data_bf20 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Li N9 Ti, 1.5(C6 H6)' _chemical_formula_sum 'C45 H39 Li N9 Ti' _chemical_formula_weight 760.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5641(5) _cell_length_b 10.7536(5) _cell_length_c 17.1299(9) _cell_angle_alpha 88.685(2) _cell_angle_beta 78.420(2) _cell_angle_gamma 82.808(2) _cell_volume 1891.38(16) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7128 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.32 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 794 _exptl_absorpt_coefficient_mu 0.273 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9105 _exptl_absorpt_correction_T_max 0.9602 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker X8 APEX II diffractometer' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29322 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8504 _reflns_number_gt 6256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SAINT+' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0461P)^2^+0.3555P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8504 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0625 _refine_ls_R_factor_gt 0.0416 _refine_ls_wR_factor_ref 0.1084 _refine_ls_wR_factor_gt 0.0987 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL bf20 in P-1 CELL 0.71073 10.5641 10.7536 17.1299 88.685 78.420 82.808 ZERR 2.00 0.0005 0.0005 0.0009 0.002 0.002 0.002 LATT 1 SFAC C H N Ti Li UNIT 90 78 18 2 2 TEMP -100 SIZE 0.150 0.250 0.350 SHEL 100 .77 OMIT 0 0 1 L.S. 12 ACTA WPDB DAMP 500 WGHT 0.046100 0.355500 FVAR 0.15642 TI1 4 0.269060 0.082909 0.234320 11.00000 0.02388 0.02196 = 0.02224 -0.00183 -0.00401 -0.00247 LI1 5 0.517895 -0.157189 0.233633 11.00000 0.03052 0.02810 = 0.03108 -0.00329 -0.00511 -0.00501 N1 3 0.141885 0.193878 0.329711 11.00000 0.02998 0.02200 = 0.02503 0.00135 -0.00438 0.00029 N2 3 0.075316 0.022079 0.246175 11.00000 0.02802 0.02595 = 0.02614 0.00353 -0.00676 -0.00386 N3 3 0.280215 -0.051250 0.139896 11.00000 0.03266 0.02414 = 0.02382 0.00121 -0.00859 -0.00134 N4 3 0.233457 0.225414 0.151743 11.00000 0.02819 0.02334 = 0.02521 -0.00200 -0.00428 -0.00291 N5 3 0.424047 0.180458 0.218279 11.00000 0.02509 0.02166 = 0.02637 -0.00130 -0.00450 -0.00289 N6 3 0.636082 -0.036264 0.163222 11.00000 0.02688 0.02950 = 0.02853 -0.00103 -0.00392 -0.00203 N7 3 0.620026 -0.142835 0.325335 11.00000 0.03065 0.03035 = 0.03036 0.00159 -0.00924 -0.00199 N8 3 0.394855 -0.015061 0.289801 11.00000 0.02513 0.02380 = 0.02329 -0.00098 -0.00530 -0.00539 N9 3 0.362226 -0.258785 0.258465 11.00000 0.02748 0.02243 = 0.02410 0.00041 -0.00747 -0.00145 C1 1 0.176660 0.286642 0.369127 11.00000 0.04115 0.02353 = 0.02881 0.00050 -0.00995 0.00036 H1 2 0.262334 0.304237 0.349505 11.00000 0.03685 C2 1 0.096021 0.351586 0.431306 11.00000 0.06057 0.02449 = 0.02877 -0.00179 -0.01151 0.00440 H2 2 0.127410 0.416831 0.453702 11.00000 0.03971 C3 1 -0.030555 0.320360 0.455279 11.00000 0.05747 0.03210 = 0.02741 0.00053 0.00520 0.01297 H3 2 -0.085339 0.364202 0.497345 11.00000 0.04101 C4 1 -0.070786 0.229223 0.415992 11.00000 0.03873 0.03486 = 0.03333 0.00585 0.00552 0.00380 H4 2 -0.157543 0.209797 0.430356 11.00000 0.04234 C5 1 0.015481 0.165668 0.350580 11.00000 0.03133 0.02731 = 0.02738 0.00512 -0.00170 0.00075 C6 1 -0.018771 0.074430 0.305056 11.00000 0.02568 0.03473 = 0.03527 0.00549 -0.00290 -0.00538 H6 2 -0.101871 0.048212 0.317025 11.00000 0.03380 C7 1 0.063506 -0.071176 