data_KH_LIT2_majucin _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common KH_LIT2_majucin _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H20 O8' _chemical_formula_weight 328.31 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 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 6.9941(3) _cell_length_b 12.1369(6) _cell_length_c 16.1722(8) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1372.80(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9967 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.35 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_F_000 696 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.260 _exptl_crystal_size_mid 0.170 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 0.130 _shelx_estimated_absorpt_T_min 0.967 _shelx_estimated_absorpt_T_max 0.987 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.705 _exptl_absorpt_correction_T_max 0.746 _exptl_absorpt_process_details SADABS _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'microfocus sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 24403 _diffrn_reflns_av_unetI/netI 0.0214 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.098 _diffrn_reflns_theta_max 28.352 _diffrn_reflns_theta_full 28.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 3431 _reflns_number_gt 3329 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.733 _reflns_Friedel_fraction_max 1.000 _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 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXT (Sheldrick 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics 'Mercury' _computing_publication_material 'WinGX' _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^)+(0.0381P)^2^+0.4848P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary iterative _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 1386 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.1(3) _chemical_absolute_configuration ad _refine_ls_number_reflns 3431 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0310 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0761 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 0.6376(3) 0.66966(14) 0.60269(11) 0.0117(3) Uani 1 1 d . . . . . H1A H 0.7604 0.6610 0.5717 0.014 Uiso 1 1 calc R U . . . C2 C 0.6079(2) 0.56948(14) 0.65906(10) 0.0099(3) Uani 1 1 d . . . . . C3 C 0.7658(2) 0.53834(13) 0.72115(10) 0.0102(3) Uani 1 1 d . . . . . C4 C 0.7814(3) 0.62188(14) 0.79332(11) 0.0130(3) Uani 1 1 d . . . . . H4A H 0.8146 0.6947 0.7714 0.019 Uiso 1 1 calc R U . . . H4B H 0.8808 0.5976 0.8319 