Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'A.Blake' 'J.B.Love' 'Andrew Novak' 'Claire Wilson' _publ_contact_author_name 'Jason B. Love' _publ_contact_author_address ; School of Chemistry University of Nottingham Nottingham NG7 2RD UK ; _publ_contact_author_email 'JASON.LOVE@NOTTINGHAM.AC.UK' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Titanium and zirconium complexes supported by dipyrrolide ligands ; data_ZRPHYR _database_code_CSD 193472 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C53 H54 N2 Zr2' _chemical_formula_sum 'C53 H54 N2 Zr2' _chemical_formula_weight 901.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.8621(13) _cell_length_b 11.2299(8) _cell_length_c 20.6506(14) _cell_angle_alpha 90.00 _cell_angle_beta 96.096(2) _cell_angle_gamma 90.00 _cell_volume 4349.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5511 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 24.65 _exptl_crystal_description tablet _exptl_crystal_colour orange _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.377 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 0.517 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.942 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'normal-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 33815 _diffrn_reflns_av_R_equivalents 0.055 _diffrn_reflns_av_sigmaI/netI 0.045 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7620 _reflns_number_gt 5686 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0164P)^2^+5.2349P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7620 _refine_ls_number_parameters 514 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.156114(16) 0.11625(3) 0.329037(15) 0.02296(8) Uani 1 1 d . . . Zr2 Zr 0.290938(15) 0.33469(3) 0.405558(15) 0.02154(8) Uani 1 1 d . . . N1 N 0.19442(13) 0.3257(2) 0.32464(12) 0.0234(6) Uani 1 1 d . . . N2 N 0.27911(12) 0.1402(2) 0.34978(12) 0.0220(6) Uani 1 1 d . . . C2 C 0.08495(17) 0.3042(3) 0.26850(16) 0.0294(8) Uani 1 1 d . . . H2A H 0.0323 0.3106 0.2563 0.035 Uiso 1 1 calc R . . C3 C 0.13606(17) 0.2623(3) 0.22851(16) 0.0285(8) Uani 1 1 d . . . H3A H 0.1267 0.2387 0.1817 0.034 Uiso 1 1 calc R . . C1 C 0.12234(16) 0.3438(3) 0.32530(16) 0.0270(7) Uani 1 1 d . . . H1A H 0.1004 0.3868 0.3607 0.032 Uiso 1 1 calc R . . C4 C 0.20232(17) 0.2773(3) 0.26331(15) 0.0248(7) Uani 1 1 d . . . C5 C 0.27664(17) 0.2510(3) 0.24615(15) 0.0270(7) Uani 1 1 d . . . C6 C 0.31656(16) 0.2092(3) 0.30931(15) 0.0259(7) Uani 1 1 d . . . C7 C 0.38605(17) 0.2265(3) 0.33730(16) 0.0295(8) Uani 1 1 d . . . H7A H 0.4256 0.2654 0.3166 0.035 Uiso 1 1 calc R . . C8 C 0.39165(16) 0.1670(3) 0.39778(16) 0.0287(8) Uani 1 1 d . . . H8A H 0.4361 0.1568 0.4283 0.034 Uiso 1 1 calc R . . C9 C 0.32658(16) 0.1146(3) 0.40343(15) 0.0259(7) Uani 1 1 d . . . H9A H 0.3176 0.0554 0.4378 0.031 Uiso 1 1 calc R . . C10 C 0.31022(19) 0.3645(3) 0.22109(17) 0.0382(9) Uani 1 1 d . . . H10A H 0.3108 0.4270 0.2542 0.057 Uiso 1 1 calc R . . H10B H 0.2821 0.3913 0.1811 0.057 Uiso 1 1 calc R . . H10C H 0.3591 0.3475 0.2120 0.057 Uiso 1 1 calc R . . C11 C 0.27526(18) 0.1524(3) 0.19457(16) 0.0357(8) Uani 1 1 d . . . H11A H 0.2535 0.0806 0.2108 0.054 Uiso 1 1 calc R . . H11B H 0.3241 0.1346 0.1855 0.054 Uiso 1 1 calc R . . H11C H 0.2473 0.1791 0.1545 0.054 Uiso 1 1 calc R . . C12 C 0.11762(17) 0.1454(3) 0.42875(16) 0.0338(8) Uani 1 1 d . . . H12A H 0.1453 0.0971 0.4627 0.041 Uiso 1 1 calc R . . H12B H 0.1203 0.2304 0.4415 0.041 Uiso 1 1 calc R . . C13 C 0.04288(17) 0.1042(3) 0.41712(15) 0.0315(8) Uani 1 1 d . . . C14 C 0.02474(19) -0.0155(3) 0.42310(16) 0.0377(9) Uani 1 1 d . . . H14A H 0.0609 -0.0713 0.4375 0.045 Uiso 1 1 calc R . . C15 C -0.0445(2) -0.0546(4) 0.40863(17) 0.0455(10) Uani 1 1 d . . . H15A H -0.0553 -0.1366 0.4132 0.055 Uiso 1 1 calc R . . C16 C -0.0977(2) 0.0235(4) 0.3878(2) 0.0603(12) Uani 1 1 d . . . H16A H -0.1452 -0.0039 0.3775 0.072 Uiso 1 1 calc R . . C17 C -0.0814(2) 0.1432(4) 0.3820(2) 0.0577(12) Uani 1 1 d . . . H17A H -0.1182 0.1983 0.3681 0.069 Uiso 1 1 calc R . . C18 C -0.01236(19) 0.1831(3) 0.39616(18) 0.0428(9) Uani 1 1 d . . . H18A H -0.0021 0.2653 0.3917 0.051 Uiso 1 1 calc R . . C19 C 0.07898(18) 0.0094(3) 0.25629(16) 0.0339(8) Uani 1 1 d . . . H19A H 0.1057 -0.0635 0.2470 0.041 Uiso 1 1 calc R . . H19B H 0.0404 -0.0173 0.2819 0.041 Uiso 1 1 calc R . . C20 C 0.04198(16) 0.0459(3) 0.19231(15) 0.0246(7) Uani 1 1 d . . . C21 C 0.07232(18) 0.0247(3) 0.13486(17) 0.0349(8) Uani 1 1 d . . . H21A H 0.1160 -0.0178 0.1367 0.042 Uiso 1 1 calc R . . C23 C -0.0229(2) 0.1242(3) 0.07098(18) 0.0433(10) Uani 1 1 d . . . H23A H -0.0443 0.1519 0.0300 0.052 Uiso 1 1 calc R . . C22 C 0.0408(2) 0.0636(3) 0.07554(18) 0.0438(10) Uani 1 1 d . . . H22A H 0.0633 0.0485 0.0373 0.053 Uiso 1 1 calc R . . C24 C -0.05487(18) 0.1438(3) 0.12613(18) 0.0373(9) Uani 1 1 d . . . H24A H -0.0994 0.1840 0.1233 0.045 Uiso 1 1 calc R . . C25 C -0.02337(16) 0.1059(3) 0.18636(16) 0.0299(8) Uani 1 1 d . . . H25A H -0.0465 0.1210 0.2242 0.036 Uiso 1 1 calc R . . C26 C 0.19240(16) -0.0717(3) 0.36071(15) 0.0280(7) Uani 1 1 d . . . H26A H 0.2216 -0.0632 0.4032 0.034 Uiso 1 1 calc R . . H26B H 0.1490 -0.1160 0.3692 0.034 Uiso 1 1 calc R . . C27 C 0.23317(17) -0.1510(3) 0.31993(15) 0.0272(7) Uani 1 1 d . . . C28 C 0.30710(17) -0.1427(3) 