data_IP-model-1 _audit_creation_date 2022-03-03 _audit_creation_method ; Olex2 1.5 (compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439) ; _shelx_SHELXL_version_number '2018/3' _audit_contact_author_address 'National University of Singapore' _audit_contact_author_email wwongpd@nus.edu.sg _audit_contact_author_name 'Walter P.D. Wong' _audit_contact_author_phone ? _publ_contact_author_id_orcid 0000-0003-4360-3920 _publ_section_references ; Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C26 H20 N4' _chemical_formula_sum 'C30 H24 F6 N4 O6' _chemical_formula_weight 650.53 _chemical_absolute_configuration ? _chemical_melting_point ? 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' 'F' 'F' 0.0727 0.0534 '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' _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. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 9 _space_group_name_H-M_alt 'C 1 c 1' _space_group_name_Hall 'C -2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 27.4671(16) _cell_length_b 8.9574(5) _cell_length_c 12.3547(7) _cell_angle_alpha 90 _cell_angle_beta 97.683(4) _cell_angle_gamma 90 _cell_volume 3012.4(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3265 _cell_measurement_temperature 100.00 _cell_measurement_theta_max 64.77 _cell_measurement_theta_min 3.25 _shelx_estimated_absorpt_T_max 0.943 _shelx_estimated_absorpt_T_min 0.747 _exptl_absorpt_coefficient_mu 1.091 _exptl_absorpt_correction_T_max 0.3795 _exptl_absorpt_correction_T_min 0.2568 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1743 before and 0.0729 after correction. The Ratio of minimum to maximum transmission is 0.6767. The \l/2 correction factor is Not present.' _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1336 _exptl_crystal_size_max 0.284 _exptl_crystal_size_mid 0.175 _exptl_crystal_size_min 0.054 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0854 _diffrn_reflns_av_unetI/netI 0.0757 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 13492 _diffrn_reflns_point_group_measured_fraction_full 0.917 _diffrn_reflns_point_group_measured_fraction_max 0.917 _diffrn_reflns_theta_full 65.133 _diffrn_reflns_theta_max 65.133 _diffrn_reflns_theta_min 3.247 _diffrn_ambient_temperature 100.0 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.839 _reflns_Friedel_fraction_full 0.837 _reflns_Friedel_fraction_max 0.837 _reflns_number_gt 2694 _reflns_number_total 4703 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _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. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_collection ? _computing_data_reduction 'SAINT V8.40B (?, 2016)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.230 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.057 _refine_ls_abs_structure_details ; Flack x determined using 886 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.7(4) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 271 _refine_ls_number_reflns 4703 _refine_ls_number_restraints 261 _refine_ls_R_factor_all 0.1237 _refine_ls_R_factor_gt 0.0755 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1316P)^2^+0.7465P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2129 _refine_ls_wR_factor_ref 0.2489 _refine_special_details ? _olex2_refinement_description ; 1. Restrained distances N25-C14 1.45 with sigma of 0.01 C16-C17 1.45 with sigma of 0.02 C14-C15 1.45 with sigma of 0.01 C15-C16 1.45 with sigma of 0.01 2. Rigid body (RIGU) restrains C17, C11, C12, C10, C24, H12, C13, H10, C9, C25, C23, H13, C8, H9, H25, C26, C22, H23, N1, H26, C21, H22, C6, C7, N3, C5, H6, N2, H7, C20, C19, C4, C1, N25, C18, C3, H4, C2, H1, C14, H3, H2, H14, C15, H17, C16, H15, H16 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002 3.a Aromatic/amide H refined with riding coordinates: C12(H12), C10(H10), C13(H13), C22(H22), C25(H25), C23(H23), C9(H9), C6(H6), C26(H26), C14(H14), C20(H20), C3(H3), C2(H2), C7(H7), C17(H17), C19(H19), C4(H4), C15(H15), C16(H16), C1(H1) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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 C11 C 0.6042(3) 0.4940(7) 0.3129(7) 0.0503(18) Uani 1 1 d . U . . . N1 N 0.6881(2) 0.4864(6) 0.0563(5) 0.0544(18) Uani 1 1 d . U . . . N3 N 0.4819(2) 0.4948(8) 0.6620(6) 0.0650(19) Uani 1 1 d . U . . . C5 C 0.7289(3) 0.4177(11) -0.0801(6) 0.059(2) Uani 1 1 d . U . . . C12 C 0.6074(2) 0.6165(7) 0.2477(6) 0.0418(16) Uani 1 1 d . U . . . H12 H 0.588248 0.701547 0.260137 0.050 Uiso 1 1 calc R U . . . C10 C 0.6253(3) 0.3668(7) 0.2858(5) 0.0436(17) Uani 1 1 d . U . . . H10 H 0.620153 0.278172 0.324870 0.052 Uiso 1 1 calc R U . . . C13 C 0.6353(2) 0.6242(8) 0.1691(6) 0.0456(17) Uani 1 1 d . U . . . H13 H 0.638801 0.715807 0.132169 0.055 Uiso 1 1 calc R U . . . C8 C 0.6592(3) 0.4993(7) 0.1411(6) 0.0471(18) Uani 1 1 d . U . . . C22 C 0.5148(3) 0.3680(10) 0.5129(6) 0.061(2) Uani 1 1 d . U . . . H22 H 0.497535 0.282249 0.532536 0.073 Uiso 1 1 calc R U . . . C25 C 0.5637(3) 0.6269(7) 0.4583(6) 0.0460(17) Uani 1 1 d . U . . . H25 H 0.576949 0.719539 0.438818 0.055 Uiso 1 1 calc R U . . . C23 C 0.5444(3) 0.3600(8) 0.4225(6) 0.0541(19) Uani 1 1 d . U . . . H23 H 0.544716 0.272710 0.378852 0.065 Uiso 1 1 calc R U . . . N2 N 0.7366(3) 0.5684(11) -0.0607(6) 0.086(2) Uani 1 1 d . U . . . C9 C 0.6538(3) 0.3607(7) 0.2045(5) 0.0403(17) Uani 1 1 d . U . . . H9 H 0.669756 0.270861 0.188568 0.048 Uiso 1 1 calc R U . . . C6 C 0.6970(3) 0.3657(11) -0.0069(6) 0.066(2) Uani 1 1 d . U . . . H6 H 0.684297 0.267505 -0.002483 0.079 Uiso 1 1 calc R U . . . C26 C 0.5331(3) 0.6185(9) 0.5458(6) 0.059(2) Uani 1 1 d . U . . . H26 H 0.527942 0.703405 0.588983 0.071 Uiso 1 1 calc R U . . . C21 C 0.5122(3) 0.4852(9) 0.5631(7) 0.0545(19) Uani 1 1 d . U . . . N25 N 0.4340(3) 0.5530(10) 0.7688(6) 0.079(2) Uani 1 1 d D U . . . C14 C 0.4060(4) 0.6498(14) 0.8349(8) 0.109(4) Uani 1 1 d D U . . . H14 H 0.402833 0.754842 0.826104 0.131 Uiso 1 1 calc R U . . . C20 C 0.4593(3) 0.6023(12) 0.6849(6) 0.065(2) Uani 1 1 d . U . . . H20 H 0.458817 0.698998 0.653214 0.078 Uiso 1 1 calc R . . . . C3 C 0.7831(3) 0.4135(11) -0.2179(7) 0.074(2) Uani 1 1 d . U . . . H3 H 0.798521 0.365009 -0.272709 0.089 Uiso 1 1 calc R U . . . C2 C 0.7922(4) 0.5625(12) -0.1970(8) 0.083(3) Uani 1 1 d . U . . . H2 H 0.814998 0.613439 -0.235244 0.099 Uiso 1 1 calc R U . . . C18 C 0.4436(4) 0.4098(13) 0.7817(7) 0.078(3) Uani 1 1 d . U . . . C7 C 0.7125(3) 0.6217(11) 0.0150(7) 0.070(2) Uani 1 1 d . U . . . H7 H 0.710712 0.722299 0.038516 0.084 Uiso 1 1 calc R U . . . C17 C 0.4209(4) 0.3382(12) 0.8673(8) 0.089(3) Uani 1 1 d D U . . . H17 H 0.426419 0.235142 0.882415 0.106 Uiso 1 1 calc R U . . . C19 C 0.4731(3) 0.3719(11) 0.7121(6) 0.065(2) Uani 1 1 d . U . . . H19 H 0.485565 0.275143 0.700350 0.078 Uiso 1 1 calc R . . . . C4 C 0.7501(3) 0.3277(12) -0.1568(6) 0.073(2) Uani 1 1 d . U . . . H4 H 0.743654 0.224173 -0.167223 0.088 Uiso 1 1 calc R U . . . C15 C 0.3855(3) 0.5700(11) 0.9090(8) 0.083(3) Uani 1 1 d D U . . . H15 H 0.365046 0.620110 0.953583 0.100 Uiso 1 1 calc R U . . . C24 C 0.5734(3) 0.4919(7) 0.4022(6) 0.0360(14) Uani 1 1 d . U . . . C16 C 0.3930(4) 0.4152(12) 0.9234(8) 0.089(3) Uani 1 1 d D U . . . H16 H 0.376916 0.365068 0.976469 0.106 Uiso 1 1 calc R U . . . C1 C 0.7694(3) 0.6385(10) -0.1234(6) 0.064(2) Uani 1 1 d . U . . . H1 H 0.775653 0.742280 -0.113736 0.077 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 C11 0.043(4) 0.051(3) 0.058(4) -0.011(3) 0.007(3) -0.011(3) N1 0.047(4) 0.071(4) 0.051(4) 0.018(3) 0.026(3) 0.007(3) N3 0.033(4) 0.113(5) 0.049(4) 0.019(3) 0.003(3) 0.020(3) C5 0.021(4) 0.123(5) 0.032(4) -0.006(4) 0.001(3) -0.006(4) C12 0.027(4) 0.050(3) 0.047(4) -0.006(3) 0.000(3) -0.005(3) C10 0.035(4) 0.052(3) 0.044(4) 0.004(3) 0.008(3) 0.001(3) C13 0.027(4) 0.061(4) 0.048(4) 0.009(3) 0.000(3) 0.002(3) C8 0.039(4) 0.057(4) 0.047(4) 0.015(3) 0.010(3) -0.002(3) C22 0.034(5) 0.087(5) 0.062(5) 0.010(4) 0.008(4) 0.004(4) C25 0.050(5) 0.040(3) 0.047(4) 0.002(3) 0.005(3) 0.007(3) C23 0.057(5) 0.050(4) 0.055(5) 0.012(3) 0.004(4) -0.004(3) N2 0.069(6) 0.131(5) 0.064(5) 0.006(4) 0.034(4) -0.014(4) C9 0.054(5) 0.033(3) 0.036(4) -0.004(3) 0.012(3) -0.002(3) C6 0.051(5) 0.095(5) 0.052(5) 0.003(4) 0.008(4) -0.001(4) C26 0.068(6) 0.061(4) 0.048(4) 0.009(4) 0.008(4) 0.022(4) C21 0.047(5) 0.081(4) 0.035(4) 0.026(3) 0.006(3) 0.007(4) N25 0.045(4) 0.138(5) 0.054(4) 0.006(4) 0.005(3) 0.000(4) C14 0.061(7) 0.177(8) 0.095(8) -0.006(6) 0.035(6) 0.007(7) C20 0.038(5) 0.114(5) 0.043(4) -0.002(4) 0.002(3) 0.010(4) C3 0.041(5) 0.116(5) 0.063(6) 0.003(5) 0.006(4) 0.007(4) C2 0.056(6) 0.125(6) 0.068(6) -0.022(5) 0.014(5) -0.009(5) C18 0.055(6) 0.118(5) 0.063(6) -0.020(5) 0.018(4) -0.026(5) C7 0.066(6) 0.099(5) 0.051(5) 