# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Philip Mountford' _publ_contact_author_email philip.mountford@chem.ox.ac.uk loop_ _publ_author_name A.Schwarz A.Nielson P.Mountford data_ADS151 _database_code_depnum_ccdc_archive 'CCDC 813857' #TrackingRef 'ADS151.cif' _audit_creation_date 11-02-18 _audit_creation_method CRYSTALS_ver_14.15 _chemical_name_systematic ; Ti(NAr)(NHAr)2(py)2 ; _chemical_melting_point ? _refine_special_details ; C-bound H atoms were placed geometrically and refined in a riding model. N-bound H atoms were placed using a difference map and their positions and isotropic temperture factors refined. Disordered solvent of crystallisation was modeled using a SQUEEZE model after unsatifactory attempts to model the disorder. ; _cell_length_a 9.69140(10) _cell_length_b 12.10820(10) _cell_length_c 22.0163(3) _cell_angle_alpha 80.7710(4) _cell_angle_beta 79.7200(5) _cell_angle_gamma 73.3185(5) _cell_volume 2418.67(5) _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C46 H63 N5 Ti1' _chemical_formula_moiety 'C46 H63 N5 Ti1' _chemical_compound_source ? _chemical_formula_weight 733.94 _cell_measurement_reflns_used 9993 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_min 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.400 _exptl_crystal_density_diffrn 1.008 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.209 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.96 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 11001 _reflns_number_total 11001 _diffrn_reflns_av_R_equivalents 0.029 _diffrn_reflns_theta_min 5.097 _diffrn_reflns_theta_max 27.486 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.936 _diffrn_measured_fraction_theta_full 0.991 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 28 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -15 _reflns_limit_k_max 15 _reflns_limit_l_min 0 _reflns_limit_l_max 28 _oxford_diffrn_Wilson_B_factor 2.30 _oxford_diffrn_Wilson_scale 6.07 _atom_sites_solution_primary Direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.45 _refine_diff_density_max 1.48 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 7786 _refine_ls_number_restraints 0 _refine_ls_number_parameters 476 _oxford_refine_ls_R_factor_ref 0.0632 _refine_ls_wR_factor_ref 0.0614 _refine_ls_goodness_of_fit_ref 0.9984 _refine_ls_shift/su_max 0.0013645 _refine_ls_shift/su_mean 0.0000261 # The values computed from all data _oxford_reflns_number_all 11001 _refine_ls_R_factor_all 0.0899 _refine_ls_wR_factor_all 0.0799 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 8501 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_gt 0.0645 _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.560 -0.488 -0.131E-01 -0.377 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.51655(4) -0.20657(3) 0.777020(17) 0.0210 1.0000 Uani . . . . . . N1 N 0.4613(2) -0.05774(15) 0.76209(8) 0.0263 1.0000 Uani . . . . . . N2 N 0.3892(2) -0.27227(17) 0.84914(9) 0.0303 1.0000 Uani . . . . . . N3 N 0.6876(2) -0.24052(16) 0.70833(8) 0.0247 1.0000 Uani . . . . . . N4 N 0.6762(2) -0.22515(16) 0.84426(9) 0.0270 1.0000 Uani . . . . . . N5 N 0.3881(2) -0.27116(17) 0.71863(9) 0.0300 1.0000 Uani . . . . . . C1 C 0.4122(3) 0.06304(19) 0.75449(11) 0.0311 1.0000 Uani . . . . . . C2 C 0.4720(3) 0.1301(2) 0.78453(12) 0.0351 1.0000 Uani . . . . . . C3 C 0.4134(3) 0.2506(2) 0.77957(15) 0.0487 1.0000 Uani . . . . . . C4 C 0.3038(4) 0.3043(2) 0.74470(18) 0.0583 1.0000 Uani . . . . . . C5 C 0.2490(3) 0.2393(2) 0.71342(16) 0.0526 1.0000 Uani . . . . . . C6 C 0.3000(3) 0.1184(2) 0.71784(12) 0.0382 1.0000 Uani . . . . . . C7 C 0.6027(3) 0.0720(2) 0.81781(13) 0.0390 1.0000 Uani . . . . . . C8 C 0.6192(4) 0.1332(3) 0.87020(16) 0.0546 1.0000 Uani . . . . . . C9 C 0.7407(3) 0.0559(3) 0.77027(16) 0.0519 1.0000 Uani . . . . . . C10 C 0.2417(3) 0.0460(3) 0.68460(14) 0.0458 1.0000 Uani . . . . . . C11 C 0.0876(4) 0.1053(3) 0.6684(2) 0.0686 1.0000 Uani . . . . . . C12 C 0.3450(4) 0.0072(3) 0.62685(15) 0.0591 1.0000 Uani . . . . . . C13 C 0.2998(2) -0.26922(19) 0.90635(10) 0.0251 1.0000 Uani . . . . . . C14 C 0.2640(2) -0.37129(19) 0.93905(10) 0.0282 1.0000 Uani . . . . . . C15 C 0.1875(3) -0.3681(2) 0.99880(11) 0.0344 1.0000 Uani . . . . . . C16 C 0.1409(3) -0.2674(2) 1.02755(11) 0.0370 1.0000 Uani . . . . . . C17 C 0.1668(2) -0.1669(2) 0.99445(11) 0.0324 1.0000 Uani . . . . . . C18 C 0.2424(2) -0.1637(2) 0.93438(10) 0.0275 1.0000 Uani . . . . . . C19 C 0.3112(3) -0.4866(2) 0.91138(11) 0.0337 1.0000 Uani . . . . . . C20 C 0.1887(3) -0.5467(3) 0.91947(15) 0.0483 1.0000 Uani . . . . . . C21 C 0.4441(3) -0.5662(2) 0.93873(15) 0.0484 1.0000 Uani . . . . . . C22 C 0.2553(3) -0.0485(2) 0.89894(11) 0.0342 1.0000 Uani . . . . . . C23 C 0.2648(4) 0.0396(3) 0.93928(15) 0.0515 1.0000 Uani . . . . . . C24 C 0.1271(3) 0.0037(2) 0.86182(13) 0.0437 1.0000 Uani . . . . . . C25 C 0.7845(2) -0.32762(18) 0.67643(10) 0.0242 1.0000 Uani . . . . . . C26 C 0.8542(2) -0.3034(2) 0.61482(10) 0.0283 1.0000 Uani . . . . . . C27 C 0.9453(3) -0.3944(2) 0.58396(11) 0.0343 1.0000 Uani . . . . . . C28 C 0.9718(3) -0.5084(2) 0.61081(12) 0.0381 1.0000 Uani . . . . . . C29 C 0.9062(3) -0.5317(2) 0.67050(12) 0.0367 1.0000 Uani . . . . . . C30 C 0.8139(2) -0.44423(19) 0.70398(10) 0.0284 1.0000 Uani . . . . . . C31 C 0.8292(3) -0.1783(2) 0.58369(11) 0.0404 1.0000 Uani . . . . . . C32 C 0.8487(6) -0.1685(4) 0.51269(18) 0.0894 1.0000 Uani . . . . . . C33 C 0.9136(6) -0.1145(4) 0.6062(2) 0.0798 1.0000 Uani . . . . . . C34 C 0.7468(3) -0.4777(2) 0.76978(12) 0.0395 1.0000 Uani . . . . . . C35 C 0.6463(4) -0.5554(3) 0.77105(17) 0.0623 1.0000 Uani . . . . . . C36 C 0.8619(4) -0.5329(3) 0.81266(15) 0.0671 1.0000 Uani . . . . . . C37 C 0.8159(3) -0.2299(3) 0.82453(13) 0.0407 1.0000 Uani . . . . . . C38 C 0.9121(3) -0.2305(3) 0.86416(15) 0.0534 1.0000 Uani . . . . . . C39 C 0.8634(3) -0.2232(3) 0.92622(14) 0.0462 1.0000 Uani . . . . . . C40 C 0.7212(3) -0.2179(2) 0.94692(12) 0.0397 1.0000 Uani . . . . . . C41 C 0.6309(3) -0.2207(2) 0.90531(11) 0.0320 1.0000 Uani . . . . . . C42 C 0.2523(3) -0.2763(4) 0.73978(16) 0.0613 1.0000 Uani . . . . . . C43 C 0.1742(4) -0.3238(4) 0.7096(2) 0.0808 1.0000 Uani . . . . . . C44 C 0.2348(4) -0.3701(3) 0.65717(19) 0.0642 1.0000 Uani . . . . . . C45 C 0.3722(4) -0.3658(4) 0.63419(19) 0.0738 1.0000 Uani . . . . . . C46 C 0.4449(3) -0.3149(3) 0.66578(14) 0.0537 1.0000 Uani . . . . . . H1 H 0.412(3) -0.342(3) 0.8387(15) 0.047(6) 1.0000 Uiso . . . . . . H2 H 0.689(3) -0.177(3) 0.6864(15) 0.047(6) 1.0000 Uiso . . . . . . H31 H 0.4500 0.2956 0.8011 0.0628 1.0000 Uiso R . . . . . H41 H 0.2658 0.3862 0.7417 0.0725 1.0000 Uiso R . . . . . H51 H 0.1749 0.2776 0.6884 0.0644 1.0000 Uiso R . . . . . H71 H 0.5945 -0.0033 0.8352 0.0492 1.0000 Uiso R . . . . . H81 H 0.7034 0.0902 0.8884 0.0702 1.0000 Uiso R . . . . . H82 H 0.5357 0.1392 0.9009 0.0702 1.0000 Uiso R . . . . . H83 H 0.6286 0.2086 0.8540 0.0702 1.0000 Uiso R . . . . . H91 H 0.8234 0.0192 0.7907 0.0676 1.0000 Uiso R . . . . . H92 H 0.7483 0.1300 0.7503 0.0676 1.0000 Uiso R . . . . . H93 H 0.7359 0.0095 0.7402 0.0676 1.0000 Uiso R . . . . . H101 H 0.2370 -0.0225 0.7119 0.0572 1.0000 Uiso R . . . . . H111 H 0.0571 0.0545 0.6482 0.0879 1.0000 Uiso R . . . . . H112 H 0.0219 0.1233 0.7053 0.0879 1.0000 Uiso R . . . . . H113 H 0.0888 0.1748 0.6415 0.0879 1.0000 Uiso R . . . . . H121 H 0.3070 -0.0388 0.6066 0.0758 1.0000 Uiso R . . . . . H122 H 0.4371 -0.0366 0.6381 0.0758 1.0000 Uiso R . . . . . H123 H 0.3559 0.0744 0.5996 0.0758 1.0000 Uiso R . . . . . H151 H 0.1669 -0.4372 1.0205 0.0447 1.0000 Uiso R . . . . . H161 H 0.0921 -0.2674 1.0690 0.0459 1.0000 Uiso R . . . . . H171 H 0.1314 -0.0968 1.0131 0.0413 1.0000 Uiso R . . . . . H191 H 0.3400 -0.4706 0.8680 0.0436 1.0000 Uiso R . . . . . H201 H 0.2229 -0.6176 0.9015 0.0642 1.0000 Uiso R . . . . . H202 H 0.1569 -0.5621 0.9626 0.0642 1.0000 Uiso R . . . . . H203 H 0.1100 -0.4971 0.8998 0.0642 1.0000 Uiso R . . . . . H211 H 0.4738 -0.6376 0.9212 0.0628 1.0000 Uiso R . . . . . H212 H 0.4189 -0.5805 0.9824 0.0628 1.0000 Uiso R . . . . . H213 H 0.5216 -0.5300 0.9301 0.0628 1.0000 Uiso R . . . . . H221 H 0.3418 -0.0631 0.8699 0.0437 1.0000 Uiso R . . . . . H231 H 0.2725 0.1094 0.9138 0.0663 1.0000 Uiso R . . . . . H232 H 0.3481 0.0090 0.9600 0.0663 1.0000 Uiso R . . . . . H233 H 0.1799 0.0554 0.9691 0.0663 1.0000 Uiso R . . . . . H241 H 0.1355 0.0760 0.8395 0.0552 1.0000 Uiso R . . . . . H242 H 0.0385 0.0153 0.8896 0.0552 1.0000 Uiso R . . . . . H243 H 0.1279 -0.0480 0.8335 0.0552 1.0000 Uiso R . . . . . H271 H 0.9924 -0.3776 0.5432 0.0432 1.0000 Uiso R . . . . . H281 H 1.0334 -0.5695 0.5885 0.0478 1.0000 Uiso R . . . . . H291 H 0.9239 -0.6098 0.6894 0.0460 1.0000 Uiso R . . . . . H311 H 0.7309 -0.1392 0.5969 0.0510 1.0000 Uiso R . . . . . H321 H 0.8310 -0.0891 0.4961 0.1494 1.0000 Uiso R . . . . . H322 H 0.9456 -0.2087 0.4980 0.1494 1.0000 Uiso R . . . . . H323 H 0.7826 -0.2018 0.4998 0.1494 1.0000 Uiso R . . . . . H331 H 0.8950 -0.0371 0.5862 0.1145 1.0000 Uiso R . . . . . H332 H 0.8928 -0.1133 0.6499 0.1145 1.0000 Uiso R . . . . . H333 H 1.0130 -0.1538 0.5953 0.1145 1.0000 Uiso R . . . . . H341 H 0.6885 -0.4082 0.7858 0.0485 1.0000 Uiso R . . . . . H351 H 0.6054 -0.5748 0.8125 0.0805 1.0000 Uiso R . . . . . H352 H 0.7012 -0.6244 0.7536 0.0805 1.0000 Uiso R . . . . . H353 H 0.5706 -0.5154 0.7471 0.0805 1.0000 Uiso R . . . . . H361 H 0.8174 -0.5528 0.8535 0.0860 1.0000 Uiso R . . . . . H362 H 0.9166 -0.4797 0.8139 0.0860 1.0000 Uiso R . . . . . H363 H 0.9247 -0.6010 0.7967 0.0860 1.0000 Uiso R . . . . . H371 H 0.8503 -0.2333 0.7815 0.0511 1.0000 Uiso R . . . . . H381 H 1.0115 -0.2358 0.8485 0.0664 1.0000 Uiso R . . . . . H391 H 0.9274 -0.2209 0.9538 0.0569 1.0000 Uiso R . . . . . H401 H 0.6846 -0.2133 0.9897 0.0495 1.0000 Uiso R . . . . . H411 H 0.5323 -0.2192 0.9205 0.0405 1.0000 Uiso R . . . . . H421 H 0.2086 -0.2473 0.7783 0.0760 1.0000 Uiso R . . . . . H431 H 0.0758 -0.3217 0.7256 0.0966 1.0000 Uiso R . . . . . H441 H 0.1834 -0.4050 0.6363 0.0796 1.0000 Uiso R . . . . . H451 H 0.4193 -0.3980 0.5969 0.0874 1.0000 Uiso R . . . . . H461 H 0.5410 -0.3113 0.6488 0.0656 1.0000 Uiso 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 0.02130(18) 0.02119(17) 0.02053(17) -0.00459(13) -0.00034(13) -0.00615(13) N1 0.0255(9) 0.0259(9) 0.0263(9) -0.0058(7) -0.0039(7) -0.0035(7) N2 0.0363(11) 0.0268(9) 0.0290(10) -0.0118(8) 0.0080(8) -0.0131(8) N3 0.0262(9) 0.0229(9) 0.0226(8) -0.0018(7) 0.0006(7) -0.0056(7) N4 0.0278(9) 0.0263(9) 0.0271(9) -0.0045(7) -0.0057(7) -0.0058(7) N5 0.0249(9) 0.0329(10) 0.0338(10) -0.0115(8) -0.0040(8) -0.0064(7) C1 0.0306(11) 0.0251(10) 0.0312(11) -0.0013(9) 0.0029(9) -0.0028(9) C2 0.0396(13) 0.0230(10) 0.0410(13) -0.0047(9) 0.0006(10) -0.0088(9) C3 0.0511(17) 0.0262(12) 0.0662(19) -0.0089(12) -0.0004(14) -0.0088(11) C4 0.0553(18) 0.0241(12) 0.086(2) -0.0011(14) -0.0077(17) 0.0002(12) C5 0.0386(15) 0.0367(14) 0.069(2) 0.0092(13) -0.0082(14) 0.0039(11) C6 0.0293(12) 0.0346(12) 0.0428(14) 0.0018(10) -0.0005(10) -0.0021(9) C7 0.0485(15) 0.0283(11) 0.0445(14) -0.0049(10) -0.0069(12) -0.0163(10) C8 0.072(2) 0.0468(16) 0.0567(18) -0.0128(14) -0.0128(16) -0.0275(15) C9 0.0411(15) 0.0524(17) 0.0622(19) -0.0081(14) -0.0078(13) -0.0113(13) C10 0.0389(14) 0.0470(15) 0.0468(15) 0.0033(12) -0.0164(12) -0.0026(12) C11 0.0461(18) 0.072(2) 0.086(3) -0.0024(19) -0.0283(18) -0.0056(16) C12 0.0580(19) 0.072(2) 0.0427(16) -0.0071(15) -0.0178(14) -0.0040(16) C13 0.0231(10) 0.0319(11) 0.0216(9) -0.0062(8) -0.0017(8) -0.0085(8) C14 0.0282(11) 0.0319(11) 0.0237(10) -0.0022(8) -0.0036(8) -0.0074(9) C15 0.0329(12) 0.0385(12) 0.0274(11) 0.0030(9) -0.0021(9) -0.0074(10) C16 0.0339(12) 0.0504(14) 0.0212(10) -0.0047(10) 0.0009(9) -0.0053(11) C17 0.0273(11) 0.0408(13) 0.0277(11) -0.0115(9) -0.0018(9) -0.0041(9) C18 0.0238(10) 0.0347(11) 0.0251(10) -0.0080(9) -0.0009(8) -0.0088(9) C19 0.0436(13) 0.0306(11) 0.0276(11) -0.0010(9) -0.0006(10) -0.0147(10) C20 0.0531(17) 0.0436(15) 0.0548(17) -0.0033(13) -0.0094(14) -0.0235(13) C21 0.0465(16) 0.0383(14) 0.0564(17) -0.0132(12) -0.0040(13) -0.0027(12) C22 0.0337(12) 0.0304(11) 0.0362(12) -0.0127(10) 0.0090(10) -0.0087(9) C23 0.0601(18) 0.0447(15) 0.0541(17) -0.0241(13) 0.0118(14) -0.0230(14) C24 0.0430(15) 0.0378(13) 0.0427(14) -0.0040(11) 0.0019(12) -0.0038(11) C25 0.0210(9) 0.0279(10) 0.0242(10) -0.0040(8) -0.0044(8) -0.0060(8) C26 0.0267(11) 0.0357(11) 0.0225(10) -0.0036(9) -0.0018(8) -0.0093(9) C27 0.0288(11) 0.0471(14) 0.0268(11) -0.0113(10) 0.0012(9) -0.0089(10) C28 0.0301(12) 0.0392(13) 0.0418(13) -0.0171(11) 0.0022(10) -0.0019(10) C29 0.0347(12) 0.0283(11) 0.0425(13) -0.0076(10) 0.0001(10) -0.0026(9) C30 0.0270(11) 0.0265(10) 0.0302(11) -0.0043(8) -0.0024(9) -0.0053(8) C31 0.0472(15) 0.0389(13) 0.0276(12) 0.0019(10) 0.0002(11) -0.0060(11) C32 0.138(4) 0.083(3) 0.0444(19) 0.0063(19) -0.010(2) -0.035(3) C33 0.114(4) 0.066(2) 0.065(2) -0.0026(19) -0.006(2) -0.040(2) C34 0.0530(15) 0.0227(11) 0.0330(12) -0.0002(9) 0.0065(11) -0.0040(10) C35 0.078(2) 0.0392(15) 0.066(2) -0.0109(14) 0.0281(18) -0.0298(15) C36 0.083(3) 0.062(2) 0.0352(15) 0.0091(14) -0.0065(15) 0.0048(18) C37 0.0280(12) 0.0571(16) 0.0380(13) -0.0135(12) -0.0032(10) -0.0095(11) C38 0.0308(14) 0.081(2) 0.0528(17) -0.0200(16) -0.0084(12) -0.0130(14) C39 0.0453(15) 0.0509(16) 0.0476(15) -0.0100(12) -0.0226(13) -0.0089(12) C40 0.0520(16) 0.0391(13) 0.0304(12) -0.0047(10) -0.0127(11) -0.0114(11) C41 0.0382(13) 0.0323(11) 0.0273(11) -0.0048(9) -0.0065(9) -0.0100(9) C42 0.0360(15) 0.102(3) 0.0601(19) -0.0368(19) 0.0026(14) -0.0314(17) C43 0.0458(19) 0.134(4) 0.087(3) -0.040(3) -0.0083(18) -0.049(2) C44 0.063(2) 0.0608(19) 0.087(3) -0.0219(18) -0.0431(19) -0.0177(16) C45 0.0501(19) 0.101(3) 0.081(2) -0.064(2) -0.0276(18) 0.0041(18) C46 0.0306(13) 0.090(2) 0.0453(16) -0.0380(16) -0.0048(12) -0.0067(14) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5320(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . N1 . 1.7208(18) yes Ti1 . N2 . 2.0337(19) yes Ti1 . N3 . 2.0291(18) yes Ti1 . N4 . 2.2684(18) yes Ti1 . N5 . 2.2948(19) yes N1 . C1 . 1.394(3) yes N2 . C13 . 1.395(3) yes N2 . H1 . 0.87(3) no N3 . C25 . 1.386(3) yes N3 . H2 . 0.84(3) no N4 . C37 . 1.334(3) yes N4 . C41 . 1.342(3) yes N5 . C42 . 1.331(3) yes N5 . C46 . 1.319(3) yes C1 . C2 . 1.418(4) yes C1 . C6 . 1.416(3) yes C2 . C3 . 1.399(3) yes C2 . C7 . 1.513(4) yes C3 . C4 . 1.369(5) yes C3 . H31 . 0.950 no C4 . C5 . 1.386(5) yes C4 . H41 . 0.950 no C5 . C6 . 1.399(4) yes C5 . H51 . 0.950 no C6 . C10 . 1.503(4) yes C7 . C8 . 1.521(4) yes C7 . C9 . 1.529(4) yes C7 . H71 . 0.950 no C8 . H81 . 0.950 no C8 . H82 . 0.950 no C8 . H83 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . C11 . 1.539(4) yes C10 . C12 . 1.519(4) yes C10 . H101 . 0.950 no C11 . H111 . 0.950 no C11 . H112 . 0.950 no C11 . H113 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . C14 . 1.428(3) yes C13 . C18 . 1.430(3) yes C14 . C15 . 1.390(3) yes C14 . C19 . 1.528(3) yes C15 . C16 . 1.385(4) yes C15 . H151 . 0.950 no C16 . C17 . 1.379(4) yes C16 . H161 . 0.950 no C17 . C18 . 1.393(3) yes C17 . H171 . 0.950 no C18 . C22 . 1.512(3) yes C19 . C20 . 1.533(4) yes C19 . C21 . 1.526(4) yes C19 . H191 . 0.950 no C20 . H201 . 0.950 no C20 . H202 . 0.950 no C20 . H203 . 0.950 no C21 . H211 . 0.950 no C21 . H212 . 0.950 no C21 . H213 . 0.950 no C22 . C23 . 1.525(3) yes C22 . C24 . 1.535(4) yes C22 . H221 . 0.950 no C23 . H231 . 0.950 no C23 . H232 . 0.950 no C23 . H233 . 0.950 no C24 . H241 . 0.950 no C24 . H242 . 0.950 no C24 . H243 . 0.950 no C25 . C26 . 1.429(3) yes C25 . C30 . 1.414(3) yes C26 . C27 . 1.386(3) yes C26 . C31 . 1.529(3) yes C27 . C28 . 1.382(4) yes C27 . H271 . 0.950 no C28 . C29 . 1.377(4) yes C28 . H281 . 0.950 no C29 . C30 . 1.392(3) yes C29 . H291 . 0.950 no C30 . C34 . 1.521(3) yes C31 . C32 . 1.530(4) yes C31 . C33 . 1.464(5) yes C31 . H311 . 0.950 no C32 . H321 . 0.950 no C32 . H322 . 0.950 no C32 . H323 . 0.950 no C33 . H331 . 0.950 no C33 . H332 . 0.950 no C33 . H333 . 0.950 no C34 . C35 . 1.530(4) yes C34 . C36 . 1.525(4) yes C34 . H341 . 0.950 no C35 . H351 . 0.950 no C35 . H352 . 0.950 no C35 . H353 . 0.950 no C36 . H361 . 0.950 no C36 . H362 . 0.950 no C36 . H363 . 0.950 no C37 . C38 . 1.384(4) yes C37 . H371 . 0.950 no C38 . C39 . 1.372(4) yes C38 . H381 . 0.950 no C39 . C40 . 1.359(4) yes C39 . H391 . 0.950 no C40 . C41 . 1.386(3) yes C40 . H401 . 0.950 no C41 . H411 . 0.950 no C42 . C43 . 1.378(4) yes C42 . H421 . 0.950 no C43 . C44 . 1.329(6) yes C43 . H431 . 0.950 no C44 . C45 . 1.350(5) yes C44 . H441 . 0.950 no C45 . C46 . 1.386(4) yes C45 . H451 . 0.950 no C46 . H461 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ti1 . N2 . 113.38(8) yes N1 . Ti1 . N3 . 99.55(8) yes N2 . Ti1 . N3 . 147.02(8) yes N1 . Ti1 . N4 . 100.01(8) yes N2 . Ti1 . N4 . 87.35(8) yes N3 . Ti1 . N4 . 88.68(7) yes N1 . Ti1 . N5 . 104.34(8) yes N2 . Ti1 . N5 . 82.94(8) yes N3 . Ti1 . N5 . 87.45(7) yes N4 . Ti1 . N5 . 155.65(7) yes Ti1 . N1 . C1 . 175.88(16) yes Ti1 . N2 . C13 . 154.03(16) yes Ti1 . N2 . H1 . 97(2) no C13 . N2 . H1 . 109(2) no Ti1 . N3 . C25 . 144.18(15) yes Ti1 . N3 . H2 . 107(2) no C25 . N3 . H2 . 107(2) no Ti1 . N4 . C37 . 121.73(16) yes Ti1 . N4 . C41 . 121.04(15) yes C37 . N4 . C41 . 116.9(2) yes Ti1 . N5 . C42 . 120.69(18) yes Ti1 . N5 . C46 . 123.67(17) yes C42 . N5 . C46 . 115.4(2) yes N1 . C1 . C2 . 120.1(2) yes N1 . C1 . C6 . 119.7(2) yes C2 . C1 . C6 . 120.2(2) yes C1 . C2 . C3 . 118.7(2) yes C1 . C2 . C7 . 120.0(2) yes C3 . C2 . C7 . 121.2(2) yes C2 . C3 . C4 . 121.2(3) yes C2 . C3 . H31 . 119.2 no C4 . C3 . H31 . 119.6 no C3 . C4 . C5 . 120.1(3) yes C3 . C4 . H41 . 120.0 no C5 . C4 . H41 . 120.0 no C4 . C5 . C6 . 121.6(3) yes C4 . C5 . H51 . 119.4 no C6 . C5 . H51 . 119.0 no C1 . C6 . C5 . 118.2(3) yes C1 . C6 . C10 . 119.3(2) yes C5 . C6 . C10 . 122.5(3) yes C2 . C7 . C8 . 115.8(2) yes C2 . C7 . C9 . 109.1(2) yes C8 . C7 . C9 . 109.5(2) yes C2 . C7 . H71 . 107.4 no C8 . C7 . H71 . 107.5 no C9 . C7 . H71 . 107.1 no C7 . C8 . H81 . 109.7 no C7 . C8 . H82 . 109.4 no H81 . C8 . H82 . 109.5 no C7 . C8 . H83 . 109.2 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no C7 . C9 . H91 . 109.7 no C7 . C9 . H92 . 108.8 no H91 . C9 . H92 . 109.5 no C7 . C9 . H93 . 109.9 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C6 . C10 . C11 . 113.7(3) yes C6 . C10 . C12 . 111.4(3) yes C11 . C10 . C12 . 110.5(3) yes C6 . C10 . H101 . 106.9 no C11 . C10 . H101 . 107.4 no C12 . C10 . H101 . 106.6 no C10 . C11 . H111 . 109.2 no C10 . C11 . H112 . 109.9 no H111 . C11 . H112 . 109.5 no C10 . C11 . H113 . 109.2 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no C10 . C12 . H121 . 110.3 no C10 . C12 . H122 . 109.7 no H121 . C12 . H122 . 109.5 no C10 . C12 . H123 . 108.4 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no N2 . C13 . C14 . 121.17(19) yes N2 . C13 . C18 . 120.90(19) yes C14 . C13 . C18 . 117.93(19) yes C13 . C14 . C15 . 119.7(2) yes C13 . C14 . C19 . 122.15(19) yes C15 . C14 . C19 . 118.2(2) yes C14 . C15 . C16 . 122.0(2) yes C14 . C15 . H151 . 118.8 no C16 . C15 . H151 . 119.2 no C15 . C16 . C17 . 118.3(2) yes C15 . C16 . H161 . 121.0 no C17 . C16 . H161 . 120.7 no C16 . C17 . C18 . 122.7(2) yes C16 . C17 . H171 . 118.9 no C18 . C17 . H171 . 118.4 no C13 . C18 . C17 . 119.0(2) yes C13 . C18 . C22 . 121.30(19) yes C17 . C18 . C22 . 119.6(2) yes C14 . C19 . C20 . 113.1(2) yes C14 . C19 . C21 . 109.9(2) yes C20 . C19 . C21 . 111.2(2) yes C14 . C19 . H191 . 107.6 no C20 . C19 . H191 . 107.5 no C21 . C19 . H191 . 107.3 no C19 . C20 . H201 . 110.2 no C19 . C20 . H202 . 108.9 no H201 . C20 . H202 . 109.5 no C19 . C20 . H203 . 109.3 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C19 . C21 . H211 . 109.8 no C19 . C21 . H212 . 108.7 no H211 . C21 . H212 . 109.5 no C19 . C21 . H213 . 109.9 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C18 . C22 . C23 . 114.4(2) yes C18 . C22 . C24 . 109.7(2) yes C23 . C22 . C24 . 109.7(2) yes C18 . C22 . H221 . 107.6 no C23 . C22 . H221 . 107.7 no C24 . C22 . H221 . 107.5 no C22 . C23 . H231 . 109.4 no C22 . C23 . H232 . 109.5 no H231 . C23 . H232 . 109.5 no C22 . C23 . H233 . 109.5 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C22 . C24 . H241 . 