Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 #=================================================================== # 0. AUDIT DETAILS _audit_creation_date 2-Jun-05 _audit_creation_method 'PLATON option' _audit_update_record ; 3-Jun-05 Updated by the Author E.H. Text writing by E.H. Checkcif OK 3-Jun-05 Updated by the Author E.H. 8-Jun-05 Updated by the Author E.H. (Autoren etc.) ; _publ_contact_author_name 'Matthias Tamm' _publ_contact_author_address ; Institut fur Anorganische und Analytische Chemie Technische Universitat Braunschweig Braunschweig 38106 GERMANY ; _publ_contact_author_email MATTHIAS.TAMM@TU-BS.DE _publ_section_title ; Imidazolin-2-iminato titanium complexes: Synthesis, structure and use in ethylene polymerization catalysis ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M. C., Polidori, G. & Camalli, M. (1994). SIR92, J. Appl. Cryst. 27, 435-436. Nonius (2001a). Data Collection Software for Nonius Kappa-CCD devices. Nonius BV, Delft, The Netherlands. Nonius (2001b). DENZO Processing Software for Nonius Kappa-CCD devices, Nonius BV, Delft, The Netherlands. Sheldrick, G. M. (1998). SHELXL97, University of Gottingen, Gottingen, Germany. Spek, A. L. (2001). PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _publ_section_table_legends ; ; loop_ _publ_author_name 'Matthias Tamm' 'G. Erker' 'Eberhardt Herdtweck' 'Gerald Kehr' 'Nina Kleigrewe' 'Soren Randoll' ; B.Rieger ; #=================================================================== data_RANJ-4415-123 _database_code_depnum_ccdc_archive 'CCDC 281530' #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C14 H21 Cl2 N3 Ti' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C14 H21 Cl2 N3 Ti' _chemical_formula_weight 350.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 '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' Cl Cl 0.1484 0.1585 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 2/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y,1/2-z -x,-y,-z x,-y,1/2+z 1/2+x,1/2+y,z 1/2-x,1/2+y,1/2-z 1/2-x,1/2-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 17.8609(2) _cell_length_b 8.3732(1) _cell_length_c 23.1179(2) _cell_angle_alpha 90 _cell_angle_beta 97.3494(3) _cell_angle_gamma 90 _cell_volume 3428.95(6) _cell_formula_units_Z 8 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 3354 _cell_measurement_theta_min 1.78 _cell_measurement_theta_max 25.35 _exptl_crystal_description fragment _exptl_crystal_colour red _exptl_crystal_size_max 0.69 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method none _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.608 _exptl_absorpt_correction_T_max 0.732 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 5 s per film repetition 1 dx 50 1139 films measured in 12 data sets set 1 to 12: omega-scans with delta_omega = 1.0 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could not be located in the difference Fourier maps and were calculated in ideal positions (riding model). ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 27779 _diffrn_reflns_av_R_equivalents 0.046 _diffrn_reflns_av_sigmaI/netI 0.0157 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3137 _reflns_number_gt 2883 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0358P)^2^+6.2540P] 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_number_reflns 3137 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0791 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.536 _refine_diff_density_min -0.251 _refine_diff_density_rms 0.048 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ti Ti Uani 0.35638(2) 0.63381(4) 0.10312(1) 1.000 0.0206(1) . . Cl1 Cl Uani 0.33941(3) 0.89845(6) 0.07608(3) 1.000 0.0411(2) . . Cl2 Cl Uani 0.46000(3) 0.66141(7) 0.17380(2) 1.000 0.0362(2) . . N1 N Uani 0.28341(8) 0.58990(17) 0.14558(6) 1.000 0.0204(4) . . N2 N Uani 0.16233(8) 0.47453(18) 0.15769(6) 1.000 0.0211(4) . . N3 N Uani 0.25131(8) 0.46563(17) 0.23198(6) 1.000 0.0200(4) . . C1 C Uani 0.23585(9) 0.5142(2) 0.17552(7) 1.000 0.0189(5) . . C2 C Uani 0.13291(10) 0.4007(2) 0.20362(8) 1.000 0.0251(5) . . C3 C Uani 0.18755(11) 0.3952(2) 0.24920(8) 1.000 0.0250(5) . . C4 C Uani 0.12326(11) 0.5006(2) 0.09837(8) 1.000 0.0270(6) . . C5 C Uani 0.05067(14) 0.5929(3) 0.10071(11) 1.000 0.0476(8) . . C6 C Uani 0.10918(13) 0.3425(3) 0.06709(9) 1.000 0.0374(7) . . C7 C Uani 0.32783(10) 0.4748(2) 0.26525(8) 1.000 0.0234(5) . . C8 C Uani 0.32239(12) 0.4928(3) 0.33001(8) 1.000 0.0360(7) . . C9 C Uani 0.37389(11) 0.3304(2) 0.25170(10) 1.000 0.0331(6) . . C10 C Uani 0.42090(14) 0.5711(4) 0.02244(11) 1.000 0.0503(9) . . C11 C Uani 0.43438(16) 0.4509(4) 0.06126(12) 1.000 0.0588(9) . . C12 C Uani 0.3628(2) 0.3742(3) 0.06703(11) 1.000 0.0663(12) . . C13 C Uani 0.30942(14) 0.4563(3) 0.02798(10) 1.000 0.0421(8) . . C14 C Uani 0.34560(14) 0.5747(3) 0.00164(10) 1.000 0.0451(8) . . H21 H Uiso 0.08300 0.36120 0.20290 1.000 0.0300 calc R H31 H Uiso 0.18330 0.35100 0.28650 1.000 0.0300 calc R H41 H Uiso 0.15690 0.56620 0.07640 1.000 0.0320 calc R H51 H Uiso 0.06190 0.69320 0.12190 1.000 0.0710 calc R H52 H Uiso 0.01600 0.52890 0.12080 1.000 0.0710 calc R H53 H Uiso 0.02720 0.61630 0.06090 1.000 0.0710 calc R H61 H Uiso 0.15670 0.28320 0.06880 1.000 0.0560 calc R H62 H Uiso 0.08900 0.36190 0.02630 1.000 0.0560 calc R H63 H Uiso 0.07270 0.28010 0.08590 1.000 0.0560 calc R H71 H Uiso 0.35320 0.57230 0.25210 1.000 0.0280 calc R H81 H Uiso 0.29050 0.58500 0.33620 1.000 0.0540 calc R H82 H Uiso 0.37300 0.50910 0.35110 1.000 0.0540 calc R H83 H Uiso 0.30020 0.39600 0.34450 1.000 0.0540 calc R H91 H Uiso 0.37530 0.32380 0.20950 1.000 0.0500 calc R H92 H Uiso 0.35070 0.23330 0.26510 1.000 0.0500 calc R H93 H Uiso 0.42540 0.34070 0.27180 1.000 0.0500 calc R H101 H Uiso 0.45790 0.64220 0.01130 1.000 0.0600 calc R H111 H Uiso 0.48220 0.42160 0.08130 1.000 0.0710 calc R H121 H Uiso 0.35400 0.28760 0.09180 1.000 0.0800 calc R H131 H Uiso 0.25690 0.43340 0.02100 1.000 0.0510 calc R H141 H Uiso 0.32220 0.64760 -0.02660 1.000 0.0540 calc R 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 Ti 0.0179(2) 0.0252(2) 0.0194(2) 0.0004(1) 0.0047(1) -0.0004(1) Cl1 0.0384(3) 0.0313(3) 0.0536(4) 0.0149(2) 0.0061(2) -0.0018(2) Cl2 0.0205(2) 0.0544(3) 0.0323(3) 0.0034(2) -0.0015(2) -0.0090(2) N1 0.0192(7) 0.0223(7) 0.0194(7) -0.0007(6) 0.0018(6) -0.0018(6) N2 0.0191(7) 0.0208(7) 0.0231(8) 0.0006(6) 0.0011(6) -0.0028(6) N3 0.0201(7) 0.0192(7) 0.0205(7) 0.0018(6) 0.0014(6) -0.0027(6) C1 0.0189(8) 0.0161(8) 0.0214(9) -0.0014(7) 0.0019(7) -0.0005(7) C2 0.0225(9) 0.0223(9) 0.0314(10) 0.0023(8) 0.0067(8) -0.0059(7) C3 0.0270(9) 0.0215(9) 0.0274(10) 0.0030(7) 0.0071(8) -0.0054(7) C4 0.0245(9) 0.0285(10) 0.0261(10) 0.0044(8) -0.0045(7) -0.0056(8) C5 0.0409(13) 0.0437(13) 0.0521(15) -0.0039(11) -0.0179(11) 0.0113(11) C6 0.0447(12) 0.0388(12) 0.0272(11) -0.0043(9) -0.0011(9) -0.0057(10) C7 0.0210(9) 0.0243(9) 0.0237(9) 0.0029(7) -0.0022(7) -0.0053(7) C8 0.0380(11) 0.0452(13) 0.0231(10) 0.0006(9) -0.0025(8) -0.0095(10) C9 0.0282(10) 0.0294(10) 0.0402(12) 0.0073(9) -0.0011(9) 0.0023(8) C10 0.0437(14) 0.0718(18) 0.0394(13) -0.0073(12) 0.0206(11) 0.0089(13) C11 0.0512(15) 0.0725(19) 0.0503(15) -0.0244(14) -0.0024(12) 0.0364(15) C12 0.141(3) 0.0260(12) 0.0364(14) -0.0087(10) 0.0281(17) 0.0129(15) C13 0.0446(13) 0.0499(14) 0.0332(12) -0.0203(10) 0.0098(10) -0.0066(11) C14 0.0505(14) 0.0618(16) 0.0240(11) -0.0058(10) 0.0081(10) 0.0014(12) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti Cl1 2.3118(6) . . yes Ti Cl2 2.3184(6) . . yes Ti N1 1.7677(15) . . yes Ti C10 2.373(3) . . yes Ti C11 2.360(3) . . yes Ti C12 2.336(3) . . yes Ti C13 2.357(2) . . yes Ti C14 2.381(2) . . yes N1 C1 1.324(2) . . yes N2 C1 1.366(2) . . yes N2 C2 1.389(2) . . yes N2 C4 1.473(2) . . yes N3 C1 1.361(2) . . yes N3 C3 1.385(2) . . yes N3 C7 1.482(2) . . yes C2 C3 1.342(3) . . no C4 C5 1.516(3) . . no C4 C6 1.514(3) . . no C7 C8 1.520(3) . . no C7 C9 1.517(2) . . no C10 C11 1.349(4) . . no C10 C14 1.369(4) . . no C11 C12 1.452(5) . . no C12 C13 1.406(4) . . no C13 C14 1.368(3) . . no C2 H21 0.9490 . . no C3 H31 0.9503 . . no C4 H41 0.9994 . . no C5 H51 0.9800 . . no C5 H52 0.9797 . . no C5 H53 0.9810 . . no C6 H61 0.9797 . . no C6 H62 0.9791 . . no C6 H63 0.9793 . . no C7 H71 0.9997 . . no C8 H81 0.9807 . . no C8 H82 0.9801 . . no C8 H83 0.9799 . . no C9 H91 0.9807 . . no C9 H92 0.9805 . . no C9 H93 0.9800 . . no C10 H101 0.9492 . . no C11 H111 0.9503 . . no C12 H121 0.9494 . . no C13 H131 0.9508 . . no C14 H141 0.9506 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ti Cl2 99.22(2) . . . yes Cl1 Ti N1 105.61(5) . . . yes Cl1 Ti C10 93.42(8) . . . yes Cl1 Ti C11 125.11(8) . . . yes Cl1 Ti C12 143.70(7) . . . yes Cl1 Ti C13 112.53(6) . . . yes Cl1 Ti C14 86.65(6) . . . yes Cl2 Ti N1 102.02(5) . . . yes Cl2 Ti C10 98.73(6) . . . yes Cl2 Ti C11 83.90(7) . . . yes Cl2 Ti C12 105.85(8) . . . yes Cl2 Ti C13 139.37(6) . . . yes Cl2 Ti C14 132.20(6) . . . yes N1 Ti C10 148.98(9) . . . yes N1 Ti C11 127.49(9) . . . yes N1 Ti C12 94.48(9) . . . yes N1 Ti C13 93.44(8) . . . yes N1 Ti C14 122.10(8) . . . yes C10 Ti C11 33.13(10) . . . yes C10 Ti C12 57.49(11) . . . yes C10 Ti C13 56.23(9) . . . yes C10 Ti C14 33.48(9) . . . yes C11 Ti C12 36.02(11) . . . yes C11 Ti C13 57.43(9) . . . yes C11 Ti C14 55.85(9) . . . yes C12 Ti C13 34.85(9) . . . yes C12 Ti C14 57.06(9) . . . yes C13 Ti C14 33.56(8) . . . yes Ti N1 C1 163.30(13) . . . yes C1 N2 C2 108.70(14) . . . yes C1 N2 C4 124.57(14) . . . yes C2 N2 C4 126.67(15) . . . yes C1 N3 C3 109.23(14) . . . yes C1 N3 C7 122.86(14) . . . yes C3 N3 C7 127.61(14) . . . yes N1 C1 N2 127.95(15) . . . yes N1 C1 N3 125.40(15) . . . yes N2 C1 N3 106.61(14) . . . yes N2 C2 C3 107.89(16) . . . yes N3 C3 C2 107.56(16) . . . yes N2 C4 C5 110.35(16) . . . yes N2 C4 C6 110.18(15) . . . yes C5 C4 C6 111.85(18) . . . no N3 C7 C8 110.20(15) . . . yes N3 C7 C9 109.87(15) . . . yes C8 C7 C9 112.76(17) . . . no Ti C10 C11 72.88(16) . . . yes Ti C10 C14 73.58(15) . . . yes C11 C10 C14 109.5(3) . . . no Ti C11 C10 73.99(18) . . . yes Ti C11 C12 71.12(16) . . . yes C10 C11 C12 107.9(2) . . . no Ti C12 C11 72.86(16) . . . yes Ti C12 C13 73.39(15) . . . yes C11 C12 C13 104.9(2) . . . no Ti C13 C12 71.76(14) . . . yes Ti C13 C14 74.18(14) . . . yes C12 C13 C14 108.7(2) . . . no Ti C14 C10 72.94(14) . . . yes Ti C14 C13 72.27(14) . . . yes C10 C14 C13 109.0(2) . . . no N2 C2 H21 126.03 . . . no C3 C2 H21 126.07 . . . no N3 C3 H31 126.20 . . . no C2 C3 H31 126.24 . . . no N2 C4 H41 108.09 . . . no C5 C4 H41 108.08 . . . no C6 C4 H41 108.17 . . . no C4 C5 H51 109.47 . . . no C4 C5 H52 109.47 . . . no C4 C5 H53 109.45 . . . no H51 C5 H52 109.46 . . . no H51 C5 H53 109.47 . . . no H52 C5 H53 109.50 . . . no C4 C6 H61 109.50 . . . no C4 C6 H62 109.46 . . . no C4 C6 H63 109.49 . . . no H61 C6 H62 109.47 . . . no H61 C6 H63 109.50 . . . no H62 C6 H63 109.41 . . . no N3 C7 H71 107.95 . . . no C8 C7 H71 107.88 . . . no C9 C7 H71 108.01 . . . no C7 C8 H81 109.47 . . . no C7 C8 H82 109.43 . . . no C7 C8 H83 109.53 . . . no H81 C8 H82 109.49 . . . no H81 C8 H83 109.48 . . . no H82 C8 H83 109.44 . . . no C7 C9 H91 109.50 . . . no C7 C9 H92 109.47 . . . no C7 C9 H93 109.44 . . . no H91 C9 H92 109.46 . . . no H91 C9 H93 109.55 . . . no H92 C9 H93 109.39 . . . no Ti C10 H101 119.96 . . . no C11 C10 H101 125.24 . . . no C14 C10 H101 125.27 . . . no Ti C11 H111 120.57 . . . no C10 C11 H111 126.12 . . . no C12 C11 H111 126.02 . . . no Ti C12 H121 118.41 . . . no C11 C12 H121 127.51 . . . no C13 C12 H121 127.57 . . . no Ti C13 H131 120.17 . . . no C12 C13 H131 125.71 . . . no C14 C13 H131 125.63 . . . no Ti C14 H141 121.08 . . . no C10 C14 H141 125.52 . . . no C13 C14 H141 125.43 . . . no #===END # CIF-file generated for RANH 4385-123 # Compound 3c #=================================================================== data_RANH-4385-123 _database_code_depnum_ccdc_archive 'CCDC 281531' #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C16 H25 Cl2 N3 Ti' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C16 H25 Cl2 N3 Ti' _chemical_formula_weight 378.