0.013(4) 0.025(4) -0.021(4) C17 0.069(7) 0.117(7) 0.081(7) 0.014(5) 0.016(5) 0.006(5) C19 0.049(5) 0.108(5) 0.038(4) 0.003(4) 0.002(3) -0.010(4) C4 0.049(5) 0.135(6) 0.037(4) 0.004(4) 0.006(4) 0.015(5) C15 0.052(6) 0.136(6) 0.063(6) -0.017(6) 0.012(5) -0.013(5) C24 0.035(4) 0.048(3) 0.023(3) -0.007(3) -0.007(2) -0.007(3) C16 0.055(6) 0.156(7) 0.055(6) 0.000(6) 0.011(4) -0.011(6) C1 0.053(5) 0.099(5) 0.043(4) 0.006(4) 0.018(4) -0.004(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 C11 C12 1.370(10) . ? C11 C10 1.342(10) . ? C11 C24 1.476(8) . ? N1 C8 1.402(9) . ? N1 C6 1.375(10) . ? N1 C7 1.506(10) . ? N3 C21 1.570(10) . ? N3 C20 1.200(11) . ? N3 C19 1.301(10) . ? C5 N2 1.383(13) . ? C5 C6 1.420(10) . ? C5 C4 1.426(11) . ? C12 H12 0.9500 . ? C12 C13 1.318(8) . ? C10 H10 0.9500 . ? C10 C9 1.353(8) . ? C13 H13 0.9500 . ? C13 C8 1.364(9) . ? C8 C9 1.486(8) . ? C22 H22 0.9500 . ? C22 C23 1.470(10) . ? C22 C21 1.226(11) . ? C25 H25 0.9500 . ? C25 C26 1.458(9) . ? C25 C24 1.436(9) . ? C23 H23 0.9500 . ? C23 C24 1.466(9) . ? N2 C7 1.307(10) . ? N2 C1 1.411(9) . ? C9 H9 0.9500 . ? C6 H6 0.9500 . ? C26 H26 0.9500 . ? C26 C21 1.354(11) . ? N25 C14 1.475(9) . ? N25 C20 1.395(10) . ? N25 C18 1.315(13) . ? C14 H14 0.9500 . ? C14 C15 1.343(10) . ? C20 H20 0.9500 . ? C3 H3 0.9500 . ? C3 C2 1.376(13) . ? C3 C4 1.472(12) . ? C2 H2 0.9500 . ? C2 C1 1.354(11) . ? C18 C17 1.448(12) . ? C18 C19 1.303(10) . ? C7 H7 0.9500 . ? C17 H17 0.9500 . ? C17 C16 1.299(12) . ? C19 H19 0.9500 . ? C4 H4 0.9500 . ? C15 H15 0.9500 . ? C15 C16 1.410(10) . ? C16 H16 0.9500 . ? C1 H1 0.9500 . ? 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 C12 C11 C24 122.5(7) . . ? C10 C11 C12 118.0(8) . . ? C10 C11 C24 119.1(7) . . ? C8 N1 C7 120.6(6) . . ? C6 N1 C8 130.6(6) . . ? C6 N1 C7 108.7(7) . . ? C20 N3 C21 125.0(8) . . ? C20 N3 C19 115.6(9) . . ? C19 N3 C21 118.3(7) . . ? N2 C5 C6 107.6(7) . . ? N2 C5 C4 126.9(7) . . ? C6 C5 C4 125.4(9) . . ? C11 C12 H12 117.8 . . ? C13 C12 C11 124.4(7) . . ? C13 C12 H12 117.8 . . ? C11 C10 H10 118.9 . . ? C11 C10 C9 122.1(7) . . ? C9 C10 H10 118.9 . . ? C12 C13 H13 120.3 . . ? C12 C13 C8 119.4(7) . . ? C8 C13 H13 120.3 . . ? N1 C8 C9 115.6(6) . . ? C13 C8 N1 126.6(6) . . ? C13 C8 C9 117.8(7) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C21 C22 C23 120.1(8) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C24 C25 C26 118.6(6) . . ? C22 C23 H23 121.3 . . ? C24 C23 C22 117.4(7) . . ? C24 C23 H23 121.3 . . ? C5 N2 C1 115.7(7) . . ? C7 N2 C5 113.6(7) . . ? C7 N2 C1 130.7(9) . . ? C10 C9 C8 117.7(6) . . ? C10 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? N1 C6 C5 106.0(7) . . ? N1 C6 H6 127.0 . . ? C5 C6 H6 127.0 . . ? C25 C26 H26 121.3 . . ? C21 C26 C25 117.4(7) . . ? C21 C26 H26 121.3 . . ? C22 C21 N3 120.9(7) . . ? C22 C21 C26 128.4(9) . . ? C26 C21 N3 110.7(7) . . ? C20 N25 C14 125.0(9) . . ? C18 N25 C14 128.1(9) . . ? C18 N25 C20 106.6(8) . . ? N25 C14 H14 124.4 . . ? C15 C14 N25 111.2(10) . . ? C15 C14 H14 124.4 . . ? N3 C20 N25 104.3(9) . . ? N3 C20 H20 127.8 . . ? N25 C20 H20 127.8 . . ? C2 C3 H3 119.4 . . ? C2 C3 C4 121.2(8) . . ? C4 C3 H3 119.4 . . ? C3 C2 H2 119.2 . . ? C1 C2 C3 121.7(9) . . ? C1 C2 H2 119.2 . . ? N25 C18 C17 114.9(9) . . ? C19 C18 N25 107.9(9) . . ? C19 C18 C17 137.2(11) . . ? N1 C7 H7 128.1 . . ? N2 C7 N1 103.9(8) . . ? N2 C7 H7 128.1 . . ? C18 C17 H17 120.1 . . ? C16 C17 C18 119.9(10) . . ? C16 C17 H17 120.1 . . ? N3 C19 C18 105.3(9) . . ? N3 C19 H19 127.3 . . ? C18 C19 H19 127.3 . . ? C5 C4 C3 112.4(9) . . ? C5 C4 H4 123.8 . . ? C3 C4 H4 123.8 . . ? C14 C15 H15 118.6 . . ? C14 C15 C16 122.8(10) . . ? C16 C15 H15 118.6 . . ? C25 C24 C11 120.8(6) . . ? C25 C24 C23 117.1(7) . . ? C23 C24 C11 121.1(6) . . ? C17 C16 C15 122.8(10) . . ? C17 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? N2 C1 H1 119.0 . . ? C2 C1 N2 122.1(9) . . ? C2 C1 H1 119.0 . . ? 