0.019 Uiso 1 1 calc R U . . . H4C H 0.6585 0.6262 0.8223 0.019 Uiso 1 1 calc R U . . . C5 C 0.7238(2) 0.42162(14) 0.75672(10) 0.0107(3) Uani 1 1 d . . . . . C6 C 0.9254(3) 0.38357(15) 0.78087(11) 0.0128(3) Uani 1 1 d . . . . . C7 C 0.9688(3) 0.52491(15) 0.68652(11) 0.0128(3) Uani 1 1 d . . . . . H7A H 0.9651 0.4994 0.6284 0.015 Uiso 1 1 calc R U . . . H7B H 1.0397 0.5954 0.6891 0.015 Uiso 1 1 calc R U . . . C8 C 0.6425(3) 0.33531(14) 0.69531(11) 0.0117(3) Uani 1 1 d . . . . . H8A H 0.5942 0.2717 0.7286 0.014 Uiso 1 1 calc R U . . . C9 C 0.8349(3) 0.34160(15) 0.56949(12) 0.0139(3) Uani 1 1 d . . . . . C10 C 0.6986(3) 0.43007(14) 0.53527(11) 0.0122(3) Uani 1 1 d . . . . . H10 H 0.6241 0.3928 0.4905 0.015 Uiso 1 1 calc R U . . . C11 C 0.5474(2) 0.47787(14) 0.59541(10) 0.0103(3) Uani 1 1 d . . . . . C12 C 0.4776(2) 0.37720(14) 0.64341(11) 0.0118(3) Uani 1 1 d . . . . . H12A H 0.3687 0.3976 0.6794 0.014 Uiso 1 1 calc R U . . . H12B H 0.4345 0.3192 0.6046 0.014 Uiso 1 1 calc R U . . . C13 C 0.3923(3) 0.54242(14) 0.54608(11) 0.0126(3) Uani 1 1 d . . . . . H13 H 0.2754 0.5444 0.5817 0.015 Uiso 1 1 calc R U . . . C14 C 0.3312(3) 0.49451(16) 0.46317(12) 0.0165(4) Uani 1 1 d . . . . . H14A H 0.4382 0.4985 0.4242 0.025 Uiso 1 1 calc R U . . . H14B H 0.2229 0.5368 0.4414 0.025 Uiso 1 1 calc R U . . . H14C H 0.2931 0.4174 0.4706 0.025 Uiso 1 1 calc R U . . . C15 C 0.4691(3) 0.66245(15) 0.54173(11) 0.0143(3) Uani 1 1 d . . . . . H15A H 0.5124 0.6799 0.4849 0.017 Uiso 1 1 calc R U . . . H15B H 0.3676 0.7153 0.5574 0.017 Uiso 1 1 calc R U . . . O1 O 0.6388(2) 0.77281(10) 0.64560(9) 0.0142(3) Uani 1 1 d . . . . . O2 O 0.43905(18) 0.59532(11) 0.70679(8) 0.0122(3) Uani 1 1 d . . . . . O3 O 0.59986(19) 0.43177(11) 0.82494(8) 0.0131(3) Uani 1 1 d . . . . . O4 O 0.96764(19) 0.31180(11) 0.82929(8) 0.0159(3) Uani 1 1 d . . . . . O5 O 1.05801(19) 0.44175(11) 0.74003(8) 0.0151(3) Uani 1 1 d . . . . . O6 O 0.79913(19) 0.29463(10) 0.64340(8) 0.0140(3) Uani 1 1 d . . . . . O7 O 0.9706(2) 0.31062(12) 0.53029(9) 0.0195(3) Uani 1 1 d . . . . . O8 O 0.8061(2) 0.51322(11) 0.49520(9) 0.0167(3) Uani 1 1 d . . . . . H1 H 0.752(5) 0.792(3) 0.6539(18) 0.038(8) Uiso 1 1 d . . . . . H2 H 0.430(4) 0.551(2) 0.7438(18) 0.026(7) Uiso 1 1 d . . . . . H3 H 0.541(4) 0.370(2) 0.8342(17) 0.028(7) Uiso 1 1 d . . . . . H8 H 0.828(5) 0.497(3) 0.450(2) 0.056(11) 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 0.0132(7) 0.0084(7) 0.0136(8) 0.0007(6) -0.0004(6) 0.0003(6) C2 0.0094(7) 0.0098(7) 0.0106(7) 0.0002(6) 0.0014(6) 0.0013(6) C3 0.0108(7) 0.0090(7) 0.0108(7) 