# Electronic Supplementary Material (ESI) for RSC Advances. # 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_150824d_tw _database_code_depnum_ccdc_archive 'CCDC 1989014' _audit_update_record ; 2020-03-09 deposited with the CCDC. 2020-08-19 downloaded from the CCDC. ; _publcif_datablock.id {ddd6e317-8049-4c29-9476-8ea307472d64} _audit_creation_method SHELXL-2018/1 _shelx_SHELXL_version_number 2018/1 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H38 N2 O17 Y2' _chemical_formula_weight 852.42 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' N N 0.0061 0.0033 '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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/n' _space_group_name_Hall '-P 2yn' _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+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3026(8) _cell_length_b 17.5625(14) _cell_length_c 11.3369(9) _cell_angle_alpha 90 _cell_angle_beta 94.3500(10) _cell_angle_gamma 90 _cell_volume 1846.9(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1712 _cell_measurement_theta_min 2.494 _cell_measurement_theta_max 28.253 _exptl_crystal_description bloc _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_F_000 868 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.130 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.100 _exptl_absorpt_coefficient_mu 3.199 _shelx_estimated_absorpt_T_min 0.681 _shelx_estimated_absorpt_T_max 0.740 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6807 _exptl_absorpt_correction_T_max 0.7402 _exptl_absorpt_process_details sadabs _exptl_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker SMART APEX II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 3171 _diffrn_reflns_av_unetI/netI 0.1804 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.143 _diffrn_reflns_theta_max 25.041 _diffrn_reflns_theta_full 25.041 _diffrn_measured_fraction_theta_max 0.971 _diffrn_measured_fraction_theta_full 0.971 _diffrn_reflns_Laue_measured_fraction_max 0.971 _diffrn_reflns_Laue_measured_fraction_full 0.971 _diffrn_reflns_point_group_measured_fraction_max 0.971 _diffrn_reflns_point_group_measured_fraction_full 0.971 _reflns_number_total 3171 _reflns_number_gt 1608 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component twin. ; _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^)+(0.0932P)^2^] 