0.31939(16) 0.0308(8) Uani 1 1 d . . . H28A H 0.3322 -0.0828 0.3449 0.037 Uiso 1 1 calc R . . C29 C 0.34475(17) -0.2179(3) 0.28334(16) 0.0309(8) Uani 1 1 d . . . H29A H 0.3949 -0.2089 0.2843 0.037 Uiso 1 1 calc R . . C30 C 0.31046(18) -0.3065(3) 0.24568(16) 0.0329(8) Uani 1 1 d . . . H30A H 0.3364 -0.3587 0.2208 0.039 Uiso 1 1 calc R . . C31 C 0.23765(18) -0.3172(3) 0.24510(17) 0.0362(9) Uani 1 1 d . . . H31A H 0.2131 -0.3780 0.2198 0.043 Uiso 1 1 calc R . . C32 C 0.19996(17) -0.2405(3) 0.28083(16) 0.0312(8) Uani 1 1 d . . . H32A H 0.1497 -0.2489 0.2787 0.037 Uiso 1 1 calc R . . C33 C 0.37461(16) 0.4771(3) 0.40453(17) 0.0312(8) Uani 1 1 d . . . H33A H 0.3520 0.5409 0.3764 0.037 Uiso 1 1 calc R . . H33B H 0.3802 0.5099 0.4493 0.037 Uiso 1 1 calc R . . C34 C 0.44847(16) 0.4668(3) 0.38589(16) 0.0275(8) Uani 1 1 d . . . C35 C 0.50274(16) 0.4126(3) 0.42697(16) 0.0301(8) Uani 1 1 d . . . H35A H 0.4931 0.3870 0.4690 0.036 Uiso 1 1 calc R . . C36 C 0.56984(17) 0.3953(3) 0.40796(17) 0.0342(8) Uani 1 1 d . . . H36A H 0.6057 0.3583 0.4369 0.041 Uiso 1 1 calc R . . C37 C 0.58523(18) 0.4311(3) 0.34741(18) 0.0373(9) Uani 1 1 d . . . H37A H 0.6312 0.4176 0.3341 0.045 Uiso 1 1 calc R . . C39 C 0.46605(17) 0.5054(3) 0.32537(17) 0.0318(8) Uani 1 1 d . . . H39A H 0.4311 0.5452 0.2967 0.038 Uiso 1 1 calc R . . C38 C 0.53319(18) 0.4871(3) 0.30614(17) 0.0372(9) Uani 1 1 d . . . H38A H 0.5436 0.5130 0.2644 0.045 Uiso 1 1 calc R . . C40 C 0.29261(17) 0.2781(3) 0.51293(15) 0.0290(8) Uani 1 1 d . . . H40A H 0.2877 0.3518 0.5384 0.035 Uiso 1 1 calc R . . H40B H 0.2489 0.2307 0.5162 0.035 Uiso 1 1 calc R . . C41 C 0.35266(17) 0.2098(3) 0.54723(14) 0.0258(7) Uani 1 1 d . . . C42 C 0.41702(18) 0.2668(3) 0.56770(16) 0.0327(8) Uani 1 1 d . . . H42A H 0.4208 0.3504 0.5619 0.039 Uiso 1 1 calc R . . C43 C 0.47544(19) 0.2042(3) 0.59623(18) 0.0425(9) Uani 1 1 d . . . H43A H 0.5187 0.2449 0.6093 0.051 Uiso 1 1 calc R . . C44 C 0.4712(2) 0.0834(4) 0.60573(18) 0.0479(10) Uani 1 1 d . . . H44A H 0.5116 0.0406 0.6247 0.057 Uiso 1 1 calc R . . C45 C 0.4079(2) 0.0246(3) 0.58767(17) 0.0403(9) Uani 1 1 d . . . H45A H 0.4044 -0.0587 0.5946 0.048 Uiso 1 1 calc R . . C46 C 0.34960(18) 0.0879(3) 0.55932(15) 0.0316(8) Uani 1 1 d . . . H46A H 0.3061 0.0468 0.5477 0.038 Uiso 1 1 calc R . . C47 C 0.21678(16) 0.4826(3) 0.43407(16) 0.0286(8) Uani 1 1 d . . . H47A H 0.1996 0.5237 0.3929 0.034 Uiso 1 1 calc R . . H47B H 0.1748 0.4416 0.4486 0.034 Uiso 1 1 calc R . . C48 C 0.23531(16) 0.5793(3) 0.48280(16) 0.0267(7) Uani 1 1 d . . . C49 C 0.22374(16) 0.5681(3) 0.54817(16) 0.0297(8) Uani 1 1 d . . . H49A H 0.2046 0.4958 0.5627 0.036 Uiso 1 1 calc R . . C50 C 0.23938(16) 0.6593(3) 0.59221(16) 0.0318(8) Uani 1 1 d . . . H50A H 0.2306 0.6491 0.6363 0.038 Uiso 1 1 calc R . . C51 C 0.26770(17) 0.7653(3) 0.57265(17) 0.0330(8) Uani 1 1 d . . . H51A H 0.2781 0.8284 0.6028 0.040 Uiso 1 1 calc R . . C52 C 0.28059(18) 0.7773(3) 0.50834(16) 0.0327(8) Uani 1 1 d . . . H52A H 0.3005 0.8492 0.4942 0.039 Uiso 1 1 calc R . . C53 C 0.26484(17) 0.6861(3) 0.46443(16) 0.0301(8) Uani 1 1 d . . . H53A H 0.2744 0.6964 0.4205 0.036 Uiso 1 1 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 Zr1 0.02437(16) 0.02233(17) 0.02140(17) -0.00010(13) -0.00117(12) 0.00017(13) Zr2 0.02189(16) 0.02045(16) 0.02166(17) -0.00302(13) -0.00051(12) 0.00228(13) N1 0.0261(14) 0.0211(14) 0.0222(15) -0.0022(12) -0.0016(11) 0.0039(11) N2 0.0241(14) 0.0198(14) 0.0214(14) -0.0034(11) -0.0002(11) 0.0010(11) C2 0.0271(18) 0.0241(18) 0.034(2) 0.0022(15) -0.0091(15) 0.0025(14) C3 0.038(2) 0.0234(18) 0.0222(18) 0.0012(14) -0.0056(15) 0.0001(15) C1 0.0239(17) 0.0233(17) 0.0328(19) -0.0033(15) -0.0014(14) 0.0049(14) C4 0.0339(19) 0.0186(16) 0.0211(18) 0.0016(14) -0.0001(14) -0.0001(14) C5 0.0313(18) 0.0277(18) 0.0214(18) -0.0005(14) 0.0009(14) 0.0003(14) C6 0.0274(18) 0.0229(17) 0.0278(19) -0.0065(14) 0.0051(14) 0.0011(14) C7 0.0266(18) 0.0281(19) 0.035(2) -0.0086(16) 0.0087(15) 0.0026(14) C8 0.0255(17) 0.0261(18) 0.033(2) -0.0106(16) -0.0042(14) 0.0082(14) C9 0.0329(18) 0.0184(16) 0.0246(18) -0.0042(14) -0.0057(14) 0.0069(14) C10 0.045(2) 0.038(2) 0.032(2) 0.0040(16) 0.0068(17) -0.0086(17) C11 0.041(2) 0.039(2) 0.027(2) -0.0050(16) 0.0034(15) 0.0014(16) C12 0.0329(19) 0.038(2) 0.031(2) 0.0041(16) 0.0059(15) 0.0043(15) C13 0.0341(19) 0.040(2) 0.0211(18) -0.0047(16) 0.0065(14) 0.0056(16) C14 0.045(2) 0.045(2) 0.025(2) -0.0015(17) 0.0097(16) 0.0068(18) C15 0.055(3) 0.047(2) 0.034(2) -0.0033(19) -0.0010(18) -0.008(2) C16 0.045(3) 0.062(3) 0.070(3) 0.001(2) -0.015(2) -0.009(2) C17 0.037(2) 0.058(3) 0.074(3) 0.002(2) -0.011(2) 0.012(2) C18 0.040(2) 0.041(2) 0.048(2) -0.0027(19) 0.0039(18) 0.0070(18) C19 0.040(2) 0.0278(19) 0.033(2) -0.0018(16) -0.0031(16) -0.0017(15) C20 0.0246(17) 0.0218(17) 0.0265(18) -0.0038(14) -0.0014(14) -0.0066(13) C21 0.033(2) 0.038(2) 0.034(2) -0.0132(17) 0.0020(16) -0.0017(16) C23 0.054(2) 0.042(2) 0.030(2) -0.0026(18) -0.0116(18) -0.0062(19) C22 0.051(2) 0.054(3) 0.026(2) -0.0129(18) 0.0028(17) -0.008(2) C24 0.034(2) 0.029(2) 0.045(2) -0.0063(17) -0.0130(17) 0.0004(15) C25 0.0277(18) 0.0295(19) 0.032(2) -0.0091(16) 0.0006(14) -0.0020(15) C26 0.0280(18) 0.0287(18) 0.0270(19) 0.0012(15) 0.0012(14) -0.0010(14) C27 0.0338(18) 0.0236(18) 0.0241(18) 0.0073(14) 0.0024(14) 