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 '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' Cl Cl 0.1484 0.1585 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,y,1/2-z 1/2-x,1/2+y,z x,1/2-y,1/2+z _cell_length_a 18.0659(2) _cell_length_b 11.2730(1) _cell_length_c 18.2918(2) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3725.25(7) _cell_formula_units_Z 8 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 3812 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 25.33 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.66 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method none _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 0.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.732 _exptl_absorpt_correction_T_max 0.845 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 22.5 s per film repetition 1 dx 40 363 films measured in 1 data set set 1: phi-scan with delta_phi = 1.0 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could not be located in the difference Fourier maps and were calculated in ideal positions (riding model). ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 27369 _diffrn_reflns_av_R_equivalents 0.032 _diffrn_reflns_av_sigmaI/netI 0.0205 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.33 _reflns_number_total 3398 _reflns_number_gt 3003 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0318P)^2^+4.2188P] 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_number_reflns 3398 _refine_ls_number_parameters 205 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0848 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.432 _refine_diff_density_min -0.438 _refine_diff_density_rms 0.050 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ti Ti Uani 0.09309(2) 0.35901(3) 0.16591(2) 1.000 0.0226(1) . . Cl1 Cl Uani 0.03400(3) 0.53854(5) 0.14540(4) 1.000 0.0504(2) . . Cl2 Cl Uani 0.10357(4) 0.34877(7) 0.29122(3) 1.000 0.0501(2) . . N1 N Uani 0.18466(9) 0.38734(14) 0.13766(8) 1.000 0.0221(5) . . N2 N Uani 0.25787(9) 0.43349(14) 0.03198(8) 1.000 0.0195(5) . . N3 N Uani 0.31561(9) 0.35753(14) 0.12610(8) 1.000 0.0192(4) . . C1 C Uani 0.24800(11) 0.39109(16) 0.10128(9) 1.000 0.0187(5) . . C2 C Uani 0.33309(11) 0.42714(17) 0.01413(10) 1.000 0.0211(5) . . C3 C Uani 0.36838(11) 0.38028(16) 0.07235(10) 1.000 0.0203(5) . . C4 C Uani 0.19572(12) 0.48421(19) -0.01035(11) 1.000 0.0269(6) . . C5 C Uani 0.36474(13) 0.4659(2) -0.05759(11) 1.000 0.0335(7) . . C6 C Uani 0.44887(11) 0.35804(19) 0.08411(12) 1.000 0.0284(6) . . C7 C Uani 0.33117(12) 0.30650(19) 0.19941(10) 1.000 0.0267(6) . . C8 C Uani 0.18023(14) 0.4149(2) -0.08001(12) 1.000 0.0379(8) . . C9 C Uani 0.20653(14) 0.6162(2) -0.02303(13) 1.000 0.0381(8) . . C10 C Uani 0.29296(13) 0.1887(2) 0.21011(12) 1.000 0.0345(7) . . C11 C Uani 0.31310(14) 0.3963(2) 0.25882(11) 1.000 0.0367(7) . . C12 C Uani 0.08037(16) 0.2216(2) 0.07090(16) 1.000 0.0515(9) . . C13 C Uani 0.0881(2) 0.1588(2) 0.1341(2) 1.000 0.0692(15) . . C14 C Uani 0.0237(3) 0.1809(3) 0.17554(17) 1.000 0.0882(16) . . C15 C Uani -0.01826(16) 0.2577(4) 0.1370(2) 1.000 0.0755(15) . . C16 C Uani 0.01590(19) 0.2828(3) 0.07349(18) 1.000 0.0627(11) . . H41 H Uiso 0.15060 0.47600 0.02100 1.000 0.0320 calc R H51 H Uiso 0.41780 0.44810 -0.05880 1.000 0.0500 calc R H52 H Uiso 0.35730 0.55150 -0.06360 1.000 0.0500 calc R H53 H Uiso 0.33980 0.42360 -0.09740 1.000 0.0500 calc R H61 H Uiso 0.46640 0.40580 0.12540 1.000 0.0430 calc R H62 H Uiso 0.47640 0.37990 0.03990 1.000 0.0430 calc R H63 H Uiso 0.45680 0.27380 0.09470 1.000 0.0430 calc R H71 H Uiso 0.38560 0.29130 0.20190 1.000 0.0320 calc R H81 H Uiso 0.13290 0.44070 -0.10080 1.000 0.0570 calc R H82 H Uiso 0.17780 0.33000 -0.06870 1.000 0.0570 calc R H83 H Uiso 0.22000 0.42940 -0.11540 1.000 0.0570 calc R H91 H Uiso 0.24640 0.62840 -0.05850 1.000 0.0570 calc R H92 H Uiso 0.21950 0.65470 0.02320 1.000 0.0570 calc R H93 H Uiso 0.16060 0.65060 -0.04200 1.000 0.0570 calc R H101 H Uiso 0.23940 0.20130 0.21400 1.000 0.0520 calc R H102 H Uiso 0.31120 0.15130 0.25500 1.000 0.0520 calc R H103 H Uiso 0.30340 0.13700 0.16830 1.000 0.0520 calc R H111 H Uiso 0.32330 0.36140 0.30690 1.000 0.0550 calc R H112 H Uiso 0.26070 0.41810 0.25580 1.000 0.0550 calc R H113 H Uiso 0.34370 0.46730 0.25210 1.000 0.0550 calc R H121 H Uiso 0.11460 0.22240 0.03150 1.000 0.0620 calc R H131 H Uiso 0.12880 0.11000 0.14760 1.000 0.0830 calc R H141 H Uiso 0.01200 0.14790 0.22190 1.000 0.1060 calc R H151 H Uiso -0.06450 0.28910 0.15230 1.000 0.0900 calc R H161 H Uiso -0.00220 0.33470 0.03670 1.000 0.0750 calc R 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 Ti 0.0198(2) 0.0238(2) 0.0242(2) -0.0081(1) 0.0038(1) -0.0010(2) Cl1 0.0333(3) 0.0322(3) 0.0858(5) -0.0085(3) 0.0005(3) 0.0107(3) Cl2 0.0449(4) 0.0820(5) 0.0233(3) -0.0144(3) 0.0111(2) -0.0178(3) N1 0.0231(9) 0.0240(8) 0.0193(8) -0.0018(7) 0.0005(7) 0.0016(7) N2 0.0215(8) 0.0210(8) 0.0161(8) 0.0005(6) -0.0008(6) 0.0023(7) N3 0.0204(8) 0.0223(8) 0.0149(7) 0.0001(6) 0.0005(6) 0.0006(7) C1 0.0216(9) 0.0179(9) 0.0166(9) -0.0023(7) -0.0001(8) 0.0012(8) C2 0.0247(10) 0.0187(9) 0.0199(9) -0.0019(7) 0.0040(8) -0.0003(8) C3 0.0212(10) 0.0189(9) 0.0208(9) -0.0040(7) 0.0031(8) -0.0004(8) C4 0.0294(11) 0.0288(11) 0.0226(10) 0.0007(8) -0.0064(8) 0.0062(9) C5 0.0388(12) 0.0366(12) 0.0250(11) 0.0063(9) 0.0108(9) 0.0012(10) C6 0.0210(10) 0.0319(11) 0.0324(11) -0.0020(9) 0.0011(9) 0.0016(9) C7 0.0271(11) 0.0358(11) 0.0171(9) 0.0041(8) -0.0019(8) 0.0056(9) C8 0.0502(15) 0.0343(12) 0.0291(12) -0.0019(10) -0.0166(10) 0.0016(11) C9 0.0519(15) 0.0273(12) 0.0350(12) 0.0005(9) -0.0123(11) 0.0103(11) C10 0.0420(13) 0.0332(12) 0.0283(11) 0.0109(9) 0.0018(10) 0.0090(11) C11 0.0470(14) 0.0463(14) 0.0169(10) -0.0040(10) -0.0060(9) 0.0057(12) C12 0.0554(17) 0.0490(16) 0.0500(16) -0.0345(14) 0.0155(13) -0.0212(14) C13 0.089(3) 0.0227(13) 0.096(3) -0.0171(15) -0.047(2) 0.0051(15) C14 0.164(4) 0.065(2) 0.0356(16) -0.0088(15) 0.013(2) -0.083(3) C15 0.0346(15) 0.089(3) 0.103(3) -0.059(2) 0.0157(17) -0.0275(17) C16 0.080(2) 0.0441(16) 0.064(2) -0.0203(14) -0.0413(18) 0.0027(16) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti Cl1 2.3187(7) . . yes Ti Cl2 2.3028(7) . . yes Ti N1 1.7623(17) . . yes Ti C12 2.339(3) . . yes Ti C13 2.333(2) . . yes Ti C14 2.374(4) . . yes Ti C15 2.373(3) . . yes Ti C16 2.354(3) . . yes N1 C1 1.324(2) . . yes N2 C1 1.366(2) . . yes N2 C2 1.399(3) . . yes N2 C4 1.479(3) . . yes N3 C1 1.357(3) . . yes N3 C3 1.393(2) . . yes N3 C7 1.486(2) . . yes C2 C3 1.349(3) . . no C2 C5 1.496(3) . . no C3 C6 1.491(3) . . no C4 C8 1.521(3) . . no C4 C9 1.519(3) . . no C7 C10 1.509(3) . . no C7 C11 1.521(3) . . no C12 C13 1.363(4) . . no C12 C16 1.355(4) . . no C13 C14 1.411(6) . . no C14 C15 1.350(6) . . no C15 C16 1.346(5) . . no C4 H41 1.0009 . . no C5 H51 0.9796 . . no C5 H52 0.9805 . . no C5 H53 0.9801 . . no C6 H61 0.9801 . . no C6 H62 0.9808 . . no C6 H63 0.9797 . . no C7 H71 0.9992 . . no C8 H81 0.9800 . . no C8 H82 0.9802 . . no C8 H83 0.9808 . . no C9 H91 0.9791 . . no C9 H92 0.9790 . . no C9 H93 0.9794 . . no C10 H101 0.9806 . . no C10 H102 0.9801 . . no C10 H103 0.9799 . . no C11 H111 0.9809 . . no C11 H112 0.9796 . . no C11 H113 0.9805 . . no C12 H121 0.9497 . . no C13 H131 0.9509 . . no C14 H141 0.9498 . . no C15 H151 0.9495 . . no C16 H161 0.9498 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ti Cl2 104.04(3) . . . yes Cl1 Ti N1 103.09(6) . . . yes Cl1 Ti C12 114.36(7) . . . yes Cl1 Ti C13 141.85(9) . . . yes Cl1 Ti C14 120.48(12) . . . yes Cl1 Ti C15 89.64(10) . . . yes Cl1 Ti C16 85.96(8) . . . yes Cl2 Ti N1 102.93(5) . . . yes Cl2 Ti C12 135.59(7) . . . yes Cl2 Ti C13 101.71(9) . . . yes Cl2 Ti C14 85.82(8) . . . yes Cl2 Ti C15 105.51(9) . . . yes Cl2 Ti C16 138.18(9) . . . yes N1 Ti C12 89.68(9) . . . yes N1 Ti C13 97.96(10) . . . yes N1 Ti C14 132.13(13) . . . yes N1 Ti C15 144.85(10) . . . yes N1 Ti C16 114.31(10) . . . yes C12 Ti C13 33.92(11) . . . yes C12 Ti C14 56.16(10) . . . yes C12 Ti C15 55.42(11) . . . yes C12 Ti C16 33.55(11) . . . yes C13 Ti C14 34.87(14) . . . yes C13 Ti C15 56.35(13) . . . yes C13 Ti C16 56.27(12) . . . yes C14 Ti C15 33.04(15) . . . yes C14 Ti C16 55.37(12) . . . yes C15 Ti C16 33.07(12) . . . yes Ti N1 C1 164.62(14) . . . yes C1 N2 C2 108.98(15) . . . yes C1 N2 C4 121.46(16) . . . yes C2 N2 C4 129.41(15) . . . yes C1 N3 C3 109.18(15) . . . yes C1 N3 C7 125.46(16) . . . yes C3 N3 C7 125.35(16) . . . yes N1 C1 N2 126.16(17) . . . yes N1 C1 N3 126.92(16) . . . yes N2 C1 N3 106.89(16) . . . yes N2 C2 C3 107.14(16) . . . yes N2 C2 C5 124.10(17) . . . yes C3 C2 C5 128.75(19) . . . no N3 C3 C2 107.81(17) . . . yes N3 C3 C6 122.31(17) . . . yes C2 C3 C6 129.84(18) . . . no N2 C4 C8 112.32(17) . . . yes N2 C4 C9 111.17(18) . . . yes C8 C4 C9 113.52(18) . . . no N3 C7 C10 111.78(16) . . . yes N3 C7 C11 110.28(17) . . . yes C10 C7 C11 113.26(17) . . . no Ti C12 C13 72.77(16) . . . yes Ti C12 C16 73.81(18) . . . yes C13 C12 C16 108.8(3) . . . no Ti C13 C12 73.32(14) . . . yes Ti C13 C14 74.15(18) . . . yes C12 C13 C14 106.2(3) . . . no Ti C14 C13 71.0(2) . . . yes Ti C14 C15 73.5(2) . . . yes C13 C14 C15 107.2(3) . . . no Ti C15 C14 73.5(2) . . . yes Ti C15 C16 72.7(2) . . . yes C14 C15 C16 109.2(3) . . . no Ti C16 C12 72.64(18) . . . yes Ti C16 C15 74.2(2) . . . yes C12 C16 C15 108.5(3) . . . no N2 C4 H41 106.41 . . . no C8 C4 H41 106.42 . . . no C9 C4 H41 106.43 . . . no C2 C5 H51 109.51 . . . no C2 C5 H52 109.47 . . . no C2 C5 H53 109.49 . . . no H51 C5 H52 109.46 . . . no H51 C5 H53 109.47 . . . no H52 C5 H53 109.42 . . . no C3 C6 H61 109.51 . . . no C3 C6 H62 109.47 . . . no C3 C6 H63 109.52 . . . no H61 C6 H62 109.48 . . . no H61 C6 H63 109.44 . . . no H62 C6 H63 109.41 . . . no N3 C7 H71 107.08 . . . no C10 C7 H71 107.05 . . . no C11 C7 H71 107.03 . . . no C4 C8 H81 109.47 . . . no C4 C8 H82 109.46 . . . no C4 C8 H83 109.43 . . . no H81 C8 H82 109.43 . . . no H81 C8 H83 109.49 . . . no H82 C8 H83 109.56 . . . no C4 C9 H91 109.48 . . . no C4 C9 H92 109.47 . . . no C4 C9 H93 109.46 . . . no H91 C9 H92 109.51 . . . no H91 C9 H93 109.44 . . . no H92 C9 H93 109.47 . . . no C7 C10 H101 109.47 . . . no C7 C10 H102 109.47 . . . no C7 C10 H103 109.52 . . . no H101 C10 H102 109.47 . . . no H101 C10 H103 109.43 . . . no H102 C10 H103 109.47 . . . no C7 C11 H111 109.48 . . . no C7 C11 H112 109.52 . . . no C7 C11 H113 109.44 . . . no H111 C11 H112 109.43 . . . no H111 C11 H113 109.51 . . . no H112 C11 H113 109.45 . . . no Ti C12 H121 119.57 . . . no C13 C12 H121 125.59 . . . no C16 C12 H121 125.56 . . . no Ti C13 H131 117.72 . . . no C12 C13 H131 126.87 . . . no C14 C13 H131 126.89 . . . no Ti C14 H141 121.00 . . . no C13 C14 H141 126.45 . . . no C15 C14 H141 126.35 . . . no Ti C15 H151 120.05 . . . no C14 C15 H151 125.41 . . . no C16 C15 H151 125.42 . . . no Ti C16 H161 119.21 . . . no C12 C16 H161 125.80 . . . no C15 C16 H161 125.69 . . . no #===END # CIF-file generated for SRAN4 1-173 # Compound 3e #=================================================================== data_SRAN4-1-173 _database_code_depnum_ccdc_archive 'CCDC 281532' #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C32 H41 Cl2 N3 Ti, C7 H8' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C39 H49 Cl2 N3 Ti' _chemical_formula_weight 678.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 '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' Cl Cl 0.1484 0.1585 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 12.8096(1) _cell_length_b 18.5630(2) _cell_length_c 15.5127(2) _cell_angle_alpha 90 _cell_angle_beta 90.8894(5) _cell_angle_gamma 90 _cell_volume 3688.24(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 6973 _cell_measurement_theta_min 1.71 _cell_measurement_theta_max 25.33 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 1.07 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method none _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.699 _exptl_absorpt_correction_T_max 0.837 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 28.5 s per film repetition 1 dx 40 536 films measured in 9 data set set 1: phi-scan with delta_phi = 1.90 set 2 to 9: omega-scans with delta_omega = 1.90 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could be located in the difference Fourier maps and were allowed to refine freely. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 79233 _diffrn_reflns_av_R_equivalents 0.057 _diffrn_reflns_av_sigmaI/netI 0.0235 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.33 _reflns_number_total 6736 _reflns_number_gt 5898 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0309P)^2^+2.4823P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_number_reflns 6736 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.0934 _refine_ls_wR_factor_gt 0.0896 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.297 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.040 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ti Ti Uani 0.26755(3) 0.19865(2) 0.18365(2) 1.000 0.0259(1) . . Cl1 Cl Uani 0.17070(6) 0.17240(3) 0.30394(4) 1.000 0.0539(2) . . Cl2 Cl Uani 0.43106(5) 0.16454(3) 0.23100(5) 1.000 0.0582(2) . . N1 N Uani 0.27299(12) 0.29436(8) 0.18191(10) 1.000 0.0233(5) . . N2 N Uani 0.20299(12) 0.41241(8) 0.14951(10) 1.000 0.0221(5) . . N3 N Uani 0.36438(11) 0.40544(8) 0.19543(9) 1.000 0.0198(5) . . C1 C Uani 0.27895(14) 0.36452(10) 0.17476(11) 1.000 0.0195(5) . . C2 C Uani 0.24168(16) 0.48239(10) 0.15643(13) 1.000 0.0261(6) . . C3 C Uani 0.34032(15) 0.47796(10) 0.18463(12) 1.000 0.0245(6) . . C4 C Uani 0.10046(14) 0.39149(10) 0.11745(12) 1.000 0.0244(6) . . C5 C Uani 0.02644(15) 0.36958(11) 0.17770(13) 1.000 0.0282(6) . . C6 C Uani -0.06974(17) 0.34699(12) 0.14445(15) 1.000 0.0366(7) . . C7 C Uani -0.09006(17) 0.34696(13) 0.05700(16) 1.000 0.0407(8) . . C8 C Uani -0.01681(17) 0.37094(13) -0.00038(15) 1.000 0.0370(8) . . C9 C Uani 0.08134(16) 0.39430(11) 0.02823(13) 1.000 0.0294(6) . . C10 C Uani 0.04820(17) 0.37459(12) 0.27440(14) 1.000 0.0337(7) . . C11 C Uani -0.0196(2) 0.32508(18) 0.32833(19) 1.000 0.0534(10) . . C12 C Uani 0.0362(3) 0.45225(16) 0.30438(18) 1.000 0.0510(10) . . C13 C Uani 0.16336(18) 0.42037(13) -0.03463(14) 1.000 0.0358(7) . . C14 C Uani 0.1178(2) 0.45302(17) -0.11738(18) 1.000 0.0516(9) . . C15 C Uani 0.2414(2) 0.36162(17) -0.05438(19) 1.000 0.0544(10) . . C16 C Uani 0.46253(14) 0.37539(10) 0.22523(12) 1.000 0.0213(5) . . C17 C Uani 0.53974(15) 0.36205(11) 0.16447(13) 1.000 0.0273(6) . . C18 C Uani 0.63322(17) 0.33290(12) 0.19529(16) 1.000 0.0372(7) . . C19 C Uani 0.64783(18) 0.31738(13) 0.28150(16) 1.000 0.0421(8) . . C20 C Uani 0.57004(18) 0.33093(13) 0.33919(15) 1.000 0.0382(8) . . C21 C Uani 0.47499(15) 0.36058(11) 0.31281(12) 1.000 0.0266(6) . . C22 C Uani 0.52463(18) 0.37742(13) 0.06906(14) 1.000 0.0374(8) . . C23 C Uani 0.6018(3) 0.43433(19) 0.0384(2) 1.000 0.0584(11) . . C24 C Uani 0.5331(3) 0.30826(19) 0.0163(2) 1.000 0.0609(11) . . C25 C Uani 0.39160(17) 0.37691(12) 0.37856(13) 1.000 0.0333(7) . . C26 C Uani 0.4311(2) 0.43311(15) 0.44297(17) 1.000 0.0440(9) . . C27 C Uani 0.3579(3) 0.30883(17) 0.4254(2) 1.000 0.0566(10) . . C28 C Uani 0.2667(2) 0.18398(14) 0.03378(15) 1.000 0.0440(8) . . C29 C Uani 0.1638(2) 0.19453(14) 0.05874(15) 1.000 0.0428(8) . . C30 C Uani 0.1360(2) 0.13369(16) 0.10723(17) 1.000 0.0516(9) . . C31 C Uani 0.2216(2) 0.08735(14) 0.11136(17) 1.000 0.0511(9) . . C32 C Uani 0.3014(2) 0.11830(14) 0.06606(17) 1.000 0.0494(9) . . C33 C Uani 0.6253(3) 0.0750(3) 0.0577(3) 1.000 0.0818(14) . . C34 C Uani 0.71517(19) 0.07978(15) 0.12176(16) 1.000 0.0474(9) . . C35 C Uani 0.7689(2) 0.01898(15) 0.1470(2) 1.000 0.0555(10) . . C36 C Uani 0.8520(2) 0.02357(18) 0.2044(2) 1.000 0.0616(11) . . C37 C Uani 0.8834(2) 0.08883(19) 0.2360(2) 1.000 0.0609(11) . . C38 C Uani 0.8303(3) 0.14897(18) 0.2115(2) 1.000 0.0749(14) . . C39 C Uani 0.7469(3) 0.14397(17) 0.1553(2) 1.000 0.0664(11) . . H10 H Uiso 0.1174(17) 0.3601(11) 0.2840(12) 1.000 0.025(5) . . H18 H Uiso -0.0318(17) 0.3718(12) -0.0576(15) 1.000 0.034(6) . . H21 H Uiso 0.1974(15) 0.5217(11) 0.1420(12) 1.000 0.022(5) . . H22 H Uiso 0.4570(17) 0.3962(11) 0.0600(13) 1.000 0.030(6) . . H31 H Uiso 0.3903(15) 0.5143(11) 0.1974(12) 1.000 0.023(5) . . H61 H Uiso -0.1230(18) 0.3323(12) 0.1847(15) 1.000 0.038(6) . . H71 H Uiso -0.154(2) 0.3303(13) 0.0345(15) 1.000 0.045(7) . . H111 H Uiso 0.005(2) 0.3266(14) 0.3905(19) 1.000 0.061(8) . . H112 H Uiso -0.016(2) 0.2765(17) 0.3087(18) 1.000 0.065(9) . . H113 H Uiso -0.091(3) 0.3395(16) 0.3278(19) 1.000 0.071(9) . . H121 H Uiso 0.050(2) 0.4550(14) 0.3675(19) 1.000 0.059(8) . . H122 H Uiso -0.035(2) 0.4636(15) 0.2961(18) 1.000 0.063(9) . . H123 H Uiso 0.081(2) 0.4865(16) 0.2744(19) 1.000 0.068(9) . . H131 H Uiso 0.1983(18) 0.4600(13) -0.0088(15) 1.000 0.041(6) . . H141 H Uiso 0.065(2) 0.4911(16) -0.1022(18) 1.000 0.070(9) . . H142 H Uiso 0.089(2) 0.4079(18) -0.155(2) 1.000 0.086(10) . . H143 H Uiso 0.174(2) 0.4745(14) -0.1503(17) 1.000 0.056(8) . . H151 H Uiso 0.297(3) 0.3794(17) -0.099(2) 1.000 0.088(10) . . H152 H Uiso 0.1876(17) 0.3300(11) -0.0957(14) 1.000 0.029(5) . . H153 H Uiso 0.277(2) 0.3427(17) 0.004(2) 1.000 0.083(10) . . H181 H Uiso 0.6858(18) 0.3244(12) 0.1574(15) 1.000 0.036(6) . . H191 H Uiso 0.708(2) 0.2981(13) 0.2985(16) 1.000 0.048(7) . . H201 H Uiso 0.5814(18) 0.3199(12) 0.3998(16) 1.000 0.042(6) . . H231 H Uiso 0.590(2) 0.4429(16) -0.021(2) 1.000 0.070(9) . . H232 H Uiso 0.669(3) 0.4157(17) 0.042(2) 1.000 0.077(10) . . H233 H Uiso 0.593(2) 0.4779(18) 0.071(2) 1.000 0.073(10) . . H241 H Uiso 0.516(2) 0.3167(16) -0.039(2) 1.000 0.074(10) . . H242 H Uiso 0.485(2) 0.2697(17) 0.037(2) 1.000 0.074(9) . . H243 H Uiso 0.606(2) 0.2906(15) 0.0206(17) 1.000 0.061(8) . . H251 H Uiso 0.3313(18) 0.3970(12) 0.3483(14) 1.000 0.037(6) . . H261 H Uiso 0.3756(19) 0.4449(12) 0.4813(15) 1.000 0.041(6) . . H262 H Uiso 0.4543(19) 0.4757(15) 0.4148(16) 1.000 0.050(7) . . H263 H Uiso 0.489(2) 0.4133(15) 0.4746(18) 1.000 0.062(8) . . H271 H Uiso 0.304(2) 0.3188(15) 0.4649(19) 1.000 0.063(8) . . H272 H Uiso 0.422(3) 0.2906(18) 0.464(2) 1.000 0.089(11) . . H273 H Uiso 0.337(2) 0.2737(18) 0.392(2) 1.000 0.076(10) . . H281 H Uiso 0.304(2) 0.2145(15) 0.0031(17) 1.000 0.056(8) . . H291 H Uiso 0.121(2) 0.2333(14) 0.0473(16) 1.000 0.053(8) . . H301 H Uiso 0.076(2) 0.1320(15) 0.1311(18) 1.000 0.063(9) . . H311 H Uiso 0.223(2) 0.0449(17) 0.143(2) 1.000 0.077(10) . . H321 H Uiso 0.368(2) 0.0984(16) 0.0588(18) 1.000 0.068(9) . . H331 H Uiso 0.613(4) 0.030(3) 0.039(4) 1.000 0.18(3) . . H332 H Uiso 0.639(4) 0.108(3) 0.010(3) 1.000 0.16(2) . . H333 H Uiso 0.574(4) 0.105(3) 0.080(3) 1.000 0.15(2) . . H351 H Uiso 0.748(2) -0.0277(17) 0.1240(19) 1.000 0.071(9) . . H361 H Uiso 0.886(2) -0.0163(17) 0.2212(19) 1.000 0.075(10) . . H371 H Uiso 0.939(2) 0.0922(16) 0.276(2) 1.000 0.074(10) . . H381 H Uiso 0.851(3) 0.192(2) 0.231(2) 1.000 0.108(13) . . H391 H Uiso 0.712(3) 0.1821(19) 0.140(2) 1.000 0.086(11) . . 