data_d1402twin _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 N2 O4 Ti, C2 H3 N' _chemical_formula_sum 'C34 H33 N3 O4 Ti' _chemical_formula_weight 595.53 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' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system tetragonal _space_group_IT_number 76 _space_group_name_H-M_alt 'P 41' _space_group_name_Hall 'P 4w' _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' '-y, x, z+1/4' 'y, -x, z+3/4' '-x, -y, z+1/2' _cell_length_a 13.3617(10) _cell_length_b 13.3617(10) _cell_length_c 16.3676(12) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2922.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 147(2) _cell_measurement_reflns_used 8413 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.38 _exptl_crystal_description 'plate' _exptl_crystal_colour yellow _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_F_000 1248 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.290 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.150 _exptl_absorpt_coefficient_mu 0.337 _shelx_estimated_absorpt_T_min 0.909 _shelx_estimated_absorpt_T_max 0.951 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6766 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 147(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube with Bruker Triumph monochromator' _diffrn_measurement_device_type 'Bruker Kappa APEX-DUO CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 6754 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.524 _diffrn_reflns_theta_max 27.560 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_point_group_measured_fraction_full 1.000 _reflns_number_total 6754 _reflns_number_gt 6336 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.932 _reflns_Friedel_fraction_max 0.998 _reflns_Friedel_fraction_full 1.000 _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 'APEX2 (Bruker, 2007)' _computing_cell_refinement 'APEX2' _computing_data_reduction 'SAINT (Bruker, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics 'PLATON (Spek, 2009)' _computing_publication_material 'SHELXTL (Sheldrick, 2008)' _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^)+(0.0442P)^2^+0.2175P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 2859 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.017(8) _chemical_absolute_configuration 'ad' _refine_ls_number_reflns 6754 _refine_ls_number_parameters 388 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0313 _refine_ls_wR_factor_ref 0.0751 _refine_ls_wR_factor_gt 0.0732 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 Ti1 Ti 0.80376(4) 0.69081(3) 0.37171(3) 0.01454(10) Uani 1 1 d . . . . . O1 O 0.79381(15) 0.61189(15) 0.46355(11) 0.0198(4) Uani 1 1 d . . . . . O2 O 0.87455(16) 0.79905(16) 0.42261(13) 0.0247(5) Uani 1 1 d . . . . . O3 O 0.71048(14) 0.61831(14) 0.30720(11) 0.0167(4) Uani 1 1 d . . . . . O4 O 0.91336(15) 0.65153(16) 0.31021(12) 0.0215(4) Uani 1 1 d . . . . . N1 N 0.67392(18) 0.77059(18) 0.42212(14) 0.0158(5) Uani 1 1 d . . . . . N2 N 0.77332(18) 0.80405(18) 0.27748(14) 0.0163(5) Uani 1 1 d . . . . . C1 C 0.64998(19) 0.86337(19) 0.37504(18) 0.0166(5) Uani 1 1 d . . . . . H1A H 0.6970 0.9175 0.3925 0.020 Uiso 1 1 calc R U . . . C2 C 0.5427(2) 0.8997(2) 0.38859(17) 0.0205(6) Uani 1 1 d . . . . . H2A H 0.4959 0.8435 0.3786 0.025 Uiso 1 1 calc R U . . . H2B H 0.5348 0.9208 0.4462 0.025 Uiso 1 1 calc R U . . . C3 C 0.5153(2) 0.9869(2) 0.33269(18) 0.0232(6) Uani 1 1 d . . . . . H3A H 0.4436 1.0035 0.3399 0.028 Uiso 1 1 calc R U . . . H3B H 0.5551 1.0464 0.3481 0.028 Uiso 1 1 calc R U . . . C4 C 0.5349(2) 0.9615(2) 0.24361(18) 0.0218(6) Uani 1 1 d . . . . . H4A H 0.5196 1.0204 0.2091 0.026 Uiso 1 1 calc R U . . . H4B H 0.4905 0.9060 0.2265 0.026 Uiso 1 1 calc R U . . . C5 C 0.6439(2) 0.9310(2) 0.23143(18) 0.0221(6) Uani 1 1 d . . . . . H5A H 0.6883 0.9876 0.2460 0.027 Uiso 1 1 calc R U . . . H5B H 0.6556 0.9140 0.1733 0.027 Uiso 1 1 calc R U . . . C6 C 0.6684(2) 0.84064(19) 0.28501(16) 0.0147(5) Uani 1 1 d . . . . . H6A H 0.6228 0.7848 0.2688 0.018 Uiso 1 1 calc R U . . . C7 C 0.6808(2) 0.7872(2) 0.51242(17) 0.0216(6) Uani 1 1 d . . . . . H7A H 0.6196 0.8248 0.5296 0.026 Uiso 1 1 calc R U . . . C8 C 0.6808(2) 0.6876(2) 0.55798(16) 0.0190(6) Uani 1 1 d . . . . . C9 C 0.6240(2) 0.6781(2) 0.62920(18) 0.0238(6) Uani 1 1 d . . . . . H9A H 0.5831 0.7323 0.6464 0.029 Uiso 1 1 calc R U . . . C10 C 0.6261(2) 0.5907(3) 0.67542(19) 0.0277(7) Uani 1 1 d . . . . . H10A H 0.5886 0.5858 0.7245 0.033 Uiso 1 1 calc R U . . . C11 C 0.6840(2) 0.5106(2) 0.64880(19) 0.0275(7) Uani 1 1 d . . . . . H11A H 0.6857 0.4506 0.6799 0.033 Uiso 1 1 calc R U . . . C12 C 0.7392(2) 0.5176(2) 0.57735(18) 0.0220(6) Uani 1 1 d . . . . . H12A H 0.7775 0.4621 0.5590 0.026 Uiso 1 1 calc R U . . . C13 C 0.7384(2) 0.6063(2) 0.53233(16) 0.0183(5) Uani 1 1 d . . . . . C14 C 0.7716(3) 0.8507(2) 0.53523(18) 0.0257(7) Uani 1 1 d . . . . . C15 C 0.7646(4) 0.9087(3) 0.60674(19) 0.0404(9) Uani 1 1 d . . . . . H15A H 0.7035 0.9099 0.6364 0.048 Uiso 1 1 calc R U . . . C16 C 0.8452(4) 0.9638(3) 0.6347(2) 0.0549(13) Uani 1 1 d . . . . . H16A H 0.8395 1.0024 0.6832 0.066 Uiso 1 1 calc R U . . . C17 C 0.9338(4) 0.9626(3) 0.5915(2) 0.0510(12) Uani 1 1 d . . . . . H17A H 0.9895 0.9999 0.6109 0.061 Uiso 1 1 calc R U . . . C18 C 0.9425(3) 0.9079(2) 0.5207(2) 0.0349(8) Uani 1 1 d . . . . . H18A H 1.0036 0.9087 0.4910 0.042 Uiso 1 1 calc R U . . . C19 C 0.8611(2) 0.8504(2) 0.49193(18) 0.0251(6) Uani 1 1 d . . . . . C20 C 0.8009(2) 0.7679(2) 0.19397(15) 0.0173(5) Uani 1 1 d . . . . . H20A H 0.7852 0.8233 0.1550 0.021 Uiso 1 1 calc R U . . . C21 C 0.7369(2) 0.6786(2) 0.16939(16) 0.0162(5) Uani 1 1 d . . . . . C22 C 0.7208(2) 0.6623(2) 0.08644(17) 0.0219(6) Uani 1 1 d . . . . . H22A H 0.7511 0.7060 0.0479 0.026 Uiso 1 1 calc R U . . . C23 C 0.6617(2) 0.5840(2) 0.05833(18) 0.0252(7) Uani 1 1 d . . . . . H23A H 0.6536 0.5726 0.0014 0.030 Uiso 1 1 calc R U . . . C24 C 0.6148(2) 0.5227(2) 0.1148(2) 0.0232(6) Uani 1 1 d . . . . . H24A H 0.5716 0.4708 0.0966 0.028 Uiso 1 1 calc R U . . . C25 C 0.6306(2) 0.5365(2) 0.19759(17) 0.0196(6) Uani 1 1 d . . . . . H25A H 0.5976 0.4942 0.2356 0.024 Uiso 1 1 calc R U . . . C26 C 0.6943(2) 0.6118(2) 0.22628(15) 0.0158(5) Uani 1 1 d . . . . . C27 C 0.9127(2) 0.7489(2) 0.18835(18) 0.0190(6) Uani 1 1 d . . . . . C28 C 0.9669(2) 0.7872(2) 0.1225(2) 0.0234(6) Uani 1 1 d . . . . . H28A H 0.9336 0.8264 0.0825 0.028 Uiso 1 1 calc R U . . . C29 C 1.0689(2) 0.7691(2) 0.1145(2) 0.0295(7) Uani 1 1 d . . . . . H29A H 1.1047 0.7959 0.0694 0.035 Uiso 1 1 calc R U . . . C30 C 1.1179(2) 0.7118(3) 0.1727(2) 0.0280(7) Uani 1 1 d . . . . . H30A H 1.1877 0.6996 0.1676 0.034 Uiso 1 1 calc R U . . . C31 C 1.0659(2) 0.6724(2) 0.23791(18) 0.0243(6) Uani 1 1 d . . . . . H31A H 1.1000 0.6329 0.2773 0.029 Uiso 1 1 calc R U . . . C32 C 0.9632(2) 0.6901(2) 0.24657(17) 0.0190(5) Uani 1 1 d . . . . . C1S C 0.8709(3) 