C8 C9 C12 . . . . -141.88(16) ? C15 C8 C9 C12 . . . . 102.5(2) ? C7 C8 C9 C12 . . . . -30.5(2) ? O3 C8 C9 C4 . . . . -40.25(14) ? C15 C8 C9 C4 . . . . -155.92(14) ? C7 C8 C9 C4 . . . . 71.16(15) ? C10 C4 C9 C14 . . . . -82.50(15) ? C3 C4 C9 C14 . . . . 49.59(16) ? C5 C4 C9 C14 . . . . 161.74(13) ? C10 C4 C9 C8 . . . . 39.98(15) ? C3 C4 C9 C8 . . . . 172.08(13) ? C5 C4 C9 C8 . . . . -75.77(14) ? C10 C4 C9 C12 . . . . 173.50(13) ? C3 C4 C9 C12 . . . . -54.41(14) ? C5 C4 C9 C12 . . . . 57.74(14) ? C8 O3 C10 O2 . . . . 177.31(15) ? C8 O3 C10 C4 . . . . -1.85(17) ? C3 C4 C10 O2 . . . . 38.6(3) ? C5 C4 C10 O2 . . . . -96.7(2) ? C9 C4 C10 O2 . . . . 156.46(17) ? C3 C4 C10 O3 . . . . -142.38(15) ? C5 C4 C10 O3 . . . . 82.36(16) ? C9 C4 C10 O3 . . . . -24.50(16) ? C6 C5 C11 O4 . . . . 27.24(19) ? C4 C5 C11 O4 . . . . 146.71(13) ? C6 C5 C11 C12 . . . . -99.17(15) ? C4 C5 C11 C12 . . . . 20.30(15) ? O4 C11 C12 C9 . . . . -109.17(15) ? C5 C11 C12 C9 . . . . 16.74(16) ? O4 C11 C12 C2 . . . . 151.51(13) ? C5 C11 C12 C2 . . . . -82.57(15) ? C14 C9 C12 C11 . . . . -158.25(13) ? C8 C9 C12 C11 . . . . 59.4(2) ? C4 C9 C12 C11 . . . . -45.59(15) ? C14 C9 C12 C2 . . . . -46.76(14) ? C8 C9 C12 C2 . . . . 170.92(16) ? C4 C9 C12 C2 . . . . 65.90(13) ? C13 C2 C12 C11 . . . . 158.39(13) ? C1 C2 C12 C11 . . . . -73.00(18) ? C3 C2 C12 C11 . . . . 52.49(16) ? C13 C2 C12 C9 . . . . 48.44(14) ? C1 C2 C12 C9 . . . . 177.05(14) ? C3 C2 C12 C9 . . . . -57.45(14) ? C1 C2 C13 C14 . . . . -163.78(16) ? C12 C2 C13 C14 . . . . -34.96(18) ? C3 C2 C13 C14 . . . . 69.35(18) ? C2 C13 C14 C9 . . . . 3.23(19) ? C8 C9 C14 C13 . . . . 179.98(14) ? C12 C9 C14 C13 . . . . 30.04(18) ? C4 C9 C14 C13 . . . . -67.01(18) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O1 H17 O4 2_456 0.84 1.83 2.6506(17) 164.2 ? O4 H18 O1 . 0.84 1.84 2.6221(17) 155.3 ? C5 H4 O3 2_566 1.00 2.49 3.3574(19) 145.2 ? C15 H14 O2 2_466 0.98 2.60 3.519(2) 156.2 ? _shelx_res_file ; TITL jar127b_0m_a.res in P2(1)2(1)2(1) jar127b_0m.res created by SHELXL-2017/1 at 11:17:36 on 08-Jan-2020 CELL 1.54178 9.5399 9.9824 13.6680 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0002 0.0003 0.000 0.000 0.000 LATT -1 SYMM x+1/2, -y+1/2, -z SYMM -x, y+1/2, -z+1/2 SYMM -x+1/2, -y, z+1/2 SFAC C H O UNIT 60 72 16 