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_number_reflns 3171 _refine_ls_number_parameters 240 _refine_ls_number_restraints 1030 _refine_ls_R_factor_all 0.1670 _refine_ls_R_factor_gt 0.0938 _refine_ls_wR_factor_ref 0.2286 _refine_ls_wR_factor_gt 0.2072 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 0.986 _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 Y1 Y 0.51485(12) 0.10100(5) 0.93409(10) 0.0341(4) Uani 1 1 d . U . . . N1 N 0.9147(14) 0.1829(8) 0.8317(12) 0.096(4) Uani 1 1 d D U . . . O1 O 0.5621(9) 0.2351(4) 0.9874(7) 0.055(2) Uani 1 1 d D U . . . O2 O 0.4114(8) 0.2103(4) 0.8316(6) 0.047(2) Uani 1 1 d D U . . . O3 O 0.3220(11) 0.1347(5) 1.0531(8) 0.067(2) Uani 1 1 d D U . . . O4 O 0.3873(9) 0.0181(4) 1.0796(7) 0.051(2) Uani 1 1 d D U . . . O5 O 0.6607(9) 0.0877(4) 1.1061(7) 0.057(2) Uani 1 1 d D U . . . O6 O 0.740(4) 0.1358(16) 0.868(2) 0.072(3) Uani 0.45(3) 1 d D U P A 1 O6' O 0.689(3) 0.1220(12) 0.825(2) 0.072(3) Uani 0.55(3) 1 d . U P A 2 O7 O 0.333(2) 0.1872(9) 0.5787(15) 0.080(5) Uani 0.5 1 d . U P . . H7C H 0.255179 0.210061 0.556929 0.096 Uiso 0.5 1 d R U P . . H7D H 0.370313 0.210455 0.639355 0.096 Uiso 0.5 1 d DR U P . . O8 O 0.6651(9) -0.0351(4) 1.1747(7) 0.062(2) Uani 1 1 d D U . . . O9 O 0.5192(18) 0.0770(8) 0.7126(9) 0.183(6) Uani 1 1 d . U . . . H9B H 0.590303 0.102724 0.691516 0.220 Uiso 1 1 d DR U . . . H9C H 0.443184 0.096584 0.679065 0.220 Uiso 1 1 d DR U . . . C1 C 0.4716(12) 0.2569(5) 0.9011(8) 0.043(3) Uani 1 1 d D U . . . C2 C 0.4411(12) 0.3402(5) 0.8877(9) 0.041(3) Uani 1 1 d D U . . . C3 C 0.5005(11) 0.3943(5) 0.9666(8) 0.038(3) Uani 1 1 d D U . . . H3 H 0.565355 0.378400 1.028124 0.045 Uiso 1 1 calc R U . . . C4 C 0.4665(12) 0.4713(5) 0.9570(9) 0.037(3) Uani 1 1 d D U . . . C5 C 0.3018(13) 0.0732(6) 1.1022(12) 0.062(4) Uani 1 1 d D U . . . C6 C 0.216(5) 0.069(2) 1.209(3) 0.085(7) Uani 0.46(3) 1 d D U P B 1 H6A H 0.119515 0.086580 1.189047 0.128 Uiso 0.46(3) 1 calc R U P B 1 H6B H 0.260478 0.099633 1.271377 0.128 Uiso 0.46(3) 1 calc R U P B 1 H6C H 0.212261 0.016745 1.235553 0.128 Uiso 0.46(3) 1 calc R U P B 1 C6' C 0.154(2) 0.0517(19) 1.140(4) 0.085(7) Uani 0.54(3) 1 d D U P B 2 H6'1 H 0.105168 0.096648 1.163921 0.128 Uiso 0.54(3) 1 calc R U P B 2 H6'2 H 0.164906 0.016793 1.205444 0.128 Uiso 0.54(3) 1 calc R U P B 2 H6'3 H 0.098851 0.028025 1.075246 0.128 Uiso 0.54(3) 1 calc R U P B 2 C7 C 0.7056(13) 0.0334(5) 1.1797(10) 