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 Ti 0.0320(2) 0.0186(2) 0.0270(2) -0.0001(1) -0.0046(2) -0.0014(2) Cl1 0.0864(5) 0.0370(3) 0.0387(3) 0.0006(3) 0.0185(3) -0.0160(3) Cl2 0.0536(4) 0.0418(3) 0.0783(5) -0.0110(3) -0.0322(3) 0.0187(3) N1 0.0218(8) 0.0218(8) 0.0263(8) -0.0001(7) -0.0032(6) -0.0004(7) N2 0.0201(8) 0.0208(8) 0.0254(8) 0.0010(6) -0.0019(7) 0.0009(6) N3 0.0193(8) 0.0199(8) 0.0202(8) 0.0010(6) -0.0008(6) -0.0013(6) C1 0.0195(9) 0.0243(10) 0.0148(9) -0.0012(7) 0.0001(7) 0.0004(8) C2 0.0278(11) 0.0200(10) 0.0305(11) 0.0025(8) -0.0018(9) 0.0021(8) C3 0.0286(11) 0.0185(10) 0.0263(10) 0.0009(8) 0.0011(8) -0.0026(8) C4 0.0190(10) 0.0221(10) 0.0319(11) -0.0012(8) -0.0046(8) 0.0025(8) C5 0.0247(10) 0.0256(10) 0.0344(11) 0.0013(9) -0.0010(9) 0.0028(8) C6 0.0245(11) 0.0403(13) 0.0450(14) 0.0019(10) 0.0006(10) -0.0028(10) C7 0.0232(11) 0.0476(14) 0.0510(15) -0.0087(11) -0.0103(11) -0.0016(10) C8 0.0336(12) 0.0445(14) 0.0325(13) -0.0048(10) -0.0084(10) 0.0029(10) C9 0.0270(11) 0.0298(11) 0.0311(11) -0.0015(9) -0.0045(9) 0.0050(9) C10 0.0248(11) 0.0432(13) 0.0332(12) 0.0056(10) 0.0002(9) 0.0019(10) C11 0.0531(18) 0.065(2) 0.0424(16) 0.0126(14) 0.0073(13) -0.0103(15) C12 0.065(2) 0.0526(17) 0.0353(15) -0.0060(12) 0.0022(13) -0.0010(15) C13 0.0360(12) 0.0425(13) 0.0289(11) 0.0012(10) -0.0031(10) -0.0018(10) C14 0.0559(17) 0.0551(17) 0.0439(15) 0.0149(13) 0.0015(13) 0.0050(15) C15 0.0499(16) 0.0657(19) 0.0477(16) 0.0114(14) 0.0086(14) 0.0140(14) C16 0.0200(9) 0.0186(9) 0.0253(10) -0.0010(7) -0.0034(8) -0.0012(7) C17 0.0241(10) 0.0266(10) 0.0312(11) -0.0015(8) 0.0019(8) -0.0024(8) C18 0.0239(11) 0.0396(13) 0.0482(14) -0.0015(11) 0.0070(10) 0.0049(9) C19 0.0268(12) 0.0491(15) 0.0502(15) 0.0050(11) -0.0102(11) 0.0110(11) C20 0.0373(13) 0.0450(14) 0.0319(12) 0.0049(10) -0.0107(10) 0.0060(10) C21 0.0259(10) 0.0266(10) 0.0272(10) -0.0010(8) -0.0042(8) -0.0001(8) C22 0.0294(12) 0.0528(15) 0.0302(12) 0.0018(10) 0.0077(9) 0.0039(11) C23 0.0545(19) 0.064(2) 0.0572(19) 0.0243(16) 0.0138(15) -0.0001(15) C24 0.075(2) 0.072(2) 0.0361(16) -0.0122(14) 0.0102(15) -0.0041(18) C25 0.0346(12) 0.0422(13) 0.0231(10) 0.0003(9) -0.0025(9) 0.0048(10) C26 0.0504(16) 0.0425(15) 0.0390(14) -0.0061(12) -0.0020(13) 0.0098(12) C27 0.076(2) 0.0515(17) 0.0430(15) -0.0065(14) 0.0230(16) -0.0150(16) C28 0.0572(16) 0.0468(15) 0.0280(12) -0.0048(11) -0.0009(11) -0.0124(13) C29 0.0500(15) 0.0425(14) 0.0352(13) -0.0077(11) -0.0193(11) 0.0022(12) C30 0.0425(15) 0.0699(19) 0.0422(14) -0.0150(13) -0.0037(12) -0.0256(14) C31 0.078(2) 0.0284(13) 0.0465(15) -0.0055(11) -0.0153(14) -0.0118(13) C32 0.0583(17) 0.0457(15) 0.0441(15) -0.0184(12) -0.0046(13) 0.0083(13) C33 0.067(2) 0.106(3) 0.072(2) 0.016(2) -0.0104(19) 0.004(2) C34 0.0455(14) 0.0564(17) 0.0406(14) 0.0092(12) 0.0116(11) 0.0059(12) C35 0.0601(18) 0.0410(16) 0.0658(18) 0.0045(14) 0.0099(15) 0.0026(13) C36 0.0566(18) 0.0573(19) 0.071(2) 0.0136(16) 0.0083(15) 0.0268(15) C37 0.0486(17) 0.080(2) 0.0541(18) 0.0035(16) 0.0053(14) 0.0026(16) C38 0.111(3) 0.0473(19) 0.066(2) -0.0047(16) -0.009(2) -0.0076(19) C39 0.097(2) 0.0454(17) 0.0567(18) 0.0048(14) -0.0056(17) 0.0250(17) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti Cl1 2.3088(7) . . yes Ti Cl2 2.2977(8) . . yes Ti N1 1.7783(15) . . yes Ti C28 2.341(2) . . yes Ti C29 2.334(2) . . yes Ti C30 2.374(3) . . yes Ti C31 2.419(3) . . yes Ti C32 2.401(3) . . yes N1 C1 1.309(2) . . yes N2 C1 1.371(2) . . yes N2 C2 1.394(2) . . yes N2 C4 1.450(2) . . yes N3 C1 1.366(2) . . yes N3 C3 1.391(2) . . yes N3 C16 1.445(2) . . yes C2 C3 1.333(3) . . no C4 C5 1.402(3) . . no C4 C9 1.403(3) . . no C5 C6 1.393(3) . . no C5 C10 1.524(3) . . no C6 C7 1.377(3) . . no C7 C8 1.377(3) . . no C8 C9 1.396(3) . . no C9 C13 1.523(3) . . no C10 C11 1.524(4) . . no C10 C12 1.523(4) . . no C13 C14 1.527(4) . . no C13 C15 1.514(4) . . no C16 C17 1.399(3) . . no C16 C21 1.393(3) . . no C17 C18 1.392(3) . . no C17 C22 1.517(3) . . no C18 C19 1.378(3) . . no C19 C20 1.373(3) . . no C20 C21 1.392(3) . . no C21 C25 1.519(3) . . no C22 C23 1.528(4) . . no C22 C24 1.527(4) . . no C25 C26 1.525(3) . . no C25 C27 1.524(4) . . no C28 C29 1.393(4) . . no C28 C32 1.388(4) . . no C29 C30 1.406(4) . . no C30 C31 1.394(4) . . no C31 C32 1.375(4) . . no C2 H21 0.95(2) . . no C3 H31 0.95(2) . . no C6 H61 0.97(2) . . no C7 H71 0.94(2) . . no C8 H18 0.91(2) . . no C10 H10 0.94(2) . . no C11 H111 1.01(3) . . no C11 H112 0.95(3) . . no C11 H113 0.95(4) . . no C12 H121 0.99(3) . . no C12 H122 0.94(3) . . no C12 H123 0.98(3) . . no C13 H131 0.95(2) . . no C14 H141 1.01(3) . . no C14 H142 1.08(3) . . no C14 H143 0.97(3) . . no C15 H151 1.05(4) . . no C15 H152 1.10(2) . . no C15 H153 1.07(3) . . no C18 H181 0.91(2) . . no C19 H191 0.89(3) . . no C20 H201 0.97(2) . . no C22 H22 0.94(2) . . no C23 H231 0.94(3) . . no C23 H232 0.93(4) . . no C23 H233 0.96(3) . . no C24 H241 0.90(3) . . no C24 H242 1.00(3) . . no C24 H243 0.99(3) . . no C25 H251 0.97(2) . . no C26 H261 0.96(2) . . no C26 H262 0.95(3) . . no C26 H263 0.96(3) . . no C27 H271 0.95(3) . . no C27 H272 1.06(4) . . no C27 H273 0.87(3) . . no C28 H281 0.88(3) . . no C29 H291 0.92(3) . . no C30 H301 0.86(3) . . no C31 H311 0.93(3) . . no C32 H321 0.94(3) . . no C33 C34 1.512(5) . . no C34 C35 1.376(4) . . no C34 C39 1.360(4) . . no C35 C36 1.380(4) . . no C36 C37 1.365(5) . . no C37 C38 1.358(5) . . no C38 C39 1.372(5) . . no C33 H331 0.90(6) . . no C33 H332 0.98(5) . . no C33 H333 0.93(5) . . no C35 H351 0.97(3) . . no C36 H361 0.90(3) . . no C37 H371 0.94(3) . . no C38 H381 0.89(4) . . no C39 H391 0.87(4) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ti Cl2 100.49(3) . . . yes Cl1 Ti N1 104.17(5) . . . yes Cl1 Ti C28 141.62(7) . . . yes Cl1 Ti C29 110.97(7) . . . yes Cl1 Ti C30 84.85(7) . . . yes Cl1 Ti C31 93.70(6) . . . yes Cl1 Ti C32 126.06(7) . . . yes Cl2 Ti N1 104.15(5) . . . yes Cl2 Ti C28 106.00(7) . . . yes Cl2 Ti C29 139.54(7) . . . yes Cl2 Ti C30 131.00(7) . . . yes Cl2 Ti C31 97.29(6) . . . yes Cl2 Ti C32 84.10(7) . . . yes N1 Ti C28 95.78(8) . . . yes N1 Ti C29 92.41(8) . . . yes N1 Ti C30 121.84(9) . . . yes N1 Ti C31 148.82(8) . . . yes N1 Ti C32 126.98(8) . . . yes C28 Ti C29 34.68(9) . . . yes C28 Ti C30 56.81(9) . . . yes C28 Ti C31 56.14(9) . . . yes C28 Ti C32 34.02(9) . . . yes C29 Ti C30 34.73(9) . . . yes C29 Ti C31 57.03(9) . . . yes C29 Ti C32 57.05(9) . . . yes C30 Ti C31 33.81(9) . . . yes C30 Ti C32 55.96(9) . . . yes C31 Ti C32 33.15(9) . . . yes Ti N1 C1 175.84(14) . . . yes C1 N2 C2 109.42(15) . . . yes C1 N2 C4 124.02(15) . . . yes C2 N2 C4 126.51(16) . . . yes C1 N3 C3 109.56(15) . . . yes C1 N3 C16 123.39(15) . . . yes C3 N3 C16 127.04(15) . . . yes N1 C1 N2 128.85(17) . . . yes N1 C1 N3 125.50(16) . . . yes N2 C1 N3 105.60(15) . . . yes N2 C2 C3 107.57(16) . . . yes N3 C3 C2 107.84(16) . . . yes N2 C4 C5 117.86(16) . . . yes N2 C4 C9 118.15(16) . . . yes C5 C4 C9 123.99(17) . . . no C4 C5 C6 116.36(19) . . . no C4 C5 C10 121.54(17) . . . no C6 C5 C10 122.00(18) . . . no C5 C6 C7 121.2(2) . . . no C6 C7 C8 121.1(2) . . . no C7 C8 C9 120.9(2) . . . no C4 C9 C8 116.41(19) . . . no C4 C9 C13 122.13(18) . . . no C8 C9 C13 121.46(19) . . . no C5 C10 C11 113.98(19) . . . no C5 C10 C12 109.90(19) . . . no C11 C10 C12 110.0(2) . . . no C9 C13 C14 113.94(19) . . . no C9 C13 C15 111.4(2) . . . no C14 C13 C15 111.1(2) . . . no N3 C16 C17 118.27(16) . . . yes N3 C16 C21 118.31(16) . . . yes C17 C16 C21 123.42(17) . . . no C16 C17 C18 116.80(19) . . . no C16 C17 C22 122.91(18) . . . no C18 C17 C22 120.29(19) . . . no C17 C18 C19 121.2(2) . . . no C18 C19 C20 120.4(2) . . . no C19 C20 C21 121.4(2) . . . no C16 C21 C20 116.83(18) . . . no C16 C21 C25 122.99(17) . . . no C20 C21 C25 120.17(18) . . . no C17 C22 C23 111.1(2) . . . no C17 C22 C24 110.8(2) . . . no C23 C22 C24 111.3(2) . . . no C21 C25 C26 110.29(18) . . . no C21 C25 C27 111.2(2) . . . no C26 C25 C27 110.4(2) . . . no Ti C28 C29 72.39(14) . . . yes Ti C28 C32 75.37(15) . . . yes C29 C28 C32 108.8(2) . . . no Ti C29 C28 72.92(14) . . . yes Ti C29 C30 74.20(15) . . . yes C28 C29 C30 106.5(2) . . . no Ti C30 C29 71.06(15) . . . yes Ti C30 C31 74.86(15) . . . yes C29 C30 C31 108.3(2) . . . no Ti C31 C30 71.33(16) . . . yes Ti C31 C32 72.70(15) . . . yes C30 C31 C32 108.0(2) . . . no Ti C32 C28 70.61(14) . . . yes Ti C32 C31 74.15(16) . . . yes C28 C32 C31 108.3(2) . . . no N2 C2 H21 119.2(12) . . . no C3 C2 H21 133.2(12) . . . no N3 C3 H31 121.0(12) . . . no C2 C3 H31 131.1(12) . . . no C5 C6 H61 118.2(14) . . . no C7 C6 H61 120.6(14) . . . no C6 C7 H71 121.2(15) . . . no C8 C7 H71 117.8(15) . . . no C7 C8 H18 120.2(14) . . . no C9 C8 H18 118.8(14) . . . no C5 C10 H10 107.3(12) . . . no C11 C10 H10 106.6(12) . . . no C12 C10 H10 108.9(13) . . . no C10 C11 H111 109.6(15) . . . no C10 C11 H112 111.4(17) . . . no C10 C11 H113 112.4(18) . . . no H111 C11 H112 108(2) . . . no H111 C11 H113 107(2) . . . no H112 C11 H113 108(2) . . . no C10 C12 H121 109.4(15) . . . no C10 C12 H122 105.8(17) . . . no C10 C12 H123 114.0(17) . . . no H121 C12 H122 106(2) . . . no H121 C12 H123 110(2) . . . no H122 C12 H123 111(2) . . . no C9 C13 H131 107.6(14) . . . no C14 C13 H131 102.7(14) . . . no C15 C13 H131 109.6(14) . . . no C13 C14 H141 109.3(16) . . . no C13 C14 H142 105.6(17) . . . no C13 C14 H143 109.1(15) . . . no H141 C14 H142 116(2) . . . no H141 C14 H143 110(2) . . . no H142 C14 H143 106(2) . . . no C13 C15 H151 111.2(18) . . . no C13 C15 H152 95.3(11) . . . no C13 C15 H153 109.9(16) . . . no H151 C15 H152 102(2) . . . no H151 C15 H153 112(2) . . . no H152 C15 H153 125(2) . . . no C17 C18 H181 119.0(15) . . . no C19 C18 H181 119.8(15) . . . no C18 C19 H191 118.5(16) . . . no C20 C19 H191 121.1(16) . . . no C19 C20 H201 119.6(14) . . . no C21 C20 H201 119.0(14) . . . no C17 C22 H22 108.6(12) . . . no C23 C22 H22 107.2(13) . . . no C24 C22 H22 107.7(13) . . . no C22 C23 H231 109.0(17) . . . no C22 C23 H232 109(2) . . . no C22 C23 H233 109.6(17) . . . no H231 C23 H232 105(3) . . . no H231 C23 H233 111(3) . . . no H232 C23 H233 113(3) . . . no C22 C24 H241 110.4(19) . . . no C22 C24 H242 112.3(18) . . . no C22 C24 H243 108.5(16) . . . no H241 C24 H242 107(2) . . . no H241 C24 H243 110(2) . . . no H242 C24 H243 109(2) . . . no C21 C25 H251 108.3(13) . . . no C26 C25 H251 107.9(13) . . . no C27 C25 H251 108.6(13) . . . no C25 C26 H261 108.7(14) . . . no C25 C26 H262 111.7(15) . . . no C25 C26 H263 108.6(17) . . . no H261 C26 H262 110(2) . . . no H261 C26 H263 110(2) . . . no H262 C26 H263 108(2) . . . no C25 C27 H271 111.1(17) . . . no C25 C27 H272 108.1(19) . . . no C25 C27 H273 115(2) . . . no H271 C27 H272 105(2) . . . no H271 C27 H273 108(2) . . . no H272 C27 H273 109(3) . . . no Ti C28 H281 117.7(18) . . . no C29 C28 H281 125.5(17) . . . no C32 C28 H281 125.7(17) . . . no Ti C29 H291 117.7(16) . . . no C28 C29 H291 128.3(16) . . . no C30 C29 H291 125.2(16) . . . no Ti C30 H301 115.9(19) . . . no C29 C30 H301 119.7(19) . . . no C31 C30 H301 131.8(19) . . . no Ti C31 H311 118.5(19) . . . no C30 C31 H311 123.8(16) . . . no C32 C31 H311 128.1(16) . . . no Ti C32 H321 120.7(17) . . . no C28 C32 H321 126.1(18) . . . no C31 C32 H321 125.6(18) . . . no C33 C34 C35 120.8(3) . . . no C33 C34 C39 121.5(3) . . . no C35 C34 C39 117.7(3) . . . no C34 C35 C36 120.7(3) . . . no C35 C36 C37 120.4(3) . . . no C36 C37 C38 119.0(3) . . . no C37 C38 C39 120.3(3) . . . no C34 C39 C38 121.9(3) . . . no C34 C33 H331 113(4) . . . no C34 C33 H332 108(3) . . . no C34 C33 H333 105(3) . . . no H331 C33 H332 112(5) . . . no H331 C33 H333 124(5) . . . no H332 C33 H333 92(4) . . . no C34 C35 H351 119.5(17) . . . no C36 C35 H351 119.8(17) . . . no C35 C36 H361 120.2(19) . . . no C37 C36 H361 119.3(19) . . . no C36 C37 H371 120.8(18) . . . no C38 C37 H371 120.1(18) . . . no C37 C38 H381 120(2) . . . no C39 C38 H381 120(2) . . . no C34 C39 H391 117(2) . . . no C38 C39 H391 121(2) . . . no #===END # CIF-file generated for RANK 4437-173 # Compound 4 #=================================================================== data_RANK-4437-173 _database_code_depnum_ccdc_archive 'CCDC 281533' #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C20 H33 Cl2 N3 Ti' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C20 H33 Cl2 N3 Ti' _chemical_formula_weight 434.