data_C31H51NOSi _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H51 N O Si' _chemical_formula_sum 'C31 H51 N O Si' _chemical_formula_weight 481.81 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' 'N' 'N' 0.0311 0.0180 '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' 'Si' 'Si' 0.2541 0.3302 '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 7.3883(3) _cell_length_b 10.3271(4) _cell_length_c 37.3224(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2847.69(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3140 _cell_measurement_theta_min 4.44 _cell_measurement_theta_max 66.46 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_method none _exptl_crystal_density_diffrn 1.124 _exptl_crystal_F_000 1064 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.240 _exptl_crystal_size_mid 0.140 _exptl_crystal_size_min 0.080 _exptl_absorpt_coefficient_mu 0.880 _shelx_estimated_absorpt_T_min 0.817 _shelx_estimated_absorpt_T_max 0.933 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.5740 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_process_details ; Sheldrick, G.M. (2013). SADABS. Bruker AXS Inc. Madison, WI USA. ; _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'microfocus sealed tube' _diffrn_source_type 'Incoatec I\uS' _diffrn_radiation_monochromator mirrors _diffrn_measurement_device_type 'Bruker Kappa DUO CCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 17845 _diffrn_reflns_av_unetI/netI 0.0964 _diffrn_reflns_av_R_equivalents 0.1240 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.368 _diffrn_reflns_theta_max 66.795 _diffrn_reflns_theta_full 66.795 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_point_group_measured_fraction_full 0.988 _reflns_number_total 4987 _reflns_number_gt 3824 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.711 _reflns_Friedel_fraction_max 0.973 _reflns_Friedel_fraction_full 0.974 _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 'APEX2 (Bruker, 2014)' _computing_cell_refinement 'SAINT (Bruker, 2014)' _computing_data_reduction 'SAINT (Bruker, 2014)' _computing_structure_solution 'SHELXL-2014 (Sheldrick, 2014)' _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^)+(0.0472P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1248 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.01(4) _chemical_absolute_configuration ad _refine_ls_number_reflns 4987 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0510 _refine_ls_wR_factor_ref 0.1182 _refine_ls_wR_factor_gt 0.1064 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 Si1 Si 0.17324(16) 0.77182(11) 0.64674(3) 0.0210(3) Uani 1 1 d . . . . . O1 O 0.2164(4) 0.6191(3) 0.63867(7) 0.0214(6) Uani 1 1 d . . . . . N1 N 0.9031(8) 0.1713(5) 0.70252(14) 0.0559(14) Uani 1 1 d . . . . . C1 C 0.7556(9) 0.2012(5) 0.70742(14) 0.0407(13) Uani 1 1 d . . . . . C2 C 0.5706(7) 0.2348(5) 0.71415(12) 0.0377(12) Uani 1 1 d . . . . . H2 H 0.4816 0.1704 0.7097 0.045 Uiso 1 1 calc R U . . . C3 C 0.5132(7) 0.3489(5) 0.72620(11) 0.0315(11) Uani 1 1 d . . . . . C4 C 0.3168(7) 0.3739(5) 0.73285(12) 0.0337(11) Uani 1 1 d . . . . . H4A H 0.3019 0.4076 0.7575 0.040 Uiso 1 1 calc R U . . . H4B H 0.2503 0.2908 0.7313 0.040 Uiso 1 1 calc R U . . . C5 