data_Compound5h _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H18 O6' _chemical_formula_weight 270.27 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' _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 7.3993(4) _cell_length_b 11.5801(6) _cell_length_c 7.7694(4) _cell_angle_alpha 90 _cell_angle_beta 103.973(3) _cell_angle_gamma 90 _cell_volume 646.02(6) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4746 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 28.65 _exptl_crystal_description 'Prismatic' _exptl_crystal_colour 'Colourless' _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_F_000 288 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_absorpt_coefficient_mu 0.110 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type 'Empirical' _exptl_absorpt_correction_T_min 0.659 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details 'Bruker SADABS (Bruker, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker D8 Venture' _diffrn_measurement_method 'Phi and Omega Scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 9943 _diffrn_reflns_av_unetI/netI 0.1236 _diffrn_reflns_av_R_equivalents 0.1927 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.701 _diffrn_reflns_theta_max 28.749 _diffrn_reflns_theta_full 25.240 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.968 _diffrn_reflns_point_group_measured_fraction_full 0.992 _reflns_number_total 3249 _reflns_number_gt 2895 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.859 _reflns_Friedel_fraction_max 0.939 _reflns_Friedel_fraction_full 0.983 _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 ApexII' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker Apex II' _computing_structure_solution 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-2014 (Sheldrick, 2014)' _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^)+(0.1318P)^2^+0.0205P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1161 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.8(10) _chemical_absolute_configuration ? _refine_ls_number_reflns 3249 _refine_ls_number_parameters 175 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0837 _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_ref 0.2014 _refine_ls_wR_factor_gt 0.1938 _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_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 0.3788(5) 0.7460(4) 0.4585(5) 0.0189(8) Uani 1 1 d . . . . . C2 C 0.4434(5) 0.7294(4) 0.7572(5) 0.0177(7) Uani 1 1 d . . . . . H2A H 0.5548 0.7098 0.8470 0.021 Uiso 1 1 calc R U . . . H2B H 0.3350 0.7085 0.7999 0.021 Uiso 1 1 calc R U . . . C3 C 0.4407(5) 0.8581(3) 0.7110(5) 0.0149(7) Uani 1 1 d . . . . . C4 C 0.6340(5) 0.9098(4) 0.7413(6) 0.0207(8) Uani 1 1 d . . . . . H4A H 0.7093 0.8625 0.6847 0.031 Uiso 1 1 d R U . . . H4B H 0.6897 0.9135 0.8663 0.031 Uiso 1 1 d R U . . . H4C H 0.6255 0.9862 0.6921 0.031 Uiso 1 1 d R U . . . C5 C 0.3036(5) 0.9250(3) 0.7922(5) 0.0122(6) Uani 1 1 d . . . . . H5 H 0.1820 0.8870 0.7559 0.015 Uiso 1 1 calc R U . . . C6 C 0.3634(5) 0.9231(3) 0.9946(5) 0.0159(7) Uani 1 1 d . . . . . H6A H 0.3727 0.8438 1.0358 0.019 Uiso 1 1 calc R U . . . H6B H 0.4853 0.9585 1.0337 0.019 Uiso 1 1 calc R U . . . C7 C 0.2251(5) 0.9875(3) 1.0737(5) 0.0148(7) Uani 1 1 d . . . . . H7 H 0.2537 0.9919 1.2035 0.018 Uiso 1 1 calc R U . . . C8 C 0.1061(5) 1.0803(3) 0.9758(5) 0.0129(7) Uani 1 1 d . . . . . C9 C 0.1208(5) 1.1106(3) 0.7892(5) 0.0128(7) Uani 1 1 d . . . . . H9 H 0.0027 1.0921 0.7052 0.015 Uiso 1 1 calc R U . . . C10 C 0.2796(5) 1.0503(3) 0.7300(5) 0.0150(7) Uani 1 1 d . . . . . H10A H 0.2547 1.0524 0.6016 0.018 Uiso 1 1 calc R U . . . H10B H 0.3948 1.0918 0.7771 0.018 Uiso 1 1 calc R U . . . C11 C 0.0181(6) 1.1686(4) 1.0716(5) 0.0178(7) Uani 1 1 d . . . . . H11A H -0.1088 1.1810 1.0081 0.027 Uiso 1 1 d R U . . . H11B H 0.0857 1.2399 1.0790 0.027 Uiso 1 1 d R U . . . H11C H 0.0212 1.1414 1.1890 0.027 Uiso 1 1 d R U . . . C12 C 0.0960(6) 1.2875(4) 0.6292(5) 0.0171(8) Uani 1 1 d . . . . . C13 C 0.1408(7) 1.4140(4) 0.6483(6) 0.0236(8) Uani 1 1 d . . . . . H13A H 0.2716 1.4251 0.6592 0.035 Uiso 1 1 d R U . . . H13B H 0.1079 1.4433 0.7522 0.035 Uiso 1 1 d R U . . . H13C H 0.0715 1.4545 0.5456 0.035 Uiso 1 1 d R U . . . O1 O 0.3410(5) 0.7199(3) 0.3054(4) 0.0279(7) Uani 1 1 d . . . . . O2 O 0.4411(4) 0.6723(3) 0.5927(4) 0.0223(6) Uani 1 1 d . . . . . O3 O 0.3636(4) 0.8540(3) 0.5181(4) 0.0172(6) Uani 1 1 d . . . . . O4 O 0.0327(4) 0.9651(2) 0.9845(4) 0.0158(6) Uani 1 1 d . . . . . O5 O 0.1515(4) 1.2339(2) 0.7876(3) 0.0144(5) Uani 1 1 d . . . . . O6 O 0.0217(5) 1.2389(3) 0.4945(4) 0.0244(7) 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 C1 0.0144(17) 0.0202(19) 0.0260(19) -0.0008(15) 0.0125(14) 0.0058(14) C2 0.0157(17) 0.0155(16) 0.0261(19) 0.0028(15) 0.0132(13) 0.0009(15) C3 0.0118(16) 0.0149(16) 0.0212(18) 0.0026(13) 0.0099(12) 0.0018(13) C4 0.0102(17) 0.022(2) 0.033(2) 0.0010(16) 0.0127(14) -0.0007(15) C5 0.0074(15) 0.0132(15) 0.0186(16) -0.0009(13) 0.0082(11) -0.0016(12) C6 0.0124(16) 0.0177(16) 0.0190(17) 0.0019(14) 0.0069(12) 0.0018(13) C7 0.0157(17) 0.0158(17) 0.0144(16) -0.0004(12) 0.0066(13) 0.0003(13) C8 0.0102(15) 0.0141(16) 0.0168(16) -0.0024(13) 0.0080(12) -0.0030(13) C9 0.0109(16) 0.0111(15) 0.0177(16) -0.0004(12) 0.0059(12) 0.0005(12) C10 0.0148(16) 0.0147(17) 0.0196(17) 0.0022(13) 0.0118(13) 0.0020(13) C11 0.0189(18) 0.0175(18) 0.0207(18) -0.0045(14) 0.0121(14) -0.0006(15) C12 0.0158(17) 0.0208(19) 0.0185(19) 0.0038(13) 0.0113(14) 0.0058(14) C13 0.033(2) 0.0195(19) 0.0220(19) 0.0057(15) 0.0137(15) 0.0052(17) O1 0.0309(17) 0.0281(16) 0.0284(16) -0.0053(13) 0.0142(13) 0.0055(14) O2 0.0271(16) 0.0164(13) 0.0275(15) -0.0014(11) 0.0148(12) 0.0031(12) O3 0.0181(14) 0.0160(13) 0.0208(14) 0.0004(10) 0.0113(10) 0.0050(11) O4 0.0125(13) 0.0150(13) 0.0233(14) 0.0004(10) 0.0113(10) -0.0032(10) O5 0.0162(12) 0.0123(11) 0.0170(12) 0.0006(10) 0.0089(9) 0.0013(11) O6 0.0320(17) 0.0251(15) 0.0182(13) 0.0030(12) 0.0099(11) 0.0079(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 C1 O1 1.193(5) . ? C1 O2 1.340(5) . ? C1 O3 1.348(5) . ? C2 O2 1.435(5) . ? C2 C3 1.531(5) . ? C3 O3 1.471(5) . ? C3 C4 1.516(5) . ? C3 