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 C11 C12 C13 C8 7.1(11) . . . . ? C11 C10 C9 C8 -3.0(11) . . . . ? N1 C8 C9 C10 -178.7(7) . . . . ? C5 N2 C7 N1 4.1(10) . . . . ? C5 N2 C1 C2 -0.7(13) . . . . ? C12 C11 C10 C9 7.3(12) . . . . ? C12 C11 C24 C25 -28.9(8) . . . . ? C12 C11 C24 C23 139.3(9) . . . . ? C12 C13 C8 N1 176.6(7) . . . . ? C12 C13 C8 C9 -2.2(11) . . . . ? C10 C11 C12 C13 -9.6(12) . . . . ? C10 C11 C24 C25 159.1(8) . . . . ? C10 C11 C24 C23 -32.8(8) . . . . ? C13 C8 C9 C10 0.3(10) . . . . ? C8 N1 C6 C5 179.7(8) . . . . ? C8 N1 C7 N2 178.8(7) . . . . ? C22 C23 C24 C11 -179.8(6) . . . . ? C22 C23 C24 C25 -11.2(10) . . . . ? C25 C26 C21 N3 178.3(6) . . . . ? C25 C26 C21 C22 -1.6(14) . . . . ? C23 C22 C21 N3 -178.3(6) . . . . ? C23 C22 C21 C26 1.6(15) . . . . ? N2 C5 C6 N1 -2.0(9) . . . . ? N2 C5 C4 C3 0.0(11) . . . . ? C6 N1 C8 C13 -150.1(9) . . . . ? C6 N1 C8 C9 28.7(12) . . . . ? C6 N1 C7 N2 -5.3(10) . . . . ? C6 C5 N2 C7 -1.6(10) . . . . ? C6 C5 N2 C1 177.5(8) . . . . ? C6 C5 C4 C3 -177.7(8) . . . . ? C26 C25 C24 C11 180.0(6) . . . . ? C26 C25 C24 C23 11.3(11) . . . . ? C21 N3 C20 N25 172.9(7) . . . . ? C21 N3 C19 C18 -173.6(7) . . . . ? C21 C22 C23 C24 5.1(12) . . . . ? N25 C14 C15 C16 3.4(15) . . . . ? N25 C18 C17 C16 0.8(14) . . . . ? N25 C18 C19 N3 2.4(10) . . . . ? C14 N25 C20 N3 171.4(9) . . . . ? C14 N25 C18 C17 4.4(14) . . . . ? C14 N25 C18 C19 -174.1(9) . . . . ? C14 C15 C16 C17 1.1(17) . . . . ? C20 N3 C21 C22 -145.3(10) . . . . ? C20 N3 C21 C26 34.7(12) . . . . ? C20 N3 C19 C18 -5.1(11) . . . . ? C20 N25 C14 C15 179.8(8) . . . . ? C20 N25 C18 C17 179.1(8) . . . . ? C20 N25 C18 C19 0.5(10) . . . . ? C3 C2 C1 N2 2.6(15) . . . . ? C2 C3 C4 C5 1.9(12) . . . . ? C18 N25 C14 C15 -6.4(15) . . . . ? C18 N25 C20 N3 -3.4(10) . . . . ? C18 C17 C16 C15 -3.5(16) . . . . ? C7 N1 C8 C13 24.8(12) . . . . ? C7 N1 C8 C9 -156.4(7) . . . . ? C7 N1 C6 C5 4.4(9) . . . . ? C7 N2 C1 C2 178.1(10) . . . . ? C17 C18 C19 N3 -175.7(11) . . . . ? C19 N3 C21 C22 22.0(12) . . . . ? C19 N3 C21 C26 -158.0(8) . . . . ? C19 N3 C20 N25 5.3(11) . . . . ? C19 C18 C17 C16 178.8(11) . . . . ? C4 C5 N2 C7 -179.6(9) . . . . ? C4 C5 N2 C1 -0.6(12) . . . . ? C4 C5 C6 N1 176.0(7) . . . . ? C4 C3 C2 C1 -3.2(15) . . . . ? C24 C11 C12 C13 178.2(6) . . . . ? C24 C11 C10 C9 179.7(6) . . . . ? C24 C25 C26 C21 -5.2(11) . . . . ? C1 N2 C7 N1 -174.8(9) . . . . ? _smtbx_masks_special_details ; A solvent mask was calculated and 532 electrons were found in a volume of 1395\%A^3^ in 1 void per unit cell. This is consistent with the presence of 2[CF3COOH2O] per Formula Unit which account for 520 electrons per unit cell. ; loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.879 -0.467 -0.510 1394.6 532.5 '8 CF3COOH2O' _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL yyj2_b.res in Cc yyj2.res created by SHELXL-2018/3 at 16:22:58 on 04-Feb-2022 REM Old TITL yyj2 in C2/c REM SHELXT solution in Cc: R1 0.312, Rweak 0.010, Alpha 0.021 REM 0.353 for 180 systematic absences, Orientation as input REM Flack x = 0.247 ( 0.465 ) from 976 Parsons' quotients REM Formula found by SHELXT: C33 N11 CELL 1.54178 27.4671 8.9574 12.3547 90 97.683 90 ZERR 4 0.0016 0.0005 0.0007 0 0.004 0 LATT -7 SYMM +X,-Y,0.5+Z SFAC C F H N O UNIT 120 24 96 16 24 DFIX 1.45 0.01 N25 C14 DFIX 1.45 C16 C17 DFIX 1.45 0.01 C14 C15 DFIX 1.45 0.01 C15 C16 RIGU 0.002 0.002 C17 C11 C12 C10 C24 H12 C13 H10 C9 C25 C23 H13 C8 H9 H25 = C26 C22 H23 N1 H26 C21 H22 C6 C7 N3 C5 H6 N2 H7 C20 C19 C4 C1 N25 C18 C3 H4 = C2 H1 C14 H3 H2 H14 C15 H17 C16 H15 H16 L.S. 5 PLAN 9 SIZE 0.054 0.175 0.284 TEMP -173.15 CONF LIST 4 MORE -1 BOND $H ABIN fmap 2 acta OMIT 4 0 2 OMIT 2 2 0 OMIT -2 2 0 REM REM REM WGHT 0.131600 0.746500 FVAR 0.23180 C11 1 0.604180 0.494047 0.312870 11.00000 0.04286 0.05054 = 0.05760 -0.01141 0.00679 -0.01084 N1 4 0.688128 0.486424 0.056345 11.00000 0.04656 0.07125 = 0.05089 0.01819 0.02625 0.00728 N3 4 0.481930 0.494829 0.662011 11.00000 0.03306 0.11269 = 0.04864 0.01900 0.00275 0.01972 C5 1 0.728893 0.417675 -0.080117 11.00000 0.02100 0.12335 = 0.03219 -0.00607 0.00067 -0.00623 C12 1 0.607412 0.616491 0.247747 11.00000 0.02736 0.04969 = 0.04718 -0.00589 0.00042 -0.00539 AFIX 43 H12 3 0.588248 0.701547 0.260137 11.00000 -1.20000 AFIX 0 C10 1 0.625324 0.366822 0.285765 11.00000 0.03521 0.05188 = 0.04441 0.00383 0.00778 0.00068 AFIX 43 H10 3 0.620153 0.278172 0.324870 11.00000 -1.20000 AFIX 0 C13 1 0.635326 0.624161 0.169072 11.00000 0.02709 0.06076 = 0.04776 0.00853 0.00027 0.00227 AFIX 43 H13 3 0.638801 0.715807 0.132169 11.00000 -1.20000 AFIX 0 C8 1 0.659180 0.499296 0.141130 11.00000 0.03890 0.05678 = 0.04682 0.01537 0.01004 -0.00201 C22 1 0.514751 0.367979 0.512944 11.00000 0.03361 0.08692 = 0.06203 0.00981 0.00776 0.00360 AFIX 43 H22 3 0.497535 0.282249 0.532536 11.00000 -1.20000 AFIX 0 C25 1 0.563709 