# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Vernon Gibson' 'David J. Jones' 'Brian S. Kimberley' 'Daniel C.H. Oakes' 'Andrew J.P. White' 'David J. WIlliams' _publ_contact_author_name 'Prof Vernon Gibson' _publ_contact_author_address ; Department of Chemistry Imperial College London Exhibition Road London SW7 2AZ UNITED KINGDOM ; _publ_contact_author_email V.GIBSON@IMPERIAL.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Olefin Polymerisation Catalysts Stabilised by Dianionic [N,O,L] Ligands: The Beneficial Effect of Soft donors on the Activity of Group 4 Metal Systems ; data_Compound_2 _database_code_depnum_ccdc_archive 'CCDC 236411' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H45 N O Zr' _chemical_formula_weight 610.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.2413(15) _cell_length_b 14.9424(15) _cell_length_c 16.766(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.462(8) _cell_angle_gamma 90.00 _cell_volume 3251.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 4.90 _cell_measurement_theta_max 27.97 _exptl_crystal_description blocks _exptl_crystal_colour 'Pale yellow' _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1288 _exptl_absorpt_coefficient_mu 2.969 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.2157 _exptl_absorpt_correction_T_max 0.3626 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4/RA' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5050 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 1 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.90 _diffrn_reflns_theta_max 59.98 _reflns_number_total 4818 _reflns_number_gt 3938 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0497P)^2^+1.5588P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00025(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4818 _refine_ls_number_parameters 362 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0530 _refine_ls_R_factor_gt 0.0389 _refine_ls_wR_factor_ref 0.0946 _refine_ls_wR_factor_gt 0.0899 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 Zr Zr 0.86562(2) 0.21337(2) 0.236499(17) 0.02571(11) Uani 1 1 d . . . O1 O 0.99079(17) 0.14572(16) 0.28179(13) 0.0277(5) Uani 1 1 d . . . C1 C 1.0804(2) 0.1299(2) 0.25392(19) 0.0245(7) Uani 1 1 d . . . C2 C 1.1391(2) 0.0533(2) 0.27765(19) 0.0235(7) Uani 1 1 d . . . C3 C 1.2290(3) 0.0442(2) 0.2459(2) 0.0269(8) Uani 1 1 d . . . H3A H 1.2711 -0.0067 0.2619 0.032 Uiso 1 1 calc R . . C4 C 1.2601(3) 0.1041(2) 0.1932(2) 0.0268(7) Uani 1 1 d . . . C5 C 1.1970(2) 0.1779(2) 0.1696(2) 0.0267(7) Uani 1 1 d . . . H5A H 1.2155 0.2197 0.1324 0.032 Uiso 1 1 calc R . . C6 C 1.1079(2) 0.1915(2) 0.1993(2) 0.0246(7) Uani 1 1 d . . . C7 C 1.0388(3) 0.2710(2) 0.1739(2) 0.0309(8) Uani 1 1 d . . . H7A H 1.0408 0.3104 0.2216 0.037 Uiso 1 1 calc R . . H7B H 1.0659 0.3054 0.1323 0.037 Uiso 1 1 calc R . . N7 N 0.9295(2) 0.2461(2) 0.14022(18) 0.0290(7) Uani 1 1 d . . . C8 C 0.9041(3) 0.2376(3) 0.0533(2) 0.0382(10) Uani 1 1 d . . . C9 C 0.8986(3) 0.1536(3) 0.0165(2) 0.0422(10) Uani 1 1 d . . . C10 C 0.8677(3) 0.1481(4) -0.0678(3) 0.0617(14) Uani 1 1 d . . . H10A H 0.8619 0.0912 -0.0935 0.074 Uiso 1 1 calc R . . C11 C 0.8455(4) 0.2236(5) -0.1139(3) 0.079(2) Uani 1 1 d . . . H11A H 0.8243 0.2184 -0.1712 0.095 Uiso 1 1 calc R . . C12 C 0.8535(4) 0.3063(5) -0.0786(3) 0.0721(18) Uani 1 1 d . . . H12A H 0.8389 0.3580 -0.1118 0.087 Uiso 1 1 calc R . . C13 C 0.8830(3) 0.3157(3) 0.0061(3) 0.0514(12) Uani 1 1 d . . . C14 C 1.1054(3) -0.0198(2) 0.3308(2) 0.0283(8) Uani 1 1 d . . . C15 C 1.0058(3) -0.0628(3) 0.2842(2) 0.0439(10) Uani 1 1 d . . . H15A H 0.9835 -0.1097 0.3178 0.066 Uiso 1 1 calc R . . H15B H 1.0183 -0.0891 0.2335 0.066 Uiso 1 1 calc R . . H15C H 0.9519 -0.0170 0.2716 0.066 Uiso 1 1 calc R . . C16 C 1.0874(3) 0.0182(3) 0.4119(2) 0.0404(9) Uani 1 1 d . . . H16A H 1.0658 -0.0301 0.4444 0.061 Uiso 1 1 calc R . . H16B H 1.0335 0.0640 0.4013 0.061 Uiso 1 1 calc R . . H16C H 1.1514 0.0449 0.4418 0.061 Uiso 1 1 calc R . . C17 C 1.1868(3) -0.0937(3) 0.3515(2) 0.0398(9) Uani 1 1 d . . . H17A H 1.1626 -0.1392 0.3854 0.060 Uiso 1 1 calc R . . H17B H 1.2514 -0.0678 0.3811 0.060 Uiso 1 1 calc R . . H17C H 1.1985 -0.1214 0.3011 0.060 Uiso 1 1 calc R . . C18 C 1.3604(3) 0.0927(3) 0.1621(2) 0.0350(9) Uani 1 1 d . . . C19 C 1.4171(4) 0.0074(3) 0.1918(3) 0.0586(13) Uani 1 1 d . . . H19A H 1.3732 -0.0442 0.1730 0.088 Uiso 1 1 calc R . . H19B H 1.4344 0.0077 0.2514 0.088 Uiso 1 1 calc R . . H19C H 1.4805 0.0036 0.1702 0.088 Uiso 1 1 calc R . . C20 C 1.4313(4) 0.1704(3) 0.1925(4) 0.085(2) Uani 1 1 d . . . H20A H 1.3966 0.2269 0.1742 0.127 Uiso 1 1 calc R . . H20B H 1.4946 0.1653 0.1709 0.127 Uiso 1 1 calc R . . H20C H 1.4485 0.1693 0.2521 0.127 Uiso 1 1 calc R . . C21 C 1.3361(4) 0.0899(4) 0.0694(3) 0.0762(18) Uani 1 1 d . . . H21A H 1.2992 0.1445 0.0484 0.114 Uiso 1 1 calc R . . H21B H 1.2931 0.0376 0.0511 0.114 Uiso 1 1 calc R . . H21C H 1.4005 0.0857 0.0492 0.114 Uiso 1 1 calc R . . C22 C 0.9225(3) 0.0688(3) 0.0648(3) 0.0491(11) Uani 1 1 d . . . H22A H 0.9962 0.0672 0.0893 0.074 Uiso 1 1 d R . . H22B H 0.9049 0.0172 0.0287 0.074 Uiso 1 1 d R . . H22C H 0.8822 0.0669 0.1079 0.074 Uiso 1 1 d R . . C23 C 0.8892(4) 0.4061(3) 0.0454(3) 0.0698(16) Uani 1 1 d . . . H23A H 0.9617 0.4224 0.0646 0.105 Uiso 1 1 d R . . H23B H 0.8541 0.4046 0.0916 0.105 Uiso 1 1 d R . . H23C H 0.8560 0.4505 0.0056 0.105 Uiso 1 1 d R . . C24 C 0.7271(3) 0.1209(3) 0.2271(2) 0.0351(9) Uani 1 1 d . . . H24A H 0.7436 0.0566 0.2239 0.042 Uiso 1 1 calc R . . H24B H 0.6848 0.1321 0.2686 0.042 Uiso 1 1 calc R . . C25 C 0.6687(3) 0.1156(3) 0.0741(2) 0.0406(9) Uani 1 1 d . . . H25A H 0.6773 0.0525 0.0744 0.049 Uiso 1 1 calc R . . C26 C 0.6388(3) 0.1596(3) 0.0013(2) 0.0484(11) Uani 1 1 d . . . H26A H 0.6261 0.1262 -0.0479 0.058 Uiso 1 1 calc R . . C27 C 0.6270(3) 0.2517(3) -0.0016(2) 0.0475(11) Uani 1 1 d . . . H27A H 0.6067 0.2813 -0.0524 0.057 Uiso 1 1 calc R . . C28 C 0.6451(3) 0.2996(3) 0.0696(2) 0.0419(10) Uani 1 1 d . . . H28A H 0.6371 0.3628 0.0683 0.050 Uiso 1 1 calc R . . C29 C 0.6751(3) 0.2556(3) 0.1439(2) 0.0335(9) Uani 1 1 d . . . H29A H 0.6880 0.2895 0.1927 0.040 Uiso 1 1 calc R . . C30 C 0.6868(3) 0.1626(3) 0.1481(2) 0.0299(8) Uani 1 1 d . . . C31 C 0.8778(3) 0.3341(3) 0.3212(2) 0.0399(9) Uani 1 1 d . . . H31A H 0.9477 0.3430 0.3544 0.048 Uiso 1 1 calc R . . H31B H 0.8517 0.3902 0.2930 0.048 Uiso 1 1 calc R . . C32 C 0.7042(3) 0.3227(3) 0.3593(2) 0.0445(10) Uani 1 1 d . . . H32A H 0.6835 0.3769 0.3311 0.053 Uiso 1 1 calc R . . C33 C 0.6334(3) 0.2756(4) 0.3922(3) 0.0586(13) Uani 1 1 d . . . H33A H 0.5655 0.2983 0.3880 0.070 Uiso 1 1 calc R . . C34 C 0.6602(4) 0.1957(4) 0.4313(3) 0.0661(15) Uani 1 1 d . . . H34A H 0.6107 0.1625 0.4529 0.079 Uiso 