0.0013(6) 0.0006(6) 0.0008(6) C4 0.0152(8) 0.0110(8) 0.0127(8) -0.0011(6) -0.0010(6) -0.0006(7) C5 0.0122(7) 0.0099(7) 0.0099(7) 0.0006(6) -0.0002(6) 0.0003(6) C6 0.0143(8) 0.0121(8) 0.0118(8) -0.0029(6) -0.0012(6) 0.0014(6) C7 0.0106(7) 0.0137(8) 0.0142(8) 0.0026(7) -0.0002(6) 0.0011(6) C8 0.0140(8) 0.0107(7) 0.0104(8) -0.0007(6) 0.0027(6) 0.0006(6) C9 0.0157(8) 0.0117(8) 0.0142(8) -0.0027(6) 0.0000(6) -0.0010(6) C10 0.0140(8) 0.0118(8) 0.0109(8) -0.0003(6) 0.0013(6) -0.0009(6) C11 0.0114(7) 0.0094(7) 0.0100(7) 0.0000(6) 0.0005(6) 0.0000(6) C12 0.0128(7) 0.0108(7) 0.0119(7) 0.0001(6) 0.0001(6) -0.0015(6) C13 0.0114(8) 0.0132(8) 0.0131(8) 0.0013(7) -0.0013(6) 0.0006(6) C14 0.0183(9) 0.0168(9) 0.0144(8) -0.0006(7) -0.0037(7) -0.0014(7) C15 0.0168(8) 0.0128(8) 0.0133(8) 0.0017(6) -0.0030(7) 0.0009(7) O1 0.0142(6) 0.0091(6) 0.0194(6) -0.0013(5) 0.0002(5) -0.0002(5) O2 0.0113(6) 0.0132(6) 0.0120(6) 0.0005(5) 0.0029(5) 0.0015(5) O3 0.0153(6) 0.0114(6) 0.0124(6) 0.0000(5) 0.0040(5) -0.0011(5) O4 0.0177(6) 0.0131(6) 0.0171(6) 0.0003(5) -0.0026(5) 0.0038(5) O5 0.0113(6) 0.0160(6) 0.0180(6) 0.0027(5) 0.0001(5) 0.0024(5) O6 0.0166(6) 0.0116(6) 0.0137(6) -0.0004(5) 0.0018(5) 0.0031(5) O7 0.0191(6) 0.0185(7) 0.0208(7) -0.0012(5) 0.0052(6) 0.0044(5) O8 0.0217(7) 0.0150(7) 0.0135(6) 0.0007(5) 0.0066(5) -0.0023(5) _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 1.431(2) . ? C1 C2 1.534(2) . ? C1 C15 1.539(2) . ? C1 H1A 1.0000 . ? C2 O2 1.446(2) . ? C2 C3 1.539(2) . ? C2 C11 1.573(2) . ? C3 C7 1.535(2) . ? C3 C4 1.550(2) . ? C3 C5 1.557(2) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 O3 1.408(2) . ? C5 C6 1.534(2) . ? C5 C8 1.551(2) . ? C6 O4 1.208(2) . ? C6 O5 1.340(2) . ? C7 O5 1.469(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O6 1.466(2) . ? C8 C12 1.514(2) . ? C8 H8A 1.0000 . ? C9 O7 1.202(2) . ? C9 O6 1.348(2) . ? C9 C10 1.539(2) . ? C10 O8 1.415(2) . ? C10 C11 1.549(2) . ? C10 H10 1.0000 . ? C11 C12 1.528(2) . ? C11 C13 1.558(2) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.523(3) . ? C13 C15 1.554(2) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? O1 H1 0.84(3) . ? O2 H2 0.81(3) . ? O3 H3 0.86(3) . ? O8 H8 0.77(4) . ? 