0.6885(4) 0.7375(3) 0.0583(13) Uani 1 1 d . . . . . H1S1 H 0.8212 0.6963 0.6939 0.087 Uiso 1 1 calc R U . . . H1S2 H 0.9186 0.6360 0.7224 0.087 Uiso 1 1 calc R U . . . H1S3 H 0.9067 0.7518 0.7452 0.087 Uiso 1 1 calc R U . . . C2S C 0.8209(3) 0.6611(3) 0.8126(3) 0.0480(10) Uani 1 1 d . . . . . N1S N 0.7793(4) 0.6414(3) 0.8710(3) 0.0748(13) Uani 1 1 d . . . . . H1N H 0.625(3) 0.737(3) 0.413(2) 0.022(9) Uiso 1 1 d . . . . . H2N H 0.811(3) 0.853(3) 0.292(2) 0.018(8) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0165(2) 0.0160(2) 0.01112(18) 0.00092(19) -0.00037(18) 0.00085(18) O1 0.0244(11) 0.0220(10) 0.0132(9) 0.0041(8) 0.0014(8) 0.0063(8) O2 0.0208(10) 0.0251(11) 0.0284(11) -0.0053(9) -0.0066(9) -0.0005(9) O3 0.0224(10) 0.0154(9) 0.0122(9) -0.0009(7) 0.0001(7) -0.0027(8) O4 0.0213(10) 0.0243(11) 0.0189(10) 0.0031(8) 0.0034(8) 0.0043(8) N1 0.0193(12) 0.0155(11) 0.0127(11) -0.0002(8) -0.0011(9) 0.0005(9) N2 0.0177(11) 0.0146(11) 0.0165(11) -0.0007(9) -0.0008(9) -0.0017(9) C1 0.0173(12) 0.0152(12) 0.0174(12) -0.0016(11) -0.0022(11) 0.0009(9) C2 0.0215(14) 0.0201(13) 0.0199(14) 0.0018(10) 0.0003(10) 0.0036(11) C3 0.0236(15) 0.0185(14) 0.0274(16) 0.0019(12) -0.0014(12) 0.0060(11) C4 0.0228(14) 0.0204(14) 0.0223(14) 0.0032(11) -0.0050(11) 0.0037(11) C5 0.0251(15) 0.0213(14) 0.0199(14) 0.0073(11) 0.0003(12) 0.0034(11) C6 0.0156(13) 0.0138(12) 0.0146(12) 0.0006(10) -0.0004(10) 0.0004(9) C7 0.0302(16) 0.0225(14) 0.0122(12) -0.0024(10) -0.0003(11) 0.0068(12) C8 0.0188(14) 0.0243(14) 0.0140(12) 0.0022(11) -0.0041(10) -0.0006(11) C9 0.0190(13) 0.0332(16) 0.0193(14) -0.0018(13) -0.0005(12) 0.0022(11) C10 0.0234(15) 0.0383(18) 0.0213(14) 0.0044(13) 0.0058(12) -0.0054(13) C11 0.0296(17) 0.0280(16) 0.0250(15) 0.0099(12) 0.0029(12) -0.0063(13) C12 0.0220(14) 0.0235(15) 0.0205(14) 0.0025(11) -0.0005(11) -0.0037(12) C13 0.0164(13) 0.0262(14) 0.0123(12) 0.0006(11) -0.0031(10) -0.0015(11) C14 0.0460(19) 0.0150(13) 0.0161(14) 0.0002(11) -0.0088(13) 0.0015(13) C15 0.080(3) 0.0243(17) 0.0168(16) -0.0026(12) -0.0026(16) -0.0044(17) C16 0.113(4) 0.0307(19) 0.0214(17) -0.0078(15) -0.013(2) -0.019(2) C17 0.088(3) 0.032(2) 0.0331(19) 0.0076(15) -0.032(2) -0.026(2) C18 0.048(2) 0.0223(16) 0.0344(18) 0.0077(13) -0.0230(16) -0.0091(15) C19 0.0374(18) 0.0161(14) 0.0218(14) 0.0033(11) -0.0146(13) -0.0019(12) C20 0.0201(14) 0.0181(13) 0.0138(13) 0.0034(10) 0.0011(10) 0.0005(10) C21 0.0166(13) 0.0172(13) 0.0149(12) 0.0005(10) 0.0003(10) 0.0030(10) C22 0.0253(15) 0.0228(15) 0.0177(13) 0.0021(11) -0.0009(11) 0.0059(12) C23 0.0309(16) 0.0290(16) 0.0156(13) -0.0047(12) -0.0078(12) 0.0083(13) C24 0.0222(14) 0.0204(14) 0.0269(15) -0.0087(12) -0.0069(12) 0.0033(11) C25 0.0187(14) 0.0182(13) 0.0219(14) -0.0020(11) 0.0012(11) 0.0016(11) C26 0.0179(13) 0.0158(12) 0.0135(12) -0.0031(10) 0.0008(10) 0.0032(10) C27 0.0199(14) 0.0183(13) 0.0187(13) 0.0005(11) 0.0027(11) -0.0025(11) C28 0.0261(14) 0.0225(14) 0.0216(13) 0.0040(13) 0.0045(13) -0.0017(11) C29 0.0271(15) 0.0316(16) 0.0297(17) 0.0028(14) 0.0097(14) -0.0075(12) C30 0.0188(14) 0.0343(18) 0.0309(16) -0.0047(13) 0.0029(12) -0.0037(12) C31 0.0213(14) 0.0285(16) 0.0230(15) -0.0039(12) -0.0016(12) -0.0001(12) C32 0.0193(13) 0.0197(13) 0.0180(13) -0.0035(11) 0.0019(11) -0.0014(11) C1S 0.041(2) 0.093(4) 0.041(2) -0.027(2) 0.0041(18) -0.003(2) C2S 0.056(3) 0.049(2) 0.039(2) -0.0103(18) 0.0002(19) 0.0161(19) N1S 0.109(4) 0.068(3) 0.048(2) -0.003(2) 0.020(3) 0.017(2) _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 