1 1 calc R . . C35 C 0.7587(4) 0.1645(4) 0.4389(2) 0.0565(13) Uani 1 1 d . . . H35A H 0.7775 0.1093 0.4660 0.068 Uiso 1 1 calc R . . C36 C 0.8315(3) 0.2122(3) 0.4075(2) 0.0425(10) Uani 1 1 d . . . H36A H 0.8998 0.1898 0.4141 0.051 Uiso 1 1 calc R . . C37 C 0.8059(3) 0.2932(3) 0.3661(2) 0.0361(9) 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 Zr 0.02527(16) 0.02600(17) 0.02593(17) 0.00273(15) 0.00525(11) 0.00202(14) O1 0.0270(12) 0.0301(13) 0.0272(12) 0.0043(11) 0.0083(10) 0.0028(11) C1 0.0243(16) 0.0243(19) 0.0241(16) -0.0014(15) 0.0027(13) -0.0004(15) C2 0.0286(16) 0.0189(17) 0.0211(16) -0.0010(14) 0.0008(13) -0.0018(14) C3 0.0315(19) 0.0193(18) 0.0291(17) -0.0024(15) 0.0040(15) 0.0028(15) C4 0.0280(17) 0.0238(19) 0.0283(18) -0.0050(15) 0.0045(14) -0.0015(15) C5 0.0280(17) 0.0250(18) 0.0270(18) 0.0038(15) 0.0054(14) -0.0021(15) C6 0.0262(16) 0.0199(18) 0.0260(17) 0.0020(14) 0.0009(13) -0.0001(14) C7 0.0301(18) 0.023(2) 0.040(2) 0.0083(16) 0.0086(15) 0.0046(15) N7 0.0254(14) 0.0296(16) 0.0316(16) 0.0064(14) 0.0048(12) 0.0030(13) C8 0.0258(18) 0.062(3) 0.0272(19) 0.0159(19) 0.0065(15) 0.0067(18) C9 0.035(2) 0.063(3) 0.029(2) -0.002(2) 0.0076(16) 0.008(2) C10 0.044(2) 0.110(5) 0.031(2) -0.005(3) 0.0088(19) 0.004(3) C11 0.052(3) 0.155(7) 0.032(3) 0.016(4) 0.011(2) 0.009(4) C12 0.056(3) 0.114(5) 0.048(3) 0.052(3) 0.015(2) 0.015(3) C13 0.038(2) 0.066(3) 0.051(3) 0.032(2) 0.013(2) 0.013(2) C14 0.0389(19) 0.0227(19) 0.0228(17) 0.0052(15) 0.0050(15) 0.0038(16) C15 0.053(2) 0.033(2) 0.044(2) 0.0086(19) 0.0060(19) -0.013(2) C16 0.057(2) 0.038(2) 0.0283(19) 0.0068(18) 0.0135(18) 0.008(2) C17 0.055(2) 0.028(2) 0.038(2) 0.0101(18) 0.0123(18) 0.0071(19) C18 0.0292(18) 0.033(2) 0.045(2) 0.0008(18) 0.0133(17) 0.0023(16) C19 0.057(3) 0.055(3) 0.072(3) 0.010(3) 0.033(2) 0.023(2) C20 0.040(3) 0.051(3) 0.173(7) -0.029(4) 0.044(3) -0.007(2) C21 0.075(3) 0.116(5) 0.045(3) 0.015(3) 0.031(3) 0.037(3) C22 0.048(2) 0.051(3) 0.048(2) -0.013(2) 0.008(2) 0.002(2) C23 0.063(3) 0.060(3) 0.087(4) 0.047(3) 0.017(3) 0.017(3) C24 0.036(2) 0.034(2) 0.037(2) 0.0006(17) 0.0088(16) -0.0020(17) C25 0.038(2) 0.040(2) 0.043(2) -0.0092(19) 0.0057(17) 0.0015(18) C26 0.044(2) 0.066(3) 0.033(2) -0.015(2) 0.0026(18) 0.005(2) C27 0.042(2) 0.068(3) 0.029(2) 0.008(2) 0.0001(18) 0.008(2) C28 0.038(2) 0.043(3) 0.044(2) 0.005(2) 0.0064(17) 0.0073(19) C29 0.0314(19) 0.042(2) 0.0267(19) -0.0041(17) 0.0044(15) 0.0032(17) C30 0.0237(17) 0.036(2) 0.0299(19) -0.0020(17) 0.0047(14) -0.0021(15) C31 0.041(2) 0.039(2) 0.037(2) -0.0043(19) 0.0027(17) 0.0018(18) C32 0.046(2) 0.056(3) 0.031(2) -0.006(2) 0.0050(18) 0.015(2) C33 0.042(2) 0.091(4) 0.045(2) -0.006(3) 0.012(2) 0.012(3) C34 0.058(3) 0.104(5) 0.041(2) 0.010(3) 0.021(2) -0.007(3) C35 0.068(3) 0.071(3) 0.029(2) 0.018(2) 0.008(2) 0.005(3) C36 0.042(2) 0.055(3) 0.0277(19) -0.002(2) -0.0006(16) 0.009(2) C37 0.039(2) 0.041(2) 0.0251(18) -0.0064(18) -0.0015(15) 0.0068(19) _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 Zr O1 1.961(2) . ? Zr N7 2.025(3) . ? Zr C24 2.277(4) . ? Zr C31 2.282(4) . ? Zr C30 2.643(3) . ? Zr C37 2.730(4) . ? Zr C29 2.759(4) . ? Zr C7 2.838(3) . ? O1 C1 1.379(4) . ? C1 C2 1.397(5) . ? C1 C6 1.397(5) . ? C2 C3 1.403(4) . ? C2 C14 1.531(4) . ? C3 C4 1.379(5) . ? C4 C5 1.391(5) . ? C4 C18 1.530(4) . ? C5 C6 1.383(4) . ? C6 C7 1.508(4) . ? C7 N7 1.492(4) . ? N7 C8 