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 C2 113.96(14) . . ? O1 C1 C15 111.41(14) . . ? C2 C1 C15 103.43(14) . . ? O1 C1 H1A 109.3 . . ? C2 C1 H1A 109.3 . . ? C15 C1 H1A 109.3 . . ? O2 C2 C1 104.82(13) . . ? O2 C2 C3 106.91(13) . . ? C1 C2 C3 119.04(14) . . ? O2 C2 C11 106.42(13) . . ? C1 C2 C11 101.99(13) . . ? C3 C2 C11 116.51(14) . . ? C7 C3 C2 116.83(14) . . ? C7 C3 C4 106.22(14) . . ? C2 C3 C4 112.40(14) . . ? C7 C3 C5 102.28(13) . . ? C2 C3 C5 109.21(14) . . ? C4 C3 C5 109.29(14) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O3 C5 C6 113.10(14) . . ? O3 C5 C8 109.57(14) . . ? C6 C5 C8 107.25(14) . . ? O3 C5 C3 109.02(13) . . ? C6 C5 C3 101.22(14) . . ? C8 C5 C3 116.56(14) . . ? O4 C6 O5 122.01(16) . . ? O4 C6 C5 127.38(16) . . ? O5 C6 C5 110.61(14) . . ? O5 C7 C3 104.53(13) . . ? O5 C7 H7A 110.8 . . ? C3 C7 H7A 110.8 . . ? O5 C7 H7B 110.8 . . ? C3 C7 H7B 110.8 . . ? H7A C7 H7B 108.9 . . ? O6 C8 C12 111.40(13) . . ? O6 C8 C5 108.67(14) . . ? C12 C8 C5 114.03(14) . . ? O6 C8 H8A 107.5 . . ? C12 C8 H8A 107.5 . . ? C5 C8 H8A 107.5 . . ? O7 C9 O6 118.83(17) . . ? O7 C9 C10 121.19(17) . . ? O6 C9 C10 119.93(15) . . ? O8 C10 C9 109.45(15) . . ? O8 C10 C11 112.52(14) . . ? C9 C10 C11 117.28(15) . . ? O8 C10 H10 105.5 . . ? C9 C10 H10 105.5 . . ? C11 C10 H10 105.5 . . ? C12 C11 C10 103.74(14) . . ? C12 C11 C13 116.10(14) . . ? C10 C11 C13 110.00(14) . . ? C12 C11 C2 108.59(13) . . ? C10 C11 C2 119.44(14) . . ? C13 C11 C2 99.62(13) . . ? C8 C12 C11 107.88(14) . . ? C8 C12 H12A 110.1 . . ? C11 C12 H12A 110.1 . . ? C8 C12 H12B 110.1 . . ? C11 C12 H12B 110.1 . . ? H12A C12 H12B 108.4 . . ? C14 C13 C15 114.52(15) . . ? C14 C13 C11 117.03(15) . . ? C15 C13 C11 104.70(14) . . ? C14 C13 H13 106.6 . . ? C15 C13 H13 106.6 . . ? C11 C13 H13 106.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C1 C15 C13 106.80(14) . . ? C1 C15 H15A 110.4 . . ? C13 C15 H15A 110.4 . . ? C1 C15 H15B 110.4 . . ? C13 C15 H15B 110.4 . . ? H15A C15 H15B 108.6 . . ? C1 O1 H1 109(2) . . ? C2 O2 H2 108(2) . . ? C5 O3 H3 110.7(19) . . ? C6 O5 C7 111.01(13) . . ? C9 O6 C8 120.28(14) . . ? C10 O8 H8 111(3) . . ? _refine_diff_density_max 0.307 _refine_diff_density_min -0.221 _refine_diff_density_rms 0.045 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in P2(1)2(1)2(1) CELL 0.71073 6.9941 12.1369 16.1722 90.000 90.000 90.000 ZERR 4.00 0.0003 0.0006 0.0008 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 60 80 32 MERG 2 FMAP 2 PLAN 20 SIZE 0.100 0.170 0.260 ACTA 56.00 BOND $H LIST 4 WPDB -2 L.S. 10 TEMP -173.00 WGHT 0.038100 0.484800 FVAR 0.25849 C1 1 0.637573 0.669661 0.602695 11.00000 0.01321 0.00836 = 0.01361 0.00075 -0.00040 0.00033 AFIX 13 H1A 2 0.760357 0.660953 0.571694 11.00000 -1.20000 AFIX 0 C2 1 0.607948 0.569483 0.659063 11.00000 0.00942 0.00977 = 0.01063 0.00024 0.00139 0.00129 C3 1 0.765778 0.538341 0.721153 11.00000 0.01080 0.00900 = 0.01081 0.00132 0.00055 0.00081 C4 1 0.781355 