0.0029(14) C28 0.0313(19) 0.0235(18) 0.036(2) 0.0015(15) -0.0016(15) -0.0003(14) C29 0.0267(18) 0.0309(19) 0.034(2) 0.0058(16) 0.0002(15) 0.0030(15) C30 0.040(2) 0.032(2) 0.0261(19) 0.0001(15) 0.0007(15) 0.0132(16) C31 0.042(2) 0.030(2) 0.034(2) -0.0007(16) -0.0074(16) 0.0021(16) C32 0.0288(18) 0.0293(19) 0.035(2) 0.0072(16) 0.0008(15) 0.0011(15) C33 0.0308(19) 0.0266(18) 0.036(2) -0.0057(15) 0.0008(15) 0.0021(15) C34 0.0248(17) 0.0215(17) 0.036(2) -0.0063(15) 0.0008(14) -0.0036(13) C35 0.0294(19) 0.0314(19) 0.0288(19) -0.0015(15) 0.0001(14) -0.0024(15) C36 0.0269(19) 0.037(2) 0.037(2) -0.0061(17) -0.0043(15) 0.0015(15) C37 0.0263(19) 0.042(2) 0.045(2) -0.0075(18) 0.0075(16) -0.0006(16) C39 0.0281(19) 0.0286(19) 0.037(2) 0.0026(16) -0.0038(15) -0.0021(15) C38 0.034(2) 0.045(2) 0.033(2) 0.0005(17) 0.0075(16) -0.0034(17) C40 0.0315(19) 0.0311(19) 0.0243(18) -0.0052(15) 0.0023(14) 0.0075(15) C41 0.0334(19) 0.0292(18) 0.0149(17) -0.0023(14) 0.0025(13) 0.0035(14) C42 0.039(2) 0.031(2) 0.0272(19) -0.0036(16) 0.0001(15) -0.0013(16) C43 0.037(2) 0.048(2) 0.040(2) -0.0064(19) -0.0093(17) 0.0032(18) C44 0.047(2) 0.051(3) 0.042(2) -0.004(2) -0.0095(18) 0.023(2) C45 0.061(3) 0.028(2) 0.030(2) -0.0028(16) -0.0031(18) 0.0105(18) C46 0.039(2) 0.032(2) 0.0226(18) -0.0020(15) -0.0001(15) -0.0051(16) C47 0.0287(18) 0.0280(18) 0.0284(19) -0.0036(15) -0.0001(14) 0.0008(14) C48 0.0205(16) 0.0276(18) 0.031(2) -0.0023(15) -0.0031(14) 0.0082(13) C49 0.0280(18) 0.0272(18) 0.034(2) -0.0018(16) 0.0041(15) -0.0009(14) C50 0.0291(18) 0.036(2) 0.0298(19) -0.0052(16) 0.0031(14) 0.0032(16) C51 0.038(2) 0.0261(19) 0.033(2) -0.0102(16) -0.0057(16) 0.0052(15) C52 0.042(2) 0.0225(18) 0.032(2) 0.0018(16) -0.0031(16) 0.0013(15) C53 0.043(2) 0.0257(19) 0.0201(18) 0.0004(14) -0.0019(15) 0.0069(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 C12 2.279(3) . ? Zr1 C26 2.293(3) . ? Zr1 C19 2.313(3) . ? Zr1 N2 2.330(2) . ? Zr1 N1 2.465(3) . ? Zr1 C4 2.475(3) . ? Zr1 C1 2.633(3) . ? Zr1 C3 2.642(3) . ? Zr1 C2 2.732(3) . ? Zr2 C33 2.248(3) . ? Zr2 C47 2.289(3) . ? Zr2 C40 2.303(3) . ? Zr2 N1 2.339(2) . ? Zr2 N2 2.468(2) . ? Zr2 C6 2.525(3) . ? Zr2 C9 2.563(3) . ? Zr2 C7 2.687(3) . ? Zr2 C8 2.692(3) . ? N1 C1 1.376(4) . ? N1 C4 1.400(4) . ? N2 C9 1.379(4) . ? N2 C6 1.386(4) . ? C2 C1 1.377(4) . ? C2 C3 1.415(4) . ? C3 C4 1.384(4) . ? C4 C5 1.511(4) . ? C5 C6 1.510(4) . ? C5 C11 1.535(4) . ? C5 C10 1.537(4) . ? C6 C7 1.389(4) . ? C7 C8 1.411(5) . ? C8 C9 1.377(4) . ? C12 C13 1.479(4) . ? C13 C14 1.395(5) . ? C13 C18 1.401(5) . ? C14 C15 1.380(5) . ? C15 C16 1.367(5) . ? C16 C17 1.387(6) . ? C17 C18 1.379(5) . ? C19 C20 1.485(4) . ? C20 C21 1.391(4) . ? C20 C25 1.399(4) . ? C21 C22 1.375(5) . ? C23 C24 1.362(5) . ? C23 C22 1.375(5) . ? C24 C25 1.387(5) . ? C26 C27 1.494(4) . ? C27 C32 1.395(4) . ? C27 C28 1.399(4) . ? C28 C29 1.372(4) . ? C29 C30 1.380(5) . ? C30 C31 1.377(5) . ? C31 C32 1.379(5) . ? C33 C34 1.489(4) . ? C34 C39 1.396(4) . ? C34 C35 1.398(4) . ? C35 C36 1.378(4) . ? C36 C37 1.374(5) . ? C37 C38 1.381(5) . ? C39 C38 1.382(5) . ? C40 C41 1.484(4) . ? C41 C46 1.394(4) . ? C41 C42 1.397(4) . ? C42 C43 1.385(5) . ? C43 C44 1.374(5) . ? C44 C45 1.379(5) . ? C45 C46 1.386(5) . ? C47 C48 1.496(4) . ? C48 C53 1.392(4) . ? C48 C49 1.396(4) . ? C49 C50 1.381(4) . ? C50 C51 1.382(5) . ? C51 C52 1.382(5) . ? C52 C53 1.379(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12 Zr1 C26 89.34(12) . . ? C12 Zr1 C19 115.00(12) . . ? C26 Zr1 C19 81.70(11) . . ? C12 Zr1 N2 102.94(10) . . ? C26 Zr1 N2 78.03(10) . . ? C19 Zr1 N2 136.45(11) . . ? C12 Zr1 N1 91.09(11) . . ? C26 Zr1 N1 144.01(10) . . ? C19 Zr1 N1 129.63(10) . . ? N2 Zr1 N1 66.82(8) . . ? C12 Zr1 C4 123.72(11) . . ? C26 Zr1 C4 135.85(11) . . ? C19 Zr1 C4 104.89(11) . . ? N2 Zr1 C4 67.32(9) . . ? N1 Zr1 C4 32.94(9) . . ? C12 Zr1 C1 77.75(11) . . ? C26 Zr1 C1 165.00(11) . . ? C19 Zr1 C1 110.56(11) . . ? N2 Zr1 C1 97.25(9) . . ? N1 Zr1 C1 31.10(8) . . ? C4 Zr1 C1 51.15(10) . . ? C12 Zr1 C3 126.03(11) . . ? C26 Zr1 C3 144.05(11) . . ? C19 Zr1 C3 77.54(11) . . ? N2 Zr1 C3 97.43(9) . . ? N1 Zr1 C3 52.88(9) . . ? C4 Zr1 C3 31.18(9) . . ? C1 Zr1 C3 50.22(10) . . ? C12 Zr1 C2 96.56(11) . . ? C26 Zr1 C2 163.57(10) . . ? C19 Zr1 C2 81.91(10) . . ? N2 Zr1 C2 115.22(9) . . ? N1 Zr1 C2 51.51(9) . . ? C4 Zr1 C2 50.87(10) . . ? C1 Zr1 C2 29.66(9) . . ? C3 Zr1 C2 30.47(10) . . ? C33 Zr2 C47 86.28(11) . . ? C33 Zr2 C40 105.51(12) . . ? C47 Zr2 C40 84.20(11) . . ? C33 Zr2 N1 121.19(11) . . ? C47 Zr2 N1 76.38(10) . . ? C40 Zr2 N1 127.29(10) . . ? C33 Zr2 N2 130.82(10) . . ? C47 Zr2 N2 137.30(10) . . ? C40 Zr2 N2 101.33(10) . . ? N1 Zr2 N2 66.64(8) . . ? C33 Zr2 C6 101.32(11) . . ? C47 Zr2 C6 141.35(11) . . ? C40 Zr2 C6 128.29(11) . . ? N1 Zr2 C6 67.23(9) . . ? N2 Zr2 C6 32.22(9) . . ? C33 Zr2 C9 120.00(11) . . ? C47 Zr2 C9 150.80(11) . . ? C40 Zr2 C9 76.92(11) . . ? N1 Zr2 C9 97.57(9) . . ? N2 Zr2 C9 31.74(8) . . ? C6 Zr2 C9 51.37(10) . . ? C33 Zr2 C7 78.94(11) . . ? C47 Zr2 C7 157.46(11) . . ? C40 Zr2 C7 116.01(11) . . ? N1 Zr2 C7 96.78(9) . . ? N2 Zr2 C7 52.21(9) . . ? C6 Zr2 C7 30.71(9) . . ? C9 Zr2 C7 50.50(10) . . ? C33 Zr2 C8 89.80(11) . . ? C47 Zr2 C8 167.87(10) . . ? C40 Zr2 C8 85.80(10) . . ? N1 Zr2 C8 115.33(9) . . ? N2 Zr2 C8 51.87(9) . . ? C6 Zr2 C8 50.74(10) . . ? C9 