1.435(5) . ? C8 C9 1.394(6) . ? C8 C13 1.406(6) . ? C9 C10 1.393(6) . ? C9 C22 1.503(6) . ? C10 C11 1.365(8) . ? C11 C12 1.365(8) . ? C12 C13 1.404(7) . ? C13 C23 1.498(7) . ? C14 C15 1.534(5) . ? C14 C17 1.534(5) . ? C14 C16 1.535(5) . ? C18 C19 1.512(6) . ? C18 C20 1.516(6) . ? C18 C21 1.523(6) . ? C24 C30 1.465(5) . ? C25 C26 1.373(6) . ? C25 C30 1.404(5) . ? C26 C27 1.385(6) . ? C27 C28 1.372(6) . ? C28 C29 1.395(5) . ? C29 C30 1.397(5) . ? C31 C37 1.460(5) . ? C32 C33 1.373(6) . ? C32 C37 1.400(5) . ? C33 C34 1.373(7) . ? C34 C35 1.368(7) . ? C35 C36 1.384(6) . ? C36 C37 1.403(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zr N7 88.76(10) . . ? O1 Zr C24 108.75(12) . . ? N7 Zr C24 123.33(13) . . ? O1 Zr C31 102.53(12) . . ? N7 Zr C31 108.42(13) . . ? C24 Zr C31 118.64(13) . . ? O1 Zr C30 131.57(11) . . ? N7 Zr C30 95.26(11) . . ? C24 Zr C30 33.62(12) . . ? C31 Zr C30 121.37(13) . . ? O1 Zr C37 105.85(10) . . ? N7 Zr C37 139.62(13) . . ? C24 Zr C37 87.91(13) . . ? C31 Zr C37 32.33(13) . . ? C30 Zr C37 101.71(11) . . ? O1 Zr C29 160.64(11) . . ? N7 Zr C29 88.62(11) . . ? C24 Zr C29 57.71(12) . . ? C31 Zr C29 96.50(13) . . ? C30 Zr C29 29.88(11) . . ? C37 Zr C29 88.36(10) . . ? O1 Zr C7 67.47(9) . . ? N7 Zr C7 30.25(11) . . ? C24 Zr C7 149.02(12) . . ? C31 Zr C7 91.60(12) . . ? C30 Zr C7 125.39(11) . . ? C37 Zr C7 123.01(11) . . ? C29 Zr C7 115.96(10) . . ? C1 O1 Zr 132.4(2) . . ? O1 C1 C2 120.8(3) . . ? O1 C1 C6 117.6(3) . . ? C2 C1 C6 121.6(3) . . ? C1 C2 C3 115.9(3) . . ? C1 C2 C14 122.7(3) . . ? C3 C2 C14 121.3(3) . . ? C4 C3 C2 124.4(3) . . ? C3 C4 C5 117.2(3) . . ? C3 C4 C18 122.5(3) . . ? C5 C4 C18 120.3(3) . . ? C6 C5 C4 121.5(3) . . ? C5 C6 C1 119.4(3) . . ? C5 C6 C7 121.9(3) . . ? C1 C6 C7 118.7(3) . . ? N7 C7 C6 113.5(3) . . ? N7 C7 Zr 43.15(14) . . ? C6 C7 Zr 98.4(2) . . ? C8 N7 C7 114.9(3) . . ? C8 N7 Zr 137.5(2) . . ? C7 N7 Zr 106.6(2) . . ? C9 C8 C13 120.8(4) . . ? C9 C8 N7 120.7(3) . . ? C13 C8 N7 118.5(4) . . ? C10 C9 C8 118.7(5) . . ? C10 C9 C22 119.1(4) . . ? C8 C9 C22 122.2(3) . . ? C11 C10 C9 120.8(5) . . ? C10 C11 C12 120.9(5) . . ? C11 C12 C13 120.7(5) . . ? C12 C13 C8 118.0(5) . . ? C12 C13 C23 121.0(5) . . ? C8 C13 C23 121.0(4) . . ? C2 C14 C15 108.8(3) . . ? C2 C14 C17 111.8(3) . . ? C15 C14 C17 108.0(3) . . ? C2 C14 C16 111.5(3) . . ? C15 C14 C16 109.7(3) . . ? C17 C14 C16 107.0(3) . . ? C19 C18 C20 107.5(4) . . ? C19 C18 C21 107.6(4) . . ? C20 C18 C21 110.9(4) . . ? C19 C18 C4 112.9(3) . . ? C20 C18 C4 108.7(3) . . ? C21 C18 C4 109.2(3) . . ? C30 C24 Zr 87.0(2) . . ? C26 C25 C30 120.9(4) . . ? C25 C26 C27 121.2(4) . . ? C28 C27 C26 119.3(4) . . ? C27 C28 C29 120.0(4) . . ? C28 C29 C30 121.5(4) . . ? C28 C29 Zr 132.6(3) . . ? C30 C29 Zr 70.4(2) . . ? C29 C30 C25 117.1(4) . . ? C29 C30 C24 119.0(3) . . ? C25 C30 C24 123.6(4) . . ? C29 C30 Zr 79.7(2) . . ? C25 C30 Zr 128.0(2) . . ? C24 C30 Zr 59.35(18) . . ? C37 C31 Zr 91.0(2) . . ? C33 C32 C37 121.9(4) . . ? C32 C33 C34 120.3(4) . . ? C35 C34 C33 119.5(4) . . ? C34 C35 C36 120.8(5) . . ? C35 C36 C37 121.0(4) . . ? C32 C37 C36 116.4(4) . . ? C32 C37 C31 122.8(4) . . ? C36 C37 C31 119.9(3) . . ? C32 C37 Zr 119.9(2) . . ? C36 C37 Zr 86.4(2) . . ? C31 C37 Zr 56.68(19) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 59.98 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.382 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.064 #===END data_Compound_3b _database_code_depnum_ccdc_archive 'CCDC 236412' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33.50 H49 N3 O2 Ti' _chemical_formula_weight 573.66 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 28.1195(8) _cell_length_b 12.6087(7) _cell_length_c 18.9179(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.379(4) _cell_angle_gamma 90.00 _cell_volume 6687.