C 0.2308(7) 0.4715(5) 0.70617(11) 0.0327(11) Uani 1 1 d . . . . . H5A H 0.1076 0.4944 0.7145 0.039 Uiso 1 1 calc R U . . . H5B H 0.3041 0.5517 0.7057 0.039 Uiso 1 1 calc R U . . . C6 C 0.2198(6) 0.4157(4) 0.66845(11) 0.0257(10) Uani 1 1 d . . . . . H6A H 0.1597 0.3301 0.6698 0.031 Uiso 1 1 calc R U . . . H6B H 0.3445 0.4011 0.6596 0.031 Uiso 1 1 calc R U . . . C7 C 0.1182(6) 0.4992(4) 0.64073(10) 0.0218(9) Uani 1 1 d . . . . . C8 C -0.0855(6) 0.5169(4) 0.65088(11) 0.0239(9) Uani 1 1 d . . . . . H8A H -0.1044 0.4969 0.6766 0.029 Uiso 1 1 calc R U . . . H8B H -0.1239 0.6074 0.6465 0.029 Uiso 1 1 calc R U . . . C9 C -0.1955(6) 0.4234(4) 0.62739(11) 0.0234(9) Uani 1 1 d . . . . . H9A H -0.2765 0.3692 0.6423 0.028 Uiso 1 1 calc R U . . . H9B H -0.2694 0.4715 0.6097 0.028 Uiso 1 1 calc R U . . . C10 C -0.0535(5) 0.3403(4) 0.60858(11) 0.0194(9) Uani 1 1 d . . . . . H10 H -0.0131 0.2740 0.6264 0.023 Uiso 1 1 calc R U . . . C11 C -0.1081(5) 0.2661(4) 0.57490(10) 0.0180(8) Uani 1 1 d . . . . . H11 H -0.1440 0.3302 0.5561 0.022 Uiso 1 1 calc R U . . . C12 C -0.2657(6) 0.1754(4) 0.58121(11) 0.0204(9) Uani 1 1 d . . . . . H12A H -0.3711 0.2254 0.5900 0.024 Uiso 1 1 calc R U . . . H12B H -0.2327 0.1114 0.5999 0.024 Uiso 1 1 calc R U . . . C13 C -0.3169(6) 0.1044(4) 0.54665(11) 0.0223(9) Uani 1 1 d . . . . . H13A H -0.4137 0.0410 0.5519 0.027 Uiso 1 1 calc R U . . . H13B H -0.3653 0.1677 0.5292 0.027 Uiso 1 1 calc R U . . . C14 C -0.1589(6) 0.0353(4) 0.53032(10) 0.0201(9) Uani 1 1 d . . . . . C15 C -0.1724(6) -0.0868(4) 0.51953(11) 0.0239(9) Uani 1 1 d . . . . . H15 H -0.2821 -0.1314 0.5244 0.029 Uiso 1 1 calc R U . . . C16 C -0.0259(6) -0.1591(4) 0.50014(12) 0.0276(10) Uani 1 1 d . . . . . H16A H -0.0799 -0.2105 0.4805 0.033 Uiso 1 1 calc R U . . . H16B H 0.0344 -0.2196 0.5169 0.033 Uiso 1 1 calc R U . . . C17 C 0.1133(6) -0.0656(4) 0.48481(11) 0.0252(10) Uani 1 1 d . . . . . H17A H 0.0606 -0.0189 0.4641 0.030 Uiso 1 1 calc R U . . . H17B H 0.2202 -0.1145 0.4763 0.030 Uiso 1 1 calc R U . . . C18 C 0.1713(6) 0.0315(4) 0.51340(10) 0.0212(9) Uani 1 1 d . . . . . H18A H 0.2670 0.0882 0.5035 0.025 Uiso 1 1 calc R U . . . H18B H 0.2229 -0.0159 0.5341 0.025 Uiso 1 1 calc R U . . . C19 C 0.0124(6) 0.1154(4) 0.52630(11) 0.0195(9) Uani 1 1 d . . . . . H19 H -0.0113 0.1816 0.5073 0.023 Uiso 1 1 calc R U . . . C20 C 0.0570(5) 0.1891(4) 0.56105(11) 0.0192(9) Uani 1 1 d . . . . . H20 H 0.0859 0.1225 0.5796 0.023 Uiso 1 1 calc R U . . . C21 C 0.2256(5) 0.2749(4) 0.55704(10) 0.0204(9) Uani 1 1 d . . . . . H21A H 0.2066 0.3355 0.5368 0.024 Uiso 1 1 calc R U . . . H21B H 0.3306 0.2194 0.5510 0.024 Uiso 1 1 calc R U . . . C22 C 0.2698(6) 0.3531(4) 0.59087(11) 0.0203(9) Uani 1 1 d . . . . . H22A H 0.3063 0.2932 0.6103 0.024 Uiso 1 1 calc R U . . . H22B H 0.3730 0.4116 0.5859 0.024 Uiso 1 1 calc R U . . . C23 C 0.1068(6) 0.4334(4) 0.60323(10) 0.0180(9) Uani 1 1 d . . . . . C24 C 0.6415(7) 0.4570(5) 0.73463(13) 0.0355(12) Uani 1 1 d . . . . . H24A H 0.7658 0.4287 0.7299 0.053 Uiso 1 1 calc R U . . . H24B H 0.6295 0.4810 0.7599 0.053 Uiso 1 1 calc R U . . . H24C H 0.6131 0.5320 0.7196 0.053 Uiso 1 1 calc R U . . . C25 C 0.0821(6) 0.7997(4) 0.69281(12) 0.0285(10) Uani 1 1 d . . . . . H25A H -0.0302 