0.200103 11.00000 0.03459 0.02897 = 0.03373 0.00578 -0.01425 -0.01226 H7 2 -0.012857 -0.109956 0.208159 11.00000 0.03725 C8 1 0.175240 -0.114902 0.142646 11.00000 0.03894 0.02420 = 0.02490 0.00392 -0.01304 -0.00462 C9 1 0.183871 -0.216794 0.090692 11.00000 0.06007 0.02773 = 0.03322 0.00226 -0.02046 -0.01164 H9 2 0.112744 -0.261694 0.096642 11.00000 0.03592 C10 1 0.296380 -0.250290 0.036862 11.00000 0.07544 0.02856 = 0.02908 -0.00609 -0.01913 -0.00017 H10 2 0.302894 -0.318451 -0.000564 11.00000 0.04654 C11 1 0.401129 -0.182859 0.032226 11.00000 0.05246 0.04130 = 0.02721 -0.00731 -0.00754 0.00889 H11 2 0.482222 -0.199694 -0.007097 11.00000 0.05147 C12 1 0.387916 -0.084319 0.084255 11.00000 0.03367 0.03783 = 0.02636 -0.00288 -0.00772 0.00079 H12 2 0.453848 -0.036020 0.084134 11.00000 0.02102 C13 1 0.128868 0.243768 0.116327 11.00000 0.03428 0.03229 = 0.03273 0.00011 -0.01016 -0.00508 H13 2 0.062663 0.189036 0.135081 11.00000 0.04090 C14 1 0.110557 0.334107 0.061444 11.00000 0.04253 0.03742 = 0.03904 0.00429 -0.01894 -0.00253 H14 2 0.032973 0.343734 0.041451 11.00000 0.04265 C15 1 0.205322 0.418644 0.040496 11.00000 0.05430 0.02949 = 0.03147 0.00481 -0.01455 -0.00255 H15 2 0.194517 0.482603 0.003262 11.00000 0.04331 C16 1 0.309920 0.405867 0.075003 11.00000 0.04294 0.02412 = 0.03345 0.00081 -0.00647 -0.00543 H16 2 0.375864 0.457833 0.062296 11.00000 0.03304 C17 1 0.328025 0.308522 0.131014 11.00000 0.03262 0.02109 = 0.02353 -0.00369 -0.00276 -0.00062 C18 1 0.431153 0.282924 0.168407 11.00000 0.02823 0.02182 = 0.02980 -0.00180 -0.00158 -0.00452 H18 2 0.505556 0.330915 0.159736 11.00000 0.03383 C19 1 0.535618 0.139034 0.255384 11.00000 0.02727 0.02497 = 0.02690 -0.00189 -0.00635 -0.00641 H19 2 0.567567 0.213301 0.278184 11.00000 0.02387 C20 1 0.647175 0.076689 0.192260 11.00000 0.02439 0.02807 = 0.02611 0.00338 -0.00876 -0.00278 C21 1 0.751769 0.141229 0.160920 11.00000 0.02745 0.03464 = 0.03408 0.00036 -0.00968 -0.00741 H21 2 0.755352 0.219581 0.184446 11.00000 0.02516 C22 1 0.842501 0.092305 0.096302 11.00000 0.02326 0.05027 = 0.03782 0.00588 -0.00336 -0.00878 H22 2 0.912012 0.137163 0.071988 11.00000 0.03665 C23 1 0.829084 -0.020856 0.065180 11.00000 0.02744 0.04425 = 0.03350 -0.00057 -0.00174 0.00240 H23 2 0.884156 -0.057382 0.019454 11.00000 0.04374 C24 1 0.726731 -0.081787 0.100275 11.00000 0.03052 0.03112 = 0.03468 -0.00144 -0.00433 0.00177 H24 2 0.714521 -0.163534 0.081553 11.00000 0.03791 C25 1 0.479360 0.054302 0.324639 11.00000 0.02696 0.02598 = 0.02334 -0.00360 -0.00498 -0.00327 H25 2 0.427774 0.110853 0.369803 11.00000 0.01784 C26 1 0.581944 -0.028609 0.358499 11.00000 0.02409 0.03150 = 0.02243 0.00074 -0.00151 -0.00772 C27 1 0.635080 0.011464 0.419437 11.00000 0.02912 0.03884 = 0.02715 -0.00485 -0.00297 -0.00806 H27 2 0.608485 0.084829 0.438849 11.00000 0.02376 C28 1 0.731910 -0.066950 0.446167 11.00000 0.03407 0.06424 = 0.02462 0.00325 -0.01186 -0.01545 H28 2 0.766724 -0.042775 0.485345 11.00000 0.04962 C29 1 0.772757 -0.181773 0.411125 11.00000 0.03252 0.04793 = 0.03764 0.01325 -0.01276 -0.00451 H29 2 0.836310 -0.237752 0.429277 11.00000 0.04154 C30 1 0.714508 -0.216873 0.351603 11.00000 0.03701 0.03386 = 0.03873 0.00449 -0.01118 -0.00133 H30 2 0.739271 -0.297249 0.329169 11.00000 0.04276 C31 1 0.288072 -0.067404 0.332483 11.00000 0.02603 0.02647 = 0.02069 -0.00111 -0.00377 -0.00262 H31 2 0.239348 -0.031422 0.381493 11.00000 0.02521 C32 1 0.267804 -0.190307 