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 22 _cell_measurement_theta_min 10.99 _cell_measurement_theta_max 24.99 _exptl_crystal_description prisms _exptl_crystal_colour Yellow/orange _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method ? _exptl_crystal_F_000 2472 _exptl_absorpt_coefficient_mu 2.401 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.3216 _exptl_absorpt_correction_T_max 0.7531 _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5084 _diffrn_reflns_av_R_equivalents 0.0444 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 59.99 _reflns_number_total 4970 _reflns_number_observed 3921 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 292 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 'calc w=1/[\s^2^(Fo^2^)+(0.0631P)^2^+3.0831P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00005(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4678 _refine_ls_number_parameters 368 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0658 _refine_ls_R_factor_obs 0.0465 _refine_ls_wR_factor_all 0.1226 _refine_ls_wR_factor_obs 0.1082 _refine_ls_goodness_of_fit_all 1.039 _refine_ls_goodness_of_fit_obs 1.082 _refine_ls_restrained_S_all 1.102 _refine_ls_restrained_S_obs 1.111 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ti Ti 0.66357(2) 0.59101(4) 0.16914(2) 0.0299(2) Uani 1 d . . O1 O 0.63462(7) 0.63096(15) 0.07998(9) 0.0348(4) Uani 1 d . . C1 C 0.63363(10) 0.7308(2) 0.05280(13) 0.0328(6) Uani 1 d . . C2 C 0.59165(10) 0.7754(2) 0.02035(15) 0.0382(6) Uani 1 d . . C3 C 0.59472(11) 0.8776(2) -0.0064(2) 0.0418(7) Uani 1 d . . H3A H 0.56673(11) 0.9080(2) -0.0293(2) 0.050 Uiso 1 calc R . C4 C 0.63620(11) 0.9382(2) -0.00172(14) 0.0360(6) Uani 1 d . . C5 C 0.67703(10) 0.8910(2) 0.03062(13) 0.0342(6) Uani 1 d . . H5A H 0.70594(10) 0.9302(2) 0.03505(13) 0.041 Uiso 1 calc R . C6 C 0.67657(10) 0.7877(2) 0.05664(13) 0.0316(6) Uani 1 d . . C7 C 0.72293(10) 0.7366(2) 0.08293(14) 0.0345(6) Uani 1 d . . H7A H 0.73411(10) 0.6923(2) 0.04432(14) 0.041 Uiso 1 calc R . H7B H 0.74687(10) 0.7933(2) 0.09292(14) 0.041 Uiso 1 calc R . N7 N 0.72156(8) 0.6703(2) 0.14673(11) 0.0313(5) Uani 1 d . . C8 C 0.76575(10) 0.6480(2) 0.18081(13) 0.0295(5) Uani 1 d . . C9 C 0.81072(10) 0.6763(2) 0.15979(14) 0.0352(6) Uani 1 d . . H9A H 0.81310(10) 0.7169(2) 0.11787(14) 0.042 Uiso 1 calc R . C10 C 0.85192(11) 0.6455(3) 0.1999(2) 0.0422(7) Uani 1 d . . H10A H 0.88206(11) 0.6663(3) 0.1851(2) 0.051 Uiso 1 calc R . C11 C 0.85025(11) 0.5858(3) 0.2605(2) 0.0452(7) Uani 1 d . . H11A H 0.87884(11) 0.5659(3) 0.2873(2) 0.054 Uiso 1 calc R . C12 C 0.80595(12) 0.5546(2) 0.28224(15) 0.0412(7) Uani 1 d . . H12A H 0.80378(12) 0.5120(2) 0.32329(15) 0.049 Uiso 1 calc R . C13 C 0.76572(10) 0.5872(2) 0.24279(14) 0.0335(6) Uani 1 d . . O14 O 0.71936(7) 0.5570(2) 0.25746(9) 0.0366(4) Uani 1 d . . C15 C 0.71887(7) 0.63255(12) 0.37473(9) 0.0415(7) Uani 1 d G . H15A H 0.73411(7) 0.69482(12) 0.35946(9) 0.050 Uiso 