Ti1 O1 1.8410(19) . ? Ti1 O4 1.853(2) . ? Ti1 O3 1.8992(19) . ? Ti1 O2 1.918(2) . ? Ti1 N1 2.197(2) . ? Ti1 N2 2.198(2) . ? O1 C13 1.350(3) . ? O2 C19 1.338(4) . ? O3 C26 1.345(3) . ? O4 C32 1.340(3) . ? N1 C1 1.494(3) . ? N1 C7 1.497(3) . ? N1 H1N 0.81(4) . ? N2 C6 1.490(3) . ? N2 C20 1.496(3) . ? N2 H2N 0.86(4) . ? C1 C6 1.524(4) . ? C1 C2 1.530(4) . ? C1 H1A 1.0000 . ? C2 C3 1.526(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.520(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.526(4) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.528(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 1.0000 . ? C7 C8 1.526(4) . ? C7 C14 1.528(4) . ? C7 H7A 1.0000 . ? C8 C13 1.395(4) . ? C8 C9 1.397(4) . ? C9 C10 1.392(5) . ? C9 H9A 0.9500 . ? C10 C11 1.390(5) . ? C10 H10A 0.9500 . ? C11 C12 1.386(4) . ? C11 H11A 0.9500 . ? C12 C13 1.396(4) . ? C12 H12A 0.9500 . ? C14 C19 1.391(5) . ? C14 C15 1.406(4) . ? C15 C16 1.382(6) . ? C15 H15A 0.9500 . ? C16 C17 1.380(7) . ? C16 H16A 0.9500 . ? C17 C18 1.375(6) . ? C17 H17A 0.9500 . ? C18 C19 1.412(4) . ? C18 H18A 0.9500 . ? C20 C27 1.518(4) . ? C20 C21 1.522(4) . ? C20 H20A 1.0000 . ? C21 C22 1.392(4) . ? C21 C26 1.410(4) . ? C22 C23 1.389(5) . ? C22 H22A 0.9500 . ? C23 C24 1.385(5) . ? C23 H23A 0.9500 . ? C24 C25 1.384(4) . ? C24 H24A 0.9500 . ? C25 C26 1.398(4) . ? C25 H25A 0.9500 . ? C27 C28 1.396(4) . ? C27 C32 1.407(4) . ? C28 C29 1.389(4) . ? C28 H28A 0.9500 . ? C29 C30 1.387(5) . ? C29 H29A 0.9500 . ? C30 C31 1.378(4) . ? C30 H30A 0.9500 . ? C31 C32 1.399(4) . ? C31 H31A 0.9500 . ? C1S C2S 1.446(6) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S N1S 1.137(6) . ? 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 Ti1 O4 109.78(9) . . ? O1 Ti1 O3 96.57(9) . . ? O4 Ti1 O3 94.14(9) . . ? O1 Ti1 O2 96.48(10) . . ? O4 Ti1 O2 93.43(9) . . ? O3 Ti1 O2 161.72(9) . . ? O1 Ti1 N1 85.08(9) . . ? O4 Ti1 N1 164.91(9) . . ? O3 Ti1 N1 86.45(9) . . ? O2 Ti1 N1 81.98(9) . . ? O1 Ti1 N2 162.48(9) . . ? O4 Ti1 N2 87.71(9) . . ? O3 Ti1 N2 80.77(9) . . ? O2 Ti1 N2 82.94(9) . . ? N1 Ti1 N2 77.49(9) . . ? C13 O1 Ti1 138.79(18) . . ? C19 O2 Ti1 133.6(2) . . ? C26 O3 Ti1 133.33(17) . . ? C32 O4 Ti1 134.94(19) . . ? C1 N1 C7 113.5(2) . . ? C1 N1 Ti1 112.20(16) . . ? C7 N1 Ti1 113.22(17) . . ? C1 N1 H1N 101(3) . . ? C7 N1 H1N 108(3) . . ? Ti1 N1 H1N 108(3) . . ? C6 N2 C20 114.4(2) . . ? C6 N2 Ti1 110.00(16) . . ? C20 N2 Ti1 111.90(16) . . ? C6 N2 H2N 106(2) . . ? C20 N2 H2N 111(2) . . ? Ti1 N2 H2N 102(2) . . ? N1 C1 C6 107.4(2) . . ? N1 C1 C2 112.9(2) . . ? C6 C1 C2 110.8(2) . . ? N1 C1 H1A 108.6 . . ? C6 C1 H1A 108.6 . . ? C2 C1 H1A 108.6 . . ? C3 C2 C1 112.3(2) . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2B 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C4 C3 C2 111.3(2) . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3B 109.4 . . ? C2 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 C5 110.4(2) . . ? C3 C4 H4A 109.6 . . ? C5 C4 H4A 109.6 . . ? C3 C4 H4B 109.6 . . ? C5 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C4 C5 C6 109.9(2) . . ? C4 C5 H5A 109.7 . . ? C6 C5 H5A 109.7 . . ? C4 C5 H5B 109.7 . . ? C6 C5 H5B 109.7 . . ? H5A C5 H5B 108.2 . . ? N2 C6 C1 107.3(2) . . ? N2 C6 C5 114.4(2) . . ? C1 C6 C5 111.3(2) . . ? N2 C6 H6A 107.9 . . ? C1 C6 H6A 107.9 . . ? C5 C6 H6A 107.9 . . ? N1 C7 C8 110.7(2) . . ? N1 C7 C14 111.8(2) . . ? C8 C7 C14 111.4(2) . . ? N1 C7 H7A 107.6 . . ? C8 C7 H7A 107.6 . . ? C14 C7 H7A 107.6 . . ? C13 C8 C9 118.7(3) . . ? C13 C8 C7 122.1(2) . . ? C9 C8 C7 119.1(3) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C11 C10 C9 119.1(3) . . ? C11 C10 H10A 120.4 . . ? C9 C10 H10A 120.4 . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C13 119.9(3) . . ? C11 C12 H12A 120.0 . . ? C13 C12 H12A 120.0 . . ? O1 C13 C8 120.7(3) . . ? O1 C13 C12 118.9(3) . . ? C8 C13 C12 120.4(3) . . ? C19 C14 C15 118.9(3) . . ? C19 C14 C7 123.9(3) . . ? C15 C14 C7 117.2(3) . . ? C16 C15 C14 121.1(4) . . ? C16 C15 H15A 119.4 . . ? C14 C15 H15A 119.4 . . ? C17 C16 C15 119.5(4) . . ? C17 C16 H16A 120.2 . . ? C15 C16 H16A 120.2 . . ? C18 C17 C16 120.7(4) . . ? C18 C17 H17A 119.6 . . ? C16 C17 H17A 119.6 . . ? C17 C18 C19 120.3(4) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? O2 C19 C14 123.3(3) . . ? O2 C19 C18 117.3(3) . . ? C14 C19 C18 119.4(3) . . ? N2 C20 C27 110.6(2) . . ? N2 C20 C21 110.9(2) . . ? C27 C20 C21 114.0(2) . . ? N2 C20 H20A 107.0 . . ? C27 C20 H20A 107.0 . . ? C21 C20 H20A 107.0 . . ? C22 C21 C26 118.8(3) . . ? C22 C21 C20 117.9(3) . . ? C26 C21 C20 123.3(2) . . ? C23 C22 C21 121.9(3) . . ? C23 C22 H22A 119.0 . . ? C21 C22 H22A 119.0 . . ? C24 C23 C22 118.8(3) . . ? C24 C23 H23A 120.6 . . ? C22 C23 H23A 120.6 . . ? C25 C24 C23 120.4(3) . . ? C25 C24 H24A 119.8 . . ? C23 C24 H24A 119.8 . . ? C24 C25 C26 121.2(3) . . ? C24 C25 H25A 119.4 . . ? C26 C25 H25A 119.4 . . ? O3 C26 C25 118.4(2) . . ? O3 C26 C21 123.0(2) . . ? C25 C26 C21 118.6(2) . . ? C28 C27 C32 118.6(3) . . ? C28 C27 C20 119.8(3) . . ? C32 C27 C20 121.6(2) . . ? C29 C28 C27 121.2(3) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C30 C29 C28 119.6(3) . . ? C30 C29 H29A 120.2 . . ? C28 C29 H29A 120.2 . . ? C31 C30 C29 120.3(3) . . ? C31 C30 H30A 119.9 . . ? C29 C30 H30A 119.9 . . ? C30 C31 C32 120.5(3) . . ? C30 C31 H31A 119.7 . . ? C32 C31 H31A 119.7 . . ? O4 C32 C31 120.1(3) . . ? O4 C32 C27 120.2(2) . . ? C31 C32 C27 119.8(3) . . ? C2S C1S H1S1 109.5 . . ? C2S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? C2S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? N1S C2S C1S 177.9(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 O4 Ti1 O1 C13 174.1(3) . . . . ? O3 Ti1 O1 C13 -89.1(3) . . . . ? O2 Ti1 O1 C13 78.1(3) . . . . ? N1 Ti1 O1 C13 -3.3(3) . . . . ? N2 Ti1 O1 C13 -9.0(5) . . . . ? O1 Ti1 O3 C26 -159.5(2) . . . . ? O4 Ti1 O3 C26 -49.0(2) . . . . ? O2 Ti1 O3 C26 65.2(4) . . . . ? N1 Ti1 O3 C26 115.9(2) . . . . ? N2 Ti1 O3 C26 38.0(2) . . . . ? O1 Ti1 O4 C32 -168.3(2) . . . . ? O3 Ti1 O4 C32 93.2(3) . . . . ? O2 Ti1 O4 C32 -70.1(3) . . . . ? N1 Ti1 O4 C32 1.5(5) . . . . ? N2 Ti1 O4 C32 12.7(3) . . . . ? C7 N1 C1 C6 167.6(2) . . . . ? Ti1 N1 C1 C6 37.6(2) . . . . ? C7 N1 C1 C2 -70.1(3) . . . . ? Ti1 N1 C1 C2 159.98(19) . . . . ? N1 C1 C2 C3 -173.2(2) . . . . ? C6 C1 C2 C3 -52.8(3) . . . . ? C1 C2 C3 C4 53.8(3) . . . . ? C2 C3 C4 C5 -56.5(3) . . . . ? C3 C4 C5 C6 58.7(3) . . . . ? C20 N2 C6 C1 173.9(2) . . . . ? Ti1 N2 C6 C1 46.9(2) . . . . ? C20 N2 C6 C5 -62.1(3) . . . . ? Ti1 N2 C6 C5 170.90(19) . . . . ? N1 C1 C6 N2 -55.2(3) . . . . ? C2 C1 C6 N2 -178.9(2) . . . . ? N1 C1 C6 C5 178.9(2) . . . . ? C2 C1 C6 C5 55.2(3) . . . . ? C4 C5 C6 N2 179.7(2) . . . . ? C4 C5 C6 C1 -58.5(3) . . . . ? C1 N1 C7 C8 166.7(2) . . . . ? Ti1 N1 C7 C8 -63.8(3) . . . . ? C1 N1 C7 C14 -68.4(3) . . . . ? Ti1 N1 C7 C14 61.1(3) . . . . ? N1 C7 C8 C13 44.4(4) . . . . ? C14 C7 C8 C13 -80.8(3) . . . . ? N1 