Zr2 C8 30.26(9) . . ? C7 Zr2 C8 30.41(10) . . ? C1 N1 C4 105.5(2) . . ? C1 N1 Zr2 132.9(2) . . ? C4 N1 Zr2 120.88(19) . . ? C1 N1 Zr1 81.21(17) . . ? C4 N1 Zr1 73.92(16) . . ? Zr2 N1 Zr1 102.93(9) . . ? C9 N2 C6 105.8(2) . . ? C9 N2 Zr1 132.3(2) . . ? C6 N2 Zr1 120.99(19) . . ? C9 N2 Zr2 77.94(16) . . ? C6 N2 Zr2 76.14(16) . . ? Zr1 N2 Zr2 103.12(9) . . ? C1 C2 C3 106.6(3) . . ? C1 C2 Zr1 71.18(18) . . ? C3 C2 Zr1 71.22(17) . . ? C4 C3 C2 106.9(3) . . ? C4 C3 Zr1 67.75(17) . . ? C2 C3 Zr1 78.31(18) . . ? N1 C1 C2 111.2(3) . . ? N1 C1 Zr1 67.69(16) . . ? C2 C1 Zr1 79.15(18) . . ? C3 C4 N1 109.9(3) . . ? C3 C4 C5 131.6(3) . . ? N1 C4 C5 118.6(3) . . ? C3 C4 Zr1 81.07(19) . . ? N1 C4 Zr1 73.15(16) . . ? C5 C4 Zr1 112.05(19) . . ? C6 C5 C4 104.4(3) . . ? C6 C5 C11 110.2(3) . . ? C4 C5 C11 110.9(3) . . ? C6 C5 C10 111.3(3) . . ? C4 C5 C10 110.0(3) . . ? C11 C5 C10 110.0(3) . . ? N2 C6 C7 110.2(3) . . ? N2 C6 C5 117.1(3) . . ? C7 C6 C5 132.7(3) . . ? N2 C6 Zr2 71.64(16) . . ? C7 C6 Zr2 81.11(18) . . ? C5 C6 Zr2 112.75(19) . . ? C6 C7 C8 106.3(3) . . ? C6 C7 Zr2 68.18(17) . . ? C8 C7 Zr2 75.00(18) . . ? C9 C8 C7 107.1(3) . . ? C9 C8 Zr2 69.69(17) . . ? C7 C8 Zr2 74.60(18) . . ? C8 C9 N2 110.6(3) . . ? C8 C9 Zr2 80.05(19) . . ? N2 C9 Zr2 70.32(15) . . ? C13 C12 Zr1 101.4(2) . . ? C14 C13 C18 117.1(3) . . ? C14 C13 C12 121.7(3) . . ? C18 C13 C12 121.1(3) . . ? C15 C14 C13 121.5(3) . . ? C16 C15 C14 120.6(4) . . ? C15 C16 C17 119.2(4) . . ? C18 C17 C16 120.6(4) . . ? C17 C18 C13 121.0(4) . . ? C20 C19 Zr1 129.7(2) . . ? C21 C20 C25 116.5(3) . . ? C21 C20 C19 121.0(3) . . ? C25 C20 C19 122.5(3) . . ? C22 C21 C20 121.8(3) . . ? C24 C23 C22 118.9(3) . . ? C21 C22 C23 120.7(3) . . ? C23 C24 C25 121.0(3) . . ? C24 C25 C20 121.1(3) . . ? C27 C26 Zr1 123.0(2) . . ? C32 C27 C28 115.5(3) . . ? C32 C27 C26 122.0(3) . . ? C28 C27 C26 122.5(3) . . ? C29 C28 C27 122.5(3) . . ? C28 C29 C30 120.7(3) . . ? C31 C30 C29 118.4(3) . . ? C30 C31 C32 120.7(3) . . ? C31 C32 C27 122.3(3) . . ? C34 C33 Zr2 128.7(2) . . ? C39 C34 C35 116.8(3) . . ? C39 C34 C33 121.7(3) . . ? C35 C34 C33 121.5(3) . . ? C36 C35 C34 121.6(3) . . ? C37 C36 C35 120.5(3) . . ? C36 C37 C38 119.3(3) . . ? C38 C39 C34 121.5(3) . . ? C37 C38 C39 120.2(3) . . ? C41 C40 Zr2 122.3(2) . . ? C46 C41 C42 116.5(3) . . ? C46 C41 C40 123.3(3) . . ? C42 C41 C40 120.1(3) . . ? C43 C42 C41 121.5(3) . . ? C44 C43 C42 120.4(3) . . ? C43 C44 C45 119.8(3) . . ? C44 C45 C46 119.6(3) . . ? C45 C46 C41 122.2(3) . . ? C48 C47 Zr2 126.5(2) . . ? C53 C48 C49 116.7(3) . . ? C53 C48 C47 120.9(3) . . ? C49 C48 C47 122.4(3) . . ? C50 C49 C48 121.7(3) . . ? C49 C50 C51 120.6(3) . . ? C52 C51 C50 118.5(3) . . ? C53 C52 C51 120.8(3) . . ? C52 C53 C48 121.7(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.41 _refine_diff_density_min -0.31 _refine_diff_density_rms 0.07 #=====END data_tipmea _database_code_CSD 193473 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H24 N4 Ti' _chemical_formula_sum 'C15 H24 N4 Ti' _chemical_formula_weight 308.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3274(6) _cell_length_b 12.3793(7) _cell_length_c 25.3112(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.705(1) _cell_angle_gamma 90.00 _cell_volume 3229.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8492 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 28.4 _exptl_crystal_description lozenge _exptl_crystal_colour yellow/orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.268 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.527 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.901 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Bruker Sadabs v2.03' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19861 _diffrn_reflns_av_R_equivalents 0.021 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 28.72 _reflns_number_total 7881 _reflns_number_gt 6261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness 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 threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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 calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0404P)^2^+1.4451P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary 'direct methods' _atom_sites_solution_secondary 'difference Fourier' _atom_sites_solution_hydrogens 'geometrically placed, Me from delta-F' _refine_ls_hydrogen_treatment 'riding model, Me as rigid rotating group' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7536 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0425 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0799 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.02728(3) 0.66575(2) 0.180201(10) 0.01864(7) Uani 1 1 d . . . Ti2 Ti 0.46372(3) 0.26621(2) 0.038006(10) 0.01842(7) Uani 1 1 d . . . N1 N -0.16184(13) 0.57486(11) 0.17618(5) 0.0245(3) Uani 1 1 d . . . N2 N -0.07929(12) 0.79964(10) 0.15955(5) 0.0205(3) Uani 1 1 d . . . N3 N 0.10482(14) 0.62774(11) 0.11690(5) 0.0260(3) Uani 1 1 d . . . N4 N 0.16839(13) 0.71099(11) 0.22593(5) 0.0236(3) Uani 1 1 d . . . N5 N 0.28260(13) 0.36470(10) 0.04374(5) 0.0230(3) Uani 1 1 d . . . N6 N 0.39725(12) 0.16692(10) 0.09400(5) 0.0203(3) Uani 1 1 d . . . N7 N 0.55975(13) 0.18145(11) -0.00775(5) 0.0262(3) Uani 1 1 d . . . N8 N 0.58965(13) 