data_Ti-PDC #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_formula_sum 'C15 H15 N3 O7 Ti' _chemical_formula_weight 397.17 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_Hall 'F 2 -2d' _symmetry_Int_Tables_number 43 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+3/4, -y+5/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+5/4, -y+3/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+5/4, -y+5/4, z+1/4' _cell_length_a 42.164(9) _cell_length_b 20.815(4) _cell_length_c 7.4780(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 6563(2) _cell_formula_units_Z 16 _cell_measurement_temperature 100.0(2) _cell_measurement_reflns_used 4692 _cell_measurement_theta_min 3.498 _cell_measurement_theta_max 25.242 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_density_diffrn 1.608 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3264 _exptl_crystal_description 'Needle' _exptl_crystal_colour 'Colorless' _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.010 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.540 _exptl_absorpt_correction_type 'EMPIRICAL' _exptl_absorpt_process_details ; SADABS(Blessing, 1995) ; _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.98 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'BL2D-SMC' _diffrn_ambient_temperature 100.0(2) _diffrn_radiation_wavelength 0.7 _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_number 4692 _diffrn_reflns_limit_h_min -59 _diffrn_reflns_limit_h_max 59 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 3.498 _diffrn_reflns_theta_max 25 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 1 _diffrn_reflns_point_group_measured_fraction_full 1 _diffrn_reflns_point_group_measured_fraction_max 1 _reflns_number_total 2884 _reflns_number_gt 2143 _reflns_threshold_expression 'I > 2\s(I)' #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refined as a 2-component inversion 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^)+(0.1924P)^2^+11.7931P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_coef 0.0077(17) _refine_ls_number_reflns 2884 _refine_ls_number_parameters 239 _refine_ls_number_restraints 1 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.1089 _refine_ls_R_factor_gt 0.0899 _refine_ls_wR_factor_ref 0.2769 _refine_ls_wR_factor_gt 0.2548 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.003 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.00(17) _refine_diff_density_max 0.997 _refine_diff_density_min -1.054 _refine_diff_density_rms 0.131 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' 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_calc_flag _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti -0.00011(3) 0.24827(11) 0.2499(6) 0.0322(5) Uani 1 d . . O1 O -0.00250(14) 0.2620(6) 0.5254(9) 0.037(2) Uani 1 d . . O3 O 0.00608(13) 0.3495(5) 0.2303(8) 0.037(2) Uani 1 d . . O4 O 0.03494(19) 0.4360(7) 0.2804(13) 0.055(3) Uani 1 d . . O5 O 0.02460(15) 0.1626(5) 0.3012(8) 0.038(2) Uani 1 d . . O6 O 0.0726(3) 0.1136(9) 0.3423(15) 0.078(5) Uani 1 d . . O7 O -0.04513(14) 0.2908(5) 0.2470(9) 0.043(2) Uani 1 d . . O8 O -0.09637(17) 0.2882(8) 0.3206(15) 0.079(5) Uani 1 d . . N1 N 0.05104(17) 0.2746(6) 0.2954(9) 0.034(2) Uani 1 d . . N2 N -0.03718(18) 0.1691(6) 0.2947(10) 0.038(3) Uani 1 d . . C1 C 0.0590(2) 0.3339(8) 0.3081(13) 0.042(3) Uani 1 d . . C2 C 0.0899(2) 0.3518(9) 0.3494(14) 0.054(5) Uani 1 d . . H2 H 0.0952 0.3949 0.3622 0.065 Uiso 1 calc . . C3 C 0.1122(2) 0.3055(9) 0.3708(17) 0.049(4) Uani 1 d . . H3 H 0.133 0.3171 0.3955 0.059 Uiso 1 calc . . C4 C 0.1046(3) 0.2442(10) 0.3569(18) 0.062(6) Uani 1 d . . H4 H 0.1198 0.2122 0.3687 0.075 Uiso 1 calc . . C5 C 0.0730(2) 0.2294(7) 0.3240(12) 0.038(3) Uani 1 d . . C6 C 0.0320(2) 0.3781(9) 0.2725(13) 0.046(3) Uani 1 d . . C7 C 0.0564(3) 0.1655(10) 0.3269(18) 0.054(4) Uani 1 d . . C8 C -0.0313(3) 0.1062(8) 0.3103(14) 0.045(3) Uani 1 d . . H8 H -0.0106 0.0916 0.2936 0.054 Uiso 1 calc . . C9 C -0.0549(3) 0.0618(10) 0.3504(16) 0.056(4) Uani 1 d . . H9 H -0.0504 0.0182 0.3589 0.067 Uiso 1 calc . . C10 C -0.0850(3) 0.0846(9) 0.3770(16) 0.057(5) Uani 1 d . . H10 H -0.1013 0.056 0.4049 0.068 Uiso 1 calc . . C11 C -0.0919(3) 0.1522(11) 0.3621(14) 0.060(5) Uani 1 d . . H11 H -0.1121 0.1685 0.383 0.073 Uiso 1 calc . . C12 C -0.0666(2) 0.1918(8) 0.3147(12) 0.044(4) Uani 1 d . . C13 C -0.0709(2) 0.2621(8) 0.2946(16) 0.043(3) Uani 1 d . . N5 N 0.0451(2) 0.0670(7) 0.7721(12) 0.047(3) Uani 1 d . . H5A H 0.0339 0.0343 0.7285 0.057 Uiso 1 d . . H5B H 0.0376 0.1033 0.7256 0.057 Uiso 1 d . . C27 C 0.0790(3) 0.0601(12) 0.735(2) 0.070(5) Uani 1 d . . H27A H 0.0829 0.0687 0.6103 0.106 Uiso 1 calc . . H27B H 0.0856 0.0172 0.7624 0.106 Uiso 1 calc . . H27C H 0.0908 0.0901 0.8063 0.106 Uiso 1 calc . . C28 C 0.0422(4) 0.0681(11) 0.967(2) 0.074(6) Uani 1 d . . H28A H 0.0204 0.0741 0.9997 0.111 Uiso 1 calc . . H28B H 0.0547 0.1027 1.0146 0.111 Uiso 1 calc . . H28C H 0.0497 0.0281 1.0154 0.111 Uiso 1 calc . . 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 0.0303(6) 0.0436(14) 0.0227(7) 0.0019(6) -0.0004(4) 0.0014(6) O1 0.040(3) 0.052(8) 0.019(4) 0.000(3) 0.0020(18) 0.000(3) O3 0.035(3) 0.043(7) 0.034(3) -0.006(3) 0.001(2) 0.006(3) O4 0.049(4) 0.041(11) 0.077(6) -0.003(5) 0.003(3) 0.000(4) O5 0.044(3) 0.035(7) 0.034(3) -0.006(3) -0.005(2) 0.013(3) O6 0.088(7) 0.072(15) 0.074(6) -0.025(6) -0.001(5) 0.033(7) O7 0.034(3) 0.063(8) 0.031(3) 0.008(3) 0.002(2) -0.001(3) O8 0.032(3) 0.118(16) 0.087(6) 0.050(8) 0.017(4) 0.014(5) N1 0.036(3) 0.046(8) 0.020(3) 