0.7504 0.6959 0.043 Uiso 1 1 calc R U . . . H25B H 0.0573 0.8922 0.6961 0.043 Uiso 1 1 calc R U . . . H25C H 0.1713 0.7712 0.7106 0.043 Uiso 1 1 calc R U . . . C26 C 0.0100(6) 0.8465(4) 0.61504(12) 0.0269(10) Uani 1 1 d . . . . . H26A H 0.0618 0.8466 0.5909 0.040 Uiso 1 1 calc R U . . . H26B H -0.0152 0.9357 0.6225 0.040 Uiso 1 1 calc R U . . . H26C H -0.1028 0.7965 0.6150 0.040 Uiso 1 1 calc R U . . . C27 C 0.4008(6) 0.8512(4) 0.64075(11) 0.0231(9) Uani 1 1 d . . . . . C28 C 0.4765(7) 0.8203(5) 0.60321(11) 0.0309(11) Uani 1 1 d . . . . . H28A H 0.3905 0.8495 0.5849 0.046 Uiso 1 1 calc R U . . . H28B H 0.4949 0.7267 0.6009 0.046 Uiso 1 1 calc R U . . . H28C H 0.5923 0.8650 0.5999 0.046 Uiso 1 1 calc R U . . . C29 C 0.5343(6) 0.7991(5) 0.66887(11) 0.0307(11) Uani 1 1 d . . . . . H29A H 0.6517 0.8421 0.6660 0.046 Uiso 1 1 calc R U . . . H29B H 0.5493 0.7056 0.6656 0.046 Uiso 1 1 calc R U . . . H29C H 0.4872 0.8165 0.6929 0.046 Uiso 1 1 calc R U . . . C30 C 0.3840(7) 0.9981(4) 0.64487(15) 0.0384(12) Uani 1 1 d . . . . . H30A H 0.3217 1.0182 0.6674 0.058 Uiso 1 1 calc R U . . . H30B H 0.3144 1.0333 0.6247 0.058 Uiso 1 1 calc R U . . . H30C H 0.5049 1.0371 0.6451 0.058 Uiso 1 1 calc R U . . . C31 C 0.0651(6) 0.5379(4) 0.57511(11) 0.0218(9) Uani 1 1 d . . . . . H31A H 0.1723 0.5923 0.5715 0.033 Uiso 1 1 calc R U . . . H31B H -0.0358 0.5916 0.5834 0.033 Uiso 1 1 calc R U . . . H31C H 0.0323 0.4964 0.5524 0.033 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 Si1 0.0175(5) 0.0218(5) 0.0236(6) -0.0009(5) -0.0005(5) 0.0007(5) O1 0.0199(15) 0.0193(13) 0.0251(15) -0.0008(12) 0.0000(12) -0.0025(12) N1 0.059(4) 0.047(3) 0.062(3) 0.008(2) 0.012(3) 0.016(3) C1 0.057(4) 0.034(3) 0.031(3) 0.003(2) 0.004(3) 0.007(3) C2 0.044(3) 0.036(3) 0.033(3) 0.003(2) -0.001(2) -0.004(3) C3 0.038(3) 0.038(3) 0.019(2) 0.008(2) -0.002(2) 0.000(2) C4 0.032(3) 0.046(3) 0.024(2) 0.008(2) -0.002(2) -0.004(3) C5 0.034(3) 0.040(3) 0.024(2) -0.001(2) -0.003(2) 0.006(2) C6 0.026(2) 0.029(2) 0.022(2) 0.0018(19) -0.0034(18) 0.002(2) C7 0.026(2) 0.024(2) 0.016(2) 0.0019(17) -0.0003(17) -0.0018(18) C8 0.023(2) 0.027(2) 0.022(2) -0.0011(19) 0.0002(19) 0.0017(19) C9 0.018(2) 0.025(2) 0.027(2) 0.0005(18) 0.0016(19) 0.0012(19) C10 0.016(2) 0.022(2) 0.021(2) 0.0012(17) 0.0012(17) 0.0006(18) C11 0.0146(19) 0.019(2) 0.021(2) 0.0031(17) 0.0012(16) 0.0004(17) C12 0.017(2) 0.022(2) 0.022(2) -0.0020(17) 0.0013(17) 0.0033(18) C13 0.016(2) 0.022(2) 0.028(2) 0.0031(17) 0.0000(19) -0.0045(19) C14 0.017(2) 0.023(2) 0.021(2) 0.0038(17) -0.0053(18) -0.0016(19) C15 0.022(2) 0.023(2) 0.026(2) 0.0030(18) 0.003(2) -0.004(2) C16 0.028(3) 0.026(2) 0.028(2) -0.005(2) 0.003(2) 0.000(2) C17 0.024(2) 0.025(2) 0.027(2) -0.0048(18) 0.0019(19) 0.0037(19) C18 0.0164(19) 0.024(2) 0.023(2) -0.0005(18) 0.0020(19) -0.002(2) C19 0.015(2) 0.021(2) 0.022(2) 0.0010(18) 0.0019(17) 0.0009(18) C20 0.017(2) 0.019(2) 0.022(2) 0.0000(17) 0.0003(17) 0.0005(18) C21 0.016(2) 0.023(2) 0.022(2) 0.0001(18) 0.0030(16) 0.0005(18) C22 0.015(2) 0.023(2) 0.023(2) -0.0018(18) -0.0003(17) -0.0030(18) C23 0.016(2) 0.019(2) 0.019(2) -0.0016(17) 0.0012(17) 0.0005(18) C24 0.033(3) 0.034(3) 0.039(3) 0.008(2) 0.001(2) -0.002(2) C25 0.023(2) 0.026(2) 0.037(3) -0.003(2) 