0.626873 0.458287 11.00000 0.05036 0.03998 = 0.04714 0.00182 0.00461 0.00668 AFIX 43 H25 3 0.576949 0.719539 0.438818 11.00000 -1.20000 AFIX 0 C23 1 0.544389 0.359963 0.422461 11.00000 0.05656 0.05022 = 0.05459 0.01190 0.00381 -0.00428 AFIX 43 H23 3 0.544716 0.272710 0.378852 11.00000 -1.20000 AFIX 0 N2 4 0.736626 0.568404 -0.060687 11.00000 0.06881 0.13103 = 0.06428 0.00611 0.03387 -0.01426 C9 1 0.653776 0.360717 0.204528 11.00000 0.05351 0.03334 = 0.03593 -0.00429 0.01235 -0.00174 AFIX 43 H9 3 0.669756 0.270861 0.188568 11.00000 -1.20000 AFIX 0 C6 1 0.696963 0.365688 -0.006879 11.00000 0.05055 0.09514 = 0.05224 0.00270 0.00843 -0.00051 AFIX 43 H6 3 0.684297 0.267505 -0.002483 11.00000 -1.20000 AFIX 0 C26 1 0.533077 0.618545 0.545796 11.00000 0.06751 0.06136 = 0.04840 0.00925 0.00833 0.02187 AFIX 43 H26 3 0.527942 0.703405 0.588983 11.00000 -1.20000 AFIX 0 C21 1 0.512223 0.485154 0.563144 11.00000 0.04737 0.08101 = 0.03525 0.02574 0.00623 0.00724 N25 4 0.433960 0.553032 0.768778 11.00000 0.04507 0.13761 = 0.05413 0.00614 0.00537 0.00008 C14 1 0.405962 0.649764 0.834856 11.00000 0.06144 0.17729 = 0.09495 -0.00558 0.03511 0.00735 AFIX 43 H14 3 0.402833 0.754842 0.826104 11.00000 -1.20000 AFIX 0 C20 1 0.459325 0.602308 0.684942 11.00000 0.03812 0.11388 = 0.04313 -0.00186 0.00226 0.01001 AFIX 43 H20 3 0.458817 0.698998 0.653214 11.00000 -1.20000 AFIX 0 C3 1 0.783148 0.413482 -0.217861 11.00000 0.04135 0.11629 = 0.06348 0.00316 0.00593 0.00714 AFIX 43 H3 3 0.798521 0.365009 -0.272709 11.00000 -1.20000 AFIX 0 C2 1 0.792187 0.562530 -0.197030 11.00000 0.05644 0.12485 = 0.06839 -0.02240 0.01399 -0.00943 AFIX 43 H2 3 0.814998 0.613439 -0.235244 11.00000 -1.20000 AFIX 0 C18 1 0.443621 0.409841 0.781671 11.00000 0.05481 0.11832 = 0.06293 -0.02045 0.01758 -0.02615 C7 1 0.712482 0.621689 0.015028 11.00000 0.06629 0.09888 = 0.05078 0.01311 0.02540 -0.02117 AFIX 43 H7 3 0.710712 0.722299 0.038516 11.00000 -1.20000 AFIX 0 C17 1 0.420904 0.338208 0.867314 11.00000 0.06936 0.11673 = 0.08121 0.01415 0.01579 0.00639 AFIX 43 H17 3 0.426419 0.235142 0.882415 11.00000 -1.20000 AFIX 0 C19 1 0.473128 0.371931 0.712060 11.00000 0.04933 0.10820 = 0.03763 0.00256 0.00231 -0.01028 AFIX 43 H19 3 0.485565 0.275143 0.700350 11.00000 -1.20000 AFIX 0 C4 1 0.750111 0.327733 -0.156768 11.00000 0.04906 0.13462 = 0.03672 0.00398 0.00585 0.01515 AFIX 43 H4 3 0.743654 0.224173 -0.167223 11.00000 -1.20000 AFIX 0 C15 1 0.385474 0.570035 0.908970 11.00000 0.05217 0.13551 = 0.06298 -0.01728 0.01196 -0.01305 AFIX 43 H15 3 0.365046 0.620110 0.953583 11.00000 -1.20000 AFIX 0 C24 1 0.573431 0.491942 0.402160 11.00000 0.03460 0.04776 = 0.02279 -0.00685 -0.00704 -0.00744 C16 1 0.392970 0.415195 0.923442 11.00000 0.05526 0.15617 = 0.05536 0.00008 0.01058 -0.01073 AFIX 43 H16 3 0.376916 0.365068 0.976469 11.00000 -1.20000 AFIX 0 C1 1 0.769390 0.638505 -0.123431 11.00000 0.05269 0.09921 = 0.04348 0.00572 0.01764 -0.00398 AFIX 43 H1 3 0.775653 0.742280 -0.113736 11.00000 -1.20000 AFIX 0 HKLF 4 REM yyj2_b.res in Cc REM wR2 = 0.2489, GooF = S = 1.047, Restrained GooF = 1.085 for all data REM R1 = 0.0755 for 2694 Fo > 4sig(Fo) and 0.1237 for all 4703 data REM 271 parameters refined using 261 restraints END WGHT 0.1316 0.7465 REM Highest difference peak 0.230, deepest hole -0.272, 1-sigma level 0.057 Q1 1 0.6202 0.5979 0.5089 11.00000 0.05 0.23 Q2 1 0.6970 0.5097 0.2804 11.00000 0.05 0.22 Q3 1 0.8306 0.5460 -0.1807 11.00000 0.05 0.21 Q4 1 0.4673 0.5088 0.9177 11.00000 0.05 0.20 Q5 1 0.6729 0.3778 0.3278 11.00000 0.05 0.20 Q6 1 0.4991 0.3612 0.3830 11.00000 0.05 0.20 Q7 1 0.6987 0.3837 0.2431 11.00000 0.05 0.20 Q8 1 0.4858 0.4893 0.4154 11.00000 0.05 0.19 Q9 1 0.5009 0.3745 0.8530 11.00000 0.05 0.19 ; _shelx_res_checksum 36629 _shelx_hkl_file ; 2 0 0 301.97 14.30 4 0 0 199.28 9.70 6 0 0 532.75 25.50 -8 0 0 241.48 13.10 8 0 0 273.67 13.10 8 0 0 281.07 13.20 10 0 0 75.29 4.50 -10 0 0 71.89 4.40 10 0 0 73.99 4.30 12 0 0 96.49 5.70 12 0 0 106.09 5.40 -12 0 0 93.59 5.50 14 0 0 1.40 1.70 14 0 0 4.50 0.70 -14 0 0 2.60 1.50 -14 0 0 2.40 1.40 16 0 0 52.89 3.40 -16 0 0 50.09 3.50 16 0 0 57.59 2.90 -16 0 0 50.49 3.60 16 0 0 49.99 4.00 18 0 0 56.09 3.00 18 0 0 50.09 4.10 18 0 0 54.39 3.40 -18 0 0 49.20 4.80 -18 0 0 52.79 3.60 -20 0 0 30.30 4.10 20 0 0 32.60 2.00 -20 0 0 32.20 2.50 20 0 0 26.10 3.30 22 0 0 64.19 5.30 -22 0 0 79.59 6.10 24 0 0 6.50 