0.621877 0.793320 11.00000 0.01523 0.01102 = 0.01274 -0.00109 -0.00098 -0.00057 AFIX 137 H4A 2 0.814588 0.694654 0.771355 11.00000 -1.50000 H4B 2 0.880799 0.597629 0.831937 11.00000 -1.50000 H4C 2 0.658526 0.626172 0.822302 11.00000 -1.50000 AFIX 0 C5 1 0.723780 0.421624 0.756716 11.00000 0.01223 0.00994 = 0.00988 0.00063 -0.00017 0.00025 C6 1 0.925368 0.383567 0.780875 11.00000 0.01435 0.01214 = 0.01177 -0.00290 -0.00124 0.00141 C7 1 0.968783 0.524910 0.686516 11.00000 0.01058 0.01366 = 0.01419 0.00260 -0.00016 0.00107 AFIX 23 H7A 2 0.965131 0.499429 0.628384 11.00000 -1.20000 H7B 2 1.039687 0.595421 0.689150 11.00000 -1.20000 AFIX 0 C8 1 0.642485 0.335309 0.695306 11.00000 0.01396 0.01068 = 0.01043 -0.00075 0.00270 0.00061 AFIX 13 H8A 2 0.594207 0.271688 0.728591 11.00000 -1.20000 AFIX 0 C9 1 0.834930 0.341603 0.569492 11.00000 0.01571 0.01169 = 0.01416 -0.00270 0.00000 -0.00102 C10 1 0.698601 0.430074 0.535269 11.00000 0.01399 0.01183 = 0.01088 -0.00027 0.00133 -0.00093 AFIX 13 H10 2 0.624073 0.392825 0.490512 11.00000 -1.20000 AFIX 0 C11 1 0.547395 0.477868 0.595411 11.00000 0.01138 0.00942 = 0.01004 0.00005 0.00047 0.00001 C12 1 0.477619 0.377203 0.643405 11.00000 0.01276 0.01077 = 0.01193 0.00015 0.00012 -0.00155 AFIX 23 H12A 2 0.368724 0.397629 0.679385 11.00000 -1.20000 H12B 2 0.434544 0.319185 0.604617 11.00000 -1.20000 AFIX 0 C13 1 0.392299 0.542419 0.546076 11.00000 0.01140 0.01317 = 0.01310 0.00135 -0.00129 0.00061 AFIX 13 H13 2 0.275423 0.544375 0.581663 11.00000 -1.20000 AFIX 0 C14 1 0.331185 0.494512 0.463165 11.00000 0.01826 0.01678 = 0.01437 -0.00058 -0.00374 -0.00139 AFIX 137 H14A 2 0.438232 0.498475 0.424178 11.00000 -1.50000 H14B 2 0.222939 0.536785 0.441392 11.00000 -1.50000 H14C 2 0.293051 0.417442 0.470565 11.00000 -1.50000 AFIX 0 C15 1 0.469124 0.662448 0.541725 11.00000 0.01675 0.01278 = 0.01330 0.00173 -0.00297 0.00090 AFIX 23 H15A 2 0.512448 0.679869 0.484933 11.00000 -1.20000 H15B 2 0.367618 0.715317 0.557412 11.00000 -1.20000 AFIX 0 O1 3 0.638822 0.772810 0.645598 11.00000 0.01420 0.00905 = 0.01943 -0.00125 0.00019 -0.00016 O2 3 0.439046 0.595317 0.706794 11.00000 0.01132 0.01317 = 0.01198 0.00049 0.00292 0.00154 O3 3 0.599855 0.431772 0.824938 11.00000 0.01534 0.01143 = 0.01239 -0.00002 0.00401 -0.00112 O4 3 0.967640 0.311800 0.829292 11.00000 0.01765 0.01308 = 0.01707 0.00028 -0.00259 0.00375 O5 3 1.058007 0.441752 0.740028 11.00000 0.01131 0.01602 = 0.01805 0.00273 0.00011 0.00242 O6 3 0.799130 0.294632 0.643404 11.00000 0.01659 0.01155 = 0.01373 -0.00035 0.00185 0.00307 O7 3 