0.004(2) 0.000(2) C26 0.024(2) 0.024(2) 0.033(2) 0.004(2) -0.005(2) 0.000(2) C27 0.020(2) 0.026(2) 0.024(2) -0.0008(19) -0.0030(19) -0.0071(19) C28 0.026(2) 0.038(3) 0.029(2) 0.000(2) 0.000(2) -0.003(2) C29 0.021(2) 0.045(3) 0.025(2) -0.002(2) -0.0040(19) -0.004(2) C30 0.035(3) 0.031(2) 0.049(3) -0.009(3) 0.000(3) -0.012(2) C31 0.020(2) 0.023(2) 0.022(2) 0.0011(18) 0.0004(18) -0.0018(19) _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 Si1 O1 1.637(3) . ? Si1 C26 1.857(4) . ? Si1 C25 1.869(4) . ? Si1 C27 1.884(4) . ? O1 C7 1.437(5) . ? N1 C1 1.147(7) . ? C1 C2 1.433(8) . ? C2 C3 1.330(7) . ? C2 H2 0.9500 . ? C3 C4 1.495(7) . ? C3 C24 1.498(7) . ? C4 C5 1.553(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.523(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.542(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C23 1.558(5) . ? C7 C8 1.562(6) . ? C8 C9 1.537(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.526(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.526(6) . ? C10 C23 1.539(6) . ? C10 H10 1.0000 . ? C11 C12 1.512(6) . ? C11 C20 1.545(5) . ? C11 H11 1.0000 . ? C12 C13 1.531(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.498(6) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.328(6) . ? C14 C19 1.519(6) . ? C15 C16 1.501(6) . ? C15 H15 0.9500 . ? C16 C17 1.522(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.525(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.537(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.539(6) . ? C19 H19 1.0000 . ? C20 C21 1.536(6) . ? C20 H20 1.0000 . ? C21 C22 1.534(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.533(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C31 1.536(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C30 1.530(6) . ? C27 C29 1.537(6) . ? C27 C28 1.542(6) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 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 O1 Si1 C26 114.15(18) . . ? O1 Si1 C25 112.84(18) . . ? C26 Si1 C25 106.7(2) . . ? O1 Si1 C27 102.91(17) . . ? C26 Si1 C27 108.9(2) . . ? C25 Si1 C27 111.3(2) . . ? C7 O1 Si1 136.2(3) . . ? N1 C1 C2 178.2(6) . . ? C3 C2 C1 125.3(5) . . ? C3 C2 H2 117.4 . . ? C1 C2 H2 117.4 . . ? C2 C3 C4 121.2(5) . . ? C2 C3 C24 122.0(5) . . ? C4 C3 C24 116.8(4) . . ? C3 C4 C5 113.7(4) . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4B 108.8 . . ? C5 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 111.6(4) . . ? C6 C5 H5A 109.3 . . ? C4 C5 H5A 109.3 . . ? C6 C5 H5B 109.3 . . ? C4 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C5 C6 C7 115.8(4) . . ? C5 C6 H6A 108.3 . . ? C7 C6 H6A 108.3 . . ? C5 C6 H6B 108.3 . . ? C7 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? O1 C7 C6 105.8(3) . . ? O1 C7 C23 110.8(3) . . ? C6 C7 C23 112.6(3) . . ? O1 C7 C8 113.5(3) . . ? C6 C7 C8 111.8(3) . . ? C23 C7 C8 102.6(3) . . ? C9 C8 C7 107.3(3) . . ? C9 C8 H8A 110.3 . . ? C7 C8 H8A 110.3 . . ? C9 C8 H8B 110.3 . . ? C7 C8 H8B 110.3 . . ? H8A C8 H8B 108.5 . . ? C10 C9 C8 104.6(4) . . ? C10 C9 H9A 110.8 . . ? C8 C9 H9A 110.8 . . ? C10 C9 H9B 110.8 . . ? C8 C9 H9B 110.8 . . ? H9A C9 H9B 108.9 . . ? C11 C10 C9 118.6(3) . . ? C11 C10 C23 114.2(3) . . ? C9 C10 C23 103.7(3) . . ? C11 C10 H10 106.5 . . ? C9 C10 H10 106.5 . . ? C23 C10 H10 106.5 . . ? C12 C11 C10 112.7(3) . . ? C12 C11 C20 109.9(3) . . ? C10 C11 C20 109.0(3) . . ? C12 C11 H11 108.4 . . ? C10 C11 H11 108.4 . . ? C20 C11 H11 108.4 . . ? C11 C12 C13 110.8(3) . . ? C11 C12 H12A 109.5 . . ? C13 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C13 C12 H12B 109.5 . . ? H12A C12 H12B 108.1 . . ? C14 C13 C12 112.2(4) . . ? C14 C13 H13A 109.2 . . ? C12 C13 H13A 109.2 . . ? C14 C13 H13B 109.2 . . ? C12 C13 H13B 109.2 . . ? H13A C13 H13B 107.9 . . ? C15 C14 C13 121.2(4) . . ? C15 C14 C19 123.4(4) . . ? C13 C14 C19 115.5(3) . . ? C14 C15 C16 124.4(4) . . ? C14 C15 H15 117.8 . . ? C16 C15 H15 117.8 . . ? C15 C16 C17 110.7(4) . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 C17 C18 110.1(3) . . ? C16 C17 H17A 109.6 . . ? C18 C17 H17A 109.6 . . ? C16 C17 H17B 109.6 . . ? C18 C17 H17B 109.6 . . ? H17A C17 H17B 108.2 . . ? C17 C18 C19 112.1(4) . . ? C17 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? C17 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C14 C19 C20 111.4(3) . . ? C14 C19 C18 111.1(3) . . ? C20 C19 C18 112.3(3) . . ? C14 C19 H19 107.3 . . ? C20 C19 H19 107.3 . . ? C18 C19 H19 107.3 . . ? C21 C20 C19 112.1(3) . . ? C21 C20 C11 112.1(3) . . ? C19 C20 C11 111.6(3) . . ? C21 C20 H20 106.9 . . ? C19 C20 H20 106.9 . . ? C11 C20 H20 106.9 . . ? C20 C21 C22 113.4(3) . . ? C20 C21 H21A 108.9 . . ? C22 C21 H21A 108.9 . . ? C20 C21 H21B 108.9 . . ? C22 C21 H21B 108.9 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C21 111.4(3) . . ? C23 C22 H22A 109.3 . . ? C21 C22 H22A 109.3 . . ? C23 C22 H22B 109.3 . . ? C21 C22 H22B 109.3 . . ? H22A C22 H22B 108.0 . . ? C22 C23 C31 109.4(3) . . ? C22 C23 C10 107.8(3) . . ? C31 C23 C10 111.9(3) . . ? C22 C23 C7 117.6(3) . . ? C31 C23 C7 108.6(3) . . ? C10 C23 C7 101.4(3) . . ? C3 C24 H24A 109.5 . . ? C3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C30 C27 C29 109.3(4) . . ? C30 C27 C28 109.0(4) . . ? C29 C27 C28 108.4(4) . . ? C30 C27 Si1 110.3(3) . . ? C29 C27 Si1 109.9(3) . . ? C28 C27 Si1 110.0(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C23 C31 H31A 109.5 . . ? C23 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C23 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 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 C26 Si1 O1 C7 -68.5(4) . . . . ? C25 Si1 O1 C7 53.6(4) . . . . ? C27 Si1 O1 C7 173.7(4) . . . . ? C1 C2 C3 C4 -179.2(4) . . . . ? C1 C2 C3 C24 -0.8(8) . . . . ? C2 C3 C4 C5 -110.9(5) . . . . ? C24 C3 C4 C5 70.6(5) . . . . ? C3 C4 C5 C6 68.3(6) . . . . ? C4 C5 C6 C7 173.8(4) . . . . ? Si1 O1 C7 C6 -118.1(4) . . . . ? Si1 O1 C7 C23 119.5(3) . . . . ? Si1 O1 C7 C8 4.8(5) . . . . ? C5 C6 C7 O1 60.9(5) . . . . ? C5 C6 C7 C23 -178.0(4) . . . . ? C5 C6 C7 C8 -63.1(5) . . . . ? O1 C7 C8 C9 138.9(3) . . . . ? C6 C7 C8 C9 -101.6(4) . . . . ? C23 C7 C8 C9 19.3(4) . . . . ? C7 C8 C9 C10 8.3(4) . . . . ? C8 C9 C10 C11 -161.2(3) . . . . ? C8 C9 C10 C23 -33.3(4) . . . . ? C9 C10 C11 C12 -57.3(5) . . . . ? C23 C10 C11 C12 179.9(3) . . . . ? C9 C10 C11 C20 -179.6(3) . . . . ? C23 C10 C11 C20 57.5(4) . . . . ? C10 C11 C12 C13 179.4(3) . . . . ? C20 C11 C12 C13 -58.9(4) . . . . ? C11 C12 C13 C14 54.5(4) . . . . ? C12 C13 C14 