C7 C8 C9 -137.8(3) . . . . ? C14 C7 C8 C9 97.1(3) . . . . ? C13 C8 C9 C10 1.7(4) . . . . ? C7 C8 C9 C10 -176.3(3) . . . . ? C8 C9 C10 C11 -1.7(5) . . . . ? C9 C10 C11 C12 0.2(5) . . . . ? C10 C11 C12 C13 1.2(4) . . . . ? Ti1 O1 C13 C8 -16.0(4) . . . . ? Ti1 O1 C13 C12 163.7(2) . . . . ? C9 C8 C13 O1 179.5(2) . . . . ? C7 C8 C13 O1 -2.7(4) . . . . ? C9 C8 C13 C12 -0.2(4) . . . . ? C7 C8 C13 C12 177.7(3) . . . . ? C11 C12 C13 O1 179.1(3) . . . . ? C11 C12 C13 C8 -1.2(4) . . . . ? N1 C7 C14 C19 -31.3(4) . . . . ? C8 C7 C14 C19 93.2(3) . . . . ? N1 C7 C14 C15 152.0(3) . . . . ? C8 C7 C14 C15 -83.5(3) . . . . ? C19 C14 C15 C16 -0.7(5) . . . . ? C7 C14 C15 C16 176.1(3) . . . . ? C14 C15 C16 C17 0.4(6) . . . . ? C15 C16 C17 C18 0.6(6) . . . . ? C16 C17 C18 C19 -1.3(6) . . . . ? Ti1 O2 C19 C14 -17.2(4) . . . . ? Ti1 O2 C19 C18 163.8(2) . . . . ? C15 C14 C19 O2 -178.9(3) . . . . ? C7 C14 C19 O2 4.5(5) . . . . ? C15 C14 C19 C18 0.1(4) . . . . ? C7 C14 C19 C18 -176.5(3) . . . . ? C17 C18 C19 O2 179.9(3) . . . . ? C17 C18 C19 C14 0.9(5) . . . . ? C6 N2 C20 C27 170.4(2) . . . . ? Ti1 N2 C20 C27 -63.6(2) . . . . ? C6 N2 C20 C21 -62.2(3) . . . . ? Ti1 N2 C20 C21 63.8(2) . . . . ? N2 C20 C21 C22 153.2(3) . . . . ? C27 C20 C21 C22 -81.2(3) . . . . ? N2 C20 C21 C26 -27.4(4) . . . . ? C27 C20 C21 C26 98.2(3) . . . . ? C26 C21 C22 C23 1.9(5) . . . . ? C20 C21 C22 C23 -178.7(3) . . . . ? C21 C22 C23 C24 2.3(5) . . . . ? C22 C23 C24 C25 -3.1(4) . . . . ? C23 C24 C25 C26 -0.4(4) . . . . ? Ti1 O3 C26 C25 168.29(19) . . . . ? Ti1 O3 C26 C21 -13.1(4) . . . . ? C24 C25 C26 O3 -176.7(3) . . . . ? C24 C25 C26 C21 4.6(4) . . . . ? C22 C21 C26 O3 176.1(3) . . . . ? C20 C21 C26 O3 -3.3(4) . . . . ? C22 C21 C26 C25 -5.3(4) . . . . ? C20 C21 C26 C25 175.3(3) . . . . ? N2 C20 C27 C28 -131.6(3) . . . . ? C21 C20 C27 C28 102.7(3) . . . . ? N2 C20 C27 C32 50.7(4) . . . . ? C21 C20 C27 C32 -75.0(3) . . . . ? C32 C27 C28 C29 -0.6(4) . . . . ? C20 C27 C28 C29 -178.4(3) . . . . ? C27 C28 C29 C30 0.1(5) . . . . ? C28 C29 C30 C31 0.4(5) . . . . ? C29 C30 C31 C32 -0.4(5) . . . . ? Ti1 O4 C32 C31 148.8(2) . . . . ? Ti1 O4 C32 C27 -31.0(4) . . . . ? C30 C31 C32 O4 -180.0(3) . . . . ? C30 C31 C32 C27 -0.2(4) . . . . ? C28 C27 C32 O4 -179.5(3) . . . . ? C20 C27 C32 O4 -1.8(4) . . . . ? C28 C27 C32 C31 0.7(4) . . . . ? C20 C27 C32 C31 178.4(3) . . . . ? _refine_diff_density_max 0.240 _refine_diff_density_min -0.241 _refine_diff_density_rms 0.040 _shelxl_version_number 2013-3 _shelx_res_file ; TITL mo_D1402_0m CELL 0.71073 13.3617 13.3617 16.3676 90.000 90.000 90.000 ZERR 4.00 0.0010 0.0010 0.0012 0.000 0.000 0.000 LATT -1 SYMM -y, x, z+1/4 SYMM y, -x, z+3/4 SYMM -x, -y, z+1/2 SFAC C H N O TI UNIT 136 132 12 16 4 TEMP -126.140 SIZE 0.150 0.200 0.290 MERG 0 ACTA L.S. 4 FMAP 2 PLAN 20 BOND $H CONF HTAB WGHT 0.044200 0.217500 BASF 0.07415 FVAR 9.94830 TI1 5 0.803765 0.690810 0.371711 11.00000 0.01649 0.01602 = 0.01112 0.00092 -0.00037 0.00085 O1 4 0.793807 0.611886 0.463548 11.00000 0.02436 0.02197 = 0.01317 0.00406 0.00144 0.00631 O2 4 0.874547 0.799049 0.422611 11.00000 0.02080 0.02505 = 0.02835 -0.00527 -0.00659 -0.00048 O3 4 0.710482 0.618312 0.307200 11.00000 0.02237 0.01544 = 0.01224 -0.00094 0.00007 -0.00267 O4 4 0.913356 0.651534 0.310210 11.00000 0.02133 0.02434 = 0.01887 0.00311 0.00339 0.00430 N1 3 0.673923 0.770590 0.422118 11.00000 0.01925 0.01551 = 0.01272 -0.00016 -0.00105 0.00051 N2 3 0.773318 0.804047 0.277485 11.00000 