0.052(3) Uani 1 1 d D U . . . C8 C 0.8725(13) 0.0074(6) 1.3601(10) 0.053(3) Uani 1 1 d D U . . . H8 H 0.850511 -0.043968 1.350036 0.064 Uiso 1 1 calc R U . . . C9 C 0.8426(12) 0.1354(5) 1.2923(9) 0.041(3) Uani 1 1 d D U . . . H9 H 0.800105 0.170930 1.239789 0.049 Uiso 1 1 calc R U . . . C11 C 0.959(2) 0.1393(13) 0.9405(15) 0.150(7) Uani 1 1 d D U . . . H11A H 0.879718 0.108537 0.962070 0.226 Uiso 1 1 calc R U . . . H11B H 0.986362 0.174017 1.003612 0.226 Uiso 1 1 calc R U . . . H11C H 1.039140 0.107136 0.926139 0.226 Uiso 1 1 calc R U . . . C12 C 1.0307(19) 0.2243(14) 0.7784(17) 0.155(9) Uani 1 1 d D U . . . H12A H 1.037506 0.207007 0.698651 0.233 Uiso 1 1 calc DR U . . . H12B H 1.120501 0.215106 0.823620 0.233 Uiso 1 1 calc R U . . . H12C H 1.010071 0.277872 0.777974 0.233 Uiso 1 1 calc R U . . . C13 C 0.7841(15) 0.1689(10) 0.7790(13) 0.103(4) Uani 1 1 d D U . . . C14 C 0.752(2) 0.1962(12) 0.6546(15) 0.145(7) Uani 1 1 d D U . . . H14A H 0.655273 0.215921 0.645780 0.218 Uiso 1 1 calc DR U . . . H14B H 0.760633 0.154545 0.600860 0.218 Uiso 1 1 calc DR U . . . H14C H 0.818580 0.235623 0.637601 0.218 Uiso 1 1 calc DR U . . . C15 C 0.8103(13) 0.0589(5) 1.2782(9) 0.050(3) Uani 1 1 d D 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 Y1 0.0393(6) 0.0125(5) 0.0470(6) 0.0017(6) -0.0184(4) -0.0019(6) N1 0.080(8) 0.094(9) 0.111(8) 0.007(8) -0.013(7) -0.010(8) O1 0.075(5) 0.027(4) 0.058(4) 0.005(4) -0.041(4) 0.003(4) O2 0.067(5) 0.009(3) 0.058(4) -0.005(3) -0.032(4) -0.002(4) O3 0.089(6) 0.048(5) 0.065(5) 0.006(5) 0.016(5) 0.022(5) O4 0.055(5) 0.028(4) 0.072(5) 0.002(4) 0.010(4) 0.010(4) O5 0.075(5) 0.021(4) 0.071(5) 0.004(4) -0.022(4) -0.007(4) O6 0.073(7) 0.052(6) 0.088(7) 0.009(6) -0.004(6) -0.015(6) O6' 0.073(7) 0.052(6) 0.088(7) 0.009(6) -0.004(6) -0.015(6) O7 0.103(10) 0.068(10) 0.066(8) -0.008(8) -0.019(8) 0.002(9) O8 0.081(6) 0.021(4) 0.075(5) 0.011(4) -0.044(5) -0.006(4) O9 0.264(15) 0.224(15) 0.060(4) -0.026(9) 0.005(9) 0.010(13) C1 0.058(6) 0.023(5) 0.045(6) -0.003(5) -0.022(5) 0.002(5) C2 0.053(6) 0.018(5) 0.048(6) -0.002(5) -0.021(5) -0.007(5) C3 0.058(6) 0.013(4) 0.038(5) -0.001(4) -0.019(5) 0.004(5) C4 0.056(7) 0.011(5) 0.039(6) -0.006(5) -0.023(5) 0.009(5) C5 0.064(8) 0.045(7) 0.079(8) 0.004(7) 0.017(7) 0.011(7) C6 0.097(13) 0.079(12) 0.083(13) -0.009(11) 0.031(11) 0.015(11) C6' 0.097(13) 0.079(12) 0.083(13) -0.009(11) 0.031(11) 