C15 132.3(4) . . . . ? C12 C13 C14 C19 -49.2(5) . . . . ? C13 C14 C15 C16 174.6(4) . . . . ? C19 C14 C15 C16 -3.8(7) . . . . ? C14 C15 C16 C17 -17.0(6) . . . . ? C15 C16 C17 C18 48.4(5) . . . . ? C16 C17 C18 C19 -62.2(5) . . . . ? C15 C14 C19 C20 -134.1(4) . . . . ? C13 C14 C19 C20 47.5(5) . . . . ? C15 C14 C19 C18 -8.1(6) . . . . ? C13 C14 C19 C18 173.5(3) . . . . ? C17 C18 C19 C14 40.5(5) . . . . ? C17 C18 C19 C20 165.9(3) . . . . ? C14 C19 C20 C21 -177.7(3) . . . . ? C18 C19 C20 C21 56.9(4) . . . . ? C14 C19 C20 C11 -51.1(4) . . . . ? C18 C19 C20 C11 -176.4(3) . . . . ? C12 C11 C20 C21 -175.4(3) . . . . ? C10 C11 C20 C21 -51.4(4) . . . . ? C12 C11 C20 C19 57.9(4) . . . . ? C10 C11 C20 C19 -178.1(3) . . . . ? C19 C20 C21 C22 178.0(3) . . . . ? C11 C20 C21 C22 51.7(5) . . . . ? C20 C21 C22 C23 -54.3(5) . . . . ? C21 C22 C23 C31 -66.1(4) . . . . ? C21 C22 C23 C10 55.8(4) . . . . ? C21 C22 C23 C7 169.5(3) . . . . ? C11 C10 C23 C22 -59.8(4) . . . . ? C9 C10 C23 C22 169.6(3) . . . . ? C11 C10 C23 C31 60.5(4) . . . . ? C9 C10 C23 C31 -70.1(4) . . . . ? C11 C10 C23 C7 176.0(3) . . . . ? C9 C10 C23 C7 45.4(4) . . . . ? O1 C7 C23 C22 82.3(4) . . . . ? C6 C7 C23 C22 -36.0(5) . . . . ? C8 C7 C23 C22 -156.4(3) . . . . ? O1 C7 C23 C31 -42.5(4) . . . . ? C6 C7 C23 C31 -160.8(4) . . . . ? C8 C7 C23 C31 78.8(4) . . . . ? O1 C7 C23 C10 -160.5(3) . . . . ? C6 C7 C23 C10 81.2(4) . . . . ? C8 C7 C23 C10 -39.1(4) . . . . ? O1 Si1 C27 C30 176.2(3) . . . . ? C26 Si1 C27 C30 54.7(4) . . . . ? C25 Si1 C27 C30 -62.7(4) . . . . ? O1 Si1 C27 C29 -63.3(3) . . . . ? C26 Si1 C27 C29 175.3(3) . . . . ? C25 Si1 C27 C29 57.8(4) . . . . ? O1 Si1 C27 C28 55.9(3) . . . . ? C26 Si1 C27 C28 -65.6(3) . . . . ? C25 Si1 C27 C28 177.0(3) . . . . ? _refine_diff_density_max 0.199 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.047 _shelx_res_file ; sad_a.res created by SHELXL-2014/7 TITL sad_a.res in P2(1)2(1)2(1) CELL 1.54178 7.3883 10.3271 37.3224 90.000 90.000 90.000 ZERR 4.000 0.0003 0.0004 0.0012 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 N O Si UNIT 124 204 4 4 4 L.S. 10 BOND $H FMAP 2 PLAN 20 SIZE 0.24 0.14 0.08 TEMP -173 CONF HTAB ACTA WGHT 0.047200 FVAR 0.39286 SI1 5 0.173237 0.771817 0.646741 11.00000 0.01747 0.02184 = 0.02365 -0.00088 -0.00052 0.00075 O1 4 0.216402 0.619093 0.638665 11.00000 0.01989 0.01927 = 0.02505 -0.00078 0.00003 -0.00248 N1 3 0.903091 0.171310 0.702519 11.00000 0.05863 0.04666 = 0.06231 0.00803 0.01179 0.01626 C1 1 0.755575 0.201227 0.707416 11.00000 0.05709 0.03386 = 0.03103 0.00328 0.00441 0.00657 C2 1 0.570554 0.234824 0.714154 11.00000 0.04361 0.03647 = 0.03291 0.00296 -0.00141 -0.00372 AFIX 43 H2 2 0.481608 0.170415 0.709656 11.00000 -1.20000 AFIX 0 C3 1 0.513207 0.348893 0.726199 11.00000 0.03759 0.03826 = 0.01853 0.00768 -0.00196 -0.00036 C4 1 0.316773 0.373858 0.732846 11.00000 0.03164 0.04576 = 0.02357 0.00808 -0.00160 -0.00414 AFIX 23 H4A 2 0.301936 0.407575 0.757503 11.00000 -1.20000 H4B 2 0.250320 0.290799 0.731308 11.00000 -1.20000 AFIX 0 C5 1 0.230807 0.471472 0.706167 11.00000 0.03366 0.04013 = 0.02424 -0.00103 -0.00290 0.00637 AFIX 23 H5A 2 0.107634 0.494373 0.714468 11.00000 -1.20000 H5B 2 0.304110 0.551704 0.705719 11.00000 -1.20000 AFIX 