0.34513(11) 0.08020(5) 0.0243(3) Uani 1 1 d . . . C1 C -0.06875(16) 0.49875(13) 0.19056(7) 0.0271(3) Uani 1 1 d . . . H1A H -0.0504 0.4334 0.1691 0.033 Uiso 1 1 calc R . . C2 C -0.01272(16) 0.51891(13) 0.24147(7) 0.0275(3) Uani 1 1 d . . . H2A H 0.0538 0.4739 0.2617 0.033 Uiso 1 1 calc R . . C3 C -0.07795(16) 0.61050(13) 0.26013(6) 0.0251(3) Uani 1 1 d . . . H3A H -0.0649 0.6438 0.2961 0.030 Uiso 1 1 calc R . . C4 C -0.16859(15) 0.64237(12) 0.21971(6) 0.0219(3) Uani 1 1 d . . . C5 C -0.25563(15) 0.74113(13) 0.21672(6) 0.0229(3) Uani 1 1 d . . . C6 C -0.20153(15) 0.81827(12) 0.17705(6) 0.0206(3) Uani 1 1 d . . . C7 C -0.25130(16) 0.91305(13) 0.15564(6) 0.0245(3) Uani 1 1 d . . . H7A H -0.3334 0.9440 0.1613 0.029 Uiso 1 1 calc R . . C8 C -0.15552(16) 0.95553(13) 0.12335(6) 0.0250(3) Uani 1 1 d . . . H8A H -0.1612 1.0206 0.1035 0.030 Uiso 1 1 calc R . . C9 C -0.05379(16) 0.88450(12) 0.12649(6) 0.0226(3) Uani 1 1 d . . . H9A H 0.0235 0.8925 0.1085 0.027 Uiso 1 1 calc R . . C10 C -0.39535(16) 0.70781(15) 0.19950(7) 0.0326(4) Uani 1 1 d . . . H10A H -0.3969 0.6731 0.1647 0.049 Uiso 1 1 calc R . . H10B H -0.4509 0.7720 0.1975 0.049 Uiso 1 1 calc R . . H10C H -0.4273 0.6571 0.2254 0.049 Uiso 1 1 calc R . . C11 C -0.25467(19) 0.79641(14) 0.27139(6) 0.0318(4) Uani 1 1 d . . . H11A H -0.1658 0.8179 0.2827 0.048 Uiso 1 1 calc R . . H11B H -0.2872 0.7459 0.2973 0.048 Uiso 1 1 calc R . . H11C H -0.3104 0.8605 0.2690 0.048 Uiso 1 1 calc R . . C12 C 0.0230(2) 0.59583(16) 0.07003(7) 0.0377(4) Uani 1 1 d . . . H12A H 0.0405 0.6433 0.0404 0.056 Uiso 1 1 calc R . . H12B H -0.0686 0.6019 0.0777 0.056 Uiso 1 1 calc R . . H12C H 0.0423 0.5210 0.0607 0.056 Uiso 1 1 calc R . . C13 C 0.24186(18) 0.61067(16) 0.10876(8) 0.0404(5) Uani 1 1 d . . . H13A H 0.2570 0.5340 0.1019 0.061 Uiso 1 1 calc R . . H13B H 0.2943 0.6330 0.1405 0.061 Uiso 1 1 calc R . . H13C H 0.2663 0.6536 0.0784 0.061 Uiso 1 1 calc R . . C14 C 0.23196(16) 0.80507(14) 0.20387(7) 0.0291(4) Uani 1 1 d . . . H14A H 0.2176 0.8686 0.2259 0.044 Uiso 1 1 calc R . . H14B H 0.1955 0.8183 0.1677 0.044 Uiso 1 1 calc R . . H14C H 0.3253 0.7913 0.2033 0.044 Uiso 1 1 calc R . . C15 C 0.2254(2) 0.68798(17) 0.27866(8) 0.0422(5) Uani 1 1 d . . . H15A H 0.3186 0.6749 0.2770 0.063 Uiso 1 1 calc R . . H15B H 0.1841 0.6237 0.2927 0.063 Uiso 1 1 calc R . . H15C H 0.2119 0.7498 0.3019 0.063 Uiso 1 1 calc R . . C16 C 0.34744(16) 0.41281(13) 0.00436(7) 0.0276(3) Uani 1 1 d . . . H16A H 0.3799 0.4889 0.0056 0.033 Uiso 1 1 calc R . . C17 C 0.34875(17) 0.34601(14) -0.03997(7) 0.0290(4) Uani 1 1 d . . . H17A H 0.3861 0.3636 -0.0744 0.035 Uiso 1 1 calc R . . C18 C 0.27715(15) 0.25268(13) -0.02821(6) 0.0235(3) Uani 1 1 d . . . H18A H 0.2555 0.1905 -0.0524 0.028 Uiso 1 1 calc R . . C19 C 0.23782(14) 0.26698(12) 0.02328(6) 0.0195(3) Uani 1 1 d . . . C20 C 0.16749(15) 0.18977(12) 0.05800(6) 0.0203(3) Uani 1 1 d . . . C21 C 0.26886(15) 0.13579(12) 0.09535(6) 0.0193(3) Uani 1 1 d . . . C22 C 0.25668(16) 0.06056(12) 0.13473(6) 0.0235(3) Uani 1 1 d . . . H22A H 0.1791 0.0254 0.1435 0.028 Uiso 1 1 calc R . . C23 C 0.38247(16) 0.04553(13) 0.15979(6) 0.0251(3) Uani 1 1 d . . . H23A H 0.4050 -0.0011 0.1887 0.030 Uiso 1 1 calc R . . C24 C 0.46502(16) 0.11108(13) 0.13425(6) 0.0242(3) Uani 1 1 d . . . H24A H 0.5556 0.1173 0.1429 0.029 Uiso 1 1 calc R . . C25 C 0.09237(17) 0.10514(14) 0.02401(6) 0.0283(4) Uani 1 1 d . . . H25A H 0.1530 0.0641 0.0035 0.042 Uiso 1 1 calc R . . H25B H 0.0286 0.1414 -0.0002 0.042 Uiso 1 1 calc R . . H25C H 0.0476 0.0558 0.0470 0.042 Uiso 1 1 calc R . . C26 C 0.07093(16) 0.25390(15) 0.08978(7) 0.0289(4) Uani 1 1 d . . . H26A H 0.1181 0.3080 0.1118 0.043 Uiso 1 1 calc R . . H26B H 0.0256 0.2043 0.1125 0.043 Uiso 1 1 calc R . . H26C H 0.0077 0.2902 0.0653 0.043 Uiso 1 1 calc R . . C27 C 0.65661(18) 0.11563(16) 0.02257(8) 0.0376(4) Uani 1 1 d . . . H27A H 0.6341 0.0390 0.0185 0.056 Uiso 1 1 calc R . . H27B H 0.6580 0.1356 0.0601 0.056 Uiso 1 1 calc R . . H27C H 0.7424 0.1283 0.0093 0.056 Uiso 1 1 calc R . . C28 C 0.5552(2) 0.14962(16) -0.06339(7) 0.0373(4) Uani 1 1 d . . . H28A H 0.6407 0.1607 -0.0772 0.056 Uiso 1 1 calc R . . H28B H 0.4907 0.1936 -0.0837 0.056 Uiso 1 1 calc R . . H28C H 0.5313 0.0732 -0.0666 0.056 Uiso 1 1 calc R . . C29 C 0.72916(17) 0.35554(15) 0.07534(7) 0.0336(4) Uani 1 1 d . . . H29A H 0.7531 0.4321 0.0760 0.050 Uiso 1 1 calc R . . H29B H 0.7522 0.3234 0.0418 0.050 Uiso 1 1 calc R . . H29C H 0.7758 0.3180 0.1049 0.050 Uiso 1 1 calc R . . C30 C 0.54822(18) 0.40238(14) 0.12678(7) 0.0326(4) Uani 1 1 d . . . H30A H 0.5895 0.3697 0.1589 0.049 Uiso 1 1 calc R . . H30B H 0.4537 0.3973 0.1278 0.049 Uiso 1 1 calc R . . H30C H 0.5737 0.4785 0.1249 0.049 Uiso 1 1 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 Ti1 0.01761(14) 0.01875(13) 0.01955(13) 0.00091(10) 0.00115(10) 0.00082(10) Ti2 0.01569(13) 0.01871(13) 0.02087(13) 0.00024(10) 0.00138(10) -0.00002(10) N1 0.0220(7) 0.0229(7) 0.0287(7) -0.0014(5) 0.0021(5) -0.0040(5) N2 0.0199(6) 0.0213(6) 0.0202(6) 0.0017(5) 0.0018(5) 0.0014(5) N3 0.0277(7) 0.0247(7) 0.0261(7) -0.0016(5) 0.0057(6) 0.0029(6) N4 0.0211(7) 0.0232(6) 0.0261(7) 0.0026(5) -0.0021(5) -0.0006(5) N5 0.0178(6) 0.0199(6) 0.0310(7) -0.0005(5) -0.0009(5) 0.0020(5) N6 0.0185(6) 0.0205(6) 0.0216(6) 0.0008(5) -0.0008(5) -0.0010(5) N7 