# Electronic Supplementary Material (ESI) for Chemical Science. # This journal is © The Royal Society of Chemistry 2020 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_mo_xlb301_0m _database_code_depnum_ccdc_archive 'CCDC 1917425' loop_ _audit_author_name _audit_author_address 'Xiaonian Li' ;Yunnan University China ; _audit_update_record ; 2019-05-21 deposited with the CCDC. 2020-01-10 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H16 O4' _chemical_formula_sum 'C18 H16 O4' _chemical_formula_weight 296.31 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 60 _space_group_name_H-M_alt 'P b c n' _space_group_name_Hall '-P 2n 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+1/2, -z' '-x, y, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 9.7263(8) _cell_length_b 11.8883(10) _cell_length_c 24.935(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2883.2(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9970 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 30.97 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_F_000 1248 _exptl_transmission_factor_min 0.4903 _exptl_transmission_factor_max 0.5649 _exptl_crystal_size_max 0.660 _exptl_crystal_size_mid 0.440 _exptl_crystal_size_min 0.360 _exptl_absorpt_coefficient_mu 0.096 _shelx_estimated_absorpt_T_min 0.939 _shelx_estimated_absorpt_T_max 0.966 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 'fine-focus sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 30553 _diffrn_reflns_av_unetI/netI 0.0211 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.633 _diffrn_reflns_theta_max 31.234 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.940 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.940 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.940 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 4416 _reflns_number_gt 3759 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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 'SHELXS-97 (Sheldrick 2008)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick 2014)' _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^)+(0.0593P)^2^+1.2533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _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_number_reflns 4416 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1148 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _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 O1 O 0.94283(8) 0.60424(6) 0.45593(3) 0.01798(17) Uani 1 1 d . . . . . H1 H 0.9348(16) 0.5337(14) 0.4411(6) 0.027 Uiso 1 1 d . U . . . O2 O 0.40655(9) 0.10059(7) 0.59176(3) 0.02113(18) Uani 1 1 d . . . . . O3 O 0.30506(9) 0.62989(7) 0.72038(3) 0.02221(18) Uani 1 1 d . . . . . O4 O 0.40319(8) 0.79160(6) 0.69344(3) 0.01724(17) Uani 1 1 d . . . . . C1 C 0.84883(10) 0.61846(8) 0.49553(4) 0.01313(19) Uani 1 1 d . . . . . C2 C 0.76629(11) 0.53050(8) 0.51404(4) 0.01487(19) Uani 1 1 d . . . . . H16 H 0.7763 0.4574 0.4991 0.018 Uiso 1 1 calc R U . . . C3 C 0.66981(11) 0.54926(8) 0.55404(4) 0.0154(2) Uani 1 1 d . . . . . H3 H 0.6141 0.4888 0.5661 0.018 Uiso 1 1 calc R U . . . C4 C 0.65331(11) 0.65658(8) 0.57696(4) 0.01341(19) Uani 1 1 d . . . . . C5 C 0.55665(11) 0.68712(8) 0.61941(4) 0.01385(19) Uani 1 1 d . . . . . H6 H 0.5488 0.7658 0.6254 0.017 Uiso 1 1 calc R U . . . C6 C 0.47646(10) 0.62362(8) 0.65165(4) 0.01292(19) Uani 1 1 d . . . . . C7 C 0.46875(10) 0.49825(8) 0.64988(4) 0.01239(18) Uani 1 1 d . . . . . C8 C 0.37567(11) 0.44561(9) 0.61545(4) 0.0169(2) Uani 1 1 d . . . . . H12 H 0.3114 0.4896 0.5959 0.020 Uiso 1 1 calc R U . . . C9 C 0.37613(11) 0.32948(9) 0.60952(4) 0.0167(2) Uani 1 1 d . . . . . H11 H 0.3138 0.2946 0.5853 0.020 Uiso 1 1 calc R U . . . C10 C 0.46793(10) 0.26405(8) 0.63901(4) 0.01285(18) Uani 1 1 d . . . . . C11 C 0.47251(11) 0.14069(8) 0.62911(4) 0.01448(19) Uani 1 1 d . . . . . C12 C 0.55981(12) 0.06674(9) 0.66413(5) 0.0209(2) Uani 1 1 d . . . . . H2 H 0.5406 -0.0124 0.6560 0.031 Uiso 1 1 calc R U . . . H10 H 0.5386 0.0817 0.7019 0.031 Uiso 1 1 calc R U . . . H9 H 0.6571 0.0826 0.6574 0.031 Uiso 1 1 calc R U . . . C13 C 0.73765(11) 0.74343(8) 0.55742(4) 0.01477(19) Uani 1 1 d . . . . . H4 H 0.7277 0.8169 0.5719 0.018 Uiso 1 1 calc R U . . . C14 C 0.83469(11) 0.72548(8) 0.51778(4) 0.0153(2) Uani 1 1 d . . . . . H5 H 0.8913 0.7856 0.5058 0.018 Uiso 1 1 calc R U . . . C15 C 0.55668(11) 0.31601(8) 0.67537(4) 0.01489(19) Uani 1 1 d . . . . . H8 H 0.6169 0.2716 0.6966 0.018 Uiso 1 1 calc R U . . . C16 C 0.55738(11) 0.43284(8) 0.68070(4) 0.01462(19) Uani 1 1 d . . . . . H7 H 0.6184 0.4678 0.7054 0.018 Uiso 1 1 calc R U . . . C17 C 0.38604(11) 0.67927(8) 0.69179(4) 0.01407(19) Uani 1 1 d . . . . . C18 C 0.31561(11) 0.85111(9) 0.73028(4) 0.0182(2) Uani 1 1 d . . . . . H15 H 0.2194 0.8314 0.7233 0.027 Uiso 1 1 calc R U . . . H14 H 0.3282 0.9323 0.7255 0.027 Uiso 1 1 calc R U . . . H13 H 0.3395 0.8302 0.7671 0.027 Uiso 1 1 calc R U . . . 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 O1 0.0186(4) 0.0142(3) 0.0212(4) -0.0036(3) 0.0068(3) -0.0007(3) O2 0.0257(4) 0.0148(3) 0.0230(4) -0.0057(3) -0.0031(3) -0.0025(3) O3 0.0282(4) 0.0153(4) 0.0231(4) 0.0004(3) 0.0104(3) -0.0021(3) O4 0.0196(4) 0.0113(3) 0.0208(4) -0.0043(3) 0.0075(3) -0.0002(3) C1 0.0134(4) 0.0128(4) 0.0133(4) -0.0001(3) -0.0006(3) 0.0018(3) C2 0.0201(5) 0.0095(4) 0.0150(4) -0.0009(3) 0.0008(4) 0.0013(3) C3 0.0202(5) 0.0100(4) 0.0159(4) 0.0001(3) 0.0025(4) -0.0004(3) C4 0.0165(4) 0.0107(4) 0.0130(4) 0.0000(3) 0.0005(3) 0.0016(3) C5 0.0181(5) 0.0097(4) 0.0137(4) -0.0007(3) 0.0005(4) 0.0021(3) C6 0.0160(4) 0.0100(4) 0.0128(4) -0.0011(3) -0.0001(3) 0.0014(3) C7 0.0147(4) 0.0102(4) 0.0123(4) -0.0006(3) 0.0019(3) 0.0001(3) C8 0.0191(5) 0.0140(4) 0.0176(5) -0.0005(3) -0.0061(4) 0.0022(4) C9 0.0191(5) 0.0137(4) 0.0172(5) -0.0025(4) -0.0056(4) -0.0003(4) C10 0.0149(4) 0.0103(4) 0.0134(4) -0.0011(3) 0.0005(3) -0.0005(3) C11 0.0164(5) 0.0109(4) 0.0162(4) -0.0012(3) 0.0028(4) -0.0017(3) C12 