0 C6 1 0.219771 0.415654 0.668451 11.00000 0.02576 0.02921 = 0.02199 0.00180 -0.00342 0.00170 AFIX 23 H6A 2 0.159650 0.330119 0.669798 11.00000 -1.20000 H6B 2 0.344504 0.401143 0.659631 11.00000 -1.20000 AFIX 0 C7 1 0.118161 0.499175 0.640726 11.00000 0.02552 0.02380 = 0.01601 0.00192 -0.00031 -0.00176 C8 1 -0.085460 0.516935 0.650880 11.00000 0.02326 0.02686 = 0.02163 -0.00106 0.00023 0.00172 AFIX 23 H8A 2 -0.104383 0.496943 0.676550 11.00000 -1.20000 H8B 2 -0.123862 0.607375 0.646454 11.00000 -1.20000 AFIX 0 C9 1 -0.195471 0.423375 0.627386 11.00000 0.01818 0.02488 = 0.02719 0.00052 0.00156 0.00117 AFIX 23 H9A 2 -0.276528 0.369161 0.642256 11.00000 -1.20000 H9B 2 -0.269394 0.471549 0.609729 11.00000 -1.20000 AFIX 0 C10 1 -0.053504 0.340270 0.608578 11.00000 0.01598 0.02163 = 0.02060 0.00124 0.00122 0.00056 AFIX 13 H10 2 -0.013072 0.274041 0.626410 11.00000 -1.20000 AFIX 0 C11 1 -0.108145 0.266091 0.574904 11.00000 0.01461 0.01864 = 0.02079 0.00306 0.00119 0.00036 AFIX 13 H11 2 -0.143998 0.330192 0.556118 11.00000 -1.20000 AFIX 0 C12 1 -0.265690 0.175397 0.581209 11.00000 0.01720 0.02160 = 0.02230 -0.00196 0.00133 0.00332 AFIX 23 H12A 2 -0.371085 0.225437 0.589961 11.00000 -1.20000 H12B 2 -0.232734 0.111408 0.599852 11.00000 -1.20000 AFIX 0 C13 1 -0.316900 0.104442 0.546651 11.00000 0.01638 0.02198 = 0.02846 0.00307 -0.00005 -0.00452 AFIX 23 H13A 2 -0.413702 0.040950 0.551920 11.00000 -1.20000 H13B 2 -0.365318 0.167721 0.529182 11.00000 -1.20000 AFIX 0 C14 1 -0.158916 0.035327 0.530323 11.00000 0.01680 0.02269 = 0.02084 0.00381 -0.00525 -0.00158 C15 1 -0.172421 -0.086793 0.519528 11.00000 0.02232 0.02349 = 0.02578 0.00297 0.00330 -0.00418 AFIX 43 H15 2 -0.282142 -0.131404 0.524402 11.00000 -1.20000 AFIX 0 C16 1 -0.025908 -0.159059 0.500139 11.00000 0.02848 0.02641 = 0.02787 -0.00480 0.00281 -0.00016 AFIX 23 H16A 2 -0.079873 -0.210525 0.480475 11.00000 -1.20000 H16B 2 0.034359 -0.219601 0.516892 11.00000 -1.20000 AFIX 0 C17 1 0.113290 -0.065606 0.484812 11.00000 0.02415 0.02499 = 0.02659 -0.00477 0.00192 0.00365 AFIX 23 H17A 2 0.060598 -0.018948 0.464120 11.00000 -1.20000 H17B 2 0.220179 -0.114535 0.476292 11.00000 -1.20000 AFIX 0 C18 1 0.171260 0.031469 0.513396 11.00000 0.01644 0.02434 = 0.02296 -0.00050 0.00196 -0.00177 AFIX 23 H18A 2 0.267012 0.088208 0.503505 11.00000 -1.20000 H18B 2 0.222932 -0.015869 0.534070 11.00000 -1.20000 AFIX 0 C19 1 0.012353 0.115426 0.526303 11.00000 0.01496 0.02109 = 0.02230 0.00101 0.00190 0.00086 AFIX 13 H19 2 -0.011272 0.181614 0.507313 11.00000 -1.20000 AFIX 0 C20 1 0.056959 0.189063 0.561046 11.00000 0.01664 0.01903 = 0.02192 0.00000 0.00034 0.00046 AFIX 13 H20 2 0.085917 0.122477 0.579635 11.00000 -1.20000 AFIX 0 C21 1 0.225606 0.274884 0.557044 11.00000 0.01574 0.02346 = 0.02191 0.00013 0.00303 0.00052 AFIX 23 H21A 2 0.206618 0.335503 0.536841 11.00000 -1.20000 H21B 2 0.330620 0.219431 0.551043 11.00000 -1.20000 AFIX 0 C22 1 0.269829 0.353114 0.590866 11.00000 0.01451 0.02289 = 0.02336 -0.00181 -0.00029 -0.00300 AFIX 23 H22A 2 0.306283 0.293223 0.610280 11.00000 -1.20000 H22B 2 0.372997 0.411594 0.585899 11.00000 -1.20000 AFIX 0 C23 1 0.106836 0.433401 0.603233 11.00000 0.01578 0.01941 = 0.01879 -0.00158 0.00119 0.00054 C24 