109.6 no C22 . C24 . H242 . 109.3 no H241 . C24 . H242 . 109.5 no C22 . C24 . H243 . 109.5 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no N3 . C25 . C26 . 121.58(19) yes N3 . C25 . C30 . 120.22(19) yes C26 . C25 . C30 . 118.18(19) yes C25 . C26 . C27 . 119.3(2) yes C25 . C26 . C31 . 120.1(2) yes C27 . C26 . C31 . 120.6(2) yes C26 . C27 . C28 . 122.3(2) yes C26 . C27 . H271 . 118.8 no C28 . C27 . H271 . 118.9 no C27 . C28 . C29 . 118.5(2) yes C27 . C28 . H281 . 120.8 no C29 . C28 . H281 . 120.6 no C28 . C29 . C30 . 121.9(2) yes C28 . C29 . H291 . 119.2 no C30 . C29 . H291 . 118.8 no C25 . C30 . C29 . 119.8(2) yes C25 . C30 . C34 . 121.77(19) yes C29 . C30 . C34 . 118.4(2) yes C26 . C31 . C32 . 113.5(3) yes C26 . C31 . C33 . 112.3(3) yes C32 . C31 . C33 . 112.4(3) yes C26 . C31 . H311 . 107.0 no C32 . C31 . H311 . 107.0 no C33 . C31 . H311 . 104.0 no C31 . C32 . H321 . 109.5 no C31 . C32 . H322 . 109.0 no H321 . C32 . H322 . 109.5 no C31 . C32 . H323 . 109.8 no H321 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no C31 . C33 . H331 . 110.1 no C31 . C33 . H332 . 112.1 no H331 . C33 . H332 . 109.5 no C31 . C33 . H333 . 106.1 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.5 no C30 . C34 . C35 . 111.9(2) yes C30 . C34 . C36 . 112.0(2) yes C35 . C34 . C36 . 111.3(3) yes C30 . C34 . H341 . 107.4 no C35 . C34 . H341 . 107.1 no C36 . C34 . H341 . 106.8 no C34 . C35 . H351 . 110.4 no C34 . C35 . H352 . 108.9 no H351 . C35 . H352 . 109.5 no C34 . C35 . H353 . 109.1 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no C34 . C36 . H361 . 110.5 no C34 . C36 . H362 . 109.3 no H361 . C36 . H362 . 109.5 no C34 . C36 . H363 . 108.6 no H361 . C36 . H363 . 109.5 no H362 . C36 . H363 . 109.5 no N4 . C37 . C38 . 122.7(3) yes N4 . C37 . H371 . 118.3 no C38 . C37 . H371 . 119.0 no C37 . C38 . C39 . 119.7(3) yes C37 . C38 . H381 . 120.3 no C39 . C38 . H381 . 120.0 no C38 . C39 . C40 . 118.2(2) yes C38 . C39 . H391 . 120.7 no C40 . C39 . H391 . 121.1 no C39 . C40 . C41 . 119.5(2) yes C39 . C40 . H401 . 120.1 no C41 . C40 . H401 . 120.4 no C40 . C41 . N4 . 122.9(2) yes C40 . C41 . H411 . 118.8 no N4 . C41 . H411 . 118.2 no N5 . C42 . C43 . 123.4(3) yes N5 . C42 . H421 . 117.8 no C43 . C42 . H421 . 118.8 no C42 . C43 . C44 . 120.2(3) yes C42 . C43 . H431 . 120.0 no C44 . C43 . H431 . 119.7 no C43 . C44 . C45 . 117.9(3) yes C43 . C44 . H441 . 121.4 no C45 . C44 . H441 . 120.7 no C44 . C45 . C46 . 119.5(3) yes C44 . C45 . H451 . 120.4 no C46 . C45 . H451 . 120.0 no C45 . C46 . N5 . 123.5(3) yes C45 . C46 . H461 . 118.6 no N5 . C46 . H461 . 117.8 no # Attachment 'ADS168.cif' data_ADS168 _database_code_depnum_ccdc_archive 'CCDC 813858' #TrackingRef 'ADS168.cif' _chemical_name_systematic ; Ti(Me)(NAr)3{Li(py)}3 ; _chemical_melting_point ? _refine_special_details ; Hydrogen atoms were placed geometrically with reference to a Fourier difference map and refined in a riding model ; _cell_length_a 10.2991(7) _cell_length_b 19.4178(12) _cell_length_c 13.0747(9) _cell_angle_alpha 90 _cell_angle_beta 101.982(4) _cell_angle_gamma 90 _cell_volume 2557.8(3) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21 1 ' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,y+1/2,-z loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Li -0.0003 0.0001 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610 0.0377 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 2 _chemical_formula_sum 'C52 H69 Li3 N6 Ti1' _chemical_formula_moiety 'C52 H69 Li3 N6 Ti1' _chemical_compound_source ? _chemical_formula_weight 846.88 _cell_measurement_reflns_used 5019 _cell_measurement_theta_min 5 _cell_measurement_theta_max 26 _cell_measurement_temperature 150 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.050 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_max 0.100 _exptl_crystal_density_diffrn 1.100 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.205 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 0.99 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 27191 _reflns_number_total 9570 _diffrn_reflns_av_R_equivalents 0.065 _diffrn_reflns_theta_min 5.100 _diffrn_reflns_theta_max 26.017 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.496 _diffrn_measured_fraction_theta_full 0.988 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -23 _reflns_limit_k_max 23 _reflns_limit_l_min 0 _reflns_limit_l_max 16 _oxford_diffrn_Wilson_B_factor 2.88 _oxford_diffrn_Wilson_scale 4.52 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.31 _refine_diff_density_max 0.21 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 5577 _refine_ls_number_restraints 1 _refine_ls_number_parameters 560 _oxford_refine_ls_R_factor_ref 0.0555 _refine_ls_wR_factor_ref 0.0493 _refine_ls_goodness_of_fit_ref 1.1051 _refine_ls_shift/su_max 0.0004448 _refine_ls_shift/su_mean 0.0000162 # The values computed from all data _oxford_reflns_number_all 9570 _refine_ls_R_factor_all 0.1163 _refine_ls_wR_factor_all 0.0841 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6557 _refine_ls_R_factor_gt 0.0708 _refine_ls_wR_factor_gt 0.0535 _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_abs_structure_details 'Flack (1983), 2291 Friedel-pairs' _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 1.54 0.226E-01 1.24 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.15392(6) 0.60399(5) -0.32009(5) 0.0340 1.0000 Uani . . . . . . N1 N 0.2468(3) 0.52223(16) -0.2934(3) 0.0389 1.0000 Uani . . . . . . N2 N 0.2206(3) 0.66380(17) -0.2111(2) 0.0374 1.0000 Uani . . . . . . N3 N 0.1892(3) 0.64135(17) -0.4402(2) 0.0376 1.0000 Uani . . . . . . N4 N 0.3988(4) 0.5494(2) -0.0060(3) 0.0514 1.0000 Uani . . . . . . N5 N 0.1987(3) 0.82455(18) -0.3640(3) 0.0463 1.0000 Uani . . . . . . N6 N 0.2449(4) 0.4867(2) -0.5745(3) 0.0559 1.0000 Uani . . . . . . Li1 Li 0.3215(8) 0.5751(4) -0.1543(6) 0.0582 1.0000 Uani . . . . . . Li2 Li 0.2436(8) 0.7253(4) -0.3373(6) 0.0500 1.0000 Uani . . . . . . Li3 Li 0.2716(8) 0.5435(4) -0.4459(6) 0.0534 1.0000 Uani . . . . . . C1 C -0.0582(4) 0.5873(2) -0.3434(3) 0.0444 1.0000 Uani . . . . . . C2 C 0.2929(4) 0.4562(2) -0.2625(3) 0.0411 1.0000 Uani . . . . . . C3 C 0.2126(4) 0.4106(2) -0.2172(3) 0.0490 1.0000 Uani . . . . . . C4 C 0.2596(5) 0.3448(3) -0.1883(4) 0.0625 1.0000 Uani . . . . . . C5 C 0.3815(5) 0.3224(3) -0.2018(4) 0.0657 1.0000 Uani . . . . . . C6 C 0.4599(5) 0.3669(3) -0.2446(4) 0.0610 1.0000 Uani . . . . . . C7 C 0.4197(4) 0.4329(2) -0.2755(3) 0.0471 1.0000 Uani . . . . . . C8 C 0.0777(5) 0.4332(3) -0.2037(4) 0.0668 1.0000 Uani . . . . . . C9 C 0.0812(7) 0.4612(4) -0.0982(6) 0.1083 1.0000 Uani . . . . . . C10 C -0.0288(5) 0.3779(3) -0.2255(4) 0.0730 1.0000 Uani . . . . . . C11 C 0.5164(5) 0.4802(3) -0.3153(4) 0.0572 1.0000 Uani . . . . . . C12 C 0.5897(6) 0.4454(3) -0.3919(5) 0.0791 1.0000 Uani . . . . . . C13 C 0.6144(6) 0.5130(3) -0.2281(5) 0.0864 1.0000 Uani . . . . . . C14 C 0.2383(4) 0.7123(2) -0.1324(3) 0.0361 1.0000 Uani . . . . . . C15 C 0.3581(4) 0.7511(2) -0.1016(3) 0.0404 1.0000 Uani . . . . . . C16 C 0.3670(5) 0.8025(2) -0.0275(3) 0.0510 1.0000 Uani . . . . . . C17 C 0.2612(5) 0.8184(2) 0.0190(3) 0.0508 1.0000 Uani . . . . . . C18 C 0.1458(4) 0.7789(2) -0.0079(3) 0.0494 1.0000 Uani . . . . . . C19 C 0.1341(4) 0.7255(2) -0.0786(3) 0.0396 1.0000 Uani . . . . . . C20 C 0.4781(4) 0.7356(3) -0.1482(4) 0.0545 1.0000 Uani . . . . . . C21 C 0.5828(5) 0.6960(3) -0.0711(5) 0.0824 1.0000 Uani . . . . . . C22 C 0.5424(5) 0.7997(3) -0.1815(4) 0.0676 1.0000 Uani . . . . . . C23 C 0.0088(4) 0.6822(3) -0.1017(3) 0.0483 1.0000 Uani . . . . . . C24 C -0.0403(5) 0.6611(3) -0.0038(4) 0.0680 1.0000 Uani . . . . . . C25 C -0.0972(5) 0.7193(3) -0.1782(4) 0.0608 1.0000 Uani . . . . . . C26 C 0.2064(4) 0.6693(2) -0.5340(3) 0.0385 1.0000 Uani . . . . . . C27 C 0.3350(4) 0.6862(2) -0.5534(3) 0.0395 1.0000 Uani . . . . . . C28 C 0.3458(5) 0.7134(2) -0.6493(4) 0.0514 1.0000 Uani . . . . . . C29 C 0.2365(5) 0.7240(3) -0.7285(4) 0.0593 1.0000 Uani . . . . . . C30 C 0.1119(5) 0.7068(2) -0.7121(3) 0.0534 1.0000 Uani . . . . . . C31 C 0.0941(4) 0.6809(2) -0.6183(3) 0.0408 1.0000 Uani . . . . . . C32 C 0.4605(4) 0.6739(2) -0.4720(4) 0.0510 1.0000 Uani . . . . . . C33 C 0.5399(5) 0.7393(3) -0.4421(4) 0.0721 1.0000 Uani . . . . . . C34 C 0.5480(4) 0.6200(3) -0.5083(4) 0.0616 1.0000 Uani . . . . . . C35 C -0.0437(4) 0.6652(2) -0.6001(3) 0.0463 1.0000 Uani . . . . . . C36 C -0.1429(5) 0.6436(3) -0.6986(4) 0.0653 1.0000 Uani . . . . . . C37 C -0.0981(4) 0.7267(3) -0.5495(4) 0.0598 1.0000 Uani . . . . . . C38 C 0.3910(4) 0.5927(3) 0.0727(4) 0.0547 1.0000 Uani . . . . . . C39 C 0.4555(5) 0.5818(3) 0.1744(4) 0.0636 1.0000 Uani . . . . . . C40 C 0.5336(5) 0.5243(3) 0.1967(4) 0.0655 1.0000 Uani . . . . . . C41 C 0.5419(5) 0.4795(3) 0.1182(4) 0.0635 1.0000 Uani . . . . . . C42 C 0.4734(5) 0.4934(2) 0.0182(4) 0.0550 1.0000 Uani . . . . . . C43 C 0.1763(5) 0.8506(2) -0.4601(4) 0.0555 1.0000 Uani . . . . . . C44 C 0.1340(5) 0.9169(3) -0.4838(4) 0.0594 1.0000 Uani . . . . . . C45 C 0.1152(5) 0.9592(3) -0.4032(4) 0.0586 1.0000 Uani . . . . . . C46 C 0.1365(5) 0.9331(2) -0.3034(4) 0.0548 1.0000 Uani . . . . . . C47 C 0.1778(4) 0.8659(2) -0.2873(4) 0.0499 1.0000 Uani . . . . . . C48 C 0.2330(5) 0.4175(3) -0.5681(4) 0.0620 1.0000 Uani . . . . . . C49 C 0.2024(5) 0.3765(3) -0.6545(5) 0.0737 1.0000 Uani . . . . . . C50 C 0.1806(6) 0.4054(3) -0.7520(5) 0.0762 1.0000 Uani . . . . . . C51 C 0.1915(6) 0.4759(3) -0.7600(5) 0.0670 1.0000 Uani . . . . . . C52 C 0.2232(5) 0.5130(3) -0.6710(4) 0.0600 1.0000 Uani . . . . . . H41 H 0.2058 0.3144 -0.1583 0.0741 1.0000 Uiso R . . . . . H51 H 0.4113 0.2771 -0.1822 0.0797 1.0000 Uiso R . . . . . H61 H 0.5449 0.3517 -0.2528 0.0717 1.0000 Uiso R . . . . . H81 H 0.0501 0.4693 -0.2524 0.0818 1.0000 Uiso R . . . . . H91 H -0.0059 0.4747 -0.0928 0.1313 1.0000 Uiso R . . . . . H92 H 0.1382 0.5002 -0.0873 0.1313 1.0000 Uiso R . . . . . H93 H 0.1132 0.4273 -0.0467 0.1313 1.0000 Uiso R . . . . . H101 H -0.1105 0.3964 -0.2150 0.0876 1.0000 Uiso R . . . . . H102 H -0.0390 0.3626 -0.2957 0.0876 1.0000 Uiso R . . . . . H103 