0.015(11) C7 0.058(7) 0.016(5) 0.076(7) -0.004(5) -0.028(6) -0.006(5) C8 0.076(8) 0.014(5) 0.063(7) 0.006(6) -0.037(6) 0.000(6) C9 0.050(7) 0.028(6) 0.042(6) 0.017(5) -0.017(5) 0.006(5) C11 0.150(15) 0.177(17) 0.128(14) 0.010(14) 0.037(13) -0.037(14) C12 0.140(17) 0.17(2) 0.154(17) 0.017(16) 0.005(15) -0.066(16) C13 0.113(10) 0.077(9) 0.118(8) 0.002(8) -0.005(9) 0.013(9) C14 0.144(15) 0.150(16) 0.141(11) 0.051(13) -0.003(13) -0.003(14) C15 0.070(8) 0.029(7) 0.047(6) -0.001(6) -0.024(6) 0.000(6) _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 Y1 O6' 2.143(19) . ? Y1 O4 2.291(7) 3_657 ? Y1 O5 2.301(8) . ? Y1 O8 2.313(7) 3_657 ? Y1 O6 2.36(3) . ? Y1 O3 2.399(9) . ? Y1 O2 2.406(7) . ? Y1 O1 2.462(8) . ? Y1 O9 2.549(11) . ? Y1 O4 2.558(8) . ? Y1 Y1 3.867(2) 3_657 ? N1 C13 1.335(9) . ? N1 C12 1.469(9) . ? N1 C11 1.483(9) . ? O1 C1 1.299(8) . ? O2 C1 1.239(8) . ? O3 C5 1.235(8) . ? O4 C5 1.290(8) . ? O5 C7 1.314(8) . ? O6 C13 1.263(10) . ? O6' C13 1.34(3) . ? O8 C7 1.261(8) . ? C1 C2 1.496(8) . ? C2 C3 1.390(8) . ? C2 C9 1.430(13) 4_565 ? C3 C4 1.392(8) . ? C4 C8 1.402(13) 4_565 ? C4 C4 1.504(18) 3_667 ? C5 C6 1.506(10) . ? C5 C6' 1.519(10) . ? C7 C15 1.495(8) . ? C8 C15 1.390(8) . ? C9 C15 1.383(9) . ? C13 C14 1.498(9) . ? 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 O6' Y1 O5 95.0(8) . . ? O4 Y1 O5 75.7(3) 3_657 . ? O4 Y1 O8 77.4(3) 3_657 3_657 ? O5 Y1 O8 139.2(3) . 3_657 ? O4 Y1 O6 81.3(7) 3_657 . ? O5 Y1 O6 79.2(8) . . ? O8 Y1 O6 125.9(9) 3_657 . ? O6' Y1 O3 155.8(6) . . ? O4 Y1 O3 125.5(3) 3_657 . ? O5 Y1 O3 88.1(3) . . ? O8 Y1 O3 83.2(3) 3_657 . ? O6 Y1 O3 146.6(8) . . ? O6' Y1 O2 82.8(6) . . ? O4 Y1 O2 147.3(3) 3_657 . ? O5 Y1 O2 132.7(2) . . ? O8 Y1 O2 84.0(2) 3_657 . ? O6 Y1 O2 88.5(6) . . ? O3 Y1 O2 77.7(3) . . ? O6' Y1 O1 81.3(7) . . ? O4 Y1 O1 145.6(3) 3_657 . ? O5 Y1 O1 78.8(2) . . ? O8 Y1 O1 135.9(2) 3_657 . ? O6 Y1 O1 71.5(8) . . ? O3 Y1 O1 75.7(3) . . ? O2 Y1 O1 54.1(2) . . ? O6' Y1 O9 52.3(9) . . ? O4 Y1 O9 75.3(4) 3_657 . ? O5 Y1 O9 139.9(4) . . ? O8 Y1 O9 57.1(4) 3_657 . ? O6 Y1 O9 69.6(9) . . ? O3 Y1 O9 131.5(4) . . ? O2 Y1 O9 72.1(4) . . ? O1 Y1 O9 112.6(4) . . ? O6' Y1 O4 151.5(6) . . ? O4 Y1 O4 74.4(3) 3_657 . ? O5 Y1 O4 70.6(3) . . ? O8 Y1 O4 72.9(3) 3_657 . ? O6 Y1 O4 144.9(7) . . ? O3 Y1 O4 51.3(3) . . ? O2 Y1 O4 125.2(3) . . ? O1 Y1 O4 117.9(3) . . ? O9 Y1 O4 125.7(4) . . ? O4 Y1 Y1 39.6(2) 3_657 3_657 ? O5 Y1 Y1 68.55(18) . 