C5 1.528(5) . ? C5 C10 1.526(5) . ? C5 C6 1.527(5) . ? C6 C7 1.512(5) . ? C7 O4 1.449(5) . ? C7 C8 1.478(5) . ? C8 O4 1.448(4) . ? C8 C11 1.502(5) . ? C8 C9 1.521(5) . ? C9 O5 1.446(4) . ? C9 C10 1.530(5) . ? C12 O6 1.199(5) . ? C12 O5 1.351(5) . ? C12 C13 1.501(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 124.6(4) . . ? O1 C1 O3 123.9(4) . . ? O2 C1 O3 111.4(3) . . ? O2 C2 C3 104.1(3) . . ? O3 C3 C4 106.9(3) . . ? O3 C3 C5 107.7(3) . . ? C4 C3 C5 115.5(3) . . ? O3 C3 C2 100.8(3) . . ? C4 C3 C2 112.9(3) . . ? C5 C3 C2 111.7(3) . . ? C10 C5 C6 108.8(3) . . ? C10 C5 C3 112.9(3) . . ? C6 C5 C3 111.2(3) . . ? C7 C6 C5 110.8(3) . . ? O4 C7 C8 59.3(2) . . ? O4 C7 C6 113.6(3) . . ? C8 C7 C6 121.8(3) . . ? O4 C8 C7 59.3(2) . . ? O4 C8 C11 113.1(3) . . ? C7 C8 C11 121.0(3) . . ? O4 C8 C9 111.7(3) . . ? C7 C8 C9 119.1(3) . . ? C11 C8 C9 117.1(3) . . ? O5 C9 C8 106.4(3) . . ? O5 C9 C10 108.4(3) . . ? C8 C9 C10 114.7(3) . . ? C5 C10 C9 112.2(3) . . ? O6 C12 O5 123.7(4) . . ? O6 C12 C13 126.0(4) . . ? O5 C12 C13 110.3(3) . . ? C1 O2 C2 109.1(3) . . ? C1 O3 C3 109.6(3) . . ? C8 O4 C7 61.4(2) . . ? C12 O5 C9 116.6(3) . . ? _refine_diff_density_max 0.532 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.120 _shelxl_version_number 2014-3 _shelx_res_file ; TITL mo_F11_01m in P2(1) CELL 0.71069 7.3993 11.5801 7.7694 90.000 103.973 90.000 ZERR 2.00 0.0004 0.0006 0.0004 0.000 0.003 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H O UNIT 26 36 12 MERG 2 acta FMAP 2 PLAN 5 LIST 1 L.S. 20 WGHT 0.131800 0.020500 FVAR 1.25936 C1 1 0.378816 0.745982 0.458540 11.00000 0.01444 0.02022 = 0.02602 -0.00078 0.01250 0.00579 C2 1 0.443376 0.729419 0.757168 11.00000 0.01573 0.01552 = 0.02610 0.00278 0.01318 0.00087 AFIX 23 H2A 2 0.554834 0.709769 0.846976 11.00000 -1.20000 H2B 2 0.334977 0.708549 0.799942 11.00000 -1.20000 AFIX 0 C3 1 0.440666 0.858059 0.711046 11.00000 0.01179 0.01486 = 0.02117 0.00264 0.00987 0.00176 C4 1 0.634034 0.909813 0.741304 11.00000 0.01023 0.02214 = 0.03341 0.00102 0.01270 -0.00071 AFIX 7 H4A 2 0.709285 0.862495 0.684748 11.00000 -1.50000 H4B 2 0.689747 0.913462 0.866297 11.00000 -1.50000 H4C 2 0.625501 0.986226 0.692079 11.00000 -1.50000 AFIX 0 C5 1 0.303563 0.924993 0.792179 11.00000 0.00740 0.01317 = 0.01858 -0.00089 0.00818 -0.00157 AFIX 13 H5 2 0.181980 0.886953 0.755866 11.00000 -1.20000 AFIX 0 C6 1 0.363432 0.923120 0.994558 11.00000 0.01244 0.01768 = 0.01904 0.00193 0.00693 0.00179 AFIX 23 H6A 2 0.372711 0.843784 1.035820 11.00000 -1.20000 H6B 2 0.485294 0.958490 1.033719 11.00000 -1.20000 AFIX 0 C7 1 0.225096 0.987513 1.073724 11.00000 0.01570 0.01576 = 0.01442 -0.00040 0.00658 0.00031 AFIX 13 H7 2 0.253697 0.991944 1.203460 11.00000 -1.20000 AFIX 0 C8 1 0.106072 1.080293 0.975847 11.00000 0.01021 0.01411 = 0.01684 -0.00242 0.00798 -0.00299 C9 1 0.120842 1.110569 0.789220 11.00000 0.01093 0.01109 = 0.01772 -0.00043 0.00586 0.00050 AFIX 13 H9 2 0.002688 1.092085 0.705238 11.00000 -1.20000 AFIX 0 C10 1 0.279621 1.050256 0.730007 11.00000 0.01478 0.01467 = 0.01957 0.00216 0.01182 0.00195 AFIX 23 H10A 2 