H -0.0037 0.3401 -0.1793 0.0876 1.0000 Uiso R . . . . . H111 H 0.4652 0.5164 -0.3525 0.0691 1.0000 Uiso R . . . . . H121 H 0.6479 0.4777 -0.4135 0.0953 1.0000 Uiso R . . . . . H122 H 0.5273 0.4295 -0.4513 0.0953 1.0000 Uiso R . . . . . H123 H 0.6395 0.4075 -0.3586 0.0953 1.0000 Uiso R . . . . . H131 H 0.6724 0.5420 -0.2565 0.1061 1.0000 Uiso R . . . . . H132 H 0.5683 0.5397 -0.1862 0.1061 1.0000 Uiso R . . . . . H133 H 0.6645 0.4783 -0.1864 0.1061 1.0000 Uiso R . . . . . H161 H 0.4474 0.8277 -0.0079 0.0621 1.0000 Uiso R . . . . . H171 H 0.2673 0.8549 0.0681 0.0612 1.0000 Uiso R . . . . . H181 H 0.0728 0.7893 0.0234 0.0596 1.0000 Uiso R . . . . . H201 H 0.4499 0.7077 -0.2084 0.0653 1.0000 Uiso R . . . . . H211 H 0.6567 0.6869 -0.1020 0.0996 1.0000 Uiso R . . . . . H212 H 0.6108 0.7227 -0.0095 0.0996 1.0000 Uiso R . . . . . H213 H 0.5462 0.6538 -0.0537 0.0996 1.0000 Uiso R . . . . . H221 H 0.6166 0.7869 -0.2099 0.0806 1.0000 Uiso R . . . . . H222 H 0.5710 0.8286 -0.1224 0.0806 1.0000 Uiso R . . . . . H223 H 0.4801 0.8239 -0.2328 0.0806 1.0000 Uiso R . . . . . H231 H 0.0292 0.6412 -0.1348 0.0580 1.0000 Uiso R . . . . . H241 H -0.1185 0.6342 -0.0233 0.0832 1.0000 Uiso R . . . . . H242 H -0.0593 0.7011 0.0323 0.0832 1.0000 Uiso R . . . . . H243 H 0.0264 0.6349 0.0405 0.0832 1.0000 Uiso R . . . . . H251 H -0.1755 0.6921 -0.1926 0.0729 1.0000 Uiso R . . . . . H252 H -0.1158 0.7622 -0.1493 0.0729 1.0000 Uiso R . . . . . H253 H -0.0672 0.7271 -0.2412 0.0729 1.0000 Uiso R . . . . . H281 H 0.4312 0.7247 -0.6609 0.0614 1.0000 Uiso R . . . . . H291 H 0.2465 0.7432 -0.7932 0.0707 1.0000 Uiso R . . . . . H301 H 0.0367 0.7128 -0.7673 0.0640 1.0000 Uiso R . . . . . H321 H 0.4351 0.6568 -0.4110 0.0620 1.0000 Uiso R . . . . . H331 H 0.6174 0.7289 -0.3910 0.0871 1.0000 Uiso R . . . . . H332 H 0.5647 0.7583 -0.5022 0.0871 1.0000 Uiso R . . . . . H333 H 0.4874 0.7717 -0.4142 0.0871 1.0000 Uiso R . . . . . H341 H 0.6257 0.6134 -0.4556 0.0745 1.0000 Uiso R . . . . . H342 H 0.5723 0.6351 -0.5709 0.0745 1.0000 Uiso R . . . . . H343 H 0.5008 0.5778 -0.5210 0.0745 1.0000 Uiso R . . . . . H351 H -0.0356 0.6280 -0.5520 0.0557 1.0000 Uiso R . . . . . H361 H -0.2266 0.6347 -0.6816 0.0780 1.0000 Uiso R . . . . . H362 H -0.1519 0.6796 -0.7488 0.0780 1.0000 Uiso R . . . . . H363 H -0.1119 0.6032 -0.7267 0.0780 1.0000 Uiso R . . . . . H371 H -0.1842 0.7160 -0.5387 0.0727 1.0000 Uiso R . . . . . H372 H -0.1029 0.7656 -0.5942 0.0727 1.0000 Uiso R . . . . . H373 H -0.0410 0.7367 -0.4843 0.0727 1.0000 Uiso R . . . . . H381 H 0.3377 0.6328 0.0572 0.0652 1.0000 Uiso R . . . . . H391 H 0.4464 0.6134 0.2280 0.0760 1.0000 Uiso R . . . . . H401 H 0.5816 0.5160 0.2658 0.0787 1.0000 Uiso R . . . . . H411 H 0.5940 0.4389 0.1325 0.0765 1.0000 Uiso R . . . . . H421 H 0.4800 0.4617 -0.0359 0.0655 1.0000 Uiso R . . . . . H431 H 0.1904 0.8217 -0.5154 0.0672 1.0000 Uiso R . . . . . H441 H 0.1179 0.9331 -0.5538 0.0714 1.0000 Uiso R . . . . . H451 H 0.0884 1.0058 -0.4164 0.0703 1.0000 Uiso R . . . . . H461 H 0.1227 0.9609 -0.2468 0.0653 1.0000 Uiso R . . . . . H471 H 0.1916 0.8480 -0.2183 0.0590 1.0000 Uiso R . . . . . H481 H 0.2476 0.3967 -0.5009 0.0752 1.0000 Uiso R . . . . . H491 H 0.1950 0.3281 -0.6468 0.0892 1.0000 Uiso R . . . . . H501 H 0.1586 0.3775 -0.8128 0.0915 1.0000 Uiso R . . . . . H511 H 0.1776 0.4978 -0.8264 0.0810 1.0000 Uiso R . . . . . H521 H 0.2306 0.5615 -0.6774 0.0725 1.0000 Uiso R . . . . . H11 H -0.0788 0.5679 -0.2819 0.0552 1.0000 Uiso R . . . . . H12 H -0.1034 0.6299 -0.3584 0.0552 1.0000 Uiso R . . . . . H13 H -0.0855 0.5566 -0.4004 0.0552 1.0000 Uiso 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 0.0285(3) 0.0360(4) 0.0385(4) 0.0002(4) 0.0096(3) -0.0002(4) N1 0.0353(19) 0.0318(19) 0.051(2) 0.0025(16) 0.0108(16) 0.0030(15) N2 0.0341(19) 0.0408(19) 0.0380(19) -0.0085(16) 0.0092(15) 0.0004(15) N3 0.0305(17) 0.0464(19) 0.0367(19) 0.0040(15) 0.0088(15) -0.0001(15) N4 0.054(2) 0.051(2) 0.048(2) 0.0012(19) 0.0067(19) 0.0004(19) N5 0.046(2) 0.046(2) 0.046(2) 0.0022(19) 0.0075(17) -0.0059(17) N6 0.048(2) 0.057(3) 0.065(3) -0.007(2) 0.017(2) 0.0081(19) Li1 0.063(5) 0.052(4) 0.056(5) 0.000(3) 0.002(4) 0.008(4) Li2 0.061(5) 0.037(4) 0.057(5) 0.002(3) 0.024(4) -0.001(3) Li3 0.060(5) 0.054(5) 0.051(4) 0.004(4) 0.023(4) 0.014(4) C1 0.033(2) 0.051(3) 0.050(2) -0.001(2) 0.0098(18) -0.0029(18) C2 0.043(3) 0.042(3) 0.037(2) -0.0048(19) 0.0047(19) -0.001(2) C3 0.051(3) 0.048(3) 0.049(3) -0.003(2) 0.012(2) -0.008(2) C4 0.071(4) 0.046(3) 0.067(3) 0.007(2) 0.005(3) -0.013(3) C5 0.070(4) 0.045(3) 0.075(3) 0.009(3) 0.000(3) 0.008(3) C6 0.059(3) 0.057(3) 0.062(3) 0.004(3) 0.002(3) 0.016(3) C7 0.048(3) 0.045(3) 0.047(3) 0.001(2) 0.008(2) 0.008(2) C8 0.071(4) 0.052(3) 0.084(4) 0.012(3) 0.030(3) -0.006(3) C9 0.072(4) 0.112(6) 0.145(7) -0.054(5) 0.033(4) -0.027(4) C10 0.065(3) 0.086(4) 0.067(3) 0.008(3) 0.012(3) -0.015(3) C11 0.040(3) 0.062(3) 0.073(3) 0.011(3) 0.018(3) 0.016(2) C12 0.064(4) 0.100(4) 0.079(4) 0.009(3) 0.029(3) 0.024(3) C13 0.067(4) 0.088(4) 0.108(5) -0.005(4) 0.028(3) -0.017(3) C14 0.031(2) 0.039(2) 0.039(2) 0.0106(19) 0.0078(18) 0.0067(18) C15 0.032(2) 0.045(3) 0.043(2) 0.001(2) 0.0033(19) -0.0044(19) C16 0.054(3) 0.055(3) 0.042(3) -0.007(2) 0.004(2) -0.015(2) C17 0.061(3) 0.053(3) 0.041(2) -0.013(2) 0.014(2) -0.002(2) C18 0.045(3) 0.058(3) 0.048(3) -0.001(2) 0.017(2) 0.006(2) C19 0.042(2) 0.044(3) 0.035(2) 0.0052(19) 0.0119(19) 0.005(2) C20 0.036(2) 0.066(3) 0.063(3) -0.014(2) 0.012(2) -0.012(2) C21 0.047(3) 0.083(4) 0.124(5) 0.032(4) 0.032(3) 0.013(3) C22 0.053(3) 0.086(4) 0.067(3) 0.007(3) 0.021(3) -0.003(3) C23 0.030(2) 0.071(3) 0.047(3) -0.003(2) 0.015(2) 0.000(2) C24 0.053(3) 0.094(4) 0.061(3) 0.004(3) 0.022(3) -0.013(3) C25 0.045(3) 0.079(4) 0.058(3) 0.000(3) 0.012(2) 0.007(2) C26 0.045(2) 0.030(2) 0.042(2) -0.0044(19) 0.013(2) 0.0007(18) C27 0.037(2) 0.040(2) 0.044(2) -0.0044(19) 0.0136(19) -0.0031(19) C28 0.054(3) 0.049(3) 0.056(3) 0.003(2) 0.025(3) 0.000(2) C29 0.067(3) 0.065(3) 0.051(3) 0.012(3) 0.022(3) 0.012(3) C30 0.056(3) 0.063(3) 0.040(3) 0.009(2) 0.006(2) 0.014(2) C31 0.045(2) 0.038(2) 0.037(2) -0.0006(19) 0.0021(19) -0.0002(19) C32 0.035(2) 0.067(3) 0.054(3) 0.001(2) 0.016(2) -0.009(2) C33 0.054(3) 0.086(4) 0.078(4) -0.020(3) 0.019(3) -0.013(3) C34 0.040(2) 0.079(4) 0.067(3) 0.008(3) 0.012(2) 0.003(2) C35 0.038(2) 0.054(3) 0.043(3) 0.004(2) 0.001(2) 0.000(2) C36 0.060(3) 0.068(3) 0.060(3) 0.005(2) -0.005(2) -0.008(3) C37 0.036(2) 0.065(3) 0.079(4) 0.004(3) 0.013(2) 0.004(2) C38 0.051(3) 0.060(3) 0.053(3) 0.010(3) 0.010(2) 0.009(2) C39 0.071(3) 0.071(4) 0.048(3) 0.002(2) 0.011(2) 0.011(3) C40 0.064(3) 0.083(4) 0.046(3) 0.012(3) 0.003(2) -0.001(3) C41 0.066(3) 0.058(3) 0.061(3) 0.007(3) 0.002(3) 0.009(2) C42 0.065(3) 0.046(3) 0.051(3) 0.002(2) 0.005(3) 0.005(2) C43 0.068(3) 0.038(3) 0.063(3) 0.003(2) 0.020(3) -0.004(2) C44 0.072(3) 0.055(3) 0.054(3) 0.009(2) 0.018(2) -0.002(2) C45 0.061(3) 0.042(3) 0.074(4) 0.009(3) 0.018(3) 0.002(2) C46 0.058(3) 0.043(3) 0.062(3) -0.005(2) 0.011(2) -0.003(2) C47 0.049(3) 0.050(3) 0.047(3) 0.001(2) 0.002(2) 0.000(2) C48 0.051(3) 0.061(4) 0.073(4) -0.007(3) 0.010(3) 0.009(2) C49 0.074(4) 0.053(3) 0.089(4) -0.012(3) 0.003(3) 0.013(3) C50 0.074(4) 0.080(4) 0.072(4) -0.031(3) 0.008(3) 0.010(3) C51 0.076(4) 0.064(4) 0.064(4) -0.011(3) 0.020(3) 0.003(3) C52 0.072(3) 0.050(3) 0.063(3) -0.011(3) 0.026(3) 0.001(3) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.5016(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . N1 . 1.849(3) yes Ti1 . N2 . 1.856(3) yes Ti1 . N3 . 1.834(3) yes Ti1 . C1 . 2.167(4) yes N1 . C2 . 1.398(5) yes N1 . Li3 . 2.103(8) yes N1 . Li1 . 2.092(9) yes N2 . C14 . 1.378(5) yes N2 . Li2 . 2.090(8) yes N2 . Li1 . 2.068(8) yes N3 . C26 . 1.385(5) yes N3 . Li2 . 2.113(8) yes N3 . Li3 . 2.088(8) yes N4 . C38 . 1.344(6) yes N4 . C42 . 1.332(6) yes N4 . Li1 . 2.000(9) yes N5 . C43 . 1.329(6) yes N5 . C47 . 1.337(5) yes N5 . Li2 . 1.996(8) yes N6 . C48 . 1.354(6) yes N6 . C52 . 1.336(6) yes N6 . Li3 . 1.982(9) yes C1 . H11 . 0.950 no C1 . H12 . 0.950 no C1 . H13 . 0.950 no C2 . C3 . 1.422(6) yes C2 . C7 . 1.425(6) yes C3 . C4 . 1.391(7) yes C3 . C8 . 1.501(7) yes C4 . C5 . 1.374(7) yes C4 . H41 . 0.950 no C5 . C6 . 1.378(7) yes C5 . H51 . 0.950 no C6 . C7 . 1.382(6) yes C6 . H61 . 0.950 no C7 . C11 . 1.523(6) yes C8 . C9 . 1.478(8) yes C8 . C10 . 1.519(7) yes C8 . H81 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . H101 . 0.950 no C10 . H102 . 0.950 no C10 . H103 . 0.950 no C11 . C12 . 1.531(7) yes C11 . C13 . 1.499(7) yes C11 . H111 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . H131 . 0.950 no C13 . H132 . 0.950 no C13 . H133 . 0.950 no C14 . C15 . 1.431(5) yes C14 . C19 . 1.424(5) yes C15 . C16 . 1.380(6) yes C15 . C20 . 1.517(6) yes C16 . C17 . 1.388(6) yes C16 . H161 . 0.950 no C17 . C18 . 1.397(6) yes C17 . H171 . 0.950 no C18 . C19 . 1.377(6) yes C18 . H181 . 0.950 no C19 . C23 . 1.517(6) yes C20 . C21 . 1.523(7) yes C20 . C22 . 1.515(7) yes C20 . H201 . 0.950 no C21 . H211 . 0.950 no C21 . H212 . 0.950 no C21 . H213 . 0.950 no C22 . H221 . 0.950 no C22 . H222 . 0.950 no C22 . H223 . 0.950 no C23 . C24 . 1.527(6) yes C23 . C25 . 1.503(6) yes C23 . H231 . 0.950 no C24 . H241 . 0.950 no C24 . H242 . 0.950 no C24 . H243 . 0.950 no C25 . H251 . 0.950 no C25 . H252 . 0.950 no C25 . H253 . 0.950 no C26 . C27 . 1.437(6) yes C26 . C31 . 1.440(6) yes C27 . C28 . 1.386(6) yes C27 . C32 . 1.513(6) yes C28 . C29 . 1.378(7) yes C28 . H281 . 0.950 no C29 . C30 . 1.385(7) yes C29 . H291 . 0.950 no C30 . C31 . 1.372(6) yes C30 . H301 . 0.950 no C31 . C35 . 1.518(6) yes C32 . C33 . 1.517(7) yes C32 . C34 . 1.521(6) yes C32 . H321 . 0.950 no C33 . H331 . 0.950 no C33 . H332 . 0.950 no C33 . H333 . 0.950 no C34 . H341 . 0.950 no C34 . H342 . 0.950 no C34 . H343 . 0.950 no C35 . C36 . 1.528(6) yes C35 . C37 . 1.525(6) yes C35 . H351 . 0.950 no C36 . H361 . 0.950 no C36 . H362 . 0.950 no C36 . H363 . 0.950 no C37 . H371 . 0.950 no C37 . H372 . 0.950 no C37 . H373 . 0.950 no C38 . C39 . 1.374(6) yes C38 . H381 . 0.950 no C39 . C40 . 1.372(7) yes C39 . H391 . 0.950 no C40 . C41 . 