3_657 ? O8 Y1 Y1 71.15(18) 3_657 3_657 ? O6 Y1 Y1 116.8(6) . 3_657 ? O3 Y1 Y1 86.0(2) . 3_657 ? O2 Y1 Y1 151.71(18) . 3_657 ? O1 Y1 Y1 143.03(18) . 3_657 ? O9 Y1 Y1 103.7(3) . 3_657 ? O4 Y1 Y1 34.78(17) . 3_657 ? C13 N1 C12 125.4(12) . . ? C13 N1 C11 117.5(11) . . ? C12 N1 C11 115.6(11) . . ? C1 O1 Y1 90.2(5) . . ? C1 O2 Y1 94.3(5) . . ? C5 O3 Y1 100.6(7) . . ? C5 O4 Y1 162.2(8) . 3_657 ? C5 O4 Y1 91.4(6) . . ? Y1 O4 Y1 105.7(3) 3_657 . ? C7 O5 Y1 138.6(6) . . ? C13 O6 Y1 136(2) . . ? C13 O6' Y1 151.4(19) . . ? C7 O8 Y1 134.7(6) . 3_657 ? O2 C1 O1 121.3(8) . . ? O2 C1 C2 120.6(7) . . ? O1 C1 C2 118.1(7) . . ? C3 C2 C9 118.8(8) . 4_565 ? C3 C2 C1 122.7(8) . . ? C9 C2 C1 118.4(7) 4_565 . ? C2 C3 C4 122.5(8) . . ? C3 C4 C8 116.4(8) . 4_565 ? C3 C4 C4 121.4(10) . 3_667 ? C8 C4 C4 122.2(10) 4_565 3_667 ? O3 C5 O4 116.7(10) . . ? O3 C5 C6 121.2(17) . . ? O4 C5 C6 119.5(17) . . ? O3 C5 C6' 121.1(16) . . ? O4 C5 C6' 117.0(15) . . ? O8 C7 O5 125.7(8) . . ? O8 C7 C15 119.7(8) . . ? O5 C7 C15 114.5(7) . . ? C15 C8 C4 123.5(9) . 4_666 ? C15 C9 C2 120.0(8) . 4_666 ? O6 C13 N1 93.8(19) . . ? N1 C13 O6' 123.2(17) . . ? O6 C13 C14 148(2) . . ? N1 C13 C14 118.2(14) . . ? O6' C13 C14 117.8(17) . . ? C9 C15 C8 118.7(9) . . ? C9 C15 C7 120.1(8) . . ? C8 C15 C7 121.2(9) . . ? _refine_diff_density_max 1.445 _refine_diff_density_min -1.117 _refine_diff_density_rms 0.181 _shelx_res_file ; TITL 150824d in P2(1)/n 150824d_tw.res created by SHELXL-2018/1 at 10:22:53 on 03-Dec-2018 CELL 0.71073 9.3026 17.5625 11.3369 90.000 94.350 90.000 ZERR 2.00 0.0008 0.0014 0.0009 0.000 0.001 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N O Y UNIT 56 76 4 34 4 omit 2 2 7 omit 3 4 6 omit 5 11 4 omit 6 10 4 omit 4 1 5 omit 3 13 1 omit 0 3 2 omit 2 0 2 omit 2 12 7 omit -1 1 10 omit 3 12 6 omit 2 6 7 omit 4 11 5 omit -3 4 8 omit -7 5 2 omit 3 8 6 omit 5 5 4 omit 3 2 6 omit 4 15 5 omit -2 6 4 omit 0 1 4 omit 0 2 4 omit 2 5 3 omit -2 1 1 omit 0 1 5 omit 1 3 3 omit 4 4 9 omit 2 8 7 omit 1 3 0 omit 3 9 1 omit -1 2 4 omit 3 9 7 omit 0 4 1 MERG 0 L.S. 16 ACTA BOND FMAP 2 PLAN 5 SIZE 0.12 0.10 0.13 dfix 1.30 0.01 c1 o1 c5 o4 c7 o5 dfix 1.24 0.01 c1 o2 c5 o3 c7 o8 dfix 1.50 0.01 c1 c2 c7 c15 c5 c6 c5 c6' dfix 1.39 0.01 c2 c3 c3 c4 c15 c8 c15 c9 DFIX 1.24 0.01 C13 O6 DFIX 1.50 0.01 C13 C14 DFIX 1.33 0.01 C13 N1 DFIX 1.47 0.01 N1 C11 N1 C12 DFIX 2.49 0.02 C11 C12 