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 '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' Cl Cl 0.1484 0.1585 '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' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z _cell_length_a 8.8141(1) _cell_length_b 17.2213(2) _cell_length_c 15.1835(2) _cell_angle_alpha 90 _cell_angle_beta 104.3295(5) _cell_angle_gamma 90 _cell_volume 2233.00(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 4257 _cell_measurement_theta_min 1.82 _cell_measurement_theta_max 25.39 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.292 _exptl_crystal_density_method none _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.766 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 40 s per film repetition 1 dx 40 557 films measured in 10 data sets set 1: phi-scan with delta_phi = 2.0 set 2 to 10: omega-scans with delta_omega = 2.0 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could not be located in the difference Fourier maps and were calculated in ideal positions (riding model). ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 54591 _diffrn_reflns_av_R_equivalents 0.068 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 25.39 _reflns_number_total 4107 _reflns_number_gt 3530 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0285P)^2^+2.5227P] 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_number_reflns 4107 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0568 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0877 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.743 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.054 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ti Ti Uani -0.06304(5) 0.31337(3) 0.31455(3) 1.000 0.0211(1) . . Cl1 Cl Uani -0.23586(7) 0.39467(4) 0.21630(4) 1.000 0.0305(2) . . Cl2 Cl Uani -0.19858(7) 0.19664(4) 0.29739(5) 1.000 0.0312(2) . . N1 N Uani 0.0820(2) 0.29810(11) 0.25357(13) 1.000 0.0213(6) . . N2 N Uani 0.2640(2) 0.34681(11) 0.17075(13) 1.000 0.0206(6) . . N3 N Uani 0.2914(2) 0.22487(11) 0.21599(14) 1.000 0.0217(6) . . C1 C Uani 0.2037(3) 0.29075(13) 0.21696(15) 1.000 0.0186(7) . . C2 C Uani 0.3890(3) 0.31540(15) 0.14311(17) 1.000 0.0246(8) . . C3 C Uani 0.4061(3) 0.24151(15) 0.17040(18) 1.000 0.0263(8) . . C4 C Uani 0.2002(3) 0.42701(14) 0.14638(17) 1.000 0.0249(8) . . C5 C Uani 0.3063(3) 0.46957(16) 0.09582(19) 1.000 0.0336(9) . . C6 C Uani 0.1992(3) 0.47189(15) 0.23259(19) 1.000 0.0351(9) . . C7 C Uani 0.0363(3) 0.41888(16) 0.08406(19) 1.000 0.0338(9) . . C8 C Uani 0.2614(3) 0.14511(14) 0.24822(18) 1.000 0.0253(8) . . C9 C Uani 0.3849(3) 0.08984(16) 0.2290(2) 1.000 0.0456(10) . . C10 C Uani 0.2726(4) 0.14716(17) 0.34994(19) 1.000 0.0416(10) . . C11 C Uani 0.1010(3) 0.11822(15) 0.19519(18) 1.000 0.0277(8) . . C12 C Uani -0.1428(3) 0.34627(15) 0.45710(16) 1.000 0.0237(8) . . C13 C Uani -0.0741(3) 0.41140(16) 0.42742(17) 1.000 0.0319(9) . . C14 C Uani 0.0810(3) 0.3947(2) 0.42772(19) 1.000 0.0423(10) . . C15 C Uani 0.1116(3) 0.3191(2) 0.45713(18) 1.000 0.0419(10) . . C16 C Uani -0.0264(3) 0.28825(16) 0.47491(17) 1.000 0.0313(8) . . C17 C Uani -0.3068(3) 0.34036(18) 0.47295(18) 1.000 0.0364(9) . . C18 C Uani -0.4330(3) 0.3533(2) 0.3876(2) 1.000 0.0551(13) . . C19 C Uani -0.3189(4) 0.3976(2) 0.5473(2) 1.000 0.0474(11) . . C20 C Uani -0.3315(4) 0.2576(2) 0.5085(3) 1.000 0.0564(12) . . H21 H Uiso 0.45210 0.34190 0.11030 1.000 0.0290 calc R H31 H Uiso 0.48320 0.20640 0.16040 1.000 0.0320 calc R H51 H Uiso 0.30450 0.44230 0.03890 1.000 0.0500 calc R H52 H Uiso 0.41370 0.47080 0.13400 1.000 0.0500 calc R H53 H Uiso 0.26840 0.52280 0.08230 1.000 0.0500 calc R H61 H Uiso 0.30350 0.46980 0.27440 1.000 0.0530 calc R H62 H Uiso 0.12260 0.44870 0.26180 1.000 0.0530 calc R H63 H Uiso 0.17080 0.52610 0.21710 1.000 0.0530 calc R H71 H Uiso 0.04330 0.39600 0.02610 1.000 0.0510 calc R H72 H Uiso -0.01280 0.47020 0.07310 1.000 0.0510 calc R H73 H Uiso -0.02700 0.38520 0.11290 1.000 0.0510 calc R H91 H Uiso 0.48940 0.10810 0.26080 1.000 0.0680 calc R H92 H Uiso 0.37650 0.08830 0.16350 1.000 0.0680 calc R H93 H Uiso 0.36790 0.03770 0.25050 1.000 0.0680 calc R H101 H Uiso 0.37520 0.16760 0.38210 1.000 0.0620 calc R H102 H Uiso 0.25990 0.09450 0.37150 1.000 0.0620 calc R H103 H Uiso 0.19000 0.18070 0.36170 1.000 0.0620 calc R H111 H Uiso 0.09820 0.11610 0.13030 1.000 0.0420 calc R H112 H Uiso 0.02130 0.15470 0.20480 1.000 0.0420 calc R H113 H Uiso 0.07970 0.06650 0.21620 1.000 0.0420 calc R H131 H Uiso -0.12530 0.45950 0.40980 1.000 0.0380 calc R H141 H Uiso 0.15280 0.42930 0.41070 1.000 0.0510 calc R H151 H Uiso 0.20830 0.29250 0.46410 1.000 0.0500 calc R H161 H Uiso -0.03870 0.23710 0.49540 1.000 0.0380 calc R H181 H Uiso -0.42390 0.31440 0.34220 1.000 0.0830 calc R H182 H Uiso -0.42180 0.40540 0.36380 1.000 0.0830 calc R H183 H Uiso -0.53580 0.34870 0.40110 1.000 0.0830 calc R H191 H Uiso -0.23980 0.38510 0.60320 1.000 0.0710 calc R H192 H Uiso -0.42340 0.39420 0.55860 1.000 0.0710 calc R H193 H Uiso -0.30140 0.45040 0.52790 1.000 0.0710 calc R H201 H Uiso -0.25410 0.24820 0.56600 1.000 0.0850 calc R H202 H Uiso -0.31870 0.21880 0.46360 1.000 0.0850 calc R H203 H Uiso -0.43710 0.25370 0.51810 1.000 0.0850 calc R 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 Ti 0.0212(2) 0.0211(2) 0.0223(2) -0.0038(2) 0.0081(2) -0.0012(2) Cl1 0.0275(3) 0.0303(4) 0.0335(4) -0.0013(3) 0.0069(3) 0.0057(3) Cl2 0.0321(3) 0.0262(3) 0.0391(4) -0.0077(3) 0.0159(3) -0.0070(3) N1 0.0246(11) 0.0182(11) 0.0217(11) 0.0006(8) 0.0068(8) 0.0001(8) N2 0.0230(11) 0.0178(10) 0.0224(10) 0.0004(8) 0.0081(8) -0.0008(8) N3 0.0202(10) 0.0184(10) 0.0276(11) 0.0013(9) 0.0078(9) 0.0010(8) C1 0.0188(12) 0.0183(12) 0.0177(12) -0.0009(10) 0.0029(9) 0.0005(9) C2 0.0233(13) 0.0262(14) 0.0271(13) -0.0009(11) 0.0117(10) -0.0025(11) C3 0.0216(13) 0.0258(14) 0.0350(15) -0.0026(11) 0.0136(11) 0.0008(11) C4 0.0310(14) 0.0166(12) 0.0267(13) 0.0028(11) 0.0061(11) 0.0015(10) C5 0.0407(16) 0.0236(14) 0.0385(16) 0.0063(12) 0.0135(13) -0.0044(12) C6 0.0503(18) 0.0184(14) 0.0387(16) -0.0009(12) 0.0149(14) 0.0025(12) C7 0.0333(15) 0.0293(15) 0.0366(16) 0.0116(12) 0.0047(12) 0.0017(12) C8 0.0265(13) 0.0174(13) 0.0328(14) 0.0069(11) 0.0087(11) 0.0015(10) C9 0.0365(16) 0.0220(15) 0.082(2) 0.0138(15) 0.0218(16) 0.0078(12) C10 0.0572(19) 0.0322(16) 0.0302(16) 0.0101(13) 0.0011(14) -0.0038(14) C11 0.0300(14) 0.0216(13) 0.0334(15) -0.0014(11) 0.0116(12) -0.0014(11) C12 0.0275(13) 0.0273(14) 0.0170(12) -0.0023(10) 0.0068(10) -0.0018(11) C13 0.0513(18) 0.0234(14) 0.0228(14) -0.0055(11) 0.0125(12) -0.0046(12) C14 0.0426(17) 0.059(2) 0.0288(16) -0.0185(15) 0.0156(13) -0.0274(16) C15 0.0233(14) 0.073(2) 0.0273(15) -0.0172(15) 0.0022(12) 0.0079(14) C16 0.0436(16) 0.0262(14) 0.0213(13) 0.0007(11) 0.0027(12) 0.0028(12) C17 0.0304(15) 0.0543(19) 0.0281(15) -0.0042(14) 0.0142(12) 0.0006(13) C18 0.0311(17) 0.092(3) 0.0450(19) -0.0083(19) 0.0149(14) 0.0012(17) C19 0.0412(18) 0.058(2) 0.0506(19) -0.0154(16) 0.0256(15) -0.0010(15) C20 0.063(2) 0.055(2) 0.061(2) 0.0014(18) 0.0342(18) -0.0158(18) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti Cl1 2.3197(8) . . yes Ti Cl2 2.3199(8) . . yes Ti N1 1.7739(19) . . yes Ti C12 2.501(2) . . yes Ti C13 2.425(3) . . yes Ti C14 2.334(3) . . yes Ti C15 2.327(3) . . yes Ti C16 2.415(3) . . yes N1 C1 1.331(3) . . yes N2 C1 1.375(3) . . yes N2 C2 1.383(3) . . yes N2 C4 1.503(3) . . yes N3 C1 1.375(3) . . yes N3 C3 1.389(3) . . yes N3 C8 1.503(3) . . yes C2 C3 1.335(4) . . no C4 C5 1.535(4) . . no C4 C6 1.522(4) . . no C4 C7 1.525(4) . . no C8 C9 1.528(4) . . no C8 C10 1.523(4) . . no C8 C11 1.516(4) . . no C12 C13 1.401(4) . . no C12 C16 1.410(4) . . no C12 C17 1.526(4) . . no C13 C14 1.396(4) . . no C14 C15 1.381(5) . . no C15 C16 1.413(4) . . no C17 C18 1.501(4) . . no C17 C19 1.522(4) . . no C17 C20 1.558(5) . . no C2 H21 0.9502 . . no C3 H31 0.9495 . . no C5 H51 0.9803 . . no C5 H52 0.9803 . . no C5 H53 0.9799 . . no C6 H61 0.9801 . . no C6 H62 0.9799 . . no C6 H63 0.9800 . . no C7 H71 0.9800 . . no C7 H72 0.9800 . . no C7 H73 0.9800 . . no C9 H91 0.9799 . . no C9 H92 0.9792 . . no C9 H93 0.9795 . . no C10 H101 0.9806 . . no C10 H102 0.9799 . . no C10 H103 0.9797 . . no C11 H111 0.9801 . . no C11 H112 0.9799 . . no C11 H113 0.9798 . . no C13 H131 0.9495 . . no C14 H141 0.9504 . . no C15 H151 0.9502 . . no C16 H161 0.9493 . . no C18 H181 0.9786 . . no C18 H182 0.9813 . . no C18 H183 0.9804 . . no C19 H191 0.9797 . . no C19 H192 0.9795 . . no C19 H193 0.9797 . . no C20 H201 0.9793 . . no C20 H202 0.9808 . . no C20 H203 0.9794 . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl1 Ti Cl2 102.29(3) . . . yes Cl1 Ti N1 101.37(7) . . . yes Cl1 Ti C12 98.01(6) . . . yes Cl1 Ti C13 84.23(7) . . . yes Cl1 Ti C14 105.20(8) . . . yes Cl1 Ti C15 138.63(9) . . . yes Cl1 Ti C16 131.24(7) . . . yes Cl2 Ti N1 103.33(7) . . . yes Cl2 Ti C12 92.65(6) . . . yes Cl2 Ti C13 124.96(7) . . . yes Cl2 Ti C14 140.71(8) . . . yes Cl2 Ti C15 110.17(9) . . . yes Cl2 Ti C16 83.95(7) . . . yes N1 Ti C12 151.48(9) . . . yes N1 Ti C13 129.23(9) . . . yes N1 Ti C14 98.18(9) . . . yes N1 Ti C15 95.49(9) . . . yes N1 Ti C16 124.47(9) . . . yes C12 Ti C13 33.01(9) . . . yes C12 Ti C14 56.29(9) . . . yes C12 Ti C15 56.51(9) . . . yes C12 Ti C16 33.27(9) . . . yes C13 Ti C14 34.05(9) . . . yes C13 Ti C15 56.36(10) . . . yes C13 Ti C16 55.30(9) . . . yes C14 Ti C15 34.47(12) . . . yes C14 Ti C16 56.80(10) . . . yes C15 Ti C16 34.62(10) . . . yes Ti N1 C1 172.62(17) . . . yes C1 N2 C2 108.5(2) . . . yes C1 N2 C4 127.1(2) . . . yes C2 N2 C4 124.2(2) . . . yes C1 N3 C3 108.4(2) . . . yes C1 N3 C8 127.3(2) . . . yes C3 N3 C8 124.0(2) . . . yes N1 C1 N2 126.8(2) . . . yes N1 C1 N3 126.6(2) . . . yes N2 C1 N3 106.5(2) . . . yes N2 C2 C3 108.4(2) . . . yes N3 C3 C2 108.1(2) . . . yes N2 C4 C5 109.0(2) . . . yes N2 C4 C6 109.7(2) . . . yes N2 C4 C7 107.9(2) . . . yes C5 C4 C6 108.8(2) . . . no C5 C4 C7 109.5(2) . . . no C6 C4 C7 112.0(2) . . . no N3 C8 C9 108.4(2) . . . yes N3 C8 C10 109.7(2) . . . yes N3 C8 C11 108.8(2) . . . yes C9 C8 C10 109.7(2) . . . no C9 C8 C11 108.9(2) . . . no C10 C8 C11 111.3(2) . . . no Ti C12 C13 70.52(15) . . . yes Ti C12 C16 70.02(14) . . . yes Ti C12 C17 126.97(17) . . . yes C13 C12 C16 106.1(2) . . . no C13 C12 C17 127.3(2) . . . no C16 C12 C17 126.5(2) . . . no Ti C13 C12 76.47(15) . . . yes Ti C13 C14 69.40(17) . . . yes C12 C13 C14 109.6(3) . . . no Ti C14 C13 76.55(16) . . . yes Ti C14 C15 72.51(18) . . . yes C13 C14 C15 107.9(3) . . . no Ti C15 C14 