1.362(7) yes C40 . H401 . 0.950 no C41 . C42 . 1.376(7) yes C41 . H411 . 0.950 no C42 . H421 . 0.950 no C43 . C44 . 1.374(6) yes C43 . H431 . 0.950 no C44 . C45 . 1.382(7) yes C44 . H441 . 0.950 no C45 . C46 . 1.374(7) yes C45 . H451 . 0.950 no C46 . C47 . 1.374(6) yes C46 . H461 . 0.950 no C47 . H471 . 0.950 no C48 . C49 . 1.365(7) yes C48 . H481 . 0.950 no C49 . C50 . 1.369(8) yes C49 . H491 . 0.950 no C50 . C51 . 1.378(8) yes C50 . H501 . 0.950 no C51 . C52 . 1.350(7) yes C51 . H511 . 0.950 no C52 . H521 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ti1 . N2 . 107.34(15) yes N1 . Ti1 . N3 . 108.35(15) yes N2 . Ti1 . N3 . 107.63(15) yes N1 . Ti1 . C1 . 111.39(15) yes N2 . Ti1 . C1 . 113.78(15) yes N3 . Ti1 . C1 . 108.17(15) yes Ti1 . N1 . C2 . 166.9(3) yes Ti1 . N1 . Li3 . 79.2(2) yes C2 . N1 . Li3 . 110.7(3) yes Ti1 . N1 . Li1 . 79.9(2) yes C2 . N1 . Li1 . 99.1(3) yes Li3 . N1 . Li1 . 129.2(4) yes Ti1 . N2 . C14 . 166.2(3) yes Ti1 . N2 . Li2 . 80.5(2) yes C14 . N2 . Li2 . 100.4(3) yes Ti1 . N2 . Li1 . 80.4(3) yes C14 . N2 . Li1 . 108.7(3) yes Li2 . N2 . Li1 . 128.9(3) yes Ti1 . N3 . C26 . 176.0(3) yes Ti1 . N3 . Li2 . 80.4(2) yes C26 . N3 . Li2 . 101.3(3) yes Ti1 . N3 . Li3 . 79.9(2) yes C26 . N3 . Li3 . 101.4(3) yes Li2 . N3 . Li3 . 131.9(3) yes C38 . N4 . C42 . 116.9(4) yes C38 . N4 . Li1 . 120.7(4) yes C42 . N4 . Li1 . 121.9(4) yes C43 . N5 . C47 . 117.2(4) yes C43 . N5 . Li2 . 121.4(4) yes C47 . N5 . Li2 . 121.1(4) yes C48 . N6 . C52 . 116.0(4) yes C48 . N6 . Li3 . 119.9(4) yes C52 . N6 . Li3 . 123.8(4) yes N4 . Li1 . N1 . 136.1(4) yes N4 . Li1 . N2 . 128.7(4) yes N1 . Li1 . N2 . 91.7(3) yes N5 . Li2 . N2 . 129.0(4) yes N5 . Li2 . N3 . 127.8(4) yes N2 . Li2 . N3 . 90.2(3) yes N6 . Li3 . N3 . 123.4(4) yes N6 . Li3 . N1 . 132.2(4) yes N3 . Li3 . N1 . 90.9(3) yes Ti1 . C1 . H11 . 109.6 no Ti1 . C1 . H12 . 109.5 no H11 . C1 . H12 . 109.5 no Ti1 . C1 . H13 . 109.3 no H11 . C1 . H13 . 109.5 no H12 . C1 . H13 . 109.5 no N1 . C2 . C3 . 119.9(4) yes N1 . C2 . C7 . 121.4(4) yes C3 . C2 . C7 . 118.7(4) yes C2 . C3 . C4 . 119.0(4) yes C2 . C3 . C8 . 120.0(4) yes C4 . C3 . C8 . 121.0(4) yes C3 . C4 . C5 . 122.1(5) yes C3 . C4 . H41 . 118.9 no C5 . C4 . H41 . 118.9 no C4 . C5 . C6 . 118.8(5) yes C4 . C5 . H51 . 120.7 no C6 . C5 . H51 . 120.5 no C5 . C6 . C7 . 122.3(5) yes C5 . C6 . H61 . 118.8 no C7 . C6 . H61 . 118.9 no C2 . C7 . C6 . 119.0(4) yes C2 . C7 . C11 . 122.0(4) yes C6 . C7 . C11 . 118.8(4) yes C3 . C8 . C9 . 111.9(5) yes C3 . C8 . C10 . 114.9(4) yes C9 . C8 . C10 . 108.2(4) yes C3 . C8 . H81 . 107.0 no C9 . C8 . H81 . 107.4 no C10 . C8 . H81 . 107.0 no C8 . C9 . H91 . 109.2 no C8 . C9 . H92 . 109.1 no H91 . C9 . H92 . 109.5 no C8 . C9 . H93 . 110.0 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C8 . C10 . H101 . 109.4 no C8 . C10 . H102 . 109.4 no H101 . C10 . H102 . 109.5 no C8 . C10 . H103 . 109.6 no H101 . C10 . H103 . 109.5 no H102 . C10 . H103 . 109.5 no C7 . C11 . C12 . 113.8(4) yes C7 . C11 . C13 . 112.4(4) yes C12 . C11 . C13 . 109.9(4) yes C7 . C11 . H111 . 106.7 no C12 . C11 . H111 . 106.8 no C13 . C11 . H111 . 106.8 no C11 . C12 . H121 . 109.3 no C11 . C12 . H122 . 109.6 no H121 . C12 . H122 . 109.5 no C11 . C12 . H123 . 109.5 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no C11 . C13 . H131 . 109.5 no C11 . C13 . H132 . 109.5 no H131 . C13 . H132 . 109.5 no C11 . C13 . H133 . 109.5 no H131 . C13 . H133 . 109.5 no H132 . C13 . H133 . 109.5 no N2 . C14 . C15 . 122.8(3) yes N2 . C14 . C19 . 119.7(3) yes C15 . C14 . C19 . 117.4(4) yes C14 . C15 . C16 . 120.4(4) yes C14 . C15 . C20 . 120.6(4) yes C16 . C15 . C20 . 119.0(4) yes C15 . C16 . C17 . 121.6(4) yes C15 . C16 . H161 . 119.2 no C17 . C16 . H161 . 119.1 no C16 . C17 . C18 . 118.1(4) yes C16 . C17 . H171 . 121.0 no C18 . C17 . H171 . 120.9 no C17 . C18 . C19 . 122.3(4) yes C17 . C18 . H181 . 118.9 no C19 . C18 . H181 . 118.8 no C14 . C19 . C18 . 119.8(4) yes C14 . C19 . C23 . 119.9(4) yes C18 . C19 . C23 . 120.2(4) yes C15 . C20 . C21 . 110.9(4) yes C15 . C20 . C22 . 113.2(4) yes C21 . C20 . C22 . 108.3(4) yes C15 . C20 . H201 . 108.1 no C21 . C20 . H201 . 108.2 no C22 . C20 . H201 . 108.0 no C20 . C21 . H211 . 109.4 no C20 . C21 . H212 . 109.6 no H211 . C21 . H212 . 109.5 no C20 . C21 . H213 . 109.5 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C20 . C22 . H221 . 109.4 no C20 . C22 . H222 . 109.3 no H221 . C22 . H222 . 109.5 no C20 . C22 . H223 . 109.7 no H221 . C22 . H223 . 109.5 no H222 . C22 . H223 . 109.5 no C19 . C23 . C24 . 113.4(4) yes C19 . C23 . C25 . 109.7(4) yes C24 . C23 . C25 . 111.5(4) yes C19 . C23 . H231 . 107.2 no C24 . C23 . H231 . 107.5 no C25 . C23 . H231 . 107.3 no C23 . C24 . H241 . 109.4 no C23 . C24 . H242 . 109.7 no H241 . C24 . H242 . 109.5 no C23 . C24 . H243 . 109.4 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no C23 . C25 . H251 . 109.5 no C23 . C25 . H252 . 109.5 no H251 . C25 . H252 . 109.5 no C23 . C25 . H253 . 109.4 no H251 . C25 . H253 . 109.5 no H252 . C25 . H253 . 109.5 no N3 . C26 . C27 . 122.5(4) yes N3 . C26 . C31 . 120.6(3) yes C27 . C26 . C31 . 116.9(4) yes C26 . C27 . C28 . 119.8(4) yes C26 . C27 . C32 . 121.6(4) yes C28 . C27 . C32 . 118.6(4) yes C27 . C28 . C29 . 122.0(4) yes C27 . C28 . H281 . 119.0 no C29 . C28 . H281 . 119.0 no C28 . C29 . C30 . 119.1(4) yes C28 . C29 . H291 . 120.4 no C30 . C29 . H291 . 120.5 no C29 . C30 . C31 . 121.8(4) yes C29 . C30 . H301 . 119.2 no C31 . C30 . H301 . 119.1 no C26 . C31 . C30 . 120.4(4) yes C26 . C31 . C35 . 118.5(3) yes C30 . C31 . C35 . 121.1(4) yes C27 . C32 . C33 . 112.7(4) yes C27 . C32 . C34 . 111.4(4) yes C33 . C32 . C34 . 109.5(4) yes C27 . C32 . H321 . 107.6 no C33 . C32 . H321 . 107.7 no C34 . C32 . H321 . 107.8 no C32 . C33 . H331 . 109.4 no C32 . C33 . H332 . 109.5 no H331 . C33 . H332 . 109.5 no C32 . C33 . H333 . 109.5 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.5 no C32 . C34 . H341 . 109.3 no C32 . C34 . H342 . 109.6 no H341 . C34 . H342 . 109.5 no C32 . C34 . H343 . 109.5 no H341 . C34 . H343 . 109.5 no H342 . C34 . H343 . 109.5 no C31 . C35 . C36 . 114.0(4) yes C31 . C35 . C37 . 110.5(4) yes C36 . C35 . C37 . 109.8(4) yes C31 . C35 . H351 . 107.4 no C36 . C35 . H351 . 107.4 no C37 . C35 . H351 . 107.4 no C35 . C36 . H361 . 109.5 no C35 . C36 . H362 . 109.4 no H361 . C36 . H362 . 109.5 no C35 . C36 . H363 . 109.5 no H361 . C36 . H363 . 109.5 no H362 . C36 . H363 . 109.5 no C35 . C37 . H371 . 109.5 no C35 . C37 . H372 . 109.4 no H371 . C37 . H372 . 109.5 no C35 . C37 . H373 . 109.5 no H371 . C37 . H373 . 109.5 no H372 . C37 . H373 . 109.5 no N4 . C38 . C39 . 123.4(4) yes N4 . C38 . H381 . 118.3 no C39 . C38 . H381 . 118.3 no C38 . C39 . C40 . 118.4(5) yes C38 . C39 . H391 . 120.8 no C40 . C39 . H391 . 120.8 no C39 . C40 . C41 . 119.1(5) yes C39 . C40 . H401 . 120.5 no C41 . C40 . H401 . 120.5 no C40 . C41 . C42 . 119.4(5) yes C40 . C41 . H411 . 120.2 no C42 . C41 . H411 . 120.4 no C41 . C42 . N4 . 122.8(5) yes C41 . C42 . H421 . 118.6 no N4 . C42 . H421 . 118.6 no N5 . C43 . C44 . 123.7(4) yes N5 . C43 . H431 . 118.1 no C44 . C43 . H431 . 118.2 no C43 . C44 . C45 . 118.3(4) yes C43 . C44 . H441 . 120.8 no C45 . C44 . H441 . 120.9 no C44 . C45 . C46 . 118.9(4) yes C44 . C45 . H451 . 120.6 no C46 . C45 . H451 . 120.5 no C45 . C46 . C47 . 118.7(4) yes C45 . C46 . H461 . 120.6 no C47 . C46 . H461 . 120.7 no C46 . C47 . N5 . 123.2(4) yes C46 . C47 . H471 . 118.4 no N5 . C47 . H471 . 118.4 no N6 . C48 . C49 . 122.5(5) yes N6 . C48 . H481 . 118.7 no C49 . C48 . H481 . 118.8 no C48 . C49 . C50 . 119.7(5) yes C48 . C49 . H491 . 120.0 no C50 . C49 . H491 . 120.2 no C49 . C50 . C51 . 118.6(5) yes C49 . C50 . H501 . 120.6 no C51 . C50 . H501 . 120.8 no C50 . C51 . C52 . 118.2(5) yes C50 . C51 . H511 . 121.0 no C52 . C51 . H511 . 120.8 no C51 . C52 . N6 . 125.0(5) yes C51 . C52 . H521 . 117.6 no N6 . C52 . H521 . 117.4 no # Attachment 'ADS173.cif' data_ads173 _database_code_depnum_ccdc_archive 'CCDC 813859' #TrackingRef 'ADS173.cif' _chemical_name_systematic ; Ti(NAr)2(NHAr)2{Li(py)}2 ; _chemical_melting_point ? _refine_special_details ; C-bound H atoms were placed geometrically and refined in a riding model. N-bound H atoms were found in a difference map and isotropically refined to a common temperature factor. One pyridine and the diethyl ether groups were positionally disordered over two sites and were refined subject to similarity restraints applied to the ADPs, bond length restraints, bond angle restraints and for pyridine planar restraints. The Flack parameter of 0.52(4)is indicative of the crystal being an intimate twin of both the enantiomers. Attempts to solve and/or refine the structure in a centrosymmetric version of Pna21 (Pbca) were unsuccessful. Molecules of ADS173 contain either two pyridines or one pyridine and one ether attached to lithium in a disordered model. ; _cell_length_a 18.4575(2) _cell_length_b 16.9731(2) _cell_length_c 17.7260(2) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 5553.22(11) _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P n a 21 ' _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz x,y,z -x+1/2,y+1/2,z+1/2 x+1/2,-y+1/2,z -x,-y,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Li -0.0003 0.0001 1.1282 3.9546 0.7508 1.0524 0.6175 85.3905 0.4653 168.2610 0.0377 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 _chemical_formula_sum 'C57.50 H82.50 Li2 N5.50 O0.50 Ti1' _chemical_formula_moiety 'C57.50 H82.50 Li2 N5.50 O0.50 Ti1' _chemical_compound_source ? _chemical_formula_weight 920.61 _cell_measurement_reflns_used 6920 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_measurement_temperature 150 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_min 0.200 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_max 0.200 _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 0.195 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _exptl_absorpt_correction_T_min 0.96 _exptl_absorpt_correction_T_max 0.96 _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_device Area _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_measurement_method \w _computing_data_collection 'COLLECT (Nonius, 2001).' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR92 (Altomare et al., 1994)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time . _diffrn_standards_interval_count . _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 150 _diffrn_reflns_number 12231 _reflns_number_total 12231 _diffrn_reflns_av_R_equivalents 0.075 _diffrn_reflns_theta_min 5.104 _diffrn_reflns_theta_max 27.494 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.944 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _reflns_limit_h_min 0 _reflns_limit_h_max 23 _reflns_limit_k_min 0 _reflns_limit_k_max 22 _reflns_limit_l_min -22 _reflns_limit_l_max 23 _oxford_diffrn_Wilson_B_factor 2.16 _oxford_diffrn_Wilson_scale 77.30 _atom_sites_solution_primary Direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.28 _refine_diff_density_max 0.28 # The current dictionary definitions do not cover the # situation where the reflections used for refinement were # selected by a user-defined sigma threshold # The values actually used during refinement _oxford_reflns_threshold_expression_ref I>3.0\s(I) _refine_ls_number_reflns 5838 _refine_ls_number_restraints 90 _refine_ls_number_parameters 657 _oxford_refine_ls_R_factor_ref 0.0523 _refine_ls_wR_factor_ref 0.0557 _refine_ls_goodness_of_fit_ref 1.1681 _refine_ls_shift/su_max 0.0006511 _refine_ls_shift/su_mean 0.0000201 # The values computed from all data _oxford_reflns_number_all 12231 _refine_ls_R_factor_all 0.1352 _refine_ls_wR_factor_all 0.1332 # The values computed with a 2 sigma cutoff - a la SHELX _reflns_threshold_expression I>2.0\s(I) _reflns_number_gt 6825 _refine_ls_R_factor_gt 0.0650 _refine_ls_wR_factor_gt 0.0624 _refine_ls_abs_structure_Flack 0.52(4) _refine_ls_abs_structure_details 'Flack (1983), 5724 Friedel-pairs' _chemical_absolute_configuration ad _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 0.353 0.229 0.155 ; _publ_section_references ; Altomare, A., Cascarano, G., Giacovazzo, C., Guagliardi, A., Burla, M.C., Polidori, G. & Camalli, M. (1994). J. Appl. Cryst. 27, 435. Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K. & Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Flack, H. D. (1983). Acta Cryst. A39, 876-881. Nonius (2001). COLLECT. Nonius BV, Delft, The Netherlands. Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994). Acta Cryst, A50, 411-437. Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996). CAMERON, Chemical Crystallography Laboratory, Oxford, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.24565(4) -0.06069(3) 0.73939(10) 0.0249 1.0000 Uani D . . . . . Li1 Li 0.2547(5) 0.0921(3) 0.7430(9) 0.0463 1.0000 Uani . . . . . . Li2 Li 0.2374(5) -0.2247(4) 0.7353(8) 0.0465 1.0000 Uani . . . . . . N1 N 0.32499(18) -0.0018(2) 0.7248(3) 0.0323 1.0000 Uani . . . . . . N2 N 0.17411(18) 0.0064(2) 0.7576(2) 0.0284 1.0000 Uani . . . . . . N3 N 0.2550(2) -0.1476(2) 0.8210(3) 0.0320 1.0000 Uani D . . . . . N4 N 0.2239(2) -0.1404(2) 0.6535(2) 0.0318 1.0000 Uani D . . . . . N5 N 0.2573(2) 0.21124(17) 0.7412(4) 0.0355 1.0000 Uani . . . . . . N6 N 0.2150(5) -0.3339(5) 0.7204(6) 0.0564 0.5000 Uani D U . 1 1 . O1 O 0.2386(7) -0.3417(5) 0.7334(7) 0.0758 0.5000 Uani D U . 1 2 . C1 C 0.3797(2) 0.0496(3) 0.7059(3) 0.0282 1.0000 Uani . . . . . . C2 C 0.4319(2) 0.0750(3) 0.7614(3) 0.0374 1.0000 Uani . . . . . . C3 C 0.4856(2) 0.1282(3) 0.7406(4) 0.0439 1.0000 Uani . . . . . . C4 C 0.4919(3) 0.1551(3) 0.6682(4) 0.0470 1.0000 Uani . . . . . . C5 C 0.4444(3) 0.1294(3) 0.6123(4) 0.0459 1.0000 Uani . . . . . . C6 C 0.3883(3) 0.0757(3) 0.6301(3) 0.0356 1.0000 Uani . . . . . . C7 C 0.4278(3) 0.0430(3) 0.8406(3) 0.0388 1.0000 Uani . . . . . . C8 C 0.4769(4) -0.0305(4) 0.8465(4) 0.0733 1.0000 Uani . . . . . . C9 C 0.4472(4) 0.1023(4) 0.9023(4) 0.0722 1.0000 Uani . . . . . . C10 C 0.3372(3) 0.0459(4) 0.5695(3) 0.0444 1.0000 Uani . . . . . . C11 C 0.2703(3) 0.0958(5) 0.5626(4) 0.0584 1.0000 Uani . . . . . . C12 C 0.3738(4) 0.0376(5) 0.4929(4) 0.0671 1.0000 Uani . . . . . . C13 C 0.1218(2) 0.0614(3) 0.7809(3) 0.0342 1.0000 Uani . . . . . . C14 C 0.1196(3) 0.0876(3) 0.8565(3) 0.0345 1.0000 Uani . . . . . . C15 C 0.0700(3) 0.1438(3) 0.8757(4) 0.0421 1.0000 Uani . . . . . . C16 C 0.0221(3) 0.1763(3) 0.8249(4) 0.0440 1.0000 Uani . . . . . . C17 C 0.0232(2) 0.1495(3) 0.7508(3) 0.0390 1.0000 Uani . . . . . . C18 C 0.0722(2) 0.0926(3) 0.7270(3) 0.0330 1.0000 Uani . . . . . . C19 C 0.1707(3) 0.0530(3) 0.9139(3) 0.0391 1.0000 Uani . . . . . . C20 C 0.1357(4) 0.0349(4) 0.9899(4) 0.0592 1.0000 Uani . . . . . . C21 C 0.2376(3) 0.1051(5) 0.9275(4) 0.0666 1.0000 Uani . . . . . . C22 C 0.0690(3) 0.0617(3) 0.6487(3) 0.0426 1.0000 Uani . . . . . . C23 C 0.0644(5) 0.1277(5) 0.5888(5) 0.0873 1.0000 Uani . . . . . . C24 C 0.0092(4) 0.0017(5) 0.6379(4) 0.0838 1.0000 Uani . . . . . . C25 C 0.2208(3) -0.1597(3) 0.8914(3) 0.0367 1.0000 Uani . . . . . . C26 C 0.1452(3) -0.1755(3) 0.8944(3) 0.0429 1.0000 Uani . . . . . . C27 C 0.1124(3) -0.1914(4) 0.9621(4) 0.0533 1.0000 Uani . . . . . . C28 C 0.1507(3) -0.1930(4) 1.0287(4) 0.0621 1.0000 Uani . . . . . . C29 C 0.2238(4) -0.1743(4) 1.0273(3) 0.0544 1.0000 Uani . . . . . . C30 C 0.2591(3) -0.1573(3) 0.9600(3) 0.0459 1.0000 Uani . . . . . . C31 C 0.3383(3) -0.1350(4) 0.9612(4) 0.0585 1.0000 Uani . . . . . . C32 C 0.3881(4) -0.2083(5) 0.9490(6) 0.1037 1.0000 Uani . . . . . . C33 C 0.3611(4) -0.0877(6) 1.0314(5) 0.0951 1.0000 Uani . . . . . . C34 C 0.0976(3) -0.1760(4) 0.8247(3) 0.0530 1.0000 Uani . . . . . . C35 C 0.0337(3) -0.1184(4) 0.8314(4) 0.0705 1.0000 Uani . . . . . . C36 C 0.0685(4) -0.2589(5) 0.8081(5) 0.0893 1.0000 Uani . . . . . . C37 C 0.2581(3) -0.1521(3) 0.5826(3) 0.0359 1.0000 Uani . . . . . . C38 C 0.2194(3) -0.1407(3) 0.5137(3) 0.0405 1.0000 Uani . . . . . . C39 C 0.2534(3) -0.1558(4) 0.4454(4) 0.0547 1.0000 Uani . . . . . . C40 C 0.3247(3) -0.1804(4) 0.4431(4) 0.0615 1.0000 Uani . . . . . . C41 C 0.3630(3) -0.1907(4) 0.5085(4) 0.0495 1.0000 Uani . . . . . . C42 C 0.3310(3) -0.1769(3) 0.5789(3) 0.0387 1.0000 Uani . . . . . . C43 C 0.1419(3) -0.1132(3) 0.5155(4) 0.0461 1.0000 Uani . . . . . . C44 C 0.1195(3) -0.0660(4) 0.4444(4) 0.0631 1.0000 Uani . . . . . . C45 C 0.0884(3) -0.1814(4) 0.5259(4) 0.0635 1.0000 Uani . . . . . . C46 C 0.3772(3) -0.1900(3) 0.6477(4) 0.0456 1.0000 Uani . . . . . . C47 C 0.3944(4) -0.2777(4) 0.6599(4) 0.0714 1.0000 Uani . . . . . . C48 C 0.4469(3) -0.1410(3) 0.6458(4) 0.0525 1.0000 Uani . . . . . . C49 C 0.1962(2) 0.2533(3) 0.7422(4) 0.0349 1.0000 Uani . . . . . . C50 C 0.1948(2) 0.3345(3) 0.7381(4) 0.0401 1.0000 Uani . . . . . . C51 C 0.2595(3) 0.3747(2) 0.7352(5) 0.0406 1.0000 Uani . . . . . . C52 C 0.3228(2) 0.3332(3) 0.7361(4) 0.0413 1.0000 Uani . . . . . . C53 C 0.3197(2) 0.2522(3) 0.7394(4) 0.0378 1.0000 Uani . . . . . . C54 C 0.1827(5) -0.3498(5) 0.6479(6) 0.0525 0.5000 Uani D U . 1 1 . C55 C 0.1378(4) -0.4121(5) 0.6392(5) 0.0613 0.5000 Uani D U . 1 1 . C56 C 0.1241(5) -0.4635(5) 0.6952(6) 0.0757 0.5000 Uani D U . 1 1 . C57 C 0.1554(5) -0.4535(5) 0.7634(6) 0.0792 0.5000 Uani D U . 1 1 . C58 C 0.2005(5) -0.3913(5) 0.7771(5) 0.0732 0.5000 Uani D U . 1 1 . C59 C 0.1476(10) -0.3501(13) 0.6349(13) 0.1302 0.5000 Uani D U . 1 2 . C60 C 0.2209(10) -0.3777(8) 0.6646(7) 0.1030 0.5000 Uani D U . 1 2 . C61 C 0.2735(10) -0.3962(8) 0.7808(6) 0.1024 0.5000 Uani D U . 1 2 . C62 C 0.2986(12) -0.3568(10) 0.8538(7) 0.1190 0.5000 Uani D U . 1 2 . H1 H 0.2954(9) -0.144(2) 0.832(2) 0.031(9) 1.0000 Uiso D . . . . . H2 H 0.1836(9) -0.131(2) 0.6449(19) 0.031(9) 1.0000 Uiso D . . . . . H31 H 0.5181 0.1463 0.7784 0.0544 1.0000 Uiso R . . . . . H41 H 0.5293 0.1911 0.6553 0.0589 1.0000 Uiso R . . . . . H51 H 0.4495 0.1477 0.5619 0.0589 1.0000 Uiso R . . . . . H71 H 0.3794 0.0261 0.8489 0.0561 1.0000 Uiso R . . . . . H81 H 0.4743 -0.0518 0.8960 0.0958 1.0000 Uiso R . . . . . H82 H 0.5253 -0.0150 0.8361 0.0958 1.0000 Uiso R . . . . . H83 H 0.4620 -0.0692 0.8110 0.0958 1.0000 Uiso R . . . . . H91 H 0.4428 0.0781 0.9504 0.0882 1.0000 Uiso R . . . . . H92 H 0.4957 0.1195 0.8951 0.0882 1.0000 Uiso R . . . . . H93 H 0.4154 0.1463 0.8995 0.0882 1.0000 Uiso R . . . . . H101 H 0.3214 -0.0051 0.5842 0.0646 1.0000 Uiso R . . . . . H111 H 0.2387 0.0756 0.5249 0.0718 1.0000 Uiso R . . . . . H112 H 0.2457 0.0971 0.6097 0.0718 1.0000 Uiso R . . . . . H113 H 0.2850 0.1475 0.5492 0.0718 1.0000 Uiso R . . . . . H121 H 0.3404 0.0186 0.4563 0.0809 1.0000 Uiso R . . . . . H122 H 0.4132 0.0018 0.4971 0.0809 1.0000 Uiso R . . . . . H123 H 0.3913 0.0878 0.4779 0.0809 1.0000 Uiso R . . . . . H151 H 0.0692 0.1617 0.9265 0.0513 1.0000 Uiso R . . . . . H161 H -0.0114 0.2156 0.8404 0.0556 1.0000 Uiso R . . . . . H171 H -0.0099 0.1708 0.7151 0.0475 1.0000 Uiso R . . . . . H191 H 0.1874 0.0043 0.8939 0.0490 1.0000 Uiso R . . . . . H201 H 0.1710 0.0119 1.0221 0.0842 1.0000 Uiso R . . . . . H202 H 0.1191 0.0830 1.0114 0.0842 1.0000 Uiso R . . . . . H203 H 0.0961 -0.0003 0.9843 0.0842 1.0000 Uiso R . . . . . H211 H 0.2685 0.0807 0.9636 0.0821 1.0000 Uiso R . . . . . H212 H 0.2222 0.1548 0.9462 0.0821 1.0000 Uiso R . . . . . H213 H 0.2633 0.1123 0.8816 0.0821 1.0000 Uiso R . . . . . H221 H 0.1128 0.0336 0.6403 0.0538 1.0000 Uiso R . . . . . H231 H 0.0630 0.1062 0.5394 0.1080 1.0000 Uiso R . . . . . H232 H 0.1061 0.1601 0.5939 0.1080 1.0000 Uiso R . . . . . H233 H 0.0221 0.1583 0.5973 0.1080 1.0000 Uiso R . . . . . H241 H 0.0088 -0.0175 0.5876 0.1004 1.0000 Uiso R . . . . . H242 H 0.0152 -0.0411 0.6719 0.1004 1.0000 Uiso R . . . . . H243 H -0.0353 0.0276 0.6482 0.1004 1.0000 Uiso R . . . . . H271 H 0.0618 -0.2018 0.9631 0.0646 1.0000 Uiso R . . . . . H281 H 0.1275 -0.2072 1.0746 0.0751 1.0000 Uiso R . . . . . H291 H 0.2499 -0.1728 1.0734 0.0637 1.0000 Uiso R . . . . . H311 H 0.3454 -0.1013 0.9191 0.0689 1.0000 Uiso R . . . . . H321 H 0.4375 -0.1928 0.9482 0.1392 1.0000 Uiso R . . . . . H322 H 0.3804 -0.2446 0.9890 0.1392 1.0000 Uiso R . . . . . H323 H 0.3760 -0.2327 0.9023 0.1392 1.0000 Uiso R . . . . . H331 H 0.4110 -0.0743 1.0289 0.1096 1.0000 Uiso R . . . . . H332 H 0.3526 -0.1191 1.0748 