0.0261(5) 0.0115(4) 0.0252(5) 0.0016(4) -0.0025(4) 0.0007(4) C13 0.0187(5) 0.0094(4) 0.0163(4) -0.0015(3) 0.0003(4) 0.0011(3) C14 0.0165(5) 0.0113(4) 0.0182(5) -0.0004(3) 0.0004(4) -0.0016(3) C15 0.0167(5) 0.0118(4) 0.0162(4) 0.0004(3) -0.0038(4) 0.0008(3) C16 0.0165(5) 0.0115(4) 0.0159(5) -0.0011(3) -0.0034(4) -0.0011(3) C17 0.0168(5) 0.0116(4) 0.0139(4) -0.0008(3) 0.0000(4) 0.0007(3) C18 0.0189(5) 0.0156(4) 0.0201(5) -0.0061(4) 0.0057(4) 0.0012(4) _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 O1 C1 1.3564(12) . ? O1 H1 0.920(17) . ? O2 C11 1.2274(13) . ? O3 C17 1.2136(13) . ? O4 C17 1.3464(12) . ? O4 C18 1.4388(12) . ? C1 C14 1.3948(13) . ? C1 C2 1.3967(14) . ? C2 C3 1.3876(14) . ? C2 H16 0.9500 . ? C3 C4 1.4072(13) . ? C3 H3 0.9500 . ? C4 C13 1.4058(14) . ? C4 C5 1.4615(14) . ? C5 C6 1.3506(14) . ? C5 H6 0.9500 . ? C6 C17 1.4878(14) . ? C6 C7 1.4930(13) . ? C7 C16 1.3923(14) . ? C7 C8 1.3957(14) . ? C8 C9 1.3885(14) . ? C8 H12 0.9500 . ? C9 C10 1.3940(14) . ? C9 H11 0.9500 . ? C10 C15 1.3959(14) . ? C10 C11 1.4877(13) . ? C11 C12 1.5021(15) . ? C12 H2 0.9800 . ? C12 H10 0.9800 . ? C12 H9 0.9800 . ? C13 C14 1.3833(14) . ? C13 H4 0.9500 . ? C14 H5 0.9500 . ? C15 C16 1.3952(13) . ? C15 H8 0.9500 . ? C16 H7 0.9500 . ? C18 H15 0.9800 . ? C18 H14 0.9800 . ? C18 H13 0.9800 . ? 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 C1 O1 H1 110.4(10) . . ? C17 O4 C18 115.71(8) . . ? O1 C1 C14 118.01(9) . . ? O1 C1 C2 122.32(9) . . ? C14 C1 C2 119.67(9) . . ? C3 C2 C1 120.38(9) . . ? C3 C2 H16 119.8 . . ? C1 C2 H16 119.8 . . ? C2 C3 C4 120.99(9) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C13 C4 C3 117.30(9) . . ? C13 C4 C5 116.35(9) . . ? C3 C4 C5 126.35(9) . . ? C6 C5 C4 131.58(9) . . ? C6 C5 H6 114.2 . . ? C4 C5 H6 114.2 . . ? C5 C6 C17 119.56(9) . . ? C5 C6 C7 124.71(9) . . ? C17 C6 C7 115.73(8) . . ? C16 C7 C8 119.38(9) . . ? C16 C7 C6 120.68(9) . . ? C8 C7 C6 119.90(9) . . ? C9 C8 C7 120.62(9) . . ? C9 C8 H12 119.7 . . ? C7 C8 H12 119.7 . . ? C8 C9 C10 120.04(9) . . ? C8 C9 H11 120.0 . . ? C10 C9 H11 120.0 . . ? C9 C10 C15 119.46(9) . . ? C9 C10 C11 118.79(9) . . ? C15 C10 C11 121.70(9) . . ? O2 C11 C10 119.55(9) . . ? O2 C11 C12 120.61(9) . . ? C10 C11 C12 119.83(9) . . ? C11 C12 H2 109.5 . . ? C11 C12 H10 109.5 . . ? H2 C12 H10 109.5 . . ? C11 C12 H9 109.5 . . ? H2 C12 H9 109.5 . . ? H10 C12 H9 109.5 . . ? C14 C13 C4 122.17(9) . . ? C14 C13 H4 118.9 . . ? C4 C13 H4 118.9 . . ? C13 C14 C1 119.48(9) . . ? C13 C14 H5 120.3 . . ? C1 C14 H5 120.3 . . ? C16 C15 C10 120.36(9) . . ? C16 C15 H8 119.8 . . ? C10 C15 H8 119.8 . . ? C7 C16 C15 120.03(9) . . ? C7 C16 H7 120.0 . . ? C15 C16 H7 120.0 . . ? O3 C17 O4 122.84(9) . . ? O3 C17 C6 124.31(9) . . ? O4 C17 C6 112.84(9) . . ? O4 C18 H15 109.5 . . ? O4 C18 H14 109.5 . . ? H15 C18 H14 109.5 . . ? O4 C18 H13 109.5 . . ? H15 C18 H13 109.5 . . ? H14 C18 H13 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 O1 C1 C2 C3 -178.92(10) . . . . ? C14 C1 C2 C3 