1 calc R . C16 C 0.70633(8) 0.62459(13) 0.44420(8) 0.0463(7) Uani 1 d G . H16A H 0.71300(12) 0.6814(2) 0.47640(10) 0.056 Uiso 1 calc R . C17 C 0.68404(8) 0.53348(15) 0.46655(7) 0.0455(7) Uani 1 d G . H17A H 0.67547(12) 0.5280(2) 0.51402(8) 0.055 Uiso 1 calc R . C18 C 0.67427(8) 0.45032(12) 0.41942(9) 0.0470(7) Uani 1 d G . H18A H 0.65904(11) 0.3880(2) 0.43470(13) 0.056 Uiso 1 calc R . C19 C 0.68681(8) 0.45827(12) 0.34996(8) 0.0416(7) Uani 1 d G . H19A H 0.68014(12) 0.4014(2) 0.31775(11) 0.050 Uiso 1 calc R . C20 C 0.70911(7) 0.54938(13) 0.32761(7) 0.0348(6) Uani 1 d G . C21 C 0.54458(12) 0.7130(3) 0.0142(2) 0.0531(8) Uani 1 d . . C22 C 0.52859(14) 0.6887(4) 0.0881(2) 0.0695(11) Uani 1 d . . H22A H 0.49857(14) 0.6489(4) 0.0836(2) 0.104 Uiso 1 calc R . H22B H 0.52386(14) 0.7553(4) 0.1134(2) 0.104 Uiso 1 calc R . H22C H 0.55310(14) 0.6464(4) 0.1147(2) 0.104 Uiso 1 calc R . C23 C 0.55064(14) 0.6093(3) -0.0268(2) 0.0650(10) Uani 1 d . . H23A H 0.56087(14) 0.6256(3) -0.0740(2) 0.098 Uiso 1 calc R . H23B H 0.52018(14) 0.5712(3) -0.0316(2) 0.098 Uiso 1 calc R . H23C H 0.57475(14) 0.5649(3) -0.0010(2) 0.098 Uiso 1 calc R . C24 C 0.50429(14) 0.7762(4) -0.0262(3) 0.0773(12) Uani 1 d . . H24A H 0.51349(14) 0.7929(4) -0.0739(3) 0.116 Uiso 1 calc R . H24B H 0.49871(14) 0.8421(4) -0.0007(3) 0.116 Uiso 1 calc R . H24C H 0.47504(14) 0.7336(4) -0.0298(3) 0.116 Uiso 1 calc R . C25 C 0.63733(13) 1.0530(2) -0.0291(2) 0.0440(7) Uani 1 d . . C26 C 0.59434(14) 1.0783(3) -0.0810(2) 0.0575(9) Uani 1 d . . H26A H 0.59414(14) 1.0304(3) -0.1218(2) 0.086 Uiso 1 calc R . H26B H 0.59652(14) 1.1518(3) -0.0973(2) 0.086 Uiso 1 calc R . H26C H 0.56488(14) 1.0690(3) -0.0572(2) 0.086 Uiso 1 calc R . C27 C 0.68207(13) 1.0741(3) -0.0690(2) 0.0521(8) Uani 1 d . . H27A H 0.68233(13) 1.0260(3) -0.1097(2) 0.078 Uiso 1 calc R . H27B H 0.71067(13) 1.0621(3) -0.0371(2) 0.078 Uiso 1 calc R . H27C H 0.68170(13) 1.1477(3) -0.0858(2) 0.078 Uiso 1 calc R . C28 C 0.6372(2) 1.1282(3) 0.0340(2) 0.0708(12) Uani 1 d . . H28A H 0.6646(2) 1.1125(3) 0.0676(2) 0.106 Uiso 1 calc R . H28B H 0.6076(2) 1.1187(3) 0.0576(2) 0.106 Uiso 1 calc R . H28C H 0.6393(2) 1.2016(3) 0.0175(2) 0.106 Uiso 1 calc R . N29 N 0.65787(9) 0.4419(2) 0.16109(12) 0.0388(5) Uani 1 d . . C30 C 0.61141(14) 0.4010(3) 0.1363(2) 0.0610(9) Uani 1 d . . H30A H 0.58793(14) 0.4585(3) 0.1353(2) 0.091 Uiso 1 d R . H30B H 0.60207(14) 0.3450(3) 0.1684(2) 0.091 Uiso 1 d R . H30C H 0.61280(14) 0.3719(3) 0.0885(2) 0.091 Uiso 1 d R . C31 C 0.69438(13) 0.3609(2) 0.1644(2) 0.0488(8) Uani 1 d . . H31A H 0.72498(13) 0.3921(2) 0.1818(2) 0.073 Uiso 1 d R . H31B H 0.69708(13) 0.3312(2) 0.1170(2) 0.073 Uiso 1 d R . H31C H 0.68585(13) 0.3044(2) 0.1967(2) 0.073 Uiso 1 d R . N32 N 0.62407(10) 0.6538(2) 0.23360(13) 0.0455(6) Uani 1 d . . C33 C 0.58829(15) 0.6060(4) 0.2751(2) 0.0748(12) Uani 1 d . . H33A H 0.58681(15) 0.5295(4) 0.2660(2) 0.112 Uiso 1 d R . H33B H 0.55711(15) 0.6379(4) 0.2619(2) 0.112 Uiso 1 d R . H33C H 0.59687(15) 0.6184(4) 0.3256(2) 0.112 Uiso 1 d R . C34 C 0.6285(2) 0.7673(3) 0.2454(2) 0.0695(11) Uani 1 d . . H34A H 0.6532(2) 0.7958(3) 0.2167(2) 0.104 Uiso 1 d R . H34B H 0.6375(2) 0.7809(3) 0.2957(2) 0.104 Uiso 1 d R . H34C H 0.5980(2) 0.8019(3) 0.2318(2) 0.104 Uiso 1 d R . C41 C 0.5127(4) -0.0413(10) 0.2339(11) 0.152(7) Uani 0.50 d PDU -1 H41A H 0.5015(4) -0.0920(10) 0.1970(11) 0.229 Uiso 0.50 