0.1096 1.0000 Uiso R . . . . . H333 H 0.3329 -0.0410 1.0343 0.1096 1.0000 Uiso R . . . . . H341 H 0.1259 -0.1594 0.7829 0.0676 1.0000 Uiso R . . . . . H351 H 0.0058 -0.1198 0.7864 0.0871 1.0000 Uiso R . . . . . H352 H 0.0045 -0.1346 0.8728 0.0871 1.0000 Uiso R . . . . . H353 H 0.0504 -0.0662 0.8399 0.0871 1.0000 Uiso R . . . . . H361 H 0.0383 -0.2589 0.7647 0.1109 1.0000 Uiso R . . . . . H362 H 0.0418 -0.2773 0.8504 0.1109 1.0000 Uiso R . . . . . H363 H 0.1089 -0.2924 0.7997 0.1109 1.0000 Uiso R . . . . . H391 H 0.2264 -0.1505 0.4001 0.0632 1.0000 Uiso R . . . . . H401 H 0.3477 -0.1887 0.3958 0.0754 1.0000 Uiso R . . . . . H411 H 0.4116 -0.2087 0.5064 0.0633 1.0000 Uiso R . . . . . H431 H 0.1366 -0.0795 0.5579 0.0565 1.0000 Uiso R . . . . . H441 H 0.0703 -0.0505 0.4494 0.0798 1.0000 Uiso R . . . . . H442 H 0.1491 -0.0205 0.4394 0.0798 1.0000 Uiso R . . . . . H443 H 0.1248 -0.0981 0.4009 0.0798 1.0000 Uiso R . . . . . H451 H 0.0400 -0.1624 0.5270 0.0801 1.0000 Uiso R . . . . . H452 H 0.0990 -0.2074 0.5720 0.0801 1.0000 Uiso R . . . . . H453 H 0.0939 -0.2173 0.4852 0.0801 1.0000 Uiso R . . . . . H461 H 0.3498 -0.1733 0.6902 0.0597 1.0000 Uiso R . . . . . H471 H 0.4225 -0.2850 0.7043 0.0939 1.0000 Uiso R . . . . . H472 H 0.3507 -0.3069 0.6640 0.0939 1.0000 Uiso R . . . . . H473 H 0.4210 -0.2955 0.6173 0.0939 1.0000 Uiso R . . . . . H481 H 0.4747 -0.1495 0.6901 0.0634 1.0000 Uiso R . . . . . H482 H 0.4743 -0.1561 0.6028 0.0634 1.0000 Uiso R . . . . . H483 H 0.4346 -0.0868 0.6421 0.0634 1.0000 Uiso R . . . . . H491 H 0.1516 0.2254 0.7453 0.0433 1.0000 Uiso R . . . . . H501 H 0.1500 0.3621 0.7372 0.0517 1.0000 Uiso R . . . . . H511 H 0.2605 0.4307 0.7335 0.0526 1.0000 Uiso R . . . . . H521 H 0.3682 0.3596 0.7345 0.0540 1.0000 Uiso R . . . . . H531 H 0.3638 0.2234 0.7402 0.0508 1.0000 Uiso R . . . . . H541 H 0.1929 -0.3143 0.6078 0.0852 0.5000 Uiso R . . 1 1 . H551 H 0.1127 -0.4168 0.5926 0.0812 0.5000 Uiso R . . 1 1 . H561 H 0.0937 -0.5076 0.6860 0.0913 0.5000 Uiso R . . 1 1 . H571 H 0.1454 -0.4903 0.8024 0.0955 0.5000 Uiso R . . 1 1 . H581 H 0.2182 -0.3821 0.8267 0.0967 0.5000 Uiso R . . 1 1 . H591 H 0.1330 -0.3790 0.5916 0.1236 0.5000 Uiso R . . 1 2 . H592 H 0.1061 -0.3364 0.6638 0.1236 0.5000 Uiso R . . 1 2 . H593 H 0.1721 -0.3036 0.6197 0.1236 0.5000 Uiso R . . 1 2 . H601 H 0.1969 -0.4243 0.6807 0.1222 0.5000 Uiso R . . 1 2 . H602 H 0.2629 -0.3915 0.6366 0.1222 0.5000 Uiso R . . 1 2 . H611 H 0.2447 -0.4423 0.7858 0.1333 0.5000 Uiso R . . 1 2 . H612 H 0.3184 -0.4094 0.7579 0.1333 0.5000 Uiso R . . 1 2 . H621 H 0.3233 -0.3907 0.8878 0.1422 0.5000 Uiso R . . 1 2 . H622 H 0.2527 -0.3432 0.8741 0.1422 0.5000 Uiso R . . 1 2 . H623 H 0.3264 -0.3103 0.8463 0.1422 0.5000 Uiso R . . 1 2 . 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 0.0250(3) 0.0237(3) 0.0259(3) -0.0014(5) -0.0003(3) 0.0000(4) Li1 0.037(3) 0.026(3) 0.076(5) 0.002(6) 0.005(4) -0.008(4) Li2 0.073(6) 0.033(3) 0.034(4) -0.004(5) 0.001(5) -0.002(4) N1 0.0261(18) 0.033(2) 0.038(3) -0.006(2) 0.0054(19) -0.0028(16) N2 0.0278(19) 0.030(2) 0.028(3) -0.0026(18) 0.0008(17) 0.0047(16) N3 0.030(2) 0.031(2) 0.035(2) 0.0060(17) -0.0059(19) -0.0003(19) N4 0.030(2) 0.037(2) 0.029(3) -0.0042(18) -0.0011(19) 0.0039(19) N5 0.0329(18) 0.0353(15) 0.0383(16) -0.003(3) 0.0123(19) 0.0014(18) N6 0.076(6) 0.020(4) 0.074(7) 0.004(5) 0.025(5) 0.006(4) O1 0.112(7) 0.033(4) 0.083(6) -0.005(5) -0.015(6) 0.027(5) C1 0.027(2) 0.030(3) 0.028(2) -0.005(2) 0.0094(19) 0.005(2) C2 0.028(2) 0.030(3) 0.054(4) -0.010(2) 0.002(2) 0.0030(19) C3 0.025(2) 0.039(3) 0.069(4) -0.009(3) 0.008(3) 0.0005(18) C4 0.027(3) 0.044(3) 0.069(4) 0.001(3) 0.010(3) -0.008(2) C5 0.043(3) 0.043(3) 0.051(4) 0.002(3) 0.024(3) 0.004(2) C6 0.031(3) 0.035(3) 0.041(3) -0.010(2) 0.006(2) 0.000(2) C7 0.042(3) 0.041(3) 0.033(3) -0.002(2) -0.004(2) -0.007(2) C8 0.067(4) 0.080(5) 0.073(5) 0.006(4) -0.018(3) 0.023(4) C9 0.082(5) 0.083(5) 0.052(4) -0.022(4) 0.001(3) -0.034(4) C10 0.057(3) 0.044(3) 0.031(3) -0.005(3) 0.010(3) -0.011(3) C11 0.052(4) 0.080(5) 0.043(4) -0.008(3) -0.003(3) -0.014(3) C12 0.076(5) 0.088(5) 0.038(4) -0.018(4) 0.005(3) -0.006(4) C13 0.024(2) 0.026(3) 0.052(4) 0.007(2) 0.003(2) -0.001(2) C14 0.038(3) 0.029(3) 0.037(3) -0.002(2) 0.014(2) -0.002(2) C15 0.038(3) 0.039(3) 0.049(4) -0.001(3) 0.013(2) 0.000(2) C16 0.032(3) 0.035(3) 0.065(4) 0.001(3) 0.023(3) 0.009(2) C17 0.016(2) 0.044(3) 0.057(4) 0.017(3) 0.001(2) 0.0045(18) C18 0.022(2) 0.036(2) 0.041(3) 0.003(2) 0.005(2) -0.0050(18) C19 0.052(3) 0.033(3) 0.032(3) -0.003(2) 0.009(2) 0.007(3) C20 0.064(4) 0.068(4) 0.045(4) -0.004(3) 0.008(3) -0.002(3) C21 0.042(4) 0.089(5) 0.068(5) 0.020(4) -0.009(3) 0.003(3) C22 0.032(3) 0.046(3) 0.049(4) 0.006(3) -0.010(2) 0.005(2) C23 0.111(6) 0.100(6) 0.051(5) 0.010(4) -0.002(4) 0.034(5) C24 0.075(4) 0.114(6) 0.063(4) -0.014(4) -0.010(4) -0.039(4) C25 0.055(3) 0.024(3) 0.031(3) 0.009(2) 0.002(3) -0.006(2) C26 0.053(3) 0.039(3) 0.037(3) 0.005(2) 0.001(3) -0.011(2) C27 0.051(3) 0.058(4) 0.050(4) 0.019(3) 0.002(3) -0.016(3) C28 0.068(4) 0.076(4) 0.042(4) 0.022(3) 0.010(3) -0.005(3) C29 0.066(4) 0.071(4) 0.026(3) 0.017(3) -0.005(3) 0.004(3) C30 0.054(3) 0.045(3) 0.038(3) 0.010(2) -0.010(3) 0.008(3) C31 0.046(3) 0.086(5) 0.044(4) 0.026(3) -0.004(3) 0.011(3) C32 0.073(5) 0.107(7) 0.132(8) 0.046(6) 0.009(5) 0.038(5) C33 0.063(4) 0.165(8) 0.058(5) 0.006(5) -0.021(4) -0.010(5) C34 0.050(3) 0.078(4) 0.030(3) -0.003(3) 0.003(3) -0.026(3) C35 0.055(4) 0.089(5) 0.068(5) 0.023(4) -0.013(3) -0.026(4) C36 0.083(5) 0.093(6) 0.092(6) -0.030(4) -0.006(4) -0.035(5) C37 0.042(3) 0.030(3) 0.035(3) -0.005(2) 0.001(2) -0.008(2) C38 0.043(3) 0.047(3) 0.031(3) -0.012(2) -0.001(2) -0.008(3) C39 0.052(4) 0.074(4) 0.038(3) -0.014(3) -0.006(3) -0.005(3) C40 0.061(4) 0.084(5) 0.039(4) -0.020(3) 0.005(3) 0.007(3) C41 0.043(3) 0.058(4) 0.048(4) -0.021(3) 0.005(3) 0.001(3) C42 0.038(3) 0.043(3) 0.036(3) -0.018(2) -0.003(2) 0.005(2) C43 0.042(3) 0.053(3) 0.043(3) -0.011(3) -0.010(3) -0.007(3) C44 0.059(4) 0.076(4) 0.054(4) 0.004(3) -0.021(3) -0.012(3) C45 0.056(4) 0.083(4) 0.051(4) -0.002(3) -0.009(3) -0.020(3) C46 0.031(3) 0.049(3) 0.056(4) -0.015(3) 0.002(2) 0.010(2) C47 0.068(4) 0.062(4) 0.084(5) 0.009(4) -0.001(4) 0.015(3) C48 0.045(3) 0.055(4) 0.058(4) -0.016(3) -0.009(3) 0.013(3) C49 0.032(2) 0.033(3) 0.039(3) 0.002(3) 0.000(3) -0.0018(18) C50 0.038(2) 0.037(3) 0.045(3) 0.000(3) 0.005(3) 0.007(2) C51 0.043(3) 0.0273(17) 0.052(3) 0.005(3) 0.000(3) -0.005(2) C52 0.032(2) 0.032(3) 0.060(4) -0.001(3) -0.008(3) -0.0031(18) C53 0.028(2) 0.039(3) 0.046(3) 0.003(3) -0.001(3) 0.0008(18) C54 0.045(6) 0.029(5) 0.084(7) -0.001(5) -0.003(5) 0.003(5) C55 0.070(6) 0.025(4) 0.089(7) -0.001(5) 0.009(5) 0.012(4) C56 0.083(6) 0.044(5) 0.100(7) -0.004(5) 0.015(6) 0.010(5) C57 0.090(7) 0.054(5) 0.094(7) 0.002(5) 0.022(6) 0.009(5) C58 0.091(7) 0.042(5) 0.086(7) 0.002(5) 0.029(6) 0.004(5) C59 0.158(12) 0.114(10) 0.118(11) -0.033(9) -0.032(10) 0.022(10) C60 0.130(9) 0.071(7) 0.107(9) -0.042(7) -0.027(8) 0.035(7) C61 0.150(9) 0.060(7) 0.097(8) 0.003(6) 0.012(8) 0.016(7) C62 0.173(11) 0.088(9) 0.096(10) 0.024(8) 0.016(10) 0.008(9) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.1326(2) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . N1 . 1.792(4) yes Ti1 . N2 . 1.773(3) yes Ti1 . N3 . 2.073(4) yes Ti1 . N4 . 2.076(4) yes Li1 . N5 . 2.023(6) yes Li1 . N2 . 2.097(8) yes Li1 . N1 . 2.081(9) yes Li2 . N3 . 2.032(11) yes Li2 . N4 . 2.053(11) yes Li2 . N6 . 1.917(11) yes Li2 . N3 . 2.032(11) yes Li2 . N4 . 2.053(11) yes Li2 . O1 . 1.987(11) yes N1 . C1 . 1.377(6) yes N2 . C13 . 1.406(6) yes N3 . C25 . 1.413(7) yes N3 . H1 . 0.773(10) no N4 . C37 . 1.420(7) yes N4 . H2 . 0.776(10) no N5 . C49 . 1.335(5) yes N5 . C53 . 1.346(6) yes N6 . C54 . 1.442(9) yes N6 . C58 . 1.426(9) yes O1 . C60 . 1.402(9) yes O1 . C61 . 1.406(9) yes C1 . C2 . 1.443(7) yes C1 . C6 . 1.423(7) yes C2 . C3 . 1.390(7) yes C2 . C7 . 1.508(8) yes C3 . C4 . 1.368(9) yes C3 . H31 . 0.950 no C4 . C5 . 1.393(9) yes C4 . H41 . 0.950 no C5 . C6 . 1.415(7) yes C5 . H51 . 0.950 no C6 . C10 . 1.517(8) yes C7 . C8 . 1.546(8) yes C7 . C9 . 1.528(8) yes C7 . H71 . 0.950 no C8 . H81 . 0.950 no C8 . H82 . 0.950 no C8 . H83 . 0.950 no C9 . H91 . 0.950 no C9 . H92 . 0.950 no C9 . H93 . 0.950 no C10 . C11 . 1.502(9) yes C10 . C12 . 1.523(8) yes C10 . H101 . 0.950 no C11 . H111 . 0.950 no C11 . H112 . 0.950 no C11 . H113 . 0.950 no C12 . H121 . 0.950 no C12 . H122 . 0.950 no C12 . H123 . 0.950 no C13 . C14 . 1.413(8) yes C13 . C18 . 1.426(7) yes C14 . C15 . 1.365(7) yes C14 . C19 . 1.507(8) yes C15 . C16 . 1.377(8) yes C15 . H151 . 0.950 no C16 . C17 . 1.391(8) yes C16 . H161 . 0.950 no C17 . C18 . 1.389(7) yes C17 . H171 . 0.950 no C18 . C22 . 1.484(8) yes C19 . C20 . 1.525(8) yes C19 . C21 . 1.537(9) yes C19 . H191 . 0.950 no C20 . H201 . 0.950 no C20 . H202 . 0.950 no C20 . H203 . 0.950 no C21 . H211 . 0.950 no C21 . H212 . 0.950 no C21 . H213 . 0.950 no C22 . C23 . 1.546(10) yes C22 . C24 . 1.514(8) yes C22 . H221 . 0.950 no C23 . H231 . 0.950 no C23 . H232 . 0.950 no C23 . H233 . 0.950 no C24 . H241 . 0.950 no C24 . H242 . 0.950 no C24 . H243 . 0.950 no C25 . C26 . 1.420(8) yes C25 . C30 . 1.408(8) yes C26 . C27 . 1.373(9) yes C26 . C34 . 1.516(8) yes C27 . C28 . 1.376(9) yes C27 . H271 . 0.950 no C28 . C29 . 1.387(9) yes C28 . H281 . 0.950 no C29 . C30 . 1.390(9) yes C29 . H291 . 0.950 no C30 . C31 . 1.511(8) yes C31 . C32 . 1.562(10) yes C31 . C33 . 1.539(10) yes C31 . H311 . 0.950 no C32 . H321 . 0.950 no C32 . H322 . 0.950 no C32 . H323 . 0.950 no C33 . H331 . 0.950 no C33 . H332 . 0.950 no C33 . H333 . 0.950 no C34 . C35 . 1.537(9) yes C34 . C36 . 1.533(9) yes C34 . H341 . 0.950 no C35 . H351 . 0.950 no C35 . H352 . 0.950 no C35 . H353 . 0.950 no C36 . H361 . 0.950 no C36 . H362 . 0.950 no C36 . H363 . 0.950 no C37 . C38 . 1.428(8) yes C37 . C42 . 1.410(7) yes C38 . C39 . 1.388(9) yes C38 . C43 . 1.505(8) yes C39 . C40 . 1.381(9) yes C39 . H391 . 0.950 no C40 . C41 . 1.367(9) yes C40 . H401 . 0.950 no C41 . C42 . 1.400(8) yes C41 . H411 . 0.950 no C42 . C46 . 1.506(8) yes C43 . C44 . 1.550(9) yes C43 . C45 . 