0.01765 0.01465 = 0.01655 -0.00072 -0.00077 -0.00172 C1 1 0.649983 0.863372 0.375038 11.00000 0.01728 0.01517 = 0.01739 -0.00162 -0.00221 0.00094 AFIX 13 H1A 2 0.697026 0.917518 0.392476 11.00000 -1.20000 AFIX 0 C2 1 0.542663 0.899660 0.388591 11.00000 0.02152 0.02011 = 0.01990 0.00179 0.00029 0.00361 AFIX 23 H2A 2 0.495871 0.843536 0.378583 11.00000 -1.20000 H2B 2 0.534810 0.920795 0.446208 11.00000 -1.20000 AFIX 0 C3 1 0.515288 0.986873 0.332695 11.00000 0.02359 0.01852 = 0.02741 0.00188 -0.00139 0.00604 AFIX 23 H3A 2 0.443641 1.003525 0.339949 11.00000 -1.20000 H3B 2 0.555136 1.046402 0.348143 11.00000 -1.20000 AFIX 0 C4 1 0.534853 0.961543 0.243609 11.00000 0.02281 0.02043 = 0.02228 0.00325 -0.00503 0.00366 AFIX 23 H4A 2 0.519582 1.020449 0.209104 11.00000 -1.20000 H4B 2 0.490454 0.906044 0.226519 11.00000 -1.20000 AFIX 0 C5 1 0.643918 0.930993 0.231428 11.00000 0.02515 0.02130 = 0.01994 0.00728 0.00033 0.00337 AFIX 23 H5A 2 0.688334 0.987554 0.245981 11.00000 -1.20000 H5B 2 0.655557 0.914011 0.173325 11.00000 -1.20000 AFIX 0 C6 1 0.668409 0.840641 0.285013 11.00000 0.01564 0.01376 = 0.01458 0.00064 -0.00041 0.00041 AFIX 13 H6A 2 0.622760 0.784763 0.268788 11.00000 -1.20000 AFIX 0 C7 1 0.680754 0.787165 0.512422 11.00000 0.03017 0.02247 = 0.01217 -0.00244 -0.00034 0.00683 AFIX 13 H7A 2 0.619559 0.824783 0.529569 11.00000 -1.20000 AFIX 0 C8 1 0.680788 0.687558 0.557984 11.00000 0.01880 0.02434 = 0.01397 0.00222 -0.00410 -0.00064 C9 1 0.623990 0.678084 0.629200 11.00000 0.01896 0.03321 = 0.01932 -0.00183 -0.00052 0.00216 AFIX 43 H9A 2 0.583125 0.732312 0.646409 11.00000 -1.20000 AFIX 0 C10 1 0.626138 0.590702 0.675417 11.00000 0.02340 0.03828 = 0.02130 0.00439 0.00577 -0.00540 AFIX 43 H10A 2 0.588557 0.585834 0.724527 11.00000 -1.20000 AFIX 0 C11 1 0.683977 0.510648 0.648797 11.00000 0.02957 0.02796 = 0.02501 0.00992 0.00289 -0.00625 AFIX 43 H11A 2 0.685681 0.450606 0.679852 11.00000 -1.20000 AFIX 0 C12 1 0.739192 0.517631 0.577347 11.00000 0.02199 0.02349 = 0.02048 0.00253 -0.00051 -0.00370 AFIX 43 H12A 2 0.777532 0.462115 0.559038 11.00000 -1.20000 AFIX 0 C13 1 0.738394 0.606324 0.532331 11.00000 0.01641 0.02620 = 0.01226 0.00061 -0.00313 -0.00150 C14 1 0.771595 0.850744 0.535228 11.00000 0.04598 0.01502 = 0.01611 0.00016 -0.00881 0.00147 C15 1 0.764610 0.908685 0.606742 11.00000 0.08015 0.02426 = 0.01681 -0.00261 -0.00258 -0.00440 AFIX 43 H15A 2 0.703478 0.909931 0.636361 11.00000 -1.20000 AFIX 0 C16 1 0.845157 0.963843 0.634671 11.00000 0.11264 0.03067 = 0.02136 -0.00783 -0.01340 -0.01947 AFIX 43 H16A 2 0.839507 1.002353 0.683243 11.00000 -1.20000 AFIX 0 C17 1 0.933837 0.962561 0.591481 11.00000 0.08833 0.03166 = 0.03305 0.00764 -0.03202 -0.02616 AFIX 43 H17A 2 0.989496 0.999875 0.610882 11.00000 -1.20000 AFIX 0 C18 1 0.942535 0.907873 0.520675 11.00000 0.04806 0.02226 = 0.03438 0.00767 -0.02302 -0.00908 AFIX 43 H18A 2 1.003603 0.908738 0.490959 11.00000 -1.20000 AFIX 0 C19 1 0.861141 0.850445 0.491930 11.00000 0.03737 0.01613 = 0.02183 0.00329 -0.01459 -0.00189 C20 1 0.800933 0.767874 0.193972 11.00000 0.02010 0.01810 = 0.01376 0.00343 0.00110 0.00048 AFIX 13 H20A 2 0.785152 0.823256 0.154950 11.00000 -1.20000 AFIX 0 C21 1 0.736921 0.678639 0.169393 11.00000 0.01661 0.01724 = 0.01489 0.00053 0.00034 0.00300 C22 1 0.720792 0.662302 0.086442 11.00000 0.02525 0.02279 = 0.01772 0.00210 -0.00090 0.00593 AFIX 43 H22A 2 0.751070 0.706008 0.047908 11.00000 -1.20000 AFIX 0 C23 1 0.661717 