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.130 SIZE 0.060 0.300 0.400 ACTA EQIV $1 x-1/2, -y+1/2, -z+1 HTAB O1 O4_$1 HTAB O4 O1 EQIV $2 x+1/2, -y+3/2, -z+1 HTAB C5 O3_$2 EQIV $3 x-1/2, -y+3/2, -z+1 HTAB C15 O2_$3 L.S. 4 FMAP 2 PLAN -4 0 0.00 HTAB BOND $H CONF WGHT 0.048400 0.261900 FVAR 1.22796 O1 3 0.298793 0.338870 0.488177 11.00000 0.01023 0.00881 = 0.04347 -0.00486 0.00185 -0.00271 AFIX 147 H17 2 0.219814 0.305521 0.500218 11.00000 -1.50000 AFIX 0 O2 3 0.409682 0.867290 0.541798 11.00000 0.01946 0.00796 = 0.01948 0.00015 -0.00171 0.00101 O3 3 0.266633 0.691964 0.562161 11.00000 0.00989 0.00917 = 0.01793 0.00050 -0.00052 0.00260 O4 3 0.571884 0.309660 0.484291 11.00000 0.01015 0.00985 = 0.03112 -0.00656 -0.00023 0.00172 AFIX 147 H18 2 0.485317 0.294276 0.484039 11.00000 -1.50000 AFIX 0 C1 1 0.772102 0.476155 0.738554 11.00000 0.01143 0.02525 = 0.02369 0.00662 -0.00359 0.00175 AFIX 137 H11 2 0.821244 0.544569 0.776866 11.00000 -1.50000 H1 2 0.827843 0.453403 0.680665 11.00000 -1.50000 H10 2 0.758697 0.395835 0.778707 11.00000 -1.50000 AFIX 0 C2 1 0.630242 0.529899 0.706646 11.00000 0.01008 0.01356 = 0.01760 0.00323 -0.00225 -0.00021 C3 1 0.636705 0.661856 0.641454 11.00000 0.01088 0.01137 = 0.01617 0.00191 -0.00135 -0.00263 AFIX 23 H7 2 0.633005 0.744013 0.681943 11.00000 -1.20000 H6 2 0.721486 0.663891 0.599710 11.00000 -1.20000 AFIX 0 C4 1 0.502851 0.643529 0.580815 11.00000 0.00864 0.00678 = 0.01394 0.00100 0.00144 -0.00148 C5 1 0.540455 0.559706 0.488062 11.00000 0.00812 0.00965 = 0.01506 -0.00165 0.00255 -0.00103 AFIX 13 H4 2 0.615905 0.605416 0.449786 11.00000 -1.20000 AFIX 0 C6 1 0.412043 0.535225 0.423216 11.00000 0.01095 0.01181 = 0.01637 -0.00332 -0.00111 0.00023 AFIX 23 H3 2 0.385373 0.620480 0.391234 11.00000 -1.20000 H2 2 0.437469 0.470729 0.371132 11.00000 -1.20000 AFIX 0 C7 1 0.285965 0.481059 0.479271 11.00000 0.00888 0.01041 = 0.02175 -0.00226 -0.00212 -0.00090 AFIX 13 H16 2 0.198586 0.502367 0.441973 11.00000 -1.20000 AFIX 0 C8 1 0.276600 0.544929 0.581217 11.00000 0.00837 0.00806 = 0.01897 0.00236 -0.00019 0.00116 C9 1 0.413855 0.539119 0.639702 11.00000 0.00778 0.00776 = 0.01535 0.00217 0.00101 0.00056 C10 1 0.396306 0.750178 0.559752 11.00000 0.01124 0.01066 = 0.01067 -0.00072 0.00060 0.00146 C11 1 0.598830 0.430451 0.537059 11.00000 