0.001(3) 0.000(2) 0.001(4) N2 0.038(3) 0.042(9) 0.033(3) 0.006(3) 0.003(2) 0.005(4) C1 0.034(4) 0.050(11) 0.041(4) -0.002(4) 0.000(3) -0.010(4) C2 0.037(4) 0.079(15) 0.046(5) -0.010(6) -0.005(3) -0.022(6) C3 0.034(4) 0.044(14) 0.070(7) -0.001(6) -0.005(4) -0.009(5) C4 0.045(5) 0.09(2) 0.054(7) 0.001(7) -0.006(4) 0.019(7) C5 0.045(4) 0.037(9) 0.031(4) 0.002(4) -0.006(3) 0.002(5) C6 0.046(4) 0.053(13) 0.039(5) 0.003(5) 0.007(3) -0.011(5) C7 0.055(6) 0.046(15) 0.061(7) -0.012(6) -0.001(5) -0.003(6) C8 0.054(5) 0.042(11) 0.040(5) 0.006(5) 0.003(4) -0.008(5) C9 0.082(7) 0.038(13) 0.048(6) 0.008(5) 0.010(5) -0.019(7) C10 0.065(6) 0.055(15) 0.050(6) 0.015(6) -0.015(5) -0.033(7) C11 0.044(5) 0.093(18) 0.044(5) 0.005(6) 0.005(4) -0.029(7) C12 0.034(4) 0.067(12) 0.031(4) -0.004(4) 0.003(3) -0.010(4) C13 0.039(4) 0.031(11) 0.059(7) 0.013(5) -0.001(4) -0.005(4) N5 0.049(4) 0.040(10) 0.052(5) -0.001(4) -0.006(3) 0.009(4) C27 0.054(6) 0.057(18) 0.100(12) 0.000(10) 0.015(6) 0.010(7) C28 0.091(9) 0.062(18) 0.069(8) -0.012(8) -0.032(7) 0.034(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 1.696(8) 6_554 ? Ti1 O1 2.082(7) . ? Ti1 O7 2.095(7) . ? Ti1 O5 2.101(9) . ? Ti1 O3 2.128(11) . ? Ti1 N1 2.251(8) . ? Ti1 N2 2.295(11) . ? O1 Ti1 1.696(8) 6 ? O3 C6 1.284(14) . ? O4 C6 1.21(2) . ? O5 C7 1.354(13) . ? O6 C7 1.28(2) . ? O7 C13 1.291(13) . ? O8 C13 1.218(16) . ? N1 C1 1.28(2) . ? N1 C5 1.336(16) . ? N2 C12 1.335(13) . ? N2 C8 1.34(2) . ? C1 C2 1.390(12) . ? C1 C6 1.489(17) . ? C2 C3 1.35(2) . ? C2 H2 0.93 . ? C3 C4 1.32(2) . ? C3 H3 0.93 . ? C4 C5 1.391(17) . ? C4 H4 0.93 . ? C5 C7 1.50(2) . ? C8 C9 1.391(17) . ? C8 H8 0.93 . ? C9 C10 1.37(2) . ? C9 H9 0.93 . ? C10 C11 1.44(2) . ? C10 H10 0.93 . ? C11 C12 1.394(17) . ? C11 H11 0.93 . ? C12 C13 1.48(2) . ? N5 C27 1.463(15) . ? N5 C28 1.464(17) . ? N5 H5A 0.8904 . ? N5 H5B 0.8904 . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? 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 O1 178.85(13) 6_554 . ? O1 Ti1 O7 95.8(4) 6_554 . ? O1 Ti1 O7 84.8(3) . . ? O1 Ti1 O5 92.4(4) 6_554 . ? O1 Ti1 O5 87.7(4) . . ? O7 Ti1 O5 144.1(4) . . ? O1 Ti1 O3 92.8(4) 6_554 . ? O1 Ti1 O3 86.5(4) . . ? O7 Ti1 O3 72.1(3) . . ? O5 Ti1 O3 142.4(3) . . ? O1 Ti1 N1 96.8(3) 6_554 . ? O1 Ti1 N1 82.1(3) . . ? O7 Ti1 N1 140.1(4) . . ? O5 Ti1 N1 72.8(4) . . ? O3 Ti1 N1 69.6(3) . . ? O1 Ti1 N2 95.7(4) 6_554 . ? O1 Ti1 N2 85.5(3) . . ? O7 Ti1 N2 71.8(4) . . ? O5 Ti1 N2 72.6(3) . . ? O3 Ti1 N2 143.5(3) . . ? N1 Ti1 N2 143.6(4) . . ? Ti1 O1 Ti1 163.6(7) 6 . ? C6 O3 Ti1 123.1(9) . . ? C7 O5 Ti1 118.6(10) . . ? C13 O7 Ti1 124.4(9) . . ? C1 N1 C5 118.9(9) . . ? C1 N1 Ti1 119.8(7) . . ? C5 N1 Ti1 121.0(9) . . ? C12 N2 C8 120.6(11) . . ? C12 N2 Ti1 113.3(10) . . ? C8 N2 Ti1 126.0(7) . . ? N1 C1 C2 