0.254652 1.052370 0.601608 11.00000 -1.20000 H10B 2 0.394757 1.091836 0.777075 11.00000 -1.20000 AFIX 0 C11 1 0.018094 1.168591 1.071642 11.00000 0.01892 0.01746 = 0.02068 -0.00451 0.01213 -0.00059 AFIX 7 H11A 2 -0.108758 1.180963 1.008111 11.00000 -1.50000 H11B 2 0.085740 1.239884 1.079001 11.00000 -1.50000 H11C 2 0.021155 1.141381 1.189019 11.00000 -1.50000 AFIX 0 C12 1 0.096007 1.287493 0.629191 11.00000 0.01576 0.02077 = 0.01852 0.00385 0.01130 0.00583 C13 1 0.140789 1.414007 0.648265 11.00000 0.03305 0.01949 = 0.02197 0.00566 0.01371 0.00523 AFIX 7 H13A 2 0.271639 1.425116 0.659208 11.00000 -1.50000 H13B 2 0.107891 1.443327 0.752197 11.00000 -1.50000 H13C 2 0.071467 1.454471 0.545584 11.00000 -1.50000 AFIX 0 O1 3 0.340957 0.719939 0.305436 11.00000 0.03088 0.02814 = 0.02840 -0.00533 0.01415 0.00548 O2 3 0.441122 0.672304 0.592692 11.00000 0.02712 0.01639 = 0.02753 -0.00140 0.01481 0.00306 O3 3 0.363552 0.853987 0.518077 11.00000 0.01812 0.01602 = 0.02080 0.00039 0.01133 0.00498 O4 3 0.032695 0.965094 0.984470 11.00000 0.01251 0.01502 = 0.02334 0.00044 0.01126 -0.00322 O5 3 0.151478 1.233869 0.787639 11.00000 0.01625 0.01234 = 0.01700 0.00060 0.00888 0.00134 O6 3 0.021672 1.238885 0.494458 11.00000 0.03196 0.02513 = 0.01822 0.00301 0.00990 0.00786 HKLF 4 REM mo_F11_01m in P2(1) REM R1 = 0.0773 for 2895 Fo > 4sig(Fo) and 0.0837 for all 3249 data REM 175 parameters refined using 1 restraints END WGHT 0.1314 0.0256 REM Highest difference peak 0.532, deepest hole -0.611, 1-sigma level 0.120 Q1 1 0.1745 1.0399 1.0379 11.00000 0.05 0.53 Q2 1 -0.0124 1.0230 0.9256 11.00000 0.05 0.46 Q3 1 -0.0654 1.0007 0.8984 11.00000 0.05 0.43 Q4 1 -0.0568 1.2827 0.4172 11.00000 0.05 0.42 Q5 1 0.2342 0.8731 0.4178 11.00000 0.05 0.42 ; _shelx_res_checksum 73299 _shelx_hkl_file ; 0 0 -1 47.89 1.28 0 0 -1 51.26 1.33 0 0 1 63.31 3.31 0 0 1 42.35 1.18 0 0 1 49.31 1.32 0 0 -2 -1.13 2.39 0 0 -2 1.41 0.89 0 0 -2 0.77 0.89 0 0 2 0.70 2.41 0 0 2 1.19 0.79 0 0 2 0.84 0.84 0 0 -3 418.83 13.75 0 0 -3 315.30 5.46 0 0 3 309.72 12.18 0 0 3 267.31 4.96 0 0 3 259.25 5.07 0 0 -4 5087.50 52.37 0 0 -4 3771.30 21.22 0 0 4 3526.97 43.69 0 0 4 3032.66 18.44 0 0 4 3030.09 19.39 0 0 -5 68.95 10.54 0 0 -5 61.70 4.06 0 0 5 53.82 10.54 0 0 5 46.21 3.54 0 0 5 42.41 3.71 0 0 -6 42.06 11.82 0 0 -6 23.94 3.38 0 0 6 23.84 11.08 0 0 6 17.25 3.07 0 0 6 11.77 2.87 0 0 -7 234.41 23.25 0 0 -7 171.18 7.63 0 0 7 107.93 18.77 0 0 7 115.51 6.29 0 0 7 117.62 6.62 0 0 -8 57.83 20.16 0 0 -8 95.22 7.71 0 0 8 46.23 21.46 0 0 8 50.83 5.51 0 0 8 53.39 6.37 0 0 -9 2.41 5.32 0 0 9 1.20 5.19 0 0 9 -7.09 2.97 0 0 10 84.26 8.75 0 0 10 70.12 7.74 0 -1 -1 1350.38 14.90 0 -1 -1 1200.28 6.53 0 -1 -1 1206.15 5.00 0 -1 1 2386.62 16.57 0 -1 1 1251.99 5.25 0 -1 1 1120.92 7.61 0 1 -1 2501.53 17.01 0 1 -1 1388.84 7.20 0 1 1 1251.16 14.28 0 1 1 1138.84 6.38 0 1 1 1152.19 4.91 0 -1 -2 227.70 8.73 0 -1 -2 227.34 3.95 0 -1 -2 238.28 3.57 0 -1 2 296.11 9.03 0 -1 2 218.37 3.36 0 -1 2 224.12 4.05 0 1 -2 394.06 10.16 0 1 -2 258.12 3.80 0 1 -2 237.47 4.18 0 1 2 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