2.80 -24 0 0 5.90 2.70 -26 0 0 3.60 3.00 -28 0 0 2.70 2.40 -30 0 0 -1.20 2.20 -32 0 0 16.00 2.40 -1 -1 0 844.22 40.90 -1 1 0 863.41 40.90 1 1 0 895.91 40.90 3 -1 0 165.98 7.90 3 1 0 160.08 7.90 5 -1 0 481.85 22.50 5 1 0 459.75 22.50 7 -1 0 212.68 9.40 7 1 0 196.38 9.40 7 1 0 162.18 9.80 -7 1 0 170.78 9.40 9 -1 0 69.79 4.10 9 1 0 63.09 4.90 -9 1 0 66.49 4.10 9 1 0 73.59 4.20 11 -1 0 7.20 1.80 11 1 0 7.70 1.90 -11 1 0 3.80 1.40 11 1 0 5.10 2.00 13 -1 0 2.30 1.70 -13 -1 0 3.70 1.20 -13 1 0 4.00 1.70 13 1 0 2.60 1.00 -13 1 0 -0.70 1.10 13 1 0 1.90 1.80 -15 -1 0 -0.80 1.00 15 -1 0 0.10 1.50 -15 1 0 0.50 1.40 15 1 0 -0.60 1.60 -15 1 0 -1.30 1.40 15 1 0 3.10 1.00 15 1 0 0.50 1.80 -17 -1 0 19.80 1.90 17 -1 0 12.00 2.30 -17 -1 0 18.10 3.30 17 1 0 17.80 2.50 17 1 0 17.30 1.80 -17 1 0 16.70 2.40 17 1 0 14.40 2.70 -19 -1 0 -3.30 2.00 19 -1 0 1.20 1.70 -19 1 0 1.20 1.30 19 1 0 0.20 0.70 -19 1 0 -3.00 1.90 19 1 0 0.90 1.80 -19 1 0 -0.30 1.30 19 1 0 1.10 1.40 21 -1 0 0.10 1.60 -21 -1 0 0.20 4.00 21 1 0 -0.40 0.80 -21 1 0 -1.80 1.30 21 1 0 -1.60 1.90 21 1 0 2.30 1.40 -21 1 0 -3.30 1.90 -21 1 0 1.60 1.40 -23 -1 0 72.39 6.20 -23 1 0 72.79 4.60 -23 1 0 67.09 5.70 23 1 0 54.49 5.10 -25 -1 0 8.40 3.00 25 1 0 5.60 2.70 -25 1 0 5.00 2.60 -27 -1 0 7.80 2.80 -27 1 0 7.70 2.60 -29 -1 0 0.90 2.10 -29 1 0 0.10 2.60 -31 -1 0 5.80 2.20 -31 1 0 5.60 2.20 0 -2 0 9999.00 474.65 -2 -2 0 1.20 0.40 2 -2 0 -0.20 0.50 2 2 0 0.80 0.80 -2 2 0 -1.60 0.80 -4 -2 0 31.20 1.80 4 -2 0 31.20 1.90 4 2 0 28.90 2.00 6 -2 0 7.60 1.30 -6 2 0 7.30 1.40 6 2 0 7.90 1.30 6 2 0 9.40 1.50 8 -2 0 10.30 1.60 8 2 0 12.00 1.80 -8 2 0 11.50 1.70 8 2 0 17.80 3.10 10 -2 0 125.19 6.80 10 2 0 126.89 6.80 12 -2 0 3.30 1.60 -12 2 0 0.30 1.50 -12 2 0 0.40 1.30 12 2 0 1.90 1.70 12 2 0 3.50 1.40 12 2 0 0.80 2.80 14 -2 0 34.10 2.90 -14 2 0 36.80 3.00 14 2 0 31.90 4.40 14 2 0 32.20 2.60 14 2 0 34.30 3.10 -14 2 0 33.60 2.90 16 -2 0 3.60 1.60 16 2 0 1.50 1.80 16 2 0 3.40 2.30 -16 2 0 3.10 1.40 16 2 0 2.60 1.40 -16 2 0 2.10 1.60 -18 -2 0 41.50 5.00 18 2 0 51.89 3.10 18 2 0 48.60 4.40 18 2 0 46.60 4.10 -18 2 0 53.29 3.70 -18 2 0 43.70 3.50 20 2 0 30.90 3.70 -20 2 0 35.60 6.10 -20 2 0 33.50 3.00 20 2 0 37.90 2.40 -20 2 0 36.20 3.10 20 2 0 30.40 3.40 -22 -2 0 49.30 5.30 -22 2 0 47.90 3.60 22 2 0 37.00 4.00 22 2 0 49.00 3.80 -24 -2 0 5.40 2.80 24 2 0 1.10 2.10 -24 2 0 -0.70 1.30 -24 2 0 1.40 1.70 -24 2 0 5.10 2.60 -24 2 0 0.20 1.80 24 2 0 2.50 1.00 -26 -2 0 7.10 3.10 -26 2 0 2.00 1.40 -26 2 0 0.50 2.70 26 2 0 6.20 3.50 -28 -2 0 0.80 2.30 -28 2 0 4.30 2.90 -30 -2 0 -0.70 2.10 -30 2 0 8.00 2.70 -1 -3 0 1481.85 66.39 1 3 0 1378.36 66.39 -1 3 0 1350.76 66.39 3 -3 0 49.40 2.60 -3 -3 0 49.90 2.50 3 3 0 44.10 2.60 3 3 0 50.59 2.80 -3 3 0 45.50 2.70 5 -3 0 63.39 3.50 -5 -3 0 67.39 3.30 5 3 0 66.59 3.70 -5 3 0 60.79 3.60 5 3 0 64.29 3.40 -7 -3 0 12.50 1.10 7 -3 0 13.60 1.50 7 3 0 11.40 2.10 7 3 0 12.30 1.60 -7 3 0 12.10 1.80 9 -3 0 244.98 12.30 -9 -3 0 248.88 12.00 9 3 0 250.17 12.40 -9 3 0 243.18 12.30 -9 3 0 249.68 13.00 9 3 0 244.78 12.10 -11 -3 0 5.80 1.10 11 -3 0 5.40 1.30 11 3 0 5.30 1.70 -11 3 0 7.50 1.60 -11 3 0 9.90 1.70 11 3 0 4.00 1.30 11 3 0 9.00 3.20 -13 -3 0 140.49 10.40 13 -3 0 157.18 8.60 -13 -3 0 134.39 7.60 -13 3 0 147.79 7.60 13 3 0 140.49 7.80 13 3 0 133.19 9.30 13 3 0 139.59 7.60 -13 3 0 147.79 7.70 -15 -3 0 -0.10 2.00 15 3 0 -0.40 1.80 15 3 0 1.20 1.60 15 3 0 0.10 3.00 -15 3 0 -0.20 1.20 -15 3 0 0.20 1.30 17 -3 0 13.50 2.70 -17 -3 0 19.00 3.70 -17 3 0 21.70 2.40 17 3 0 18.90 2.60 17 3 0 19.60 2.30 17 3 0 18.60 3.80 -17 3 0 19.10 2.20 19 -3 0 -1.60 2.40 -19 -3 0 0.00 2.40 19 3 0 2.00 2.60 -19 3 0 4.30 1.50 19 3 0 1.00 1.30 -19 3 0 1.40 1.30 19 3 0 2.70 1.50 -21 -3 0 7.90 2.80 21 -3 0 12.10 2.90 21 3 0 11.90 1.80 -21 3 0 12.20 1.90 -21 3 0 14.30 2.10 21 3 0 6.10 1.90 21 3 0 10.50 2.80 23 -3 0 19.60 4.60 -23 -3 0 26.40 4.70 -23 3 0 27.40 3.20 23 3 0 26.30 2.00 -23 3 0 23.70 2.50 23 3 0 24.50 4.00 -23 3 0 23.40 3.30 -25 -3 0 12.10 3.10 25 3 0 10.60 1.30 -25 3 0 8.70 1.90 25 3 0 11.30 3.70 -25 3 0 8.60 2.00 -25 3 0 12.00 1.80 -27 -3 0 3.90 2.70 -27 3 0 -2.10 1.40 -27 3 0 0.70 1.10 -29 -3 0 2.90 2.70 0 4 0 71.69 4.40 0 4 0 69.79 3.80 0 4 0 74.39 3.70 -2 4 0 116.59 6.00 -2 4 0 119.59 7.10 2 4 0 117.79 6.00 2 4 0 129.89 6.80 -4 -4 0 17.00 1.30 4 4 0 18.20 1.40 4 4 0 15.90 1.70 -4 4 0 17.30 1.50 6 4 0 1.70 1.10 6 4 0 2.80 1.60 8 4 0 2.30 0.80 -8 4 0 2.40 