DFIX 2.45 0.02 C13 C11 C13 C12 SIMU 0.04 0.08 4.8 EADP c6 c6' EADP o6 o6' DELU 0.002 0.001 y1 o9 c13 c14 DFIX 2.16 0.01 h12a h14c h9b h14a h9b h14b h7d h9c ISOR 0.01 c6 c3 ISOR 0.01 o7 FREE Y1 C1 FREE Y1 C5 FREE O6 N1 TEMP 25 WGHT 0.093200 BASF 0.28869 FVAR 10.81356 0.44774 0.46311 Y1 5 0.514849 0.100996 0.934086 11.00000 0.03934 0.01253 = 0.04704 0.00169 -0.01841 -0.00193 N1 3 0.914687 0.182938 0.831675 11.00000 0.08036 0.09394 = 0.11142 0.00674 -0.01320 -0.01042 O1 4 0.562107 0.235061 0.987418 11.00000 0.07494 0.02681 = 0.05759 0.00517 -0.04099 0.00257 O2 4 0.411400 0.210283 0.831645 11.00000 0.06713 0.00937 = 0.05842 -0.00516 -0.03198 -0.00184 O3 4 0.321986 0.134651 1.053150 11.00000 0.08901 0.04822 = 0.06451 0.00623 0.01642 0.02166 O4 4 0.387323 0.018105 1.079617 11.00000 0.05475 0.02831 = 0.07214 0.00157 0.01039 0.00995 O5 4 0.660663 0.087696 1.106069 11.00000 0.07461 0.02071 = 0.07065 0.00421 -0.02249 -0.00673 PART 1 O6 4 0.739993 0.135796 0.868413 21.00000 0.07335 0.05197 = 0.08850 0.00877 -0.00370 -0.01454 PART 2 O6' 4 0.688533 0.122000 0.824577 -21.00000 0.07335 0.05197 = 0.08850 0.00877 -0.00370 -0.01454 PART 0 O7 4 0.333270 0.187201 0.578669 10.50000 0.10325 0.06841 = 0.06551 -0.00762 -0.01882 0.00179 AFIX 3 H7C 2 0.255179 0.210061 0.556929 10.50000 -1.20000 H7D 2 0.370313 0.210455 0.639355 10.50000 -1.20000 AFIX 0 O8 4 0.665116 -0.035086 1.174663 11.00000 0.08121 0.02090 = 0.07491 0.01076 -0.04413 -0.00576 O9 4 0.519224 0.077014 0.712625 11.00000 0.26431 0.22366 = 0.05989 -0.02624 0.00473 0.01019 AFIX 3 H9B 2 0.590303 0.102724 0.691516 11.00000 -1.20000 H9C 2 0.443184 0.096584 0.679065 11.00000 -1.20000 AFIX 0 C1 1 0.471623 0.256860 0.901060 11.00000 0.05788 0.02276 = 0.04458 -0.00312 -0.02202 0.00232 C2 1 0.441146 0.340164 0.887703 11.00000 0.05338 0.01823 = 0.04822 -0.00166 -0.02145 -0.00674 C3 1 0.500484 0.394288 0.966585 11.00000 0.05839 0.01318 = 0.03786 -0.00094 -0.01892 0.00366 AFIX 43 H3 2 0.565355 0.378400 1.028124 11.00000 -1.20000 AFIX 0 C4 1 0.466543 0.471316 0.957001 11.00000 0.05573 0.01129 = 0.03879 -0.00644 -0.02335 0.00883 C5 1 0.301827 0.073203 1.102178 11.00000 0.06432 0.04526 = 0.07862 0.00394 0.01716 0.01140 PART 1 C6 1 0.215712 0.068625 1.209247 31.00000 0.09725 0.07940 = 0.08304 -0.00895 0.03066 0.01505 AFIX 137 H6A 2 0.119515 0.086580 1.189047 31.00000 -1.50000 H6B 2 0.260478 0.099633 1.271377 31.00000 -1.50000 H6C 2 0.212261 0.016745 1.235553 31.00000 -1.50000 PART 2 AFIX 0 C6' 1 0.154099 0.051688 1.140194 -31.00000 0.09725 0.07940 = 0.08304 -0.00895 0.03066 0.01505 AFIX 137 H6'1 2 0.105168 0.096648 1.163921 -31.00000 -1.50000 H6'2 2 0.164906 0.016793 1.205444 -31.00000 -1.50000 H6'3 2 0.098851 0.028025 1.075246 -31.00000 -1.50000 PART 0 AFIX 0 C7 1 0.705602 0.033424 1.179656 11.00000 0.05794 0.01604 = 0.07631 -0.00380 -0.02752 -0.00572 C8 1 0.872494 0.007392 1.360097 11.00000 0.07626 0.01381 = 0.06287 0.00574 -0.03709 0.00011 AFIX 43 H8 2 0.850511 -0.043968 1.350036 11.00000 -1.20000 AFIX 0 C9 1 0.842566 0.135392 1.292347 11.00000 0.04997 0.02799 = 0.04232 0.01719 -0.01709 0.00641 AFIX 43 H9 2 0.800105 0.170930 1.239789 11.00000 -1.20000 AFIX 0 C11 1 0.958874 0.139308 0.940471 11.00000 0.15047 0.17662 = 0.12836 0.01026 0.03663 -0.03685 AFIX 137 H11A 2 0.879718 0.108537 0.962070 11.00000 -1.50000 H11B 2 0.986362 0.174017 1.003612 11.00000 -1.50000 H11C 2 1.039140 0.107136 0.926139 11.00000 -1.50000 AFIX 0 C12 1 1.030745 0.224315 0.778362 11.00000 0.13956 0.17078 = 0.15372 0.01689 0.00483 -0.06603 AFIX 137 H12A 2 1.037506 0.207007 0.698651 11.00000 -1.50000 H12B 2 1.120501 0.215106 0.823620 11.00000 -1.50000 H12C 2 1.010071 0.277872 0.777974 11.00000 -1.50000 AFIX 0 C13 1 0.784069 0.168915 0.779039 11.00000 0.11304 0.07744 = 0.11766 0.00217 -0.00483 0.01324 C14 1 0.751735 0.196201 0.654650 11.00000 0.14351 0.14974 = 0.14063 0.05114 -0.00292 -0.00344 AFIX 137 H14A 2 0.655273 0.215921 0.645780 11.00000 -1.50000 H14B 2 0.760633 0.154545 0.600860 11.00000 -1.50000 H14C 2 0.818580 0.235623 0.637601 11.00000 -1.50000 AFIX 0 C15 1 0.810332 0.058924 1.278242 11.00000 0.06976 0.02916 = 0.04730 -0.00130 -0.02357 0.00012 HKLF 5 REM 150824d in P2(1)/n REM R1 = 0.0938 for 1608 Fo > 4sig(Fo) and 0.1670 for all 3171 data REM 240 parameters refined using 1030 restraints END WGHT 0.1342 0.0000 REM Highest difference peak 1.445, deepest hole -1.117, 1-sigma level 0.181 Q1 1 0.4254 0.1027 0.9844 11.00000 0.05 1.45 Q2 1 0.6062 0.1033 0.8783 11.00000 0.05 1.15 Q3 1 0.2891 0.1027 0.7184 11.00000 0.05 0.98 Q4 1 0.4842 0.0763 0.6000 11.00000 0.05 0.93 Q5 1 0.4608 0.0315 0.5344 11.00000 0.05 0.87 ; _shelx_res_checksum 27162 loop_ _publcif_info_exptl_table_extra_item sin_theta_over_lambda_max loop_ _publcif_info_exptl_table_header_item ? _publcif_funding_html ; ;