1.531(8) yes C43 . H431 . 0.950 no C44 . H441 . 0.950 no C44 . H442 . 0.950 no C44 . H443 . 0.950 no C45 . H451 . 0.950 no C45 . H452 . 0.950 no C45 . H453 . 0.950 no C46 . C47 . 1.537(8) yes C46 . C48 . 1.532(7) yes C46 . H461 . 0.950 no C47 . H471 . 0.950 no C47 . H472 . 0.950 no C47 . H473 . 0.950 no C48 . H481 . 0.950 no C48 . H482 . 0.950 no C48 . H483 . 0.950 no C49 . C50 . 1.381(6) yes C49 . H491 . 0.950 no C50 . C51 . 1.376(6) yes C50 . H501 . 0.950 no C51 . C52 . 1.365(6) yes C51 . H511 . 0.950 no C52 . C53 . 1.376(6) yes C52 . H521 . 0.950 no C53 . H531 . 0.950 no C54 . C55 . 1.353(8) yes C54 . H541 . 0.950 no C55 . C56 . 1.346(8) yes C55 . H551 . 0.950 no C56 . C57 . 1.349(9) yes C56 . H561 . 0.950 no C57 . C58 . 1.365(9) yes C57 . H571 . 0.950 no C58 . H581 . 0.950 no C59 . C60 . 1.525(4) yes C59 . H591 . 0.950 no C59 . H592 . 0.950 no C59 . H593 . 0.950 no C60 . H601 . 0.950 no C60 . H602 . 0.950 no C61 . C62 . 1.528(4) yes C61 . H611 . 0.950 no C61 . H612 . 0.950 no C62 . H621 . 0.950 no C62 . H622 . 0.950 no C62 . H623 . 0.950 no loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag N1 . Ti1 . N2 . 106.08(14) yes N1 . Ti1 . N3 . 115.43(19) yes N2 . Ti1 . N3 . 113.05(19) yes N1 . Ti1 . N4 . 114.6(2) yes N2 . Ti1 . N4 . 114.06(18) yes N3 . Ti1 . N4 . 93.72(15) yes N5 . Li1 . N2 . 135.4(5) yes N5 . Li1 . N1 . 138.5(5) yes N2 . Li1 . N1 . 86.0(3) yes N3 . Li2 . N4 . 95.7(3) yes N3 . Li2 . N6 . 139.5(8) yes N4 . Li2 . N6 . 123.4(7) yes N3 . Li2 . N4 . 95.7(3) yes N3 . Li2 . O1 . 130.9(7) yes N4 . Li2 . O1 . 133.4(7) yes Ti1 . N1 . C1 . 171.4(4) yes Ti1 . N1 . Li1 . 84.0(2) yes C1 . N1 . Li1 . 90.6(3) yes Ti1 . N2 . C13 . 172.7(4) yes Ti1 . N2 . Li1 . 84.0(3) yes C13 . N2 . Li1 . 93.6(4) yes Ti1 . N3 . C25 . 133.0(3) yes Ti1 . N3 . H1 . 101.6(10) no C25 . N3 . H1 . 103(3) no Ti1 . N3 . Li2 . 85.6(3) yes C25 . N3 . Li2 . 119.6(4) yes H1 . N3 . Li2 . 113(4) no Ti1 . N4 . C37 . 130.8(3) yes Ti1 . N4 . H2 . 101.3(10) no C37 . N4 . H2 . 106(3) no Ti1 . N4 . Li2 . 85.0(3) yes C37 . N4 . Li2 . 118.2(4) yes H2 . N4 . Li2 . 113(4) no C49 . N5 . C53 . 116.6(3) yes C49 . N5 . Li1 . 120.9(4) yes C53 . N5 . Li1 . 122.5(4) yes C54 . N6 . C58 . 115.0(6) yes C54 . N6 . Li2 . 113.1(7) yes C58 . N6 . Li2 . 127.2(8) yes C60 . O1 . C61 . 109.90(10) yes C60 . O1 . Li2 . 116.6(9) yes C61 . O1 . Li2 . 130.7(9) yes N1 . C1 . C2 . 120.8(5) yes N1 . C1 . C6 . 120.6(4) yes C2 . C1 . C6 . 118.5(4) yes C1 . C2 . C3 . 119.2(6) yes C1 . C2 . C7 . 119.6(4) yes C3 . C2 . C7 . 121.1(5) yes C2 . C3 . C4 . 121.8(6) yes C2 . C3 . H31 . 118.3 no C4 . C3 . H31 . 120.0 no C3 . C4 . C5 . 120.6(5) yes C3 . C4 . H41 . 120.2 no C5 . C4 . H41 . 119.2 no C4 . C5 . C6 . 120.3(6) yes C4 . C5 . H51 . 120.2 no C6 . C5 . H51 . 119.5 no C1 . C6 . C5 . 119.4(5) yes C1 . C6 . C10 . 119.8(4) yes C5 . C6 . C10 . 120.8(5) yes C2 . C7 . C8 . 108.9(5) yes C2 . C7 . C9 . 114.6(5) yes C8 . C7 . C9 . 110.2(5) yes C2 . C7 . H71 . 107.5 no C8 . C7 . H71 . 107.3 no C9 . C7 . H71 . 108.0 no C7 . C8 . H81 . 109.9 no C7 . C8 . H82 . 108.4 no H81 . C8 . H82 . 109.5 no C7 . C8 . H83 . 110.1 no H81 . C8 . H83 . 109.5 no H82 . C8 . H83 . 109.5 no C7 . C9 . H91 . 109.6 no C7 . C9 . H92 . 109.1 no H91 . C9 . H92 . 109.5 no C7 . C9 . H93 . 109.6 no H91 . C9 . H93 . 109.5 no H92 . C9 . H93 . 109.5 no C6 . C10 . C11 . 112.4(5) yes C6 . C10 . C12 . 112.7(5) yes C11 . C10 . C12 . 110.1(6) yes C6 . C10 . H101 . 107.5 no C11 . C10 . H101 . 106.5 no C12 . C10 . H101 . 107.2 no C10 . C11 . H111 . 111.0 no C10 . C11 . H112 . 109.5 no H111 . C11 . H112 . 109.5 no C10 . C11 . H113 . 107.8 no H111 . C11 . H113 . 109.5 no H112 . C11 . H113 . 109.5 no C10 . C12 . H121 . 110.6 no C10 . C12 . H122 . 109.2 no H121 . C12 . H122 . 109.5 no C10 . C12 . H123 . 108.6 no H121 . C12 . H123 . 109.5 no H122 . C12 . H123 . 109.5 no N2 . C13 . C14 . 120.5(5) yes N2 . C13 . C18 . 119.5(5) yes C14 . C13 . C18 . 120.0(5) yes C13 . C14 . C15 . 118.4(5) yes C13 . C14 . C19 . 120.0(4) yes C15 . C14 . C19 . 121.6(5) yes C14 . C15 . C16 . 123.2(6) yes C14 . C15 . H151 . 118.0 no C16 . C15 . H151 . 118.8 no C15 . C16 . C17 . 118.5(5) yes C15 . C16 . H161 . 120.7 no C17 . C16 . H161 . 120.8 no C16 . C17 . C18 . 121.6(5) yes C16 . C17 . H171 . 119.7 no C18 . C17 . H171 . 118.7 no C13 . C18 . C17 . 118.2(5) yes C13 . C18 . C22 . 121.3(4) yes C17 . C18 . C22 . 120.3(5) yes C14 . C19 . C20 . 114.1(5) yes C14 . C19 . C21 . 112.6(5) yes C20 . C19 . C21 . 108.5(5) yes C14 . C19 . H191 . 106.7 no C20 . C19 . H191 . 107.0 no C21 . C19 . H191 . 107.4 no C19 . C20 . H201 . 108.8 no C19 . C20 . H202 . 108.5 no H201 . C20 . H202 . 109.5 no C19 . C20 . H203 . 111.1 no H201 . C20 . H203 . 109.5 no H202 . C20 . H203 . 109.5 no C19 . C21 . H211 . 109.6 no C19 . C21 . H212 . 108.9 no H211 . C21 . H212 . 109.5 no C19 . C21 . H213 . 109.9 no H211 . C21 . H213 . 109.5 no H212 . C21 . H213 . 109.5 no C18 . C22 . C23 . 112.8(5) yes C18 . C22 . C24 . 112.6(5) yes C23 . C22 . C24 . 111.1(6) yes C18 . C22 . H221 . 106.9 no C23 . C22 . H221 . 107.6 no C24 . C22 . H221 . 105.3 no C22 . C23 . H231 . 110.9 no C22 . C23 . H232 . 108.1 no H231 . C23 . H232 . 109.5 no C22 . C23 . H233 . 109.5 no H231 . C23 . H233 . 109.5 no H232 . C23 . H233 . 109.5 no C22 . C24 . H241 . 110.8 no C22 . C24 . H242 . 110.4 no H241 . C24 . H242 . 109.5 no C22 . C24 . H243 . 107.2 no H241 . C24 . H243 . 109.5 no H242 . C24 . H243 . 109.5 no N3 . C25 . C26 . 119.9(5) yes N3 . C25 . C30 . 122.2(5) yes C26 . C25 . C30 . 117.8(6) yes C25 . C26 . C27 . 120.2(5) yes C25 . C26 . C34 . 122.7(5) yes C27 . C26 . C34 . 117.1(5) yes C26 . C27 . C28 . 121.9(6) yes C26 . C27 . H271 . 119.0 no C28 . C27 . H271 . 119.1 no C27 . C28 . C29 . 118.7(6) yes C27 . C28 . H281 . 120.5 no C29 . C28 . H281 . 120.8 no C28 . C29 . C30 . 121.3(6) yes C28 . C29 . H291 . 119.0 no C30 . C29 . H291 . 119.7 no C25 . C30 . C29 . 120.0(6) yes C25 . C30 . C31 . 120.4(6) yes C29 . C30 . C31 . 119.6(5) yes C30 . C31 . C32 . 111.5(6) yes C30 . C31 . C33 . 114.0(6) yes C32 . C31 . C33 . 111.6(6) yes C30 . C31 . H311 . 105.8 no C32 . C31 . H311 . 106.9 no C33 . C31 . H311 . 106.5 no C31 . C32 . H321 . 110.2 no C31 . C32 . H322 . 109.0 no H321 . C32 . H322 . 109.5 no C31 . C32 . H323 . 109.3 no H321 . C32 . H323 . 109.5 no H322 . C32 . H323 . 109.5 no C31 . C33 . H331 . 110.6 no C31 . C33 . H332 . 108.5 no H331 . C33 . H332 . 109.5 no C31 . C33 . H333 . 109.2 no H331 . C33 . H333 . 109.5 no H332 . C33 . H333 . 109.5 no C26 . C34 . C35 . 112.2(5) yes C26 . C34 . C36 . 111.4(6) yes C35 . C34 . C36 . 109.3(5) yes C26 . C34 . H341 . 108.2 no C35 . C34 . H341 . 107.1 no C36 . C34 . H341 . 108.5 no C34 . C35 . H351 . 109.4 no C34 . C35 . H352 . 108.1 no H351 . C35 . H352 . 109.5 no C34 . C35 . H353 . 110.8 no H351 . C35 . H353 . 109.5 no H352 . C35 . H353 . 109.5 no C34 . C36 . H361 . 111.2 no C34 . C36 . H362 . 109.4 no H361 . C36 . H362 . 109.5 no C34 . C36 . H363 . 107.8 no H361 . C36 . H363 . 109.5 no H362 . C36 . H363 . 109.5 no N4 . C37 . C38 . 120.9(5) yes N4 . C37 . C42 . 120.5(5) yes C38 . C37 . C42 . 118.5(5) yes C37 . C38 . C39 . 119.6(5) yes C37 . C38 . C43 . 120.0(5) yes C39 . C38 . C43 . 120.4(5) yes C38 . C39 . C40 . 120.9(6) yes C38 . C39 . H391 . 118.8 no C40 . C39 . H391 . 120.3 no C39 . C40 . C41 . 120.3(6) yes C39 . C40 . H401 . 119.7 no C41 . C40 . H401 . 119.9 no C40 . C41 . C42 . 121.1(5) yes C40 . C41 . H411 . 119.8 no C42 . C41 . H411 . 119.1 no C37 . C42 . C41 . 119.6(5) yes C37 . C42 . C46 . 123.1(5) yes C41 . C42 . C46 . 117.3(5) yes C38 . C43 . C44 . 113.3(5) yes C38 . C43 . C45 . 112.4(5) yes C44 . C43 . C45 . 108.5(5) yes C38 . C43 . H431 . 107.4 no C44 . C43 . H431 . 107.7 no C45 . C43 . H431 . 107.1 no C43 . C44 . H441 . 108.7 no C43 . C44 . H442 . 110.1 no H441 . C44 . H442 . 109.5 no C43 . C44 . H443 . 109.6 no H441 . C44 . H443 . 109.5 no H442 . C44 . H443 . 109.5 no C43 . C45 . H451 . 110.6 no C43 . C45 . H452 . 108.8 no H451 . C45 . H452 . 109.5 no C43 . C45 . H453 . 108.9 no H451 . C45 . H453 . 109.5 no H452 . C45 . H453 . 109.5 no C42 . C46 . C47 . 112.0(5) yes C42 . C46 . C48 . 112.2(5) yes C47 . C46 . C48 . 110.8(4) yes C42 . C46 . H461 . 107.2 no C47 . C46 . H461 . 106.7 no C48 . C46 . H461 . 107.6 no C46 . C47 . H471 . 110.8 no C46 . C47 . H472 . 110.0 no H471 . C47 . H472 . 109.5 no C46 . C47 . H473 . 107.6 no H471 . C47 . H473 . 109.5 no H472 . C47 . H473 . 109.5 no C46 . C48 . H481 . 110.7 no C46 . C48 . H482 . 108.6 no H481 . C48 . H482 . 109.5 no C46 . C48 . H483 . 109.1 no H481 . C48 . H483 . 109.5 no H482 . C48 . H483 . 109.5 no N5 . C49 . C50 . 123.2(4) yes N5 . C49 . H491 . 117.8 no C50 . C49 . H491 . 119.0 no C49 . C50 . C51 . 118.8(4) yes C49 . C50 . H501 . 120.6 no C51 . C50 . H501 . 120.7 no C50 . C51 . C52 . 119.1(4) yes C50 . C51 . H511 . 120.9 no C52 . C51 . H511 . 120.0 no C51 . C52 . C53 . 118.7(4) yes C51 . C52 . H521 . 120.7 no C53 . C52 . H521 . 120.6 no C52 . C53 . N5 . 123.5(4) yes C52 . C53 . H531 . 118.6 no N5 . C53 . H531 . 117.9 no N6 . C54 . C55 . 120.1(6) yes N6 . C54 . H541 . 117.8 no C55 . C54 . H541 . 122.1 no C54 . C55 . C56 . 122.5(6) yes C54 . C55 . H551 . 117.7 no C56 . C55 . H551 . 119.7 no C55 . C56 . C57 . 119.9(6) yes C55 . C56 . H561 . 119.6 no C57 . C56 . H561 . 120.4 no C56 . C57 . C58 . 121.2(6) yes C56 . C57 . H571 . 119.0 no C58 . C57 . H571 . 119.8 no N6 . C58 . C57 . 121.1(6) yes N6 . C58 . H581 . 118.4 no C57 . C58 . H581 . 120.1 no C60 . C59 . H591 . 111.9 no C60 . C59 . H592 . 127.1 no H591 . C59 . H592 . 109.5 no C60 . C59 . H593 . 86.1 no H591 . C59 . H593 . 109.5 no H592 . C59 . H593 . 109.5 no C59 . C60 . O1 . 111.9(14) yes C59 . C60 . H601 . 86.9 no O1 . C60 . H601 . 102.1 no C59 . C60 . H602 . 128.2 no O1 . C60 . H602 . 111.9 no H601 . C60 . H602 . 109.5 no O1 . C61 . C62 . 111.0(11) yes O1 . C61 . H611 . 109.8 no C62 . C61 . H611 . 116.9 no O1 . C61 . H612 . 107.4 no C62 . C61 . H612 . 101.5 no H611 . C61 . H612 . 109.5 no C61 . C62 . H621 . 114.7 no C61 . C62 . H622 . 99.0 no H621 . C62 . H622 . 109.5 no C61 . C62 . H623 . 114.1 no H621 . C62 . H623 . 109.5 no H622 . C62 . H623 . 109.5 no