73.02(16) . . . yes Ti C15 C16 76.08(15) . . . yes C14 C15 C16 107.9(2) . . . no Ti C16 C12 76.71(15) . . . yes Ti C16 C15 69.31(15) . . . yes C12 C16 C15 108.5(2) . . . no C12 C17 C18 112.5(2) . . . no C12 C17 C19 108.5(2) . . . no C12 C17 C20 109.5(2) . . . no C18 C17 C19 111.8(3) . . . no C18 C17 C20 107.3(3) . . . no C19 C17 C20 107.1(3) . . . no N2 C2 H21 125.81 . . . no C3 C2 H21 125.78 . . . no N3 C3 H31 125.89 . . . no C2 C3 H31 125.98 . . . no C4 C5 H51 109.46 . . . no C4 C5 H52 109.46 . . . no C4 C5 H53 109.46 . . . no H51 C5 H52 109.53 . . . no H51 C5 H53 109.46 . . . no H52 C5 H53 109.45 . . . no C4 C6 H61 109.53 . . . no C4 C6 H62 109.49 . . . no C4 C6 H63 109.44 . . . no H61 C6 H62 109.44 . . . no H61 C6 H63 109.47 . . . no H62 C6 H63 109.46 . . . no C4 C7 H71 109.49 . . . no C4 C7 H72 109.47 . . . no C4 C7 H73 109.50 . . . no H71 C7 H72 109.48 . . . no H71 C7 H73 109.43 . . . no H72 C7 H73 109.47 . . . no C8 C9 H91 109.47 . . . no C8 C9 H92 109.43 . . . no C8 C9 H93 109.42 . . . no H91 C9 H92 109.55 . . . no H91 C9 H93 109.43 . . . no H92 C9 H93 109.53 . . . no C8 C10 H101 109.48 . . . no C8 C10 H102 109.46 . . . no C8 C10 H103 109.50 . . . no H101 C10 H102 109.47 . . . no H101 C10 H103 109.45 . . . no H102 C10 H103 109.47 . . . no C8 C11 H111 109.48 . . . no C8 C11 H112 109.50 . . . no C8 C11 H113 109.48 . . . no H111 C11 H112 109.45 . . . no H111 C11 H113 109.53 . . . no H112 C11 H113 109.40 . . . no Ti C13 H131 120.51 . . . no C12 C13 H131 125.16 . . . no C14 C13 H131 125.27 . . . no Ti C14 H141 116.97 . . . no C13 C14 H141 125.97 . . . no C15 C14 H141 126.09 . . . no Ti C15 H151 116.85 . . . no C14 C15 H151 126.05 . . . no C16 C15 H151 126.03 . . . no Ti C16 H161 119.94 . . . no C12 C16 H161 125.73 . . . no C15 C16 H161 125.80 . . . no C17 C18 H181 109.52 . . . no C17 C18 H182 109.46 . . . no C17 C18 H183 109.47 . . . no H181 C18 H182 109.46 . . . no H181 C18 H183 109.45 . . . no H182 C18 H183 109.47 . . . no C17 C19 H191 109.56 . . . no C17 C19 H192 109.43 . . . no C17 C19 H193 109.45 . . . no H191 C19 H192 109.48 . . . no H191 C19 H193 109.46 . . . no H192 C19 H193 109.45 . . . no C17 C20 H201 109.50 . . . no C17 C20 H202 109.41 . . . no C17 C20 H203 109.49 . . . no H201 C20 H202 109.42 . . . no H201 C20 H203 109.51 . . . no H202 C20 H203 109.50 . . . no #===END # CIF-file generated for SRAN2 1-173 # Compound 6 #=================================================================== data_SRAN2-1-173 _database_code_depnum_ccdc_archive 'CCDC 281534' #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ; _chemical_name_common ? _chemical_formula_moiety 'C24 H46 N6 Ti' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C24 H46 N6 Ti' _chemical_formula_weight 466.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_Hall '-P 2ac 2ab' _symmetry_space_group_name_H-M 'P b c a' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,-y,1/2+z 1/2+x,1/2-y,-z -x,1/2+y,1/2-z -x,-y,-z 1/2+x,y,1/2-z 1/2-x,1/2+y,z x,1/2-y,1/2+z _cell_length_a 18.4995(1) _cell_length_b 16.2737(1) _cell_length_c 18.6379(1) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5611.04(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used 5679 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 25.36 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.105 _exptl_crystal_density_method none _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.325 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.863 _exptl_absorpt_correction_T_max 0.973 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 15 s per film repetition 1 dx 40 1075 films measured in 8 data set set 1: phi-scan with delta_phi = 1.0 set 2 to 8: omega-scans with delta_omega = 1.0 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could be located in the difference Fourier maps and were allowed to refine freely. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 128752 _diffrn_reflns_av_R_equivalents 0.051 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.36 _reflns_number_total 5141 _reflns_number_gt 4482 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0535P)^2^+1.9445P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_number_reflns 5141 _refine_ls_number_parameters 464 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0984 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.324 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.036 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ti Ti Uani 0.52241(1) 0.27042(2) 0.13874(1) 1.000 0.0289(1) . . N1 N Uani 0.50557(7) 0.29919(8) 0.04590(7) 1.000 0.0325(4) . . N2 N Uani 0.43823(7) 0.37048(8) -0.04612(7) 1.000 0.0332(4) . . N3 N Uani 0.54086(7) 0.31207(9) -0.07738(7) 1.000 0.0349(4) . . N4 N Uani 0.44299(7) 0.24532(9) 0.19279(7) 1.000 0.0346(4) . . N5 N Uani 0.34487(7) 0.15100(9) 0.21321(8) 1.000 0.0407(4) . . N6 N Uani 0.34244(7) 0.26828(9) 0.27270(8) 1.000 0.0406(5) . . C1 C Uani 0.49544(8) 0.32456(9) -0.01945(8) 1.000 0.0301(4) . . C2 C Uani 0.44952(10) 0.38457(11) -0.11871(9) 1.000 0.0405(6) . . C3 C Uani 0.51122(10) 0.34936(12) -0.13770(9) 1.000 0.0424(6) . . C4 C Uani 0.37870(8) 0.40626(10) -0.00178(9) 1.000 0.0350(5) . . C5 C Uani 0.41170(10) 0.46651(11) 0.05170(10) 1.000 0.0395(5) . . C6 C Uani 0.33857(10) 0.33712(12) 0.03639(13) 1.000 0.0460(6) . . C7 C Uani 0.32612(11) 0.45209(14) -0.05064(12) 1.000 0.0503(7) . . C8 C Uani 0.61195(9) 0.26800(11) -0.07357(9) 1.000 0.0407(6) . . C9 C Uani 0.66055(10) 0.31145(14) -0.01995(12) 1.000 0.0455(6) . . C10 C Uani 0.59848(11) 0.17880(12) -0.05277(12) 1.000 0.0480(7) . . C11 C Uani 0.64769(14) 0.27170(19) -0.14736(13) 1.000 0.0632(9) . . C12 C Uani 0.38244(8) 0.22399(10) 0.22282(8) 1.000 0.0342(5) . . C13 C Uani 0.28462(10) 0.15211(15) 0.25830(11) 1.000 0.0510(7) . . C14 C Uani 0.28346(10) 0.22201(15) 0.29339(11) 1.000 0.0516(7) . . C15 C Uani 0.36511(10) 0.08419(11) 0.16229(11) 1.000 0.0455(6) . . C16 C Uani 0.30884(15) 0.01546(16) 0.16714(18) 1.000 0.0675(9) . . C17 C Uani 0.43858(12) 0.04940(13) 0.18388(14) 1.000 0.0524(7) . . C18 C Uani 0.36644(13) 0.11765(14) 0.08594(11) 1.000 0.0520(7) . . C19 C Uani 0.36155(10) 0.35148(12) 0.30112(10) 1.000 0.0450(6) . . C20 C Uani 0.30232(14) 0.3812(2) 0.35229(15) 1.000 0.0704(10) . . C21 C Uani 0.43216(11) 0.34543(15) 0.34255(12) 1.000 0.0510(7) . . C22 C Uani 0.36754(15) 0.41146(15) 0.23897(13) 1.000 0.0621(8) . . C23 C Uani 0.57791(12) 0.37087(14) 0.18493(13) 1.000 0.0503(7) . . C24 C Uani 0.59667(11) 0.17207(14) 0.14233(12) 1.000 0.0454(7) . . H21 H Uiso 0.4182(11) 0.4132(13) -0.1452(11) 1.000 0.049(6) . . H31 H Uiso 0.5336(10) 0.3440(12) -0.1825(11) 1.000 0.047(5) . . H51 H Uiso 0.4332(11) 0.5115(14) 0.0279(11) 1.000 0.053(6) . . H52 H Uiso 0.4499(10) 0.4389(11) 0.0806(10) 1.000 0.041(5) . . H53 H Uiso 0.3753(11) 0.4875(12) 0.0835(11) 1.000 0.048(5) . . H61 H Uiso 0.3195(12) 0.3026(14) 0.0010(12) 1.000 0.061(6) . . H62 H Uiso 0.2983(12) 0.3594(13) 0.0630(11) 1.000 0.058(6) . . H63 H Uiso 0.3672(11) 0.3103(12) 0.0703(11) 1.000 0.045(5) . . H71 H Uiso 0.3491(11) 0.4988(14) -0.0752(11) 1.000 0.055(6) . . H72 H Uiso 0.2873(12) 0.4731(13) -0.0217(12) 1.000 0.058(6) . . H73 H Uiso 0.3053(12) 0.4145(14) -0.0856(12) 1.000 0.064(6) . . H91 H Uiso 0.6684(11) 0.3673(15) -0.0369(11) 1.000 0.060(6) . . H92 H Uiso 0.7044(12) 0.2815(12) -0.0171(11) 1.000 0.055(6) . . H93 H Uiso 0.6403(11) 0.3151(12) 0.0264(12) 1.000 0.051(5) . . H101 H Uiso 0.5700(11) 0.1497(13) -0.0885(12) 1.000 0.055(6) . . H102 H Uiso 0.5690(11) 0.1720(13) -0.0090(12) 1.000 0.052(6) . . H103 H Uiso 0.6464(13) 0.1514(14) -0.0425(12) 1.000 0.066(6) . . H111 H Uiso 0.6170(12) 0.2423(14) -0.1809(13) 1.000 0.058(6) . . H112 H Uiso 0.6904(17) 0.2454(18) -0.1428(14) 1.000 0.084(9) . . H113 H Uiso 0.6539(15) 0.3285(19) -0.1668(15) 1.000 0.093(9) . . H131 H Uiso 0.2543(12) 0.1113(13) 0.2574(11) 1.000 0.053(6) . . H141 H Uiso 0.2523(13) 0.2416(14) 0.3286(13) 1.000 0.064(6) . . H161 H Uiso 0.3055(14) -0.0052(17) 0.2148(15) 1.000 0.085(9) . . H162 H Uiso 0.3219(15) -0.0247(18) 0.1290(15) 1.000 0.088(9) . . H163 H Uiso 0.2624(14) 0.0361(14) 0.1520(13) 1.000 0.070(7) . . H171 H Uiso 0.4348(12) 0.0236(14) 0.2320(13) 1.000 0.065(6) . . H172 H Uiso 0.4746(10) 0.0898(13) 0.1845(10) 1.000 0.047(5) . . H173 H Uiso 0.4518(12) 0.0091(14) 0.1493(11) 1.000 0.056(6) . . H181 H Uiso 0.3187(13) 0.1395(14) 0.0723(12) 1.000 0.068(7) . . H182 H Uiso 0.3781(11) 0.0738(14) 0.0545(12) 1.000 0.057(6) . . H183 H Uiso 0.4022(11) 0.1596(13) 0.0800(10) 1.000 0.047(5) . . H201 H Uiso 0.2561(15) 0.3810(15) 0.3280(14) 1.000 0.079(8) . . H202 H Uiso 0.3167(15) 0.4382(19) 0.3689(15) 1.000 0.094(9) . . H203 H Uiso 0.2970(13) 0.3419(16) 0.3919(14) 1.000 0.074(8) . . H211 H Uiso 0.4299(13) 0.3092(16) 0.3862(14) 1.000 0.073(7) . . H212 H Uiso 0.4414(12) 0.3984(16) 0.3621(12) 1.000 0.062(6) . . H213 H Uiso 0.4703(10) 0.3255(12) 0.3123(11) 1.000 0.045(5) . . H221 H Uiso 0.3221(14) 0.4106(15) 0.2156(13) 1.000 0.072(7) . . H222 H Uiso 0.4044(12) 0.3974(14) 0.2046(13) 1.000 0.067(7) . . H223 H Uiso 0.3759(13) 0.4653(17) 0.2583(14) 1.000 0.083(8) . . H231 H Uiso 0.5883(14) 0.3728(17) 0.2287(16) 1.000 0.087(9) . . H232 H Uiso 0.5499(15) 0.4246(19) 0.1805(15) 1.000 0.092(8) . . H233 H Uiso 0.6178(17) 0.3791(18) 0.1636(17) 1.000 0.098(10) . . H241 H Uiso 0.6073(14) 0.1560(16) 0.1865(16) 1.000 0.084(8) . . H242 H Uiso 0.6384(15) 0.1868(17) 0.1217(14) 1.000 0.080(8) . . H243 H Uiso 0.5944(14) 0.1207(18) 0.1210(14) 1.000 0.084(8) . . 