0.00795 0.00969 = 0.02038 -0.00203 0.00116 0.00048 AFIX 13 H12 2 0.702783 0.440656 0.542797 11.00000 -1.20000 AFIX 0 C12 1 0.537070 0.436547 0.640727 11.00000 0.00833 0.00873 = 0.01960 0.00384 0.00067 0.00114 AFIX 13 H5 2 0.513944 0.347547 0.670175 11.00000 -1.20000 AFIX 0 C13 1 0.528270 0.567157 0.786502 11.00000 0.01827 0.01557 = 0.01479 0.00440 0.00077 0.00008 AFIX 43 H8 2 0.550562 0.580968 0.853488 11.00000 -1.20000 AFIX 0 C14 1 0.402005 0.577209 0.746606 11.00000 0.01359 0.01375 = 0.01415 0.00318 0.00409 0.00061 AFIX 43 H9 2 0.318670 0.603683 0.779377 11.00000 -1.20000 AFIX 0 C15 1 0.143687 0.503933 0.633569 11.00000 0.00919 0.02071 = 0.02310 0.00393 0.00227 -0.00047 AFIX 137 H15 2 0.130519 0.560521 0.691434 11.00000 -1.50000 H13 2 0.150898 0.409985 0.653760 11.00000 -1.50000 H14 2 0.063518 0.514726 0.589436 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM jar127b_0m_a.res in P2(1)2(1)2(1) REM R1 = 0.0306 for 2533 Fo > 4sig(Fo) and 0.0308 for all 2554 data REM 176 parameters refined using 0 restraints END WGHT 0.0484 0.2619 REM Instructions for potential hydrogen bonds HTAB O1 O4_$1 HTAB O4 O1 HTAB C5 O3_$2 HTAB C15 O2_$3 REM Highest difference peak 0.249, deepest hole -0.300, 1-sigma level 0.077 Q1 1 0.5494 0.9994 0.5249 11.00000 0.05 0.25 Q2 1 0.4926 0.9134 0.5538 11.00000 0.05 0.24 Q3 1 0.5714 0.9407 0.5542 11.00000 0.05 0.23 Q4 1 0.4715 1.0599 0.5634 11.00000 0.05 0.23 ; _shelx_res_checksum 31609 _shelx_hkl_file ; -2 0 0 430.86 18.30 -2 0 0 421.96 18.20 -3 0 0 1.90 1.10 -3 0 0 0.90 0.70 -4 0 0 153.48 9.00 -4 0 0 164.18 9.50 -5 0 0 -0.80 0.80 -5 0 0 -0.80 1.20 -6 0 0 5988.20 208.38 -6 0 0 4941.31 209.38 -6 0 0 4843.62 207.28 -6 0 0 4998.90 205.88 -6 0 0 5173.98 206.48 -7 0 0 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406.26 18.40 -9 3 0 431.16 18.20 -9 3 0 404.06 19.20 -10 3 0 358.66 15.30 -10 3 0 350.66 15.70 -10 -3 0 352.46 16.20 -10 -3 0 360.46 16.30 -10 3 0 342.67 16.40 -10 3 0 352.66 15.10 -10 3 0 349.96 15.80 -10 -3 0 371.06 16.80 -10 3 0 353.06 16.80 -11 -3 0 239.28 10.60 -11 -3 0 228.18 10.80 -11 -3 0 231.88 10.50 0 4 0 719.03 31.60 -1 4 0 4225.78 164.48 -1 4 0 3951.00 163.58 -2 4 0 1390.16 61.79 -2 4 0 1503.75 60.49 -3 4 0 10.00 2.40 -3 4 0 7.00 2.70 -4 4 0 108.99 9.70 -4 4 0 108.19 7.80 -5 -4 0 336.37 16.30 -5 -4 0 304.77 15.90 -5 4 0 370.76 18.70 -5 4 0 339.87 18.30 -5 4 0 349.77 16.60 -5 -4 0 306.77 15.90 -5 4 0 323.47 20.80 -5 4 0 376.46 19.20 -6 4 0 316.97 13.40 -6 4 0 295.37 13.80 -6 4 0 263.67 16.80 -6 4 0 276.17 14.50 6 4 0 243.58 15.40 -6 4 0 293.57 14.30 -6 -4 0 284.57 13.80 -6 4 0 243.18 22.40 -6 -4 0 296.07 14.70 -6 -4 0 283.17 14.20 -6 -4 0 282.57 14.20 -7 4 0 843.22 53.19 -7 -4 0 1032.60 43.80 -7 -4 0 1009.70 42.10 -7 4 0 965.50 43.20 -7 4 0 1072.29 44.20 -7 4 0 1101.49 42.00 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6 0 142.89 10.20 -4 6 0 136.79 14.10 -4 6 0 154.78 8.40 -5 -6 0 140.89 7.70 -5 6 0 125.99 8.20 -5 -6 0 141.59 8.20 -5 -6 0 156.48 8.30 -5 -6 0 123.39 7.60 5 6 0 135.49 10.00 -5 6 0 127.69 16.10 -5 6 0 139.19 8.60 -6 6 0 54.99 4.50 -6 -6 0 51.89 4.40 -6 6 0 52.59 9.40 -6 -6 0 53.69 4.40 -6 -6 0 58.29 4.20 -6 6 0 45.50 8.30 6 6 0 48.10 5.70 -6 -6 0 49.50 4.50 -6 6 0 60.19 4.90 -6 6 0 44.90 4.50 -7 -6 0 600.64 26.00 -7 6 0 580.24 26.30 -7 6 0 587.74 25.80 7 6 0 552.74 28.20 -7 -6 0 589.04 25.70 -7 6 0 598.94 26.40 -7 -6 0 576.34 25.80 -7 -6 0 578.64 25.50 -8 -6 0 13.80 2.00 -8 -6 0 11.60 1.60 8 6 0 15.40 2.80 -8 6 0 12.10 2.00 -8 6 0 8.60 1.70 -8 -6 0 10.80 1.80 -8 6 0 12.30 2.10 -8 -6 0 12.20 1.40 -9 6 0 281.77 13.30 -9 6 0 306.57 14.30 -9 -6 0 304.77 13.00 9 6 0 312.37 14.80 -9 6 0 280.07 13.50 -9 -6 0 293.07 13.30 -10 6 0 25.00 2.30 -10 6 0 24.80 1.90 -10 -6 0 29.20 1.80 0 7 0 9.60 1.90 0 -7 0 11.70 2.90 1 -7 0 10.90 2.40 1 7 0 14.10 2.50 -1 7 0 10.10 3.40 -1 -7 0 8.10 2.40 -1 -7 0 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2.00 -2 -2 16 15.10 1.90 -2 -2 16 12.30 1.60 3 2 -16 37.30 3.00 -3 -2 -16 36.80 3.10 -3 2 16 37.60 2.70 -3 2 16 36.50 2.60 -3 -2 16 38.10 2.70 -3 -2 16 36.00 3.40 3 -2 -16 31.90 4.10 0 -3 16 26.00 2.60 0 -3 -16 24.40 2.30 0 3 16 28.20 2.20 0 -3 -16 24.50 2.30 0 3 16 24.80 2.40 -1 -3 -16 117.49 6.50 -1 3 16 126.39 6.60 1 -3 16 112.59 6.70 -1 3 16 127.79 6.30 1 -3 -16 126.49 8.50 -1 -3 16 131.99 7.10 -1 -3 16 121.09 6.10 1 3 16 127.09 6.20 1 3 16 119.69 6.50 -2 3 16 35.30 2.60 2 3 -16 32.30 3.10 -2 3 16 36.70 3.50 -2 -3 -16 34.50 2.60 -2 3 16 37.00 2.60 -2 -3 16 37.50 2.50 2 3 16 33.80 2.70 -2 -3 16 35.60 2.90 2 -3 -16 33.20 3.50 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 39017