0.50(15) . . . . ? C1 C2 C3 C4 -0.28(16) . . . . ? C2 C3 C4 C13 0.40(15) . . . . ? C2 C3 C4 C5 -179.53(10) . . . . ? C13 C4 C5 C6 -169.50(11) . . . . ? C3 C4 C5 C6 10.44(18) . . . . ? C4 C5 C6 C17 -179.65(10) . . . . ? C4 C5 C6 C7 -0.68(18) . . . . ? C5 C6 C7 C16 89.40(13) . . . . ? C17 C6 C7 C16 -91.59(12) . . . . ? C5 C6 C7 C8 -88.02(13) . . . . ? C17 C6 C7 C8 90.98(12) . . . . ? C16 C7 C8 C9 -3.63(16) . . . . ? C6 C7 C8 C9 173.83(10) . . . . ? C7 C8 C9 C10 1.51(16) . . . . ? C8 C9 C10 C15 1.55(16) . . . . ? C8 C9 C10 C11 -175.93(10) . . . . ? C9 C10 C11 O2 7.44(15) . . . . ? C15 C10 C11 O2 -169.97(10) . . . . ? C9 C10 C11 C12 -173.77(10) . . . . ? C15 C10 C11 C12 8.81(15) . . . . ? C3 C4 C13 C14 -0.79(15) . . . . ? C5 C4 C13 C14 179.15(10) . . . . ? C4 C13 C14 C1 1.03(16) . . . . ? O1 C1 C14 C13 178.58(9) . . . . ? C2 C1 C14 C13 -0.87(15) . . . . ? C9 C10 C15 C16 -2.48(15) . . . . ? C11 C10 C15 C16 174.92(10) . . . . ? C8 C7 C16 C15 2.68(15) . . . . ? C6 C7 C16 C15 -174.75(9) . . . . ? C10 C15 C16 C7 0.35(16) . . . . ? C18 O4 C17 O3 -2.00(15) . . . . ? C18 O4 C17 C6 178.11(9) . . . . ? C5 C6 C17 O3 175.75(10) . . . . ? C7 C6 C17 O3 -3.31(15) . . . . ? C5 C6 C17 O4 -4.35(14) . . . . ? C7 C6 C17 O4 176.59(8) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O2 0.920(17) 1.816(17) 2.7328(11) 174.9(15) 2_556 O1 H1 O2 0.920(17) 1.816(17) 2.7328(11) 174.9(15) 2_556 O1 H1 O2 0.920(17) 1.816(17) 2.7328(11) 174.9(15) 2_556 O1 H1 O2 0.920(17) 1.816(17) 2.7328(11) 174.9(15) 2_556 O1 H1 O2 0.920(17) 1.816(17) 2.7328(11) 174.9(15) 2_556 O1 H1 O2 0.920(17) 1.816(17) 2.7328(11) 174.9(15) 2_556 O1 H1 O2 0.920(17) 1.816(17) 2.7328(11) 174.9(15) 2_556 O1 H1 O2 0.920(17) 1.816(17) 2.7328(11) 174.9(15) 2_556 _refine_diff_density_max 0.550 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.056 _shelx_res_file ; mo_xlb301_0m.res created by SHELXL-2014/7 TITL mo_xlb301_0m in Pbcn CELL 0.71073 9.7263 11.8883 24.9346 90.000 90.000 90.000 ZERR 8.00 0.0008 0.0010 0.0021 0.000 0.000 0.000 LATT 1 SYMM x+1/2, -y+1/2, -z SYMM -x, y, -z+1/2 SYMM -x+1/2, -y+1/2, z+1/2 SFAC C H O UNIT 144 128 32 L.S. 10 ACTA BOND $H FMAP 2 PLAN -4 HTAB O1 O2_$1 HTAB O1 O2_$1 HTAB O1 O2_$1 HTAB O1 O2_$1 HTAB O1 O2_$1 EQIV $1 x+1/2, -y+1/2, -z+1 CONF HTAB SIZE 0.360 0.440 0.660 HTAB O1 O2_$1 HTAB O1 O2_$1 HTAB O1 O2_$1 TEMP -173.000 WGHT 0.059300 1.253300 FVAR 0.10025 O1 3 0.942826 0.604241 0.455925 11.00000 0.01859 0.01421 = 0.02115 -0.00358 0.00679 -0.00074 H1 2 0.934796 0.533681 0.441131 11.00000 -1.50000 O2 3 0.406552 0.100592 0.591760 11.00000 0.02567 0.01476 = 0.02296 -0.00574 -0.00305 -0.00250 O3 3 0.305062 0.629894 0.720376 11.00000 0.02821 0.01527 = 0.02314 0.00037 0.01042 -0.00209 O4 3 0.403194 0.791598 0.693437 11.00000 0.01961 0.01129 = 0.02083 -0.00429 0.00748 -0.00017 C1 1 0.848835 0.618456 0.495535 11.00000 0.01336 0.01276 = 0.01328 -0.00013 -0.00058 0.00182 C2 1 0.766294 0.530495 0.514036 11.00000 0.02011 0.00953 = 0.01498 -0.00090 0.00075 