121.4(13) . . ? N1 C1 C6 112.4(9) . . ? C2 C1 C6 126.2(15) . . ? C3 C2 C1 119.0(16) . . ? C3 C2 H2 120.5 . . ? C1 C2 H2 120.5 . . ? C4 C3 C2 120.7(11) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 117.4(14) . . ? C3 C4 H4 121.3 . . ? C5 C4 H4 121.3 . . ? N1 C5 C4 122.4(14) . . ? N1 C5 C7 107.7(10) . . ? C4 C5 C7 129.8(14) . . ? O4 C6 O3 124.0(13) . . ? O4 C6 C1 121.9(10) . . ? O3 C6 C1 114.1(14) . . ? O6 C7 O5 120.3(17) . . ? O6 C7 C5 119.7(12) . . ? O5 C7 C5 119.8(14) . . ? N2 C8 C9 122.3(13) . . ? N2 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? C10 C9 C8 117.7(18) . . ? C10 C9 H9 121.1 . . ? C8 C9 H9 121.1 . . ? C9 C10 C11 120.9(13) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 116.3(13) . . ? C12 C11 H11 121.9 . . ? C10 C11 H11 121.9 . . ? N2 C12 C11 122.1(16) . . ? N2 C12 C13 116.8(10) . . ? C11 C12 C13 121.0(12) . . ? O8 C13 O7 125.4(16) . . ? O8 C13 C12 122.2(12) . . ? O7 C13 C12 112.4(10) . . ? C27 N5 C28 105.9(11) . . ? C27 N5 H5A 111.9 . . ? C28 N5 H5A 109.4 . . ? C27 N5 H5B 110.7 . . ? C28 N5 H5B 110.3 . . ? H5A N5 H5B 108.5 . . ? N5 C27 H27A 109.5 . . ? N5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N5 C28 H28A 109.5 . . ? N5 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N5 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 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 C5 N1 C1 C2 0.5(14) . . . . ? Ti1 N1 C1 C2 175.1(8) . . . . ? C5 N1 C1 C6 -180.0(8) . . . . ? Ti1 N1 C1 C6 -5.3(11) . . . . ? N1 C1 C2 C3 2.2(17) . . . . ? C6 C1 C2 C3 -177.3(10) . . . . ? C1 C2 C3 C4 -1.6(19) . . . . ? C2 C3 C4 C5 -1.5(19) . . . . ? C1 N1 C5 C4 -3.8(14) . . . . ? Ti1 N1 C5 C4 -178.4(8) . . . . ? C1 N1 C5 C7 172.0(9) . . . . ? Ti1 N1 C5 C7 -2.6(10) . . . . ? C3 C4 C5 N1 4.3(17) . . . . ? C3 C4 C5 C7 -170.5(12) . . . . ? Ti1 O3 C6 O4 -171.9(8) . . . . ? Ti1 O3 C6 C1 9.5(11) . . . . ? N1 C1 C6 O4 179.1(10) . . . . ? C2 C1 C6 O4 -1.3(16) . . . . ? N1 C1 C6 O3 -2.2(12) . . . . ? C2 C1 C6 O3 177.4(10) . . . . ? Ti1 O5 C7 O6 -173.6(10) . . . . ? Ti1 O5 C7 C5 1.9(13) . . . . ? N1 C5 C7 O6 176.0(11) . . . . ? C4 C5 C7 O6 -9(2) . . . . ? N1 C5 C7 O5 0.5(14) . . . . ? C4 C5 C7 O5 175.9(11) . . . . ? C12 N2 C8 C9 -1.1(16) . . . . ? Ti1 N2 C8 C9 175.2(8) . . . . ? N2 C8 C9 C10 -1.0(18) . . . . ? C8 C9 C10 C11 0.5(17) . . . . ? C9 C10 C11 C12 1.8(17) . . . . ? C8 N2 C12 C11 3.7(15) . . . . ? Ti1 N2 C12 C11 -173.0(8) . . . . ? C8 N2 C12 C13 -179.8(9) . . . . ? Ti1 N2 C12 C13 3.4(11) . . . . ? C10 C11 C12 N2 -4.0(15) . . . . ? C10 C11 C12 C13 179.7(10) . . . . ? Ti1 O7 C13 O8 167.9(10) . . . . ? Ti1 O7 C13 C12 -12.3(14) . . . . ? N2 C12 C13 O8 -175.5(11) . . . . ? C11 C12 C13 O8 1.0(18) . . . . ? N2 C12 C13 O7 4.7(14) . . . . ? C11 C12 C13 O7 -178.8(10) . . . . ? # END of CIF