0.970600 0.310617 0.530294 11.00000 0.01913 0.01848 = 0.02083 -0.00117 0.00524 0.00441 O8 3 0.806086 0.513224 0.495202 11.00000 0.02170 0.01501 = 0.01354 0.00066 0.00655 -0.00235 H1 2 0.751785 0.792158 0.653866 11.00000 0.03841 H2 2 0.430062 0.550927 0.743818 11.00000 0.02611 H3 2 0.541142 0.370344 0.834220 11.00000 0.02846 H8 2 0.828031 0.497072 0.450170 11.00000 0.05572 HKLF 4 REM shelxt_a.res in P2(1)2(1)2(1) REM R1 = 0.0300 for 3329 Fo > 4sig(Fo) and 0.0310 for all 3431 data REM 226 parameters refined using 0 restraints END WGHT 0.0379 0.4862 REM Highest difference peak 0.307, deepest hole -0.221, 1-sigma level 0.045 Q1 1 0.6215 0.6235 0.6301 11.00000 0.05 0.31 Q2 1 0.6919 0.3791 0.7222 11.00000 0.05 0.29 Q3 1 0.8180 0.3981 0.7703 11.00000 0.05 0.27 Q4 1 0.7733 0.5780 0.7554 11.00000 0.05 0.27 Q5 1 0.5501 0.6665 0.5746 11.00000 0.05 0.25 Q6 1 0.5607 0.3601 0.6708 11.00000 0.05 0.24 Q7 1 0.5873 0.5224 0.6242 11.00000 0.05 0.23 Q8 1 0.6875 0.5549 0.6914 11.00000 0.05 0.23 Q9 1 0.4716 0.5095 0.5643 11.00000 0.05 0.22 Q10 1 0.7688 0.3930 0.5587 11.00000 0.05 0.22 Q11 1 0.6299 0.4550 0.5665 11.00000 0.05 0.22 Q12 1 0.4345 0.5994 0.5406 11.00000 0.05 0.21 Q13 1 0.7394 0.4840 0.7372 11.00000 0.05 0.21 Q14 1 0.5139 0.4257 0.6171 11.00000 0.05 0.20 Q15 1 0.3571 0.5247 0.5023 11.00000 0.05 0.18 Q16 1 0.5605 0.7946 0.6759 11.00000 0.05 0.18 Q17 1 0.8570 0.5273 0.6999 11.00000 0.05 0.18 Q18 1 0.7843 0.3078 0.6018 11.00000 0.05 0.16 Q19 1 0.6833 0.4404 0.8012 11.00000 0.05 0.16 Q20 1 0.6456 0.7076 0.6180 11.00000 0.05 0.16 ; _shelx_res_checksum 60507 _shelx_hkl_file ; -1 0 0 0.20 0.03 -1 0 0 0.15 0.02 -1 0 0 0.15 0.06 -1 0 0 0.20 0.03 1 0 0 0.14 0.03 1 0 0 0.21 0.04 1 0 0 0.15 0.04 2 0 0 118.36 4.62 2 0 0 124.90 4.63 2 0 0 122.78 4.63 3 0 0 0.05 0.06 3 0 0 0.17 0.07 3 0 0 0.09 0.06 4 0 0 5.15 0.32 4 0 0 5.63 0.33 -4 0 0 5.39 0.47 -4 0 0 4.96 0.28 -4 0 0 4.36 0.26 -5 0 0 0.35 0.21 5 0 0 0.31 0.12 -5 0 0 0.27 0.10 -5 0 0 0.55 0.15 5 0 0 0.58 0.16 6 0 0 0.52 0.17 -6 0 0 0.45 0.24 -6 0 0 0.85 0.21 -7 0 0 0.24 0.16 7 0 0 0.18 0.15 -7 0 0 0.47 0.31 8 0 0 7.33 0.55 -8 0 0 7.40 0.85 -8 0 0 7.02 0.56 -9 0 0 -0.02 0.18 -9 0 0 -0.01 0.36 0 1 0 0.71 0.06 0 -1 0 0.76 0.07 0 1 0 0.67 0.07 0 1 0 0.75 0.06 0 1 0 0.75 0.07 0 -1 0 0.69 0.07 0 1 0 0.69 0.07 0 1 0 0.71 0.09 0 -1 0 0.69 0.06 0 -1 0 0.70 0.07 1 1 0 999.33 36.86 1 1 0 1000.00 36.83 1 1 0 961.41 36.91 1 1 0 980.17 36.85 -1 -1 0 961.27 36.84 -1 -1 0 995.34 36.85 -1 -1 0 941.79 36.91 -1 -1 0 977.17 36.87 -1 -1 0 975.03 36.93 -1 -1 0 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