0.0238(7) 0.0268(7) 0.0286(7) -0.0011(6) 0.0064(6) 0.0018(6) N8 0.0200(7) 0.0234(7) 0.0290(7) 0.0026(5) -0.0017(5) -0.0025(5) C1 0.0261(8) 0.0191(7) 0.0363(9) 0.0008(6) 0.0040(7) -0.0017(6) C2 0.0265(8) 0.0232(8) 0.0331(9) 0.0103(6) 0.0031(7) 0.0008(6) C3 0.0258(8) 0.0273(8) 0.0226(7) 0.0066(6) 0.0040(6) -0.0021(7) C4 0.0194(7) 0.0227(7) 0.0241(7) 0.0017(6) 0.0045(6) -0.0032(6) C5 0.0217(8) 0.0245(8) 0.0228(7) 0.0003(6) 0.0041(6) 0.0014(6) C6 0.0187(7) 0.0236(7) 0.0193(7) -0.0021(6) 0.0005(6) 0.0001(6) C7 0.0226(8) 0.0245(8) 0.0259(8) -0.0006(6) -0.0012(6) 0.0044(6) C8 0.0305(9) 0.0208(7) 0.0229(7) 0.0026(6) -0.0045(6) 0.0006(6) C9 0.0239(8) 0.0238(8) 0.0201(7) 0.0016(6) 0.0008(6) -0.0034(6) C10 0.0206(8) 0.0376(9) 0.0399(10) 0.0053(8) 0.0048(7) 0.0001(7) C11 0.0414(10) 0.0303(9) 0.0247(8) 0.0003(7) 0.0090(7) 0.0042(8) C12 0.0433(11) 0.0435(11) 0.0261(9) -0.0045(8) 0.0011(8) 0.0047(9) C13 0.0315(10) 0.0406(11) 0.0507(11) -0.0138(9) 0.0148(9) 0.0018(8) C14 0.0211(8) 0.0266(8) 0.0395(9) 0.0017(7) 0.0023(7) -0.0016(6) C15 0.0407(11) 0.0485(11) 0.0351(10) 0.0095(9) -0.0152(8) -0.0106(9) C16 0.0245(8) 0.0204(8) 0.0377(9) 0.0078(7) 0.0002(7) 0.0018(6) C17 0.0263(9) 0.0346(9) 0.0260(8) 0.0100(7) 0.0016(7) 0.0005(7) C18 0.0217(8) 0.0282(8) 0.0202(7) 0.0013(6) -0.0019(6) 0.0002(6) C19 0.0148(7) 0.0207(7) 0.0227(7) 0.0006(6) -0.0012(6) 0.0019(6) C20 0.0175(7) 0.0228(7) 0.0207(7) -0.0015(6) 0.0016(6) -0.0015(6) C21 0.0196(7) 0.0189(7) 0.0195(7) -0.0035(5) 0.0028(6) -0.0003(6) C22 0.0270(8) 0.0208(7) 0.0233(7) -0.0008(6) 0.0062(6) -0.0020(6) C23 0.0331(9) 0.0219(8) 0.0202(7) 0.0021(6) 0.0014(6) 0.0031(6) C24 0.0247(8) 0.0230(8) 0.0241(7) -0.0005(6) -0.0040(6) 0.0022(6) C25 0.0268(9) 0.0312(9) 0.0264(8) -0.0016(7) -0.0022(7) -0.0099(7) C26 0.0217(8) 0.0386(9) 0.0270(8) 0.0011(7) 0.0060(6) 0.0066(7) C27 0.0298(9) 0.0368(10) 0.0474(11) 0.0045(8) 0.0106(8) 0.0137(8) C28 0.0414(11) 0.0383(10) 0.0337(9) -0.0103(8) 0.0133(8) -0.0025(8) C29 0.0213(8) 0.0410(10) 0.0377(9) 0.0080(8) -0.0046(7) -0.0066(7) C30 0.0357(10) 0.0288(8) 0.0326(9) -0.0064(7) -0.0040(7) -0.0030(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N4 1.8866(13) . ? Ti1 N3 1.8962(13) . ? Ti1 N2 2.0389(13) . ? Ti1 N1 2.2507(13) . ? Ti1 C1 2.3152(16) . ? Ti1 C4 2.3317(15) . ? Ti1 C2 2.4419(16) . ? Ti1 C3 2.4548(15) . ? Ti2 N7 1.8906(14) . ? Ti2 N8 1.8993(13) . ? Ti2 N6 2.0289(13) . ? Ti2 N5 2.2452(13) . ? Ti2 C16 2.3084(16) . ? Ti2 C19 2.3386(15) . ? Ti2 C17 2.4451(16) . ? Ti2 C18 2.4764(15) . ? N1 C1 1.378(2) . ? N1 C4 1.388(2) . ? N2 C9 1.3789(19) . ? N2 C6 1.3840(19) . ? N3 C13 1.459(2) . ? N3 C12 1.466(2) . ? N4 C15 1.452(2) . ? N4 C14 1.465(2) . ? N5 C16 1.372(2) . ? N5 C19 1.3836(19) . ? N6 C24 1.3832(19) . ? N6 C21 1.3833(19) . ? N7 C28 1.460(2) . ? N7 C27 1.468(2) . ? N8 C29 1.460(2) . ? N8 C30 1.463(2) . ? C1 C2 1.401(2) . ? C2 C3 1.415(2) . ? C3 C4 1.398(2) . ? C4 C5 1.516(2) . ? C5 C6 1.518(2) . ? C5 C10 1.537(2) . ? C5 C11 1.543(2) . ? C6 C7 1.378(2) . ? C7 C8 1.424(2) . ? C8 C9 1.368(2) . ? C16 C17 1.395(2) . ? C17 C18 1.414(2) . ? C18 C19 1.401(2) . ? C19 C20 1.515(2) . ? C20 C21 1.519(2) . ? C20 C25 1.534(2) . ? C20 C26 1.541(2) . ? C21 C22 1.376(2) . ? C22 C23 1.420(2) . ? C23 C24 1.369(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Ti1 N3 103.91(6) . . ? N4 Ti1 N2 107.38(6) . . ? N3 Ti1 N2 103.63(6) . . ? N4 Ti1 N1 144.08(5) . . ? N3 Ti1 N1 104.50(6) . . ? N2 Ti1 N1 86.70(5) . . ? N4 Ti1 C1 121.01(6) . . ? N3 Ti1 C1 94.67(6) . . ? N2 Ti1 C1 121.79(6) . . ? N1 Ti1 C1 35.10(5) . . ? N4 Ti1 C4 115.52(6) . . ? N3 Ti1 C4 139.20(6) . . ? N2 Ti1 C4 75.05(5) . . ? N1 Ti1 C4 35.21(5) . . ? C1 Ti1 C4 56.69(6) . . ? N4 Ti1 C2 89.25(6) . . ? N3 Ti1 C2 116.74(6) . . ? N2 Ti1 C2 131.09(6) . . ? N1 Ti1 C2 58.31(5) . . ? C1 Ti1 C2 34.11(6) . . ? C4 Ti1 C2 56.51(5) . . ? N4 Ti1 C3 86.71(6) . . ? N3 Ti1 C3 149.41(6) . . ? N2 Ti1 C3 100.22(5) . . ? N1 Ti1 C3 57.92(5) . . ? C1 Ti1 C3 56.10(6) . . ? C4 Ti1 C3 33.85(5) . . ? C2 Ti1 C3 33.60(5) . . ? N7 Ti2 N8 105.23(6) . . ? N7 Ti2 N6 107.83(6) . . ? N8 Ti2 N6 99.74(5) . . ? N7 Ti2 N5 144.41(6) . . ? N8 Ti2 N5 103.14(5) . . ? N6 Ti2 N5 87.88(5) . . ? N7 Ti2 C16 119.43(6) . . ? N8 Ti2 C16 97.13(6) . . ? N6 Ti2 C16 122.86(6) . . ? N5 Ti2 C16 35.04(5) . . ? N7 Ti2 C19 117.52(6) . . ? N8 Ti2 C19 136.66(6) . . ? N6 Ti2 C19 74.62(5) . . ? N5 Ti2 C19 35.06(5) . . ? C16 Ti2 C19 56.51(6) . . ? N7 Ti2 C17 88.65(6) . . ? N8 Ti2 C17 121.69(6) . . ? N6 Ti2 C17 129.80(6) . . ? N5 Ti2 C17 57.97(5) . . ? C16 Ti2 C17 33.97(6) . . ? C19 Ti2 C17 56.11(5) . . ? N7 Ti2 C18 87.93(6) . . ? N8 Ti2 C18 152.87(6) . . ? N6 Ti2 C18 98.52(5) . . ? N5 Ti2 C18 57.69(5) . . ? C16 Ti2 C18 55.94(6) . . ? C19 Ti2 C18 33.68(5) . . ? C17 Ti2 C18 33.38(5) . . ? C1 N1 C4 105.78(13) . . ? C1 N1 Ti1 75.01(9) . . ? C4 N1 Ti1 75.58(8) . . ? C9 N2 C6 106.33(13) . . ? C9 N2 Ti1 130.83(11) . . ? C6 N2 Ti1 122.81(10) . . ? C13 N3 C12 111.13(14) . . ? C13 N3 Ti1 128.45(12) . . ? C12 N3 Ti1 119.86(12) . . ? C15 N4 C14 109.96(14) . . ? C15 N4 Ti1 139.20(12) . . ? C14 N4 Ti1 110.46(10) . . ? C16 N5 C19 105.94(13) . . ? C16 N5 Ti2 74.99(9) . . ? C19 N5 Ti2 76.16(8) . . ? C24 N6 C21 106.42(13) . . ? C24 N6 Ti2 129.74(11) . . ? C21 N6 Ti2 123.66(10) . . ? C28 N7 C27 109.43(14) . . ? C28 N7 Ti2 139.04(12) . . ? C27 N7 Ti2 