1 0.641494 0.457014 0.734633 11.00000 0.03335 0.03402 = 0.03925 0.00806 0.00075 -0.00153 AFIX 137 H24A 2 0.765849 0.428735 0.729918 11.00000 -1.50000 H24B 2 0.629459 0.480992 0.759926 11.00000 -1.50000 H24C 2 0.613096 0.532044 0.719571 11.00000 -1.50000 AFIX 0 C25 1 0.082066 0.799715 0.692808 11.00000 0.02332 0.02579 = 0.03653 -0.00277 0.00409 0.00031 AFIX 137 H25A 2 -0.030168 0.750393 0.695905 11.00000 -1.50000 H25B 2 0.057265 0.892169 0.696112 11.00000 -1.50000 H25C 2 0.171293 0.771211 0.710564 11.00000 -1.50000 AFIX 0 C26 1 0.010004 0.846451 0.615039 11.00000 0.02425 0.02370 = 0.03264 0.00359 -0.00525 0.00026 AFIX 137 H26A 2 0.061841 0.846601 0.590869 11.00000 -1.50000 H26B 2 -0.015217 0.935660 0.622470 11.00000 -1.50000 H26C 2 -0.102756 0.796477 0.615046 11.00000 -1.50000 AFIX 0 C27 1 0.400841 0.851199 0.640755 11.00000 0.02006 0.02555 = 0.02368 -0.00083 -0.00296 -0.00707 C28 1 0.476547 0.820287 0.603214 11.00000 0.02583 0.03759 = 0.02942 -0.00042 0.00022 -0.00256 AFIX 137 H28A 2 0.390502 0.849505 0.584939 11.00000 -1.50000 H28B 2 0.494940 0.726669 0.600937 11.00000 -1.50000 H28C 2 0.592313 0.865042 0.599908 11.00000 -1.50000 AFIX 0 C29 1 0.534342 0.799148 0.668867 11.00000 0.02127 0.04523 = 0.02547 -0.00160 -0.00396 -0.00408 AFIX 137 H29A 2 0.651667 0.842143 0.665950 11.00000 -1.50000 H29B 2 0.549301 0.705581 0.665641 11.00000 -1.50000 H29C 2 0.487174 0.816534 0.692932 11.00000 -1.50000 AFIX 0 C30 1 0.383952 0.998144 0.644867 11.00000 0.03505 0.03145 = 0.04859 -0.00904 -0.00001 -0.01206 AFIX 137 H30A 2 0.321729 1.018153 0.667385 11.00000 -1.50000 H30B 2 0.314398 1.033309 0.624737 11.00000 -1.50000 H30C 2 0.504915 1.037070 0.645111 11.00000 -1.50000 AFIX 0 C31 1 0.065118 0.537856 0.575111 11.00000 0.02045 0.02254 = 0.02245 0.00109 0.00044 -0.00179 AFIX 137 H31A 2 0.172278 0.592278 0.571546 11.00000 -1.50000 H31B 2 -0.035825 0.591557 0.583439 11.00000 -1.50000 H31C 2 0.032290 0.496362 0.552408 11.00000 -1.50000 AFIX 0 HKLF 4 REM sad_a.res in P2(1)2(1)2(1) REM R1 = 0.0510 for 3824 Fo > 4sig(Fo) and 0.0786 for all 4987 data REM 314 parameters refined using 0 restraints END WGHT 0.0421 0.0000 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.199, deepest hole -0.247, 1-sigma level 0.047 Q1 1 0.3042 0.8195 0.6463 11.00000 0.05 0.20 Q2 1 0.8072 0.0831 0.6811 11.00000 0.05 0.19 Q3 1 0.3994 0.5382 0.6714 11.00000 0.05 0.17 Q4 1 0.1012 0.7145 0.6107 11.00000 0.05 0.17 Q5 1 0.5155 0.7552 0.6941 11.00000 0.05 0.17 Q6 1 0.0580 0.8034 0.6309 11.00000 0.05 0.16 Q7 1 0.2027 0.3969 0.5934 11.00000 0.05 0.16 Q8 1 0.4741 0.5876 0.6140 11.00000 0.05 0.16 Q9 1 -0.0043 0.4144 0.6806 11.00000 0.05 0.16 Q10 1 0.0772 0.4660 0.5912 11.00000 0.05 0.16 Q11 1 0.1047 0.5993 0.6795 11.00000 0.05 0.16 Q12 1 0.4203 0.9421 0.7027 11.00000 0.05 0.16 Q13 1 0.4698 0.1089 0.7343 11.00000 0.05 0.16 Q14 1 0.6673 0.7696 0.6799 11.00000 0.05 0.15 Q15 1 0.6794 0.3876 0.7140 11.00000 0.05 0.15 Q16 1 0.1828 1.0587 0.6163 11.00000 0.05 0.15 Q17 1 0.0959 0.0785 0.5213 11.00000 0.05 0.15 Q18 1 -0.1706 0.3731 0.5524 11.00000 0.05 0.15 Q19 1 0.2209 0.1429 0.6032 11.00000 0.05 0.15 Q20 1 -0.1290 -0.3476 0.4598 11.00000 0.05 0.15 ; _shelx_res_checksum 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