calc PR -1 H41B H 0.5057(4) -0.0687(10) 0.2804(11) 0.229 Uiso 0.50 calc PR -1 H41C H 0.5472(4) -0.0313(10) 0.2328(11) 0.229 Uiso 0.50 calc PR -1 C42 C 0.4896(7) 0.0556(10) 0.2217(9) 0.160(7) Uani 0.50 d PDU -1 H42A H 0.4962(7) 0.0782(10) 0.1733(9) 0.191 Uiso 0.50 calc PR -1 H42B H 0.4550(7) 0.0412(10) 0.2205(9) 0.191 Uiso 0.50 calc PR -1 C43 C 0.4985(8) 0.1428(9) 0.2657(4) 0.110(5) Uani 0.50 d PD -1 H43A H 0.5218(8) 0.1211(9) 0.3049(4) 0.132 Uiso 0.50 calc PR -1 H43B H 0.4684(8) 0.1609(9) 0.2871(4) 0.132 Uiso 0.50 calc PR -1 C44 C 0.5157(5) 0.2354(10) 0.2352(9) 0.124(5) Uani 0.50 d PD -1 H44A H 0.5194(5) 0.2204(10) 0.1845(9) 0.149 Uiso 0.50 calc PR -1 H44B H 0.5480(5) 0.2495(10) 0.2579(9) 0.149 Uiso 0.50 calc PR -1 C45 C 0.4886(5) 0.3302(10) 0.2388(14) 0.138(7) Uani 0.50 d PDU -1 H45A H 0.5048(5) 0.3879(10) 0.2155(14) 0.207 Uiso 0.50 calc PR -1 H45B H 0.4855(5) 0.3488(10) 0.2885(14) 0.207 Uiso 0.50 calc PR -1 H45C H 0.4569(5) 0.3194(10) 0.2148(14) 0.207 Uiso 0.50 calc PR -1 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 0.0312(3) 0.0281(2) 0.0307(2) 0.0006(2) 0.0039(2) -0.0029(2) O1 0.0336(10) 0.0340(10) 0.0364(9) 0.0005(8) -0.0007(8) -0.0030(8) C1 0.0325(15) 0.0338(14) 0.0322(12) -0.0018(11) 0.0029(10) 0.0013(11) C2 0.0296(15) 0.043(2) 0.0410(14) -0.0015(12) -0.0029(11) 0.0024(12) C3 0.035(2) 0.043(2) 0.046(2) -0.0012(12) -0.0040(12) 0.0097(13) C4 0.043(2) 0.0305(14) 0.0337(13) 0.0002(11) -0.0010(12) 0.0059(12) C5 0.0356(15) 0.0350(14) 0.0315(12) 0.0017(11) -0.0005(11) -0.0008(11) C6 0.0326(14) 0.0348(14) 0.0273(12) 0.0011(10) 0.0011(10) 0.0018(11) C7 0.0305(14) 0.0373(14) 0.0357(13) 0.0086(11) 0.0032(11) -0.0007(12) N7 0.0319(12) 0.0331(11) 0.0287(10) 0.0043(9) 0.0005(9) 0.0012(9) C8 0.0310(14) 0.0267(12) 0.0304(12) -0.0018(10) -0.0004(10) 0.0029(10) C9 0.0348(15) 0.0341(14) 0.0366(13) 0.0003(11) 0.0028(11) -0.0002(12) C10 0.0310(15) 0.049(2) 0.046(2) -0.0064(13) 0.0021(12) 0.0034(13) C11 0.036(2) 0.054(2) 0.044(2) -0.0029(14) -0.0057(12) 0.0097(14) C12 0.045(2) 0.044(2) 0.0339(13) 0.0040(12) -0.0024(12) 0.0051(13) C13 0.0339(14) 0.0319(13) 0.0345(13) -0.0013(11) 0.0015(11) 0.0000(12) O14 0.0385(11) 0.0417(10) 0.0292(9) 0.0060(8) 0.0005(8) -0.0048(8) C15 0.054(2) 0.0345(14) 0.0367(14) 0.0045(12) 0.0056(13) -0.0028(13) C16 0.058(2) 0.044(2) 0.0369(15) -0.0057(12) 0.0041(14) 0.0046(15) C17 0.054(2) 0.050(2) 0.0335(14) 0.0064(13) 0.0090(13) 0.0117(15) C18 0.058(2) 0.041(2) 0.044(2) 0.0119(13) 0.0140(14) -0.0007(14) C19 0.052(2) 0.0360(14) 0.0364(14) 0.0023(12) 0.0040(13) -0.0044(13) C20 0.040(2) 0.0352(14) 0.0295(13) 0.0067(11) 0.0035(11) 0.0032(12) C21 0.030(2) 0.061(2) 0.066(2) 0.001(2) -0.0070(14) -0.0050(15) C22 0.039(2) 0.089(3) 0.082(3) 0.005(2) 0.012(2) -0.011(2) C23 0.053(2) 0.063(2) 0.076(2) -0.006(2) -0.015(2) -0.019(2) C24 0.034(2) 0.084(3) 0.110(3) 0.010(3) -0.019(2) 0.000(2) C25 0.058(2) 0.0342(15) 0.0385(14) 0.0022(12) -0.0050(13) 0.0091(14) C26 0.060(2) 0.053(2) 0.058(2) 0.015(2) -0.009(2) 0.015(2) C27 0.057(2) 0.037(2) 0.061(2) 0.0111(14) -0.005(2) -0.0029(15) C28 0.126(4) 0.037(2) 0.048(2) -0.0014(15) -0.003(2) 0.015(2) N29 0.0435(14) 0.0342(12) 0.0390(12) 0.0020(10) 0.0037(10) -0.0036(11) C30 0.054(2) 0.048(2) 0.082(2) -0.002(2) 0.004(2) -0.016(2) C31 0.063(2) 0.0363(15) 0.047(2) -0.0005(13) 0.0035(15) 0.0061(15) N32 0.046(2) 0.0518(15) 0.0395(13) -0.0013(11) 0.0086(11) 