0.583959 0.058334 11.00000 0.03086 0.02900 = 0.01562 -0.00465 -0.00781 0.00830 AFIX 43 H23A 2 0.653635 0.572638 0.001414 11.00000 -1.20000 AFIX 0 C24 1 0.614845 0.522695 0.114817 11.00000 0.02223 0.02040 = 0.02687 -0.00868 -0.00686 0.00326 AFIX 43 H24A 2 0.571608 0.470839 0.096626 11.00000 -1.20000 AFIX 0 C25 1 0.630600 0.536547 0.197593 11.00000 0.01871 0.01817 = 0.02194 -0.00197 0.00123 0.00156 AFIX 43 H25A 2 0.597569 0.494185 0.235616 11.00000 -1.20000 AFIX 0 C26 1 0.694283 0.611799 0.226282 11.00000 0.01795 0.01581 = 0.01352 -0.00308 0.00083 0.00321 C27 1 0.912709 0.748884 0.188347 11.00000 0.01990 0.01832 = 0.01873 0.00049 0.00274 -0.00250 C28 1 0.966945 0.787220 0.122544 11.00000 0.02610 0.02246 = 0.02162 0.00395 0.00453 -0.00171 AFIX 43 H28A 2 0.933555 0.826421 0.082522 11.00000 -1.20000 AFIX 0 C29 1 1.068857 0.769127 0.114471 11.00000 0.02707 0.03160 = 0.02969 0.00281 0.00971 -0.00748 AFIX 43 H29A 2 1.104728 0.795855 0.069358 11.00000 -1.20000 AFIX 0 C30 1 1.117925 0.711790 0.172690 11.00000 0.01876 0.03430 = 0.03087 -0.00470 0.00295 -0.00367 AFIX 43 H30A 2 1.187694 0.699619 0.167577 11.00000 -1.20000 AFIX 0 C31 1 1.065905 0.672408 0.237912 11.00000 0.02130 0.02848 = 0.02301 -0.00386 -0.00162 -0.00011 AFIX 43 H31A 2 1.100029 0.632897 0.277313 11.00000 -1.20000 AFIX 0 C32 1 0.963236 0.690148 0.246568 11.00000 0.01934 0.01965 = 0.01803 -0.00349 0.00192 -0.00140 C1S 1 0.870874 0.688516 0.737462 11.00000 0.04081 0.09323 = 0.04090 -0.02690 0.00412 -0.00306 AFIX 133 H1S1 2 0.821204 0.696337 0.693873 11.00000 -1.50000 H1S2 2 0.918584 0.635970 0.722363 11.00000 -1.50000 H1S3 2 0.906691 0.751806 0.745245 11.00000 -1.50000 AFIX 0 C2S 1 0.820915 0.661120 0.812579 11.00000 0.05626 0.04894 = 0.03874 -0.01033 0.00017 0.01613 N1S 3 0.779311 0.641416 0.871011 11.00000 0.10868 0.06811 = 0.04761 -0.00288 0.01954 0.01692 H1N 2 0.624602 0.737312 0.413217 11.00000 0.02157 H2N 2 0.811112 0.852576 0.292265 11.00000 0.01788 HKLF 5 1 1 0 0 0 1 0 0 0 1 REM mo_D1402_0m REM R1 = 0.0313 for 6336 Fo > 4sig(Fo) and 0.0356 for all 6754 data REM 388 parameters refined using 1 restraints END WGHT 0.0449 0.1910 REM Instructions for potential hydrogen bonds EQIV $1 y, -x+2, z-1/4 HTAB C5 O2_$1 REM Highest difference peak 0.240, deepest hole -0.241, 1-sigma level 0.040 Q1 1 0.7948 0.7929 0.0211 11.00000 0.05 0.24 Q2 1 0.7021 0.6791 0.1261 11.00000 0.05 0.22 Q3 1 0.6912 0.6609 0.5177 11.00000 0.05 0.22 Q4 1 0.6962 0.7366 0.5270 11.00000 0.05 0.20 Q5 1 0.6772 0.8564 0.3302 11.00000 0.05 0.19 Q6 1 0.7907 0.7862 0.2363 11.00000 0.05 0.19 Q7 1 0.7622 0.6773 0.4147 11.00000 0.05 0.17 Q8 1 0.7368 0.6572 0.5631 11.00000 0.05 0.17 Q9 1 0.7358 0.8205 0.5260 11.00000 0.05 0.17 Q10 1 0.6830 0.6816 0.6091 11.00000 0.05 0.17 Q11 1 0.6765 0.6372 0.0720 11.00000 0.05 0.16 Q12 1 0.8529 0.7586 0.1851 11.00000 0.05 0.16 Q13 1 0.6217 0.5524 0.1548 11.00000 0.05 0.16 Q14 1 0.7546 0.6634 0.1261 11.00000 0.05 0.16 Q15 1 0.7563 0.6399 0.3330 11.00000 0.05 0.16 Q16 1 0.6598 0.8912 0.2637 11.00000 0.05 0.16 Q17 1 1.0964 0.7616 0.1573 11.00000 0.05 0.15 Q18 1 0.8591 0.6848 0.3363 11.00000 0.05 0.15 Q19 1 0.7324 0.6387 0.1992 11.00000 0.05 0.15 Q20 1 0.7350 0.5648 0.5602 11.00000 0.05 0.15 ; _shelx_res_checksum 67511 _shelx_hkl_file ; 0 -1 21 57782 3071 -2 0 1 -21 57782 3071 1 1 -1 21 3105 1860 -2 1 1 -21 3105 1860 1 -1 -2 21 78719 3475 -2 -1 2 -21 78719 3475 1 0 -2 21 11781 1812 -2 0 2 -21 11781 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