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 Ti 0.0248(2) 0.0315(2) 0.0303(2) 0.0001(1) 0.0009(1) -0.0007(1) N1 0.0282(6) 0.0356(7) 0.0337(7) 0.0010(6) 0.0016(5) 0.0004(6) N2 0.0324(7) 0.0342(7) 0.0331(7) 0.0001(6) -0.0033(5) -0.0015(6) N3 0.0352(7) 0.0393(8) 0.0302(7) -0.0031(6) 0.0014(6) 0.0005(6) N4 0.0322(7) 0.0362(7) 0.0354(7) 0.0029(6) 0.0035(6) 0.0004(6) N5 0.0315(7) 0.0456(8) 0.0451(8) 0.0106(7) -0.0024(6) -0.0053(6) N6 0.0271(7) 0.0584(10) 0.0362(8) 0.0049(7) 0.0041(6) 0.0031(6) C1 0.0280(7) 0.0289(8) 0.0334(8) -0.0030(6) -0.0001(6) -0.0047(6) C2 0.0472(10) 0.0409(10) 0.0334(9) 0.0012(7) -0.0074(8) -0.0003(8) C3 0.0521(11) 0.0472(11) 0.0280(9) -0.0018(7) -0.0002(8) -0.0017(9) C4 0.0292(8) 0.0335(9) 0.0422(9) 0.0019(7) -0.0009(7) 0.0013(6) C5 0.0398(9) 0.0352(9) 0.0435(10) -0.0019(8) 0.0039(8) 0.0004(8) C6 0.0296(9) 0.0416(10) 0.0667(13) 0.0062(10) 0.0040(9) -0.0039(8) C7 0.0432(11) 0.0535(12) 0.0541(12) 0.0011(10) -0.0085(9) 0.0109(10) C8 0.0348(9) 0.0486(11) 0.0386(9) -0.0052(8) 0.0068(7) 0.0042(7) C9 0.0289(9) 0.0528(12) 0.0547(12) -0.0027(10) 0.0042(8) -0.0001(9) C10 0.0470(11) 0.0448(11) 0.0522(12) -0.0114(9) -0.0018(9) 0.0075(9) C11 0.0546(14) 0.0863(19) 0.0486(13) -0.0048(13) 0.0161(11) 0.0151(13) C12 0.0276(8) 0.0414(9) 0.0337(8) 0.0092(7) -0.0015(6) 0.0018(7) C13 0.0292(9) 0.0717(14) 0.0520(11) 0.0207(11) -0.0018(8) -0.0138(9) C14 0.0292(9) 0.0816(16) 0.0439(11) 0.0078(11) 0.0052(8) -0.0015(9) C15 0.0425(10) 0.0370(9) 0.0569(11) 0.0082(8) -0.0076(8) -0.0062(8) C16 0.0568(14) 0.0527(14) 0.093(2) 0.0076(14) -0.0081(14) -0.0186(11) C17 0.0512(12) 0.0366(10) 0.0694(14) 0.0088(10) -0.0061(10) 0.0020(9) C18 0.0603(13) 0.0436(11) 0.0520(12) -0.0027(9) -0.0110(10) -0.0031(10) C19 0.0398(9) 0.0530(11) 0.0422(9) -0.0014(8) 0.0053(8) 0.0133(8) C20 0.0534(14) 0.094(2) 0.0637(15) -0.0153(15) 0.0145(12) 0.0183(14) C21 0.0469(11) 0.0545(13) 0.0517(12) -0.0085(10) -0.0025(9) 0.0058(9) C22 0.0743(16) 0.0536(14) 0.0583(13) 0.0054(11) 0.0079(12) 0.0248(12) C23 0.0514(12) 0.0516(12) 0.0480(12) -0.0071(9) -0.0025(10) -0.0124(10) C24 0.0360(10) 0.0544(13) 0.0458(11) 0.0045(10) -0.0025(8) 0.0045(9) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti N1 1.8194(13) . . yes Ti N4 1.8276(13) . . yes Ti C23 2.114(2) . . yes Ti C24 2.110(2) . . yes N1 C1 1.300(2) . . yes N2 C1 1.388(2) . . yes N2 C2 1.388(2) . . yes N2 C4 1.495(2) . . yes N3 C1 1.383(2) . . yes N3 C3 1.390(2) . . yes N3 C8 1.500(2) . . yes N4 C12 1.299(2) . . yes N5 C12 1.388(2) . . yes N5 C13 1.396(2) . . yes N5 C15 1.491(2) . . yes N6 C12 1.390(2) . . yes N6 C14 1.381(2) . . yes N6 C19 1.496(2) . . yes C2 C3 1.325(3) . . no C4 C5 1.526(2) . . no C4 C6 1.524(3) . . no C4 C7 1.527(3) . . no C8 C9 1.519(3) . . no C8 C10 1.523(3) . . no C8 C11 1.527(3) . . no C13 C14 1.312(3) . . no C15 C16 1.531(3) . . no C15 C17 1.526(3) . . no C15 C18 1.524(3) . . no C19 C20 1.531(3) . . no C19 C21 1.521(3) . . no C19 C22 1.519(3) . . no C2 H21 0.89(2) . . no C3 H31 0.94(2) . . no C5 H51 0.94(2) . . no C5 H52 0.996(19) . . no C5 H53 0.96(2) . . no C6 H61 0.94(2) . . no C6 H62 0.97(2) . . no C6 H63 0.93(2) . . no C7 H71 0.98(2) . . no C7 H72 0.96(2) . . no C7 H73 0.97(2) . . no C9 H91 0.97(2) . . no C9 H92 0.95(2) . . no C9 H93 0.94(2) . . no C10 H101 0.97(2) . . no C10 H102 0.99(2) . . no C10 H103 1.01(2) . . no C11 H111 0.97(2) . . no C11 H112 0.90(3) . . no C11 H113 1.00(3) . . no C13 H131 0.87(2) . . no C14 H141 0.93(2) . . no C16 H161 0.95(3) . . no C16 H162 1.00(3) . . no C16 H163 0.96(3) . . no C17 H171 0.99(2) . . no C17 H172 0.94(2) . . no C17 H173 0.95(2) . . no C18 H181 0.99(2) . . no C18 H182 0.95(2) . . no C18 H183 0.96(2) . . no C20 H201 0.97(3) . . no C20 H202 1.01(3) . . no C20 H203 0.98(3) . . no C21 H211 1.01(3) . . no C21 H212 0.95(3) . . no C21 H213 0.960(19) . . no C22 H221 0.95(3) . . no C22 H222 0.96(2) . . no C22 H223 0.96(3) . . no C23 H231 0.84(3) . . no C23 H232 1.02(3) . . no C23 H233 0.85(3) . . no C24 H241 0.89(3) . . no C24 H242 0.90(3) . . no C24 H243 0.93(3) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti N4 116.36(6) . . . yes N1 Ti C23 105.75(8) . . . yes N1 Ti C24 109.68(7) . . . yes N4 Ti C23 109.81(8) . . . yes N4 Ti C24 109.65(8) . . . yes C23 Ti C24 104.92(8) . . . yes Ti N1 C1 176.13(12) . . . yes C1 N2 C2 108.87(13) . . . yes C1 N2 C4 125.00(13) . . . yes C2 N2 C4 125.83(13) . . . yes C1 N3 C3 109.12(13) . . . yes C1 N3 C8 124.48(13) . . . yes C3 N3 C8 126.36(13) . . . yes Ti N4 C12 171.93(12) . . . yes C12 N5 C13 108.12(15) . . . yes C12 N5 C15 125.49(13) . . . yes C13 N5 C15 126.38(16) . . . yes C12 N6 C14 108.95(15) . . . yes C12 N6 C19 125.47(14) . . . yes C14 N6 C19 125.55(15) . . . yes N1 C1 N2 128.08(14) . . . yes N1 C1 N3 126.68(14) . . . yes N2 C1 N3 105.24(12) . . . yes N2 C2 C3 108.57(15) . . . yes N3 C3 C2 108.21(15) . . . yes N2 C4 C5 108.46(13) . . . yes N2 C4 C6 109.23(14) . . . yes N2 C4 C7 109.26(14) . . . yes C5 C4 C6 111.37(15) . . . no C5 C4 C7 109.31(15) . . . no C6 C4 C7 109.19(14) . . . no N3 C8 C9 109.12(14) . . . yes N3 C8 C10 108.93(14) . . . yes N3 C8 C11 108.55(15) . . . yes C9 C8 C10 111.91(16) . . . no C9 C8 C11 108.54(16) . . . no C10 C8 C11 109.73(18) . . . no N4 C12 N5 127.21(15) . . . yes N4 C12 N6 127.49(15) . . . yes N5 C12 N6 105.28(13) . . . yes N5 C13 C14 108.92(18) . . . yes N6 C14 C13 108.70(17) . . . yes N5 C15 C16 108.93(17) . . . yes N5 C15 C17 109.04(16) . . . yes N5 C15 C18 109.75(15) . . . yes C16 C15 C17 108.60(17) . . . no C16 C15 C18 109.10(19) . . . no C17 C15 C18 111.37(18) . . . no N6 C19 C20 109.71(17) . . . yes N6 C19 C21 108.91(16) . . . yes N6 C19 C22 109.20(16) . . . yes C20 C19 C21 108.60(17) . . . no C20 C19 C22 108.92(19) . . . no C21 C19 C22 111.48(18) . . . no N2 C2 H21 121.9(13) . . . no C3 C2 H21 129.6(13) . . . no N3 C3 H31 120.4(12) . . . no C2 C3 H31 131.3(12) . . . no C4 C5 H51 111.1(13) . . . no C4 C5 H52 110.3(11) . . . no C4 C5 H53 110.6(12) . . . no H51 C5 H52 107.8(16) . . . no H51 C5 H53 108.0(17) . . . no H52 C5 H53 108.9(16) . . . no C4 C6 H61 107.3(14) . . . no C4 C6 H62 109.8(13) . . . no C4 C6 H63 112.6(12) . . . no H61 C6 H62 107.3(19) . . . no H61 C6 H63 114.3(19) . . . no H62 C6 H63 105.4(18) . . . no C4 C7 H71 112.3(12) . . . no C4 C7 H72 108.4(13) . . . no C4 C7 H73 110.1(14) . . . no H71 C7 H72 108.0(18) . . . no H71 C7 H73 110.2(18) . . . no H72 C7 H73 107.7(19) . . . no C8 C9 H91 108.0(12) . . . no C8 C9 H92 107.7(12) . . . no C8 C9 H93 113.4(13) . . . no H91 C9 H92 111.8(17) . . . no H91 C9 H93 107.3(17) . . . no H92 C9 H93 108.7(18) . . . no C8 C10 H101 112.2(13) . . . no C8 C10 H102 114.0(12) . . . no C8 C10 H103 109.0(13) . . . no H101 C10 H102 102.2(18) . . . no H101 C10 H103 113.0(18) . . . no H102 C10 H103 106.2(18) . . . no C8 C11 H111 107.9(14) . . . no C8 C11 H112 106.0(17) . . . no C8 C11 H113 114.4(16) . . . no H111 C11 H112 110(2) . . . no H111 C11 H113 107(2) . . . no H112 C11 H113 112(2) . . . no N5 C13 H131 119.6(14) . . . no C14 C13 H131 131.4(14) . . . no N6 C14 H141 120.0(14) . . . no C13 C14 H141 131.2(14) . . . no C15 C16 H161 110.9(16) . . . no C15 C16 H162 105.8(17) . . . no C15 C16 H163 109.5(14) . . . no H161 C16 H162 117(2) . . . no H161 C16 H163 110(2) . . . no H162 C16 H163 104(2) . . . no C15 C17 H171 109.4(13) . . . no C15 C17 H172 112.1(12) . . . no C15 C17 H173 107.8(13) . . . no H171 C17 H172 109.6(18) . . . no H171 C17 H173 109.8(19) . . . no H172 C17 H173 108.0(18) . . . no C15 C18 H181 110.8(13) . . . no C15 C18 H182 108.2(14) . . . no C15 C18 H183 112.0(11) . . . no H181 C18 H182 108.4(18) . . . no H181 C18 H183 109.4(18) . . . no H182 C18 H183 107.9(18) . . . no C19 C20 H201 109.9(16) . . . no C19 C20 H202 107.0(16) . . . no C19 C20 H203 109.5(15) . . . no H201 C20 H202 112(2) . . . no H201 C20 H203 105(2) . . . no H202 C20 H203 113(2) . . . no C19 C21 H211 114.4(14) . . . no C19 C21 H212 106.9(14) . . . no C19 C21 H213 110.8(12) . . . no H211 C21 H212 103(2) . . . no H211 C21 H213 107.9(19) . . . no H212 C21 H213 113.5(18) . . . no C19 C22 H221 106.1(15) . . . no C19 C22 H222 114.0(14) . . . no C19 C22 H223 108.2(16) . . . no H221 C22 H222 109(2) . . . no H221 C22 H223 109(2) . . . no H222 C22 H223 111(2) . . . no Ti C23 H231 122.4(19) . . . no Ti C23 H232 112.5(16) . . . no Ti C23 H233 111(2) . . . no H231 C23 H232 99(2) . . . no H231 C23 H233 105(3) . . . no H232 C23 H233 106(3) . . . no Ti C24 H241 113.4(17) . . . no Ti C24 H242 110.2(18) . . . no Ti C24 H243 129.9(16) . . . no H241 C24 H242 107(2) . . . no H241 C24 H243 98(2) . . . no H242 C24 H243 96(2) . . . no #===END # CIF-file generated for RANI 4414-123 # Compound 7 #=================================================================== data_RANI-4414-123 _database_code_depnum_ccdc_archive 'CCDC 281535' #=================================================================== #=================================================================== # 5. CHEMICAL DATA #=================================================================== _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C18 H31 N3 Ti' _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H31 N3 Ti' _chemical_formula_weight 337.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ti Ti 0.2776 0.4457 '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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' #=================================================================== # 6. CRYSTAL DATA #=================================================================== _symmetry_cell_setting Monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 11.0252(1) _cell_length_b 10.1497(1) _cell_length_c 16.7456(2) _cell_angle_alpha 90 _cell_angle_beta 90.3793(5) _cell_angle_gamma 90 _cell_volume 1873.83(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used 3647 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.39 _exptl_crystal_description fragment _exptl_crystal_colour orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.196 _exptl_crystal_density_method none _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 0.458 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.794 _exptl_absorpt_correction_T_max 0.878 _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_special_details ; Diffractometer operator E. Herdtweck scanspeed 2 x 10 s per film repetition 1 dx 40 526 films measured in 9 data sets set 1: phi-scan with delta_phi = 2.0 set 2 to 9: omega-scans with delta_omega = 2.0 ; _publ_section_exptl_prep ; The crystal was fixed in a capillary with perfluorinated ether and transferred to the diffractometer. ; _publ_section_exptl_refinement ; Straight forward after integration with the program NPROCESS, source: Nonius (2001b). Hydrogen atoms could be located in the difference Fourier maps and were allowed to refine freely. ; #=================================================================== # 7. EXPERIMENTAL DATA #=================================================================== _diffrn_ambient_temperature 123(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 # 9 for binned mode _diffrn_standards_decay_% 0 # number of measured reflections (redundant set) _diffrn_reflns_number 43438 _diffrn_reflns_av_R_equivalents 0.042 _diffrn_reflns_av_sigmaI/netI 0.0189 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.39 _reflns_number_total 3434 _reflns_number_gt 3034 # number of observed reflections (> n sig(I)) _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' #=================================================================== # 8. REFINEMENT DATA #=================================================================== _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme sigma _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0371P)^2^+1.2374P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_number_reflns 3434 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0381 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0760 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.39 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.243 _refine_diff_density_min -0.312 _refine_diff_density_rms 0.044 #=================================================================== # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS #=================================================================== loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags Ti Ti Uani 0.42704(3) 0.17524(3) 0.36094(2) 1.000 0.0182(1) . . N1 N Uani 0.48217(12) 0.27405(13) 0.27925(8) 1.000 0.0181(4) . . N2 N Uani 0.49703(11) 0.32847(13) 0.13896(7) 1.000 0.0178(4) . . N3 N Uani 0.57916(12) 0.46741(13) 0.22511(8) 1.000 0.0194(4) . . C1 C Uani 0.51490(14) 0.35025(15) 0.22006(9) 1.000 0.0168(4) . . C2 C Uani 0.55467(15) 0.42749(18) 0.09660(10) 1.000 0.0244(5) . . C3 C Uani 0.60397(16) 0.51184(18) 0.14852(10) 1.000 0.0254(5) . . C4 C Uani 0.43283(14) 0.21329(16) 0.10225(9) 1.000 0.0197(5) . . C5 C Uani 0.42204(17) 0.2358(2) 0.01208(10) 1.000 0.0265(6) . . C6 C Uani 0.30601(15) 0.20145(19) 0.13685(11) 1.000 0.0239(5) . . C7 C Uani 0.50808(17) 0.08991(18) 0.11784(11) 1.000 0.0277(6) . . C8 C Uani 0.61794(14) 0.53468(16) 0.30049(10) 1.000 0.0209(5) . . C9 C Uani 0.68365(18) 0.66310(18) 0.27985(12) 1.000 0.0285(6) . . C10 C Uani 0.50487(17) 0.5681(2) 0.34863(12) 1.000 0.0300(6) . . C11 C Uani 0.70345(17) 0.44377(18) 0.34594(11) 1.000 0.0267(6) . . C12 C Uani 0.4573(2) -0.02464(18) 0.32134(13) 1.000 0.0281(6) . . C13 C Uani 0.57229(19) 0.1777(2) 0.44819(12) 1.000 0.0275(6) . . C14 C Uani 0.25415(17) 0.0871(2) 0.43226(12) 1.000 0.0347(6) . . C15 C Uani 0.30097(17) 0.1878(2) 0.47900(11) 1.000 0.0328(6) . . C16 C Uani 0.2894(2) 0.3062(2) 0.43730(14) 1.000 0.0428(7) . . C17 C Uani 0.2330(2) 0.2784(3) 0.36459(15) 1.000 0.0553(9) . . C18 C Uani 0.21212(18) 0.1429(3) 0.36083(13) 1.000 0.0499(8) . . H21 H Uiso 0.5572(17) 0.4300(19) 0.0405(12) 1.000 0.029(5) . . H31 H Uiso 0.6473(17) 0.5886(19) 0.1386(10) 1.000 0.024(5) . . H51 H Uiso 0.3789(19) 0.161(2) -0.0105(12) 1.000 0.034(5) . . H52 H Uiso 0.3759(19) 0.316(2) 0.0000(12) 1.000 0.033(5) . . H53 H Uiso 0.4997(19) 0.2398(19) -0.0130(11) 1.000 0.030(5) . . H61 H Uiso 0.3084(19) 0.1821(19) 0.1920(13) 1.000 0.035(5) . . H62 H Uiso 0.2662(19) 0.133(2) 0.1109(12) 1.000 0.035(5) . . H63 H Uiso 0.261(2) 0.278(2) 0.1298(13) 1.000 0.041(6) . . H71 H Uiso 0.5202(18) 0.0760(19) 0.1723(13) 1.000 0.033(5) . . H72 H Uiso 0.587(2) 0.096(2) 0.0919(12) 1.000 0.040(6) . . H73 H Uiso 0.4624(18) 0.013(2) 0.0955(12) 1.000 0.035(5) . . H91 H Uiso 0.7538(19) 0.6468(18) 0.2505(12) 1.000 0.025(5) . . H92 H Uiso 0.6297(19) 0.722(2) 0.2512(12) 1.000 0.036(5) . . H93 H Uiso 0.7066(19) 0.705(2) 0.3313(13) 1.000 0.040(6) . . H101 H Uiso 0.455(2) 0.630(2) 0.3164(13) 1.000 0.046(6) . . H102 H Uiso 0.4549(17) 0.490(2) 0.3600(10) 1.000 0.025(5) . . H103 H Uiso 0.528(2) 0.612(2) 0.3984(13) 1.000 0.046(6) . . H111 H Uiso 0.6660(19) 0.360(2) 0.3551(12) 1.000 0.035(5) . . H112 H Uiso 0.7240(18) 0.482(2) 0.3964(13) 1.000 0.035(5) . . H113 H Uiso 0.778(2) 0.432(2) 0.3178(12) 1.000 0.037(5) . . H121 H Uiso 0.449(2) -0.075(3) 0.3618(15) 1.000 0.056(7) . . H122 H Uiso 0.411(2) -0.040(2) 0.2859(14) 1.000 0.040(7) . . H123 H Uiso 0.535(2) -0.025(2) 0.3046(14) 1.000 0.052(7) . . H131 H Uiso 0.632(2) 0.159(2) 0.4232(15) 1.000 0.045(7) . . H132 H Uiso 0.575(2) 0.251(3) 0.4690(14) 1.000 0.047(7) . . H133 H Uiso 0.556(2) 0.118(3) 0.4807(15) 1.000 0.051(7) . . H141 H Uiso 0.2533(19) -0.004(2) 0.4444(12) 1.000 0.042(6) . . H151 H Uiso 0.340(2) 0.179(2) 0.5307(15) 1.000 0.052(7) . . H161 H Uiso 0.320(2) 0.390(3) 0.4539(15) 1.000 0.059(7) . . H171 H Uiso 0.222(3) 0.338(3) 0.3314(19) 1.000 0.083(10) . . H181 H Uiso 0.181(2) 0.096(3) 0.3218(16) 1.000 0.065(8) . . 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 Ti 0.0184(2) 0.0199(2) 0.0164(2) 0.0027(1) 0.0016(1) -0.0026(1) N1 0.0180(7) 0.0187(7) 0.0177(7) -0.0007(5) 0.0003(5) -0.0022(5) N2 0.0174(7) 0.0213(7) 0.0147(6) 0.0007(5) 0.0010(5) -0.0004(5) N3 0.0206(7) 0.0193(7) 0.0183(7) 0.0016(5) 0.0020(5) -0.0040(5) C1 0.0150(7) 0.0192(8) 0.0163(7) -0.0005(6) 0.0019(6) 0.0015(6) C2 0.0235(9) 0.0315(9) 0.0182(8) 0.0076(7) 0.0049(7) -0.0022(7) C3 0.0252(9) 0.0273(9) 0.0237(9) 0.0077(7) 0.0044(7) -0.0060(8) C4 0.0187(8) 0.0222(8) 0.0183(8) -0.0030(6) -0.0009(6) 0.0015(6) C5 0.0281(10) 0.0335(11) 0.0180(9) -0.0023(8) -0.0015(7) 0.0028(8) C6 0.0183(8) 0.0296(10) 0.0239(9) -0.0018(8) -0.0019(7) -0.0013(7) C7 0.0289(10) 0.0273(10) 0.0269(10) -0.0032(8) -0.0036(8) 0.0077(8) C8 0.0221(8) 0.0189(8) 0.0217(8) -0.0032(6) -0.0001(6) -0.0047(6) C9 0.0294(10) 0.0224(9) 0.0338(10) -0.0013(8) 0.0028(8) -0.0058(8) C10 0.0286(10) 0.0280(10) 0.0336(10) -0.0087(9) 0.0080(8) -0.0042(8) C11 0.0243(9) 0.0244(10) 0.0313(10) 0.0002(8) -0.0062(8) -0.0072(7) C12 0.0362(11) 0.0222(9) 0.0260(10) 0.0063(8) 0.0042(9) -0.0046(8) C13 0.0304(11) 0.0339(11) 0.0183(9) 0.0098(9) -0.0010(8) -0.0087(9) C14 0.0296(10) 0.0365(11) 0.0381(11) 0.0021(9) 0.0141(8) -0.0099(8) C15 0.0311(10) 0.0430(12) 0.0243(9) -0.0002(8) 0.0105(8) -0.0031(8) C16 0.0441(12) 0.0336(12) 0.0511(14) 0.0005(10) 0.0278(11) 0.0034(10) C17 0.0313(11) 0.0809(19) 0.0540(15) 0.0385(14) 0.0221(11) 0.0288(12) C18 0.0177(10) 0.098(2) 0.0339(12) -0.0067(13) 0.0022(8) -0.0089(11) #================================================================== # 10. MOLECULAR GEOMETRY #=================================================================== loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti N1 1.8049(14) . . yes Ti C12 2.1609(19) . . yes Ti C13 2.161(2) . . yes Ti C14 2.427(2) . . yes Ti C15 2.4276(19) . . yes Ti C16 2.394(2) . . yes Ti C17 2.383(2) . . yes Ti C18 2.392(2) . . yes N1 C1 1.310(2) . . yes N2 C1 1.3887(19) . . yes N2 C2 1.387(2) . . yes N2 C4 1.497(2) . . yes N3 C1 1.386(2) . . yes N3 C3 1.388(2) . . yes N3 C8 1.495(2) . . yes C2 C3 1.333(2) . . no C4 C5 1.531(2) . . no C4 C6 1.522(2) . . no C4 C7 1.524(2) . . no C8 C9 1.532(2) . . no C8 C10 1.527(2) . . no C8 C11 1.520(2) . . no C14 C15 1.385(3) . . no C14 C18 1.400(3) . . no C15 C16 1.395(3) . . no C16 C17 1.392(3) . . no C17 C18 1.396(4) . . no C2 H21 0.94(2) . . no C3 H31 0.929(19) . . no C5 H51 0.97(2) . . no C5 H52 0.98(2) . . no C5 H53 0.96(2) . . no C6 H61 0.94(2) . . no C6 H62 0.93(2) . . no C6 H63 0.93(2) . . no C7 H71 0.93(2) . . no C7 H72 0.98(2) . . no C7 H73 1.00(2) . . no C9 H91 0.93(2) . . no C9 H92 0.97(2) . . no C9 H93 0.99(2) . . no C10 H101 0.99(2) . . no C10 H102 0.98(2) . . no C10 H103 0.98(2) . . no C11 H111 0.96(2) . . no C11 H112 0.96(2) . . no C11 H113 0.96(2) . . no C12 H121 0.85(3) . . no C12 H122 0.80(2) . . no C12 H123 0.90(2) . . no C13 H131 0.81(2) . . no C13 H132 0.82(3) . . no C13 H133 0.83(3) . . no C14 H141 0.95(2) . . no C15 H151 0.97(2) . . no C16 H161 0.96(3) . . no C17 H171 0.83(3) . . no C18 H181 0.88(3) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti C12 103.63(7) . . . yes N1 Ti C13 104.73(7) . . . yes N1 Ti C14 147.92(6) . . . yes N1 Ti C15 141.77(7) . . . yes N1 Ti C16 108.31(7) . . . yes N1 Ti C17 94.71(8) . . . yes N1 Ti C18 114.47(7) . . . yes C12 Ti C13 95.92(8) . . . yes C12 Ti C14 85.89(8) . . . yes C12 Ti C15 112.93(8) . . . yes C12 Ti C16 141.71(8) . . . yes C12 Ti C17 124.11(9) . . . yes C12 Ti C18 91.48(9) . . . yes C13 Ti C14 104.63(7) . . . yes C13 Ti C15 82.79(7) . . . yes C13 Ti C16 95.85(8) . . . yes C13 Ti C17 129.72(8) . . . yes C13 Ti C18 137.04(8) . . . yes C14 Ti C15 33.15(7) . . . yes C14 Ti C16 55.88(7) . . . yes C14 Ti C17 56.03(8) . . . yes C14 Ti C18 33.76(7) . . . yes C15 Ti C16 33.63(7) . . . yes C15 Ti C17 55.74(8) . . . yes C15 Ti C18 55.62(7) . . . yes C16 Ti C17 33.89(8) . . . yes C16 Ti C18 56.30(8) . . . yes C17 Ti C18 33.99(10) . . . yes Ti N1 C1 175.96(12) . . . yes C1 N2 C2 108.80(13) . . . yes C1 N2 C4 126.13(12) . . . yes C2 N2 C4 124.97(12) . . . yes C1 N3 C3 109.02(13) . . . yes C1 N3 C8 125.90(13) . . . yes C3 N3 C8 125.07(13) . . . yes N1 C1 N2 127.45(14) . . . yes N1 C1 N3 127.12(14) . . . yes N2 C1 N3 105.39(13) . . . yes N2 C2 C3 108.54(15) . . . yes N3 C3 C2 108.17(15) . . . yes N2 C4 C5 108.78(13) . . . yes N2 C4 C6 109.79(13) . . . yes N2 C4 C7 108.43(13) . . . yes C5 C4 C6 108.77(14) . . . no C5 C4 C7 109.29(14) . . . no C6 C4 C7 111.74(14) . . . no N3 C8 C9 109.34(14) . . . yes N3 C8 C10 108.50(13) . . . yes N3 C8 C11 108.57(13) . . . yes C9 C8 C10 108.60(14) . . . no C9 C8 C11 109.68(14) . . . no C10 C8 C11 112.11(15) . . . no Ti C14 C15 73.45(11) . . . yes Ti C14 C18 71.76(12) . . . yes C15 C14 C18 107.7(2) . . . no Ti C15 C14 73.40(11) . . . yes Ti C15 C16 71.86(12) . . . yes C14 C15 C16 108.68(18) . . . no Ti C16 C15 74.51(12) . . . yes Ti C16 C17 72.63(14) . . . yes C15 C16 C17 107.6(2) . . . no Ti C17 C16 73.48(13) . . . yes Ti C17 C18 73.37(14) . . . yes C16 C17 C18 108.2(2) . . . no Ti C18 C14 74.49(11) . . . yes Ti C18 C17 72.64(13) . . . yes C14 C18 C17 107.9(2) . . . no N2 C2 H21 123.2(12) . . . no C3 C2 H21 128.3(12) . . . no N3 C3 H31 122.8(11) . . . no C2 C3 H31 129.0(11) . . . no C4 C5 H51 107.6(12) . . . no C4 C5 H52 111.4(12) . . . no C4 C5 H53 112.0(11) . . . no H51 C5 H52 108.5(17) . . . no H51 C5 H53 107.4(17) . . . no H52 C5 H53 109.8(17) . . . no C4 C6 H61 111.7(13) . . . no C4 C6 H62 108.3(13) . . . no C4 C6 H63 112.1(14) . . . no H61 C6 H62 108.2(17) . . . no H61 C6 H63 108.0(18) . . . no H62 C6 H63 108.4(19) . . . no C4 C7 H71 111.5(12) . . . no C4 C7 H72 110.9(12) . . . no C4 C7 H73 107.8(12) . . . no H71 C7 H72 108.8(17) . . . no H71 C7 H73 108.4(17) . . . no H72 C7 H73 109.3(17) . . . no C8 C9 H91 111.3(11) . . . no C8 C9 H92 110.3(12) . . . no C8 C9 H93 106.7(12) . . . no H91 C9 H92 110.9(17) . . . no H91 C9 H93 109.0(17) . . . no H92 C9 H93 108.5(17) . . . no C8 C10 H101 107.8(13) . . . no C8 C10 H102 112.5(11) . . . no C8 C10 H103 110.0(13) . . . no H101 C10 H102 107.8(17) . . . no H101 C10 H103 108.4(17) . . . no H102 C10 H103 110.2(16) . . . no C8 C11 H111 110.6(13) . . . no C8 C11 H112 109.8(12) . . . no C8 C11 H113 111.2(12) . . . no H111 C11 H112 108.6(17) . . . no H111 C11 H113 109.9(18) . . . no H112 C11 H113 106.6(17) . . . no Ti C12 H121 107.5(19) . . . no Ti C12 H122 108.3(15) . . . no Ti C12 H123 104.3(13) . . . no H121 C12 H122 114(2) . . . no H121 C12 H123 111(2) . . . no H122 C12 H123 112(2) . . . no Ti C13 H131 104.5(17) . . . no Ti C13 H132 108.8(16) . . . no Ti C13 H133 105.7(16) . . . no H131 C13 H132 114(2) . . . no H131 C13 H133 110(2) . . . no H132 C13 H133 113(3) . . . no Ti C14 H141 118.3(13) . . . no C15 C14 H141 127.1(12) . . . no C18 C14 H141 125.1(12) . . . no Ti C15 H151 118.0(13) . . . no C14 C15 H151 126.8(12) . . . no C16 C15 H151 124.4(12) . . . no Ti C16 H161 115.2(14) . . . no C15 C16 H161 126.2(15) . . . no C17 C16 H161 126.1(15) . . . no Ti C17 H171 115(2) . . . no C16 C17 H171 120(2) . . . no C18 C17 H171 132(2) . . . no Ti C18 H181 117.2(15) . . . no C14 C18 H181 123(2) . . . no C17 C18 H181 129(2) . . . no # End of Crystallographic Information File