0.0045(12) C33 0.057(2) 0.099(3) 0.072(2) 0.003(2) 0.030(2) 0.004(2) C34 0.078(3) 0.060(2) 0.071(2) -0.020(2) 0.015(2) 0.014(2) C41 0.065(9) 0.198(13) 0.185(15) -0.040(12) -0.054(9) 0.054(8) C42 0.155(10) 0.151(10) 0.169(11) -0.015(8) -0.013(8) -0.007(9) C43 0.132(10) 0.141(10) 0.055(11) 0.005(5) -0.005(11) -0.014(11) C44 0.091(10) 0.135(12) 0.148(13) 0.023(11) 0.020(8) -0.010(9) C45 0.081(13) 0.166(11) 0.172(15) 0.019(12) 0.047(12) 0.028(8) _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 Ti O1 1.885(2) . ? Ti N32 1.886(3) . ? Ti N29 1.892(2) . ? Ti N7 1.986(2) . ? Ti O14 2.244(2) . ? O1 C1 1.359(3) . ? C1 C6 1.402(4) . ? C1 C2 1.406(4) . ? C2 C3 1.389(4) . ? C2 C21 1.537(4) . ? C3 C4 1.392(4) . ? C4 C5 1.393(4) . ? C4 C25 1.538(4) . ? C5 C6 1.393(4) . ? C6 C7 1.504(4) . ? C7 N7 1.471(3) . ? N7 C8 1.384(4) . ? C8 C9 1.400(4) . ? C8 C13 1.401(4) . ? C9 C10 1.391(4) . ? C10 C11 1.376(5) . ? C11 C12 1.397(5) . ? C12 C13 1.370(4) . ? C13 O14 1.406(3) . ? O14 C20 1.383(2) . ? C15 C16 1.39 . ? C15 C20 1.39 . ? C16 C17 1.39 . ? C17 C18 1.39 . ? C18 C19 1.39 . ? C19 C20 1.39 . ? C21 C22 1.532(5) . ? C21 C23 1.537(5) . ? C21 C24 1.540(5) . ? C25 C28 1.524(5) . ? C25 C26 1.532(4) . ? C25 C27 1.540(5) . ? N29 C31 1.446(4) . ? N29 C30 1.449(4) . ? N32 C34 1.452(5) . ? N32 C33 1.454(5) . ? C41 C42 1.395(9) . ? C42 C43 1.391(9) . ? C43 C44 1.406(9) . ? C44 C45 1.422(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ti N32 103.36(10) . . ? O1 Ti N29 99.52(9) . . ? N32 Ti N29 114.77(12) . . ? O1 Ti N7 88.86(8) . . ? N32 Ti N7 117.41(11) . . ? N29 Ti N7 123.29(10) . . ? O1 Ti O14 161.27(8) . . ? N32 Ti O14 90.66(10) . . ? N29 Ti O14 85.43(9) . . ? N7 Ti O14 73.52(8) . . ? C1 O1 Ti 125.5(2) . . ? O1 C1 C6 117.5(2) . . ? O1 C1 C2 121.9(3) . . ? C6 C1 C2 120.6(3) . . ? C3 C2 C1 117.2(3) . . ? C3 C2 C21 121.7(3) . . ? C1 C2 C21 121.2(3) . . ? C2 C3 C4 124.2(3) . . ? C3 C4 C5 116.8(3) . . ? C3 C4 C25 122.3(3) . . ? C5 C4 C25 120.9(3) . . ? C6 C5 C4 121.7(3) . . ? C5 C6 C1 119.5(3) . . ? C5 C6 C7 119.1(2) . . ? C1 C6 C7 121.3(2) . . ? N7 C7 C6 116.0(2) . . ? C8 N7 C7 114.7(2) . . ? C8 N7 Ti 121.4(2) . . ? C7 N7 Ti 122.3(2) . . ? N7 C8 C9 127.9(2) . . ? N7 C8 C13 116.3(2) . . ? C9 C8 C13 115.8(2) . . ? C10 C9 C8 120.4(3) . . ? C11 C10 C9 121.9(3) . . ? C10 C11 C12 119.1(3) . . ? C13 C12 C11 118.3(3) . . ? C12 C13 C8 124.5(3) . . ? C12 C13 O14 123.4(2) . . ? C8 C13 O14 111.9(2) . . ? C20 O14 C13 118.2(2) . . ? C20 O14 Ti 122.88(15) . . ? C13 O14 Ti 114.04(15) . . ? C16 C15 C20 120.0 . . ? C17 C16 C15 120.0 . . ? C18 C17 C16 120.0 . . ? C19 C18 C17 120.0 . . ? C18 C19 C20 120.0 . . ? O14 C20 C19 118.78(14) . . ? O14 C20 C15 121.16(14) . . ? C19 C20 C15 120.0 . . ? C22 C21 C2 110.2(3) . . ? C22 C21 C23 110.1(3) . . ? C2 C21 C23 110.2(3) . . ? C22 C21 C24 107.5(3) . . ? C2 C21 C24 111.7(3) . . ? C23 C21 C24 107.1(3) . . ? C28 C25 C26 108.9(3) . . ? C28 C25 C4 108.7(2) . . ? C26 C25 C4 112.1(3) . . ? C28 C25 C27 109.1(3) . . ? C26 C25 C27 106.5(3) . . ? C4 C25 C27 111.5(3) . . ? C31 N29 C30 112.5(3) . . ? C31 N29 Ti 130.0(2) . . ? C30 N29 Ti 116.7(2) . . ? C34 N32 C33 112.4(3) . . ? C34 N32 Ti 117.7(2) . . ? C33 N32 Ti 129.9(3) . . ? C43 C42 C41 122.3(11) . . ? C42 C43 C44 117.5(9) . . ? C43 C44 C45 118.4(10) . . ? _refine_diff_density_max 0.276 _refine_diff_density_min -0.316 _refine_diff_density_rms 0.047 #===END