110.78(11) . . ? C29 N8 C30 111.53(14) . . ? C29 N8 Ti2 129.92(12) . . ? C30 N8 Ti2 118.49(11) . . ? N1 C1 C2 111.15(14) . . ? N1 C1 Ti1 69.89(8) . . ? C2 C1 Ti1 77.91(10) . . ? C1 C2 C3 105.82(14) . . ? C1 C2 Ti1 67.98(9) . . ? C3 C2 Ti1 73.70(9) . . ? C4 C3 C2 107.00(14) . . ? C4 C3 Ti1 68.24(9) . . ? C2 C3 Ti1 72.70(9) . . ? N1 C4 C3 110.21(14) . . ? N1 C4 C5 120.39(13) . . ? C3 C4 C5 129.09(14) . . ? N1 C4 Ti1 69.21(8) . . ? C3 C4 Ti1 77.91(9) . . ? C5 C4 Ti1 113.98(10) . . ? C4 C5 C6 107.32(12) . . ? C4 C5 C10 109.91(13) . . ? C6 C5 C10 111.11(13) . . ? C4 C5 C11 110.09(13) . . ? C6 C5 C11 109.44(13) . . ? C10 C5 C11 108.96(14) . . ? C7 C6 N2 109.92(13) . . ? C7 C6 C5 130.69(14) . . ? N2 C6 C5 119.28(13) . . ? C6 C7 C8 106.56(14) . . ? C9 C8 C7 106.77(14) . . ? C8 C9 N2 110.42(14) . . ? N5 C16 C17 110.96(14) . . ? N5 C16 Ti2 69.97(8) . . ? C17 C16 Ti2 78.40(10) . . ? C16 C17 C18 106.42(14) . . ? C16 C17 Ti2 67.64(9) . . ? C18 C17 Ti2 74.52(9) . . ? C19 C18 C17 106.23(14) . . ? C19 C18 Ti2 67.76(8) . . ? C17 C18 Ti2 72.10(9) . . ? N5 C19 C18 110.40(13) . . ? N5 C19 C20 119.71(13) . . ? C18 C19 C20 129.67(14) . . ? N5 C19 Ti2 68.78(8) . . ? C18 C19 Ti2 78.56(9) . . ? C20 C19 Ti2 114.56(9) . . ? C19 C20 C21 107.55(12) . . ? C19 C20 C25 110.46(12) . . ? C21 C20 C25 110.60(13) . . ? C19 C20 C26 109.17(13) . . ? C21 C20 C26 110.17(12) . . ? C25 C20 C26 108.89(13) . . ? C22 C21 N6 109.83(13) . . ? C22 C21 C20 131.07(14) . . ? N6 C21 C20 119.02(13) . . ? C21 C22 C23 106.75(14) . . ? C24 C23 C22 106.92(14) . . ? C23 C24 N6 110.07(14) . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.341 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.049 #===========END data_tidpcl _database_code_CSD 193474 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H26 Cl2 N4 Ti' _chemical_formula_weight 477.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 11.107(2) _cell_length_b 14.926(2) _cell_length_c 6.7163(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1113.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1136 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.4 _exptl_crystal_description lath _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 496 _exptl_absorpt_coefficient_mu 0.642 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.887 _exptl_absorpt_correction_T_max 0.949 _exptl_absorpt_process_details 'XPREP SHElXTLv6.12' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD area detector' _diffrn_measurement_method omega _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 4543 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.0856 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 28.63 _reflns_number_total 2522 _reflns_number_gt 1666 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART version 5.624 (Bruker, 2001)' _computing_cell_refinement 'Bruker SAINT version 6.02a (Bruker, 2000)' _computing_data_reduction 'Bruker SAINT; Bruker SHELXTL (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97; PLATON (Spek, 2002)' _refine_special_details ; Disorder in one ring, modelled as two sites with occupancy 0.54 and 0.46. Restraints applied to geometry. All partially occupied sites modelled with isotropic adps. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0442P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geometrically placed' _refine_ls_hydrogen_treatment 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(5) _refine_ls_number_reflns 2506 _refine_ls_number_parameters 128 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0480 _refine_ls_wR_factor_ref 0.1009 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 0.913 _refine_ls_restrained_S_all 0.916 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.0000 0.0000 0.74229(12) 0.0240(2) Uani 1 2 d S . . N1 N -0.1419(2) -0.02932(16) 0.9237(4) 0.0231(6) Uani 1 1 d . A . C1 C -0.2100(3) 0.0280(2) 1.0410(5) 0.0316(9) Uani 1 1 d . . . H1A H -0.1993 0.0911 1.0473 0.038 Uiso 1 1 calc R A . C2 C -0.2936(3) -0.0182(2) 1.1452(5) 0.0377(10) Uani 1 1 d . A . H2A H -0.3501 0.0063 1.2362 0.045 Uiso 1 1 calc R . . C3 C -0.2815(3) -0.1100(2) 1.0939(5) 0.0357(9) Uani 1 1 d . . . H3A H -0.3279 -0.1585 1.1436 0.043 Uiso 1 1 calc R A . C4 C -0.1894(3) -0.1145(2) 0.9585(5) 0.0243(7) Uani 1 1 d . A . C5 C -0.1397(3) -0.1922(2) 0.8413(5) 0.0295(8) Uani 1 1 d . . . C6 C -0.0443(3) -0.1546(2) 0.7063(5) 0.0303(9) Uiso 1 1 d D A . N2 N 0.0674(4) -0.1461(4) 0.7950(9) 0.0175(17) Uiso 0.54 1 d PD A 1 C7 C -0.0458(7) -0.1228(6) 0.5101(9) 0.039(3) Uiso 0.54 1 d PD A 1 H7A H -0.1126 -0.1265 0.4106 0.047 Uiso 0.54 1 calc PR A 1 C8 C 0.0755(7) -0.0977(5) 0.4775(13) 0.0288(17) Uiso 0.54 1 d PD A 1 H8A H 0.1100 -0.0771 0.3478 0.035 Uiso 0.54 1 calc PR A 1 C9 C 0.1389(6) -0.1122(4) 0.6468(10) 0.0258(17) Uiso 0.54 1 d PD A 1 H9A H 0.2283 -0.1057 0.6573 0.031 Uiso 0.54 1 calc PR A 1 N2' N 0.0755(4) -0.1399(5) 0.7349(13) 0.033(3) Uiso 0.46 1 d PD A 2 C7' C -0.0717(9) -0.1141(7) 0.5220(11) 0.041(4) Uiso 0.46 1 d PD A 2 H7'A H -0.1529 -0.1145 0.4574 0.049 Uiso 0.46 1 calc PR A 2 C8' C 0.0336(8) -0.0766(5) 0.4373(13) 0.035(2) Uiso 0.46 1 d PD A 2 H8'A H 0.0436 -0.0502 0.3015 0.042 Uiso 0.46 1 calc PR A 2 C9' C 0.1223(8) -0.0954(5) 0.5756(15) 0.029(2) Uiso 0.46 1 d PD A 2 H9'A H 0.2103 -0.0852 0.5532 0.034 Uiso 0.46 1 calc PR A 2 C10 C -0.2402(3) -0.2359(2) 0.7177(6) 0.0412(10) Uani 1 1 d . A . H10A H -0.2741 -0.1917 0.6257 0.062 Uiso 1 1 calc R . . H10B H -0.3036 -0.2578 0.8068 0.062 Uiso 1 1 calc R . . H10C H -0.2069 -0.2862 0.6417 0.062 Uiso 1 1 calc R . . C11 C -0.0863(4) -0.2618(2) 0.9841(6) 0.0477(12) Uani 1 1 d . A . H11A H -0.0217 -0.2342 1.0622 0.072 Uiso 1 1 calc R . . H11B H -0.0538 -0.3121 0.9074 0.072 Uiso 1 1 calc R . . H11C H -0.1494 -0.2835 1.0740 0.072 Uiso 1 1 calc R . . C1S C 0.5000 0.0000 0.7291(8) 0.091(2) Uani 1 2 d S . . H1S1 H 0.5714 -0.0076 0.8158 0.110 Uiso 0.50 1 calc PR . . H1S2 H 0.4286 0.0076 0.8158 0.110 Uiso 0.50 1 calc PR . . Cl1 Cl 0.48141(11) -0.09639(7) 0.58117(17) 0.0650(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0271(4) 0.0222(4) 0.0228(4) 0.000 0.000 -0.0033(4) N1 0.0206(14) 0.0222(14) 0.0265(15) -0.0035(12) 0.0011(13) 0.0003(11) C1 0.029(2) 0.0325(18) 0.034(2) -0.0131(15) -0.0017(18) 0.0060(16) C2 0.028(2) 0.054(3) 0.031(2) -0.0134(18) 0.0035(18) -0.0018(19) C3 0.026(2) 0.044(2) 0.037(2) 0.0061(18) -0.0009(19) -0.0116(18) C4 0.0217(17) 0.0249(17) 0.0262(19) 0.0019(14) -0.0027(16) -0.0009(15) C5 0.0250(19) 0.0218(17) 0.042(2) -0.0027(15) -0.0035(17) 0.0010(15) C10 0.032(2) 0.0345(18) 0.057(3) -0.0176(19) -0.006(2) -0.0031(16) C11 0.045(3) 0.0293(19) 0.069(3) 0.010(2) -0.004(2) 0.0044(19) C1S 0.059(4) 0.187(8) 0.029(3) 0.000 0.000 -0.038(5) Cl1 0.0466(7) 0.0809(8) 0.0675(7) 0.0296(6) -0.0062(7) 0.0008(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N1 2.040(3) 2 ? Ti1 N1 2.040(3) . ? Ti1 N2' 2.251(8) 2 ? Ti1 N2' 2.251(8) . ? Ti1 C9' 2.264(8) 2 ? Ti1 C9' 2.264(8) . ? Ti1 N2 2.333(6) 2 ? Ti1 N2 2.333(6) . ? Ti1 C9 2.366(7) 2 ? Ti1 C9 2.366(7) . ? Ti1 C6 2.371(3) . ? Ti1 C6 2.371(3) 2 ? N1 C1 1.387(4) . ? N1 C4 1.397(4) . ? C1 C2 1.352(5) . ? C2 C3 1.418(4) . ? C3 C4 1.370(5) . ? C4 C5 1.506(4) . ? C5 C6 1.504(5) . ? C5 C11 1.533(5) . ? C5 C10 1.536(5) . ? C6 N2' 1.363(5) . ? C6 N2 1.382(4) . ? C6 C7 1.400(6) . ? C6 C7' 1.411(6) . ? N2 C9 1.371(7) . ? C7 C8 1.415(7) . ? C8 C9 1.355(11) . ? N2' C9' 1.363(7) . ? C7' C8' 1.416(8) . ? C8' C9' 1.382(13) . ? C1S Cl1 1.761(3) . ? C1S Cl1 1.761(3) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ti1 N1 106.63(15) 2 . ? N1 Ti1 N2' 95.87(18) 2 2 ? N1 Ti1 N2' 85.65(16) . 2 ? N1 Ti1 N2' 85.65(16) 2 . ? N1 Ti1 N2' 95.87(18) . . ? N2' Ti1 N2' 177.5(4) 2 . ? N1 Ti1 C9' 128.63(19) 2 2 ? N1 Ti1 C9' 88.1(3) . 2 ? N2' Ti1 C9' 35.1(2) 2 2 ? N2' Ti1 C9' 142.7(3) . 2 ? N1 Ti1 C9' 88.1(3) 2 . ? N1 Ti1 C9' 128.63(19) . . ? N2' Ti1 C9' 142.7(3) 2 . ? N2' Ti1 C9' 35.1(2) . . ? C9' Ti1 C9' 120.7(6) 2 . ? N1 Ti1 N2 87.52(16) 2 2 ? N1 Ti1 N2 82.07(12) . 2 ? N2' Ti1 N2 10.4(2) 2 2 ? N2' Ti1 N2 172.0(3) . 2 ? C9' Ti1 N2 45.1(3) 2 2 ? C9' Ti1 N2 148.8(2) . 2 ? N1 Ti1 N2 82.07(12) 2 . ? N1 Ti1 N2 87.52(16) . . ? N2' Ti1 N2 172.0(3) 2 . ? N2' Ti1 N2 10.4(2) . . ? C9' Ti1 N2 148.8(2) 2 . ? C9' Ti1 N2 45.1(3) . . ? N2 Ti1 N2 162.5(3) 2 . ? N1 Ti1 C9 120.94(17) 2 2 ? N1 Ti1 C9 79.03(19) . 2 ? N2' Ti1 C9 25.1(2) 2 2 ? N2' Ti1 C9 153.4(2) . 2 ? C9' Ti1 C9 13.9(2) 2 2 ? C9' Ti1 C9 134.6(4) . 2 ? N2 Ti1 C9 33.91(18) 2 2 ? N2 Ti1 C9 155.80(16) . 2 ? N1 Ti1 C9 79.03(19) 2 . ? N1 Ti1 C9 120.94(17) . . ? N2' Ti1 C9 153.4(2) 2 . ? N2' Ti1 C9 25.1(2) . . ? C9' Ti1 C9 134.6(4) 2 . ? C9' Ti1 C9 13.9(2) . . ? N2 Ti1 C9 155.80(16) 2 . ? N2 Ti1 C9 33.91(18) . . ? C9 Ti1 C9 148.5(4) 2 . ? N1 Ti1 C6 115.47(11) 2 . ? N1 Ti1 C6 72.06(11) . . ? N2' Ti1 C6 145.37(13) 2 . ? N2' Ti1 C6 34.17(13) . . ? C9' Ti1 C6 115.89(19) 2 . ? C9' Ti1 C6 57.5(2) . . ? N2 Ti1 C6 149.15(13) 2 . ? N2 Ti1 C6 34.16(11) . . ? C9 Ti1 C6 121.71(17) 2 . ? C9 Ti1 C6 54.48(17) . . ? N1 Ti1 C6 72.06(11) 2 2 ? N1 Ti1 C6 115.47(11) . 2 ? N2' Ti1 C6 34.17(13) 2 2 ? N2' Ti1 C6 145.37(13) . 2 ? C9' Ti1 C6 57.5(2) 2 2 ? C9' Ti1 C6 115.89(19) . 2 ? N2 Ti1 C6 34.16(11) 2 2 ? N2 Ti1 C6 149.15(13) . 2 ? C9 Ti1 C6 54.48(17) 2 2 ? C9 Ti1 C6 121.71(17) . 2 ? C6 Ti1 C6 168.28(18) . 2 ? C1 N1 C4 105.1(3) . . ? C1 N1 Ti1 128.9(2) . . ? C4 N1 Ti1 126.0(2) . . ? C2 C1 N1 110.7(3) . . ? C1 C2 C3 107.6(3) . . ? C4 C3 C2 106.2(3) . . ? C3 C4 N1 110.3(3) . . ? C3 C4 C5 131.2(3) . . ? N1 C4 C5 118.4(3) . . ? C6 C5 C4 106.6(3) . . ? C6 C5 C11 110.9(3) . . ? C4 C5 C11 109.6(3) . . ? C6 C5 C10 110.2(3) . . ? C4 C5 C10 110.1(3) . . ? C11 C5 C10 109.3(3) . . ? N2 C6 C7 112.7(5) . . ? N2' C6 C7' 105.4(6) . . ? N2 C6 C5 114.0(4) . . ? C7 C6 C5 133.3(4) . . ? N2' C6 Ti1 68.1(4) . . ? N2 C6 Ti1 71.4(3) . . ? C7 C6 Ti1 76.7(4) . . ? C7' C6 Ti1 73.6(5) . . ? C5 C6 Ti1 116.6(2) . . ? C9 N2 C6 103.9(5) . . ? C9 N2 Ti1 74.4(4) . . ? C6 N2 Ti1 74.4(3) . . ? C6 C7 C8 102.9(6) . . ? C6 C7 Ti1 69.7(4) . . ? C8 C7 Ti1 72.8(5) . . ? C9 C8 C7 108.8(6) . . ? C9 C8 Ti1 70.3(4) . . ? C7 C8 Ti1 73.7(5) . . ? C8 C9 N2 111.5(6) . . ? C8 C9 Ti1 77.0(4) . . ? N2 C9 Ti1 71.7(4) . . ? C9' N2' C6 109.9(7) . . ? C9' N2' Ti1 73.0(5) . . ? C6 N2' Ti1 77.7(4) . . ? C6 C7' C8' 110.1(7) . . ? C6 C7' Ti1 72.0(4) . . ? C8' C7' Ti1 72.1(5) . . ? C9' C8' C7' 103.8(7) . . ? C9' C8' Ti1 68.3(5) . . ? C7' C8' Ti1 73.4(6) . . ? N2' C9' C8' 110.8(7) . . ? N2' C9' Ti1 71.9(5) . . ? C8' C9' Ti1 77.1(5) . . ? Cl1 C1S Cl1 111.3(3) . 2_655 ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.437 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.063 #========END