1.10 8 4 0 0.80 1.20 -8 4 0 1.40 1.00 8 4 0 1.40 1.10 10 4 0 215.08 10.40 -10 4 0 207.58 10.50 -10 4 0 206.78 10.50 10 4 0 204.68 10.70 12 4 0 147.79 8.00 -12 4 0 149.88 7.60 12 4 0 155.68 9.80 -12 4 0 150.98 7.70 12 4 0 125.59 7.80 14 -4 0 16.00 2.60 -14 -4 0 17.00 3.00 14 4 0 13.00 2.30 -14 4 0 16.30 2.10 14 4 0 16.10 4.50 14 4 0 16.70 2.50 -14 4 0 15.80 2.00 16 -4 0 15.60 2.80 -16 -4 0 19.30 3.30 16 4 0 17.90 2.50 16 4 0 17.60 4.50 -16 4 0 16.00 2.20 -16 4 0 19.20 2.20 16 4 0 17.70 2.60 -18 -4 0 2.30 2.30 18 -4 0 2.60 2.70 18 4 0 3.20 3.60 18 4 0 1.40 1.80 -18 4 0 1.70 1.30 -18 4 0 0.10 1.20 18 4 0 -0.20 1.80 -20 -4 0 4.20 2.70 20 -4 0 2.30 2.50 -20 4 0 0.30 1.20 20 4 0 4.30 1.70 20 4 0 3.70 2.70 -20 4 0 3.90 1.60 20 4 0 -1.50 3.00 -22 -4 0 6.70 2.90 22 -4 0 10.30 3.20 -22 4 0 7.70 2.00 -22 4 0 6.30 1.50 22 4 0 7.30 3.00 22 4 0 10.10 1.70 -22 4 0 13.00 2.80 22 4 0 12.10 2.60 24 -4 0 -1.80 2.30 -24 -4 0 0.70 2.50 24 4 0 6.50 2.90 24 4 0 -0.80 2.00 -24 4 0 -1.50 1.60 -24 4 0 0.10 1.50 24 4 0 -0.10 1.00 -24 4 0 0.50 1.10 -26 -4 0 4.50 2.50 -26 4 0 3.20 1.50 26 4 0 5.10 1.00 -26 4 0 2.10 1.70 -26 4 0 4.20 1.20 -28 -4 0 -0.70 2.00 1 -5 0 91.09 4.80 -1 -5 0 92.89 4.80 -1 5 0 95.79 5.00 -1 5 0 89.39 5.30 1 5 0 91.09 4.80 1 5 0 99.09 4.90 1 5 0 94.49 5.30 -1 5 0 98.49 4.90 3 -5 0 39.70 2.40 3 5 0 41.40 2.50 -3 5 0 39.60 2.60 -3 5 0 41.30 2.40 3 5 0 40.80 2.90 5 -5 0 59.29 3.30 5 5 0 61.99 3.30 -5 5 0 58.19 3.40 5 5 0 63.59 3.90 5 5 0 63.49 3.60 -5 5 0 61.59 3.40 -7 -5 0 5.90 1.80 7 -5 0 1.40 2.10 7 -5 0 6.10 1.90 7 5 0 5.90 1.00 -7 5 0 7.30 1.20 7 5 0 6.60 1.70 -7 5 0 6.10 1.10 7 5 0 6.30 1.30 -9 -5 0 49.80 4.80 9 -5 0 34.60 4.80 9 5 0 41.40 3.40 9 5 0 38.10 3.00 -9 5 0 40.70 2.70 -9 5 0 43.30 2.80 9 5 0 40.70 3.30 -11 -5 0 21.20 3.60 11 -5 0 21.60 3.90 11 5 0 20.60 2.10 -11 5 0 19.10 2.00 11 5 0 17.80 2.30 -13 -5 0 45.80 4.80 13 -5 0 56.69 5.40 13 5 0 47.00 3.70 13 5 0 39.20 3.40 13 5 0 47.40 6.60 -13 5 0 50.29 3.30 -13 5 0 53.99 3.30 -15 -5 0 12.50 3.00 15 5 0 15.50 2.70 15 5 0 7.70 1.90 15 5 0 12.40 4.60 -15 5 0 16.30 2.10 -15 5 0 13.90 1.90 -17 -5 0 2.80 2.50 -17 5 0 3.20 1.40 17 5 0 2.40 1.90 17 5 0 3.60 4.10 17 5 0 2.70 2.20 -17 5 0 4.30 1.40 -19 -5 0 1.90 2.40 19 5 0 -1.30 1.80 -19 5 0 1.00 1.10 19 5 0 1.00 1.60 19 5 0 -0.60 3.80 -19 5 0 1.70 1.30 -19 5 0 1.60 1.60 21 -5 0 1.60 3.30 -21 -5 0 1.00 2.70 -21 5 0 0.80 1.40 -21 5 0 0.60 0.90 21 5 0 0.20 1.90 21 5 0 2.50 3.30 -21 5 0 2.30 1.80 21 5 0 1.00 1.50 23 -5 0 2.90 2.80 -23 -5 0 1.10 2.10 -23 5 0 2.00 1.50 23 5 0 -9.20 3.50 23 5 0 2.10 1.30 -23 5 0 0.50 1.50 -23 5 0 -0.50 0.90 23 5 0 0.50 2.40 -25 -5 0 3.70 2.10 25 5 0 -2.20 1.70 -25 5 0 1.10 1.40 -25 5 0 0.60 0.80 25 5 0 0.40 0.90 -25 5 0 -2.30 1.30 -27 -5 0 1.80 1.70 -27 5 0 -2.10 1.30 -27 5 0 -0.80 0.80 0 6 0 76.39 4.20 0 6 0 77.79 4.30 0 6 0 77.49 4.10 2 -6 0 84.99 5.60 -2 -6 0 80.39 5.10 2 -6 0 75.29 4.30 -2 6 0 79.59 4.30 2 6 0 74.19 4.80 2 6 0 78.19 4.30 -2 6 0 74.29 4.30 2 6 0 77.09 4.10 -2 6 0 78.99 4.10 4 -6 0 3.50 1.40 -4 -6 0 0.50 1.40 -4 6 0 2.10 1.00 4 6 0 1.30 1.00 4 6 0 1.60 0.80 4 6 0 1.00 1.40 -4 6 0 0.70 1.00 -4 6 0 2.30 0.90 6 -6 0 2.50 1.40 6 -6 0 -2.10 2.20 -6 -6 0 1.60 1.60 6 6 0 1.10 0.80 6 6 0 1.00 1.60 -6 6 0 0.70 0.80 -6 6 0 2.00 1.10 8 -6 0 23.70 3.00 -8 -6 0 18.30 3.40 8 -6 0 24.90 4.50 -8 6 0 21.60 2.00 8 6 0 20.10 2.60 -8 6 0 19.20 2.20 -8 6 0 20.20 1.80 8 6 0 20.30 2.70 8 6 0 21.60 1.90 10 -6 0 25.20 3.30 10 -6 0 46.30 9.40 -10 -6 0 21.70 3.90 10 6 0 27.00 2.90 -10 6 0 26.00 2.30 -10 6 0 26.30 2.70 10 6 0 27.20 2.40 -10 6 0 24.10 2.20 12 -6 0 24.40 3.40 -12 -6 0 23.20 4.00 12 6 0 24.00 2.60 12 6 0 20.40 2.70 12 6 0 28.80 5.50 -12 6 0 23.40 2.20 -12 6 0 26.50 2.40 -12 6 0 23.30 2.70 -14 -6 0 1.90 2.30 14 -6 0 4.90 2.20 14 6 0 2.60 4.40 -14 6 0 5.20 1.80 -14 6 0 5.20 1.40 14 6 0 6.30 2.20 -14 6 0 2.30 1.20 -16 -6 0 3.50 2.30 16 -6 0 6.50 2.30 16 6 0 7.60 2.10 -16 6 0 4.40 1.20 16 6 0 4.40 4.50 16 6 0 6.50 2.40 -16 6 0 8.70 2.10 18 -6 0 38.10 6.80 -18 -6 0 18.10 3.20 18 -6 0 17.00 3.30 18 6 0 18.80 4.90 -18 6 0 21.80 2.10 18 6 0 17.90 2.90 -18 6 0 27.80 2.60 18 6 0 22.50 3.20 -18 6 0 23.70 2.80 20 -6 0 10.60 2.80 -20 -6 0 11.40 2.60 20 -6 0 9.90 2.50 -20 6 0 13.50 2.30 20 6 0 11.50 2.10 20 6 0 10.90 4.10 -20 6 0 13.40 1.70 -20 6 0 13.10 2.30 22 -6 0 1.80 1.90 22 -6 0 3.80 2.80 -22 -6 0 3.60 1.90 -22 6 0 2.30 1.50 22 6 0 2.50 1.50 -22 6 0 0.90 