0.00133 AFIX 43 H16 2 0.776263 0.457395 0.499144 11.00000 -1.20000 AFIX 0 C3 1 0.669814 0.549264 0.554042 11.00000 0.02020 0.00999 = 0.01594 0.00014 0.00248 -0.00041 AFIX 43 H3 2 0.614068 0.488753 0.566140 11.00000 -1.20000 AFIX 0 C4 1 0.653306 0.656582 0.576960 11.00000 0.01651 0.01071 = 0.01302 0.00000 0.00052 0.00157 C5 1 0.556649 0.687122 0.619408 11.00000 0.01812 0.00974 = 0.01368 -0.00071 0.00046 0.00205 AFIX 43 H6 2 0.548810 0.765776 0.625404 11.00000 -1.20000 AFIX 0 C6 1 0.476464 0.623623 0.651645 11.00000 0.01599 0.01000 = 0.01278 -0.00110 -0.00008 0.00140 C7 1 0.468749 0.498255 0.649876 11.00000 0.01470 0.01018 = 0.01228 -0.00057 0.00189 0.00009 C8 1 0.375671 0.445610 0.615453 11.00000 0.01910 0.01400 = 0.01762 -0.00053 -0.00612 0.00218 AFIX 43 H12 2 0.311401 0.489645 0.595901 11.00000 -1.20000 AFIX 0 C9 1 0.376129 0.329479 0.609517 11.00000 0.01910 0.01372 = 0.01721 -0.00251 -0.00560 -0.00031 AFIX 43 H11 2 0.313840 0.294592 0.585339 11.00000 -1.20000 AFIX 0 C10 1 0.467934 0.264047 0.639014 11.00000 0.01488 0.01031 = 0.01335 -0.00106 0.00054 -0.00052 C11 1 0.472515 0.140695 0.629114 11.00000 0.01637 0.01091 = 0.01616 -0.00121 0.00280 -0.00175 C12 1 0.559810 0.066739 0.664129 11.00000 0.02607 0.01150 = 0.02521 0.00156 -0.00252 0.00072 AFIX 137 H2 2 0.540594 -0.012357 0.655981 11.00000 -1.50000 H10 2 0.538640 0.081709 0.701886 11.00000 -1.50000 H9 2 0.657149 0.082613 0.657365 11.00000 -1.50000 AFIX 0 C13 1 0.737648 0.743434 0.557422 11.00000 0.01867 0.00936 = 0.01627 -0.00148 0.00029 0.00108 AFIX 43 H4 2 0.727671 0.816877 0.571924 11.00000 -1.20000 AFIX 0 C14 1 0.834689 0.725482 0.517776 11.00000 0.01646 0.01127 = 0.01816 -0.00043 0.00035 -0.00156 AFIX 43 H5 2 0.891255 0.785583 0.505791 11.00000 -1.20000 AFIX 0 C15 1 0.556675 0.316011 0.675373 11.00000 0.01671 0.01178 = 0.01618 0.00039 -0.00383 0.00084 AFIX 43 H8 2 0.616913 0.271590 0.696608 11.00000 -1.20000 AFIX 0 C16 1 0.557381 0.432838 0.680697 11.00000 0.01646 0.01149 = 0.01591 -0.00113 -0.00339 -0.00111 AFIX 43 H7 2 0.618364 0.467767 0.705362 11.00000 -1.20000 AFIX 0 C17 1 0.386037 0.679272 0.691794 11.00000 0.01679 0.01155 = 0.01388 -0.00076 -0.00005 0.00072 C18 1 0.315607 0.851112 0.730279 11.00000 0.01895 0.01561 = 0.02008 -0.00605 0.00573 0.00118 AFIX 137 H15 2 0.219448 0.831376 0.723262 11.00000 -1.50000 H14 2 0.328182 0.932294 0.725537 11.00000 -1.50000 H13 2 0.339535 0.830200 0.767133 11.00000 -1.50000 AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM mo_xlb301_0m in Pbcn REM R1 = 0.0417 for 3759 Fo > 4sig(Fo) and 0.0511 for all 4416 data REM 204 parameters refined using 0 restraints END WGHT 0.0593 1.2384 REM Instructions for potential hydrogen bonds HTAB O1 O2_$1 REM Highest difference peak 0.550, deepest hole -0.248, 1-sigma level 0.056 Q1 1 0.4719 0.5614 0.6507 11.00000 0.05 0.55 Q2 1 0.4682 0.2030 0.6374 11.00000 0.05 0.54 Q3 1 0.5611 0.3762 0.6745 11.00000 0.05 0.53 Q4 1 0.3706 0.3873 0.6155 11.00000 0.05 0.45 ; _shelx_res_checksum 80452