0.80 22 6 0 5.20 3.80 -22 6 0 0.80 1.60 -24 -6 0 1.10 2.10 24 6 0 -0.60 0.90 24 6 0 -3.20 1.90 -24 6 0 0.00 0.80 -24 6 0 -1.10 1.30 -24 6 0 -1.80 1.20 26 -6 0 0.50 1.30 -26 -6 0 0.10 1.40 -26 6 0 -0.60 0.70 26 6 0 -1.70 0.70 -1 -7 0 69.19 4.90 1 -7 0 67.79 4.80 1 7 0 75.29 4.40 -1 7 0 76.09 4.10 1 7 0 74.19 4.10 -1 7 0 77.69 4.40 3 -7 0 38.30 5.20 3 -7 0 37.50 3.40 -3 -7 0 38.10 3.70 -3 7 0 42.20 2.90 3 7 0 37.50 3.60 3 7 0 41.20 3.20 -3 7 0 39.30 2.50 3 7 0 42.70 2.60 -3 7 0 38.60 2.70 -5 -7 0 12.50 2.90 5 -7 0 11.80 3.50 5 7 0 11.80 2.50 5 7 0 8.50 1.40 -5 7 0 6.60 1.10 -5 7 0 12.80 1.90 5 7 0 10.70 1.90 7 -7 0 4.60 3.30 7 -7 0 3.80 1.50 -7 -7 0 1.00 2.10 7 7 0 3.30 1.80 -7 7 0 3.60 0.90 -7 7 0 2.80 1.30 -7 7 0 6.50 1.30 7 7 0 3.90 1.30 7 7 0 5.30 2.10 9 -7 0 10.50 3.50 -9 -7 0 2.90 2.20 9 -7 0 1.60 1.40 -9 7 0 1.40 0.90 -9 7 0 1.40 1.10 -9 7 0 1.30 1.40 9 7 0 2.10 1.80 9 7 0 1.20 1.20 -11 -7 0 0.30 2.00 11 -7 0 1.10 1.50 11 -7 0 5.90 3.30 -11 7 0 2.60 1.00 -11 7 0 0.90 1.50 -11 7 0 2.80 1.30 11 7 0 1.30 1.50 11 7 0 3.90 2.20 11 7 0 1.90 4.80 -13 -7 0 3.90 2.30 13 -7 0 9.90 2.00 13 7 0 7.90 2.10 -13 7 0 7.60 1.30 15 -7 0 -1.00 1.50 15 -7 0 3.60 2.60 -15 -7 0 2.20 2.30 15 7 0 2.20 2.00 15 7 0 -4.20 4.70 -15 7 0 0.70 0.90 -15 7 0 1.50 1.30 -15 7 0 0.40 1.40 17 -7 0 10.30 3.00 -17 -7 0 7.50 2.20 17 -7 0 4.90 1.80 -17 7 0 3.80 1.50 17 7 0 2.30 4.60 -17 7 0 7.70 1.70 17 7 0 4.40 2.20 -17 7 0 4.00 1.00 17 7 0 4.00 1.90 19 -7 0 2.10 1.70 19 -7 0 4.80 2.40 -19 -7 0 5.20 2.00 -19 7 0 2.40 0.90 19 7 0 3.50 4.00 19 7 0 -1.10 1.80 -19 7 0 2.30 1.60 -19 7 0 4.30 1.70 21 -7 0 2.80 2.00 -21 -7 0 7.20 2.30 21 -7 0 5.50 1.70 -21 7 0 4.10 1.00 21 7 0 7.70 3.20 -21 7 0 4.00 1.60 -21 7 0 6.60 1.60 -23 -7 0 0.90 1.30 -23 7 0 0.00 0.80 -23 7 0 -1.40 1.30 23 7 0 -0.30 1.10 -23 7 0 1.90 1.50 0 8 0 117.89 6.50 0 8 0 110.59 6.00 -2 8 0 64.39 4.20 2 8 0 66.79 4.50 -2 8 0 60.69 3.70 2 8 0 61.79 3.80 4 -8 0 6.50 2.80 4 8 0 7.50 1.40 -4 8 0 4.40 1.10 -4 8 0 5.90 1.80 4 8 0 7.70 2.10 -4 8 0 9.20 1.80 6 -8 0 -0.50 2.40 -6 8 0 1.40 0.90 6 8 0 1.10 1.10 -6 8 0 1.70 1.70 -6 8 0 1.70 1.90 6 8 0 -0.70 3.10 8 -8 0 3.20 3.70 -8 8 0 0.70 0.80 -8 8 0 0.00 1.20 8 8 0 -1.10 1.20 -8 8 0 0.80 1.10 8 8 0 4.60 2.20 10 -8 0 3.10 2.50 -10 8 0 0.30 0.80 10 8 0 0.60 1.50 -10 8 0 0.50 1.30 -10 8 0 1.70 1.40 10 8 0 -2.00 4.70 12 -8 0 3.20 2.60 -12 8 0 0.50 0.90 -12 8 0 -2.00 1.30 12 8 0 -1.80 4.70 -12 8 0 0.50 1.30 12 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1.00 0 10 0 5.80 1.80 2 10 0 0.50 0.90 -2 10 0 -0.50 0.80 -2 10 0 -1.40 1.50 -4 10 0 0.20 0.80 4 10 0 -0.70 0.90 -4 10 0 -1.10 1.40 4 10 0 -1.60 3.90 -6 10 0 0.60 0.80 6 10 0 0.20 1.00 6 10 0 -8.20 3.30 -6 10 0 -0.10 1.40 8 10 0 12.50 3.90 -8 10 0 1.50 0.80 -8 10 0 3.20 1.50 10 10 0 2.00 1.60 -10 10 0 0.40 0.70 -32 0 1 -0.70 1.90 -30 0 1 -0.20 2.10 -28 0 1 -0.60 2.40 26 0 -1 6.40 2.70 24 0 -1 1.30 3.30 -24 0 1 2.40 2.70 22 0 -1 1.60 2.20 -22 0 1 0.10 2.10 22 0 -1 1.50 0.90 -20 0 1 -3.10 1.90 20 0 -1 0.00 0.80 20 0 -1 -0.70 1.20 20 0 -1 -1.30 2.20 -18 0 1 0.70 1.90 -18 0 1 1.10 0.90 18 0 -1 0.40 1.90 18 0 -1 1.80 1.10 18 0 -1 0.80 1.20 16 0 -1 0.40 1.10 -16 0 1 2.80 1.10 16 0 -1 0.10 0.60 16 0 -1 -1.30 1.70 -14 0 1 0.30 1.00 14 0 -1 -0.90 1.80 14 0 -1 0.00 0.60 -14 0 1 -0.30 0.90 12 0 -1 0.10 1.00 -12 0 1 -1.80 0.90 12 0 -1 -1.30 1.70 -10 0 1 -0.90 0.90 10 0 -1 -0.70 1.40 10 0 -1 -0.80 1.00 8 0 -1 -1.00 1.30 8 0 -1 -0.90 1.10 6 0 -1 -0.10 1.00 4 0 -1 0.20 0.50 2 0 -1 0.10 0.20 0 0 1 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_shelx_fab_checksum 6597 _olex2_submission_special_instructions 'No special instructions were received' # start Validation Reply Form _vrf_PLAT110_IP-model-1 ; PROBLEM: ADDSYM Detects Potential Lattice Translation ... ? Check RESPONSE: artefact arising from solvent masking ; _vrf_PLAT111_IP-model-1 ; PROBLEM: ADDSYM Detects New (Pseudo) Centre of Symmetry . 100 %Fit RESPONSE: artefact arising from solvent masking ; _vrf_PLAT112_IP-model-1 ; PROBLEM: ADDSYM Detects New (Pseudo) Symm. Elem c/2 100 %Fit RESPONSE: artefact arising from solvent masking ; _vrf_PLAT113_IP-model-1 ; PROBLEM: ADDSYM Suggests Possible Pseudo/New Space Group I2/n Check RESPONSE: artefact arising from solvent masking ; _vrf_PLAT340_IP-model-1 ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.011 Ang. RESPONSE: low data quality and strong disorder present ;