0.312746 11.00000 0.02718 0.02314 = 0.02003 0.00385 -0.00813 -0.00159 C33 1 0.150328 -0.238408 0.344761 11.00000 0.02978 0.02847 = 0.02781 0.00145 -0.00287 -0.00259 H33 2 0.087534 -0.190335 0.380492 11.00000 0.03360 C34 1 0.129330 -0.353913 0.321612 11.00000 0.03189 0.03113 = 0.03537 0.00506 -0.00620 -0.00925 H34 2 0.051167 -0.386738 0.340996 11.00000 0.04018 C35 1 0.224592 -0.423001 0.265830 11.00000 0.03713 0.02132 = 0.03533 0.00020 -0.01232 -0.00597 H35 2 0.214681 -0.503144 0.246568 11.00000 0.02499 C36 1 0.336699 -0.370727 0.236425 11.00000 0.02979 0.02407 = 0.02943 -0.00173 -0.00944 0.00113 H36 2 0.403222 -0.414641 0.197650 11.00000 0.02495 C1S 1 0.827799 -0.410011 0.161812 11.00000 0.04256 0.05412 = 0.03528 0.00340 -0.00682 -0.00198 H1S 2 0.853314 -0.355552 0.118379 11.00000 0.06091 C2S 1 0.698547 -0.428324 0.186396 11.00000 0.03835 0.05394 = 0.04212 -0.00139 -0.01705 0.00286 H2S 2 0.633470 -0.389514 0.157125 11.00000 0.05012 C3S 1 0.661003 -0.501249 0.252588 11.00000 0.03704 0.04540 = 0.05143 -0.00119 -0.01247 -0.00685 H3S 2 0.572221 -0.513648 0.269418 11.00000 0.05460 C4S 1 0.753698 -0.557127 0.292856 11.00000 0.05056 0.03473 = 0.05123 0.00665 -0.01743 -0.00879 H4S 2 0.726925 -0.606852 0.339243 11.00000 0.05733 C5S 1 0.882977 -0.540778 0.267507 11.00000 0.04599 0.03733 = 0.05298 0.00271 -0.02359 0.00153 H5S 2 0.945795 -0.578351 0.295935 11.00000 0.04789 C6S 1 0.919790 -0.467065 0.202479 11.00000 0.03394 0.05160 = 0.04739 -0.00348 -0.00999 -0.00104 H6S 2 1.007600 -0.454631 0.185294 11.00000 0.04514 C7S 1 0.468734 0.615451 0.467745 11.00000 0.05775 0.06621 = 0.05691 0.01973 -0.00789 -0.01515 H7S 2 0.446005 0.693512 0.445306 11.00000 0.06327 C8S 1 0.418092 0.512954 0.446590 11.00000 0.04894 0.09060 = 0.04348 0.00745 -0.01360 -0.02042 H8S 2 0.365134 0.521836 0.409398 11.00000 0.05907 C9S 1 0.449594 0.397673 0.478840 11.00000 0.06784 0.07204 = 0.06018 0.00057 -0.01273 -0.03349 H9S 2 0.419285 0.328110 0.463881 11.00000 0.08206 HKLF 4 REM bf20 in P-1 REM R1 = 0.0416 for 6256 Fo > 4sig(Fo) and 0.0625 for all 8504 data REM 661 parameters refined using 0 restraints END WGHT 0.0435 0.4688 REM Highest difference peak 0.238, deepest hole -0.422, 1-sigma level 0.047 Q1 1 0.2410 0.1447 0.1723 11.00000 0.05 0.24 Q2 1 0.6375 0.0011 0.3659 11.00000 0.05 0.23 Q3 1 0.4196 -0.2183 0.2709 11.00000 0.05 0.23 Q4 1 0.1405 0.0701 0.2517 11.00000 0.05 0.22 Q5 1 0.8655 -0.4695 0.1745 11.00000 0.05 0.22 Q6 1 0.3645 0.1370 0.2148 11.00000 0.05 0.22 Q7 1 0.4582 0.4554 0.4443 11.00000 0.05 0.22 Q8 1 0.2969 -0.1478 0.3316 11.00000 0.05 0.21 Q9 1 0.5489 0.0184 0.3409 11.00000 0.05 0.20 Q10 1 0.6285 -0.0588 0.3290 11.00000 0.05 0.20 Q11 1 0.1982 0.1714 0.2873 11.00000 0.05 0.20 Q12 1 0.1900 0.1193 0.3008 11.00000 0.05 0.20 Q13 1 0.2183 0.2981 0.3620 11.00000 0.05 0.20 Q14 1 0.4221 0.5756 0.4900 11.00000 0.05 0.19 Q15 1 0.0466 0.3054 0.4461 11.00000 0.05 0.19 Q16 1 0.5310 0.0973 0.2968 11.00000 0.05 0.19 Q17 1 0.1177 0.3304 0.3889 11.00000 0.05 0.19 Q18 1 0.2634 0.0098 0.1815 11.00000 0.05 0.19 Q19 1 0.3180 0.5985 0.4284 11.00000 0.05 0.19 Q20 1 0.1848 -0.1525 0.1134 11.00000 0.05 0.18 ; loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.26906(2) 0.08291(2) 0.234320(14) 0.02278(6) Uani 1 1 d . . . Li1 Li 0.5179(2) -0.1572(2) 0.23363(14) 0.0299(6) Uani 1 1 d . . . N1 N 0.14188(11) 0.19388(11) 0.32971(7) 0.0261(3) Uani 1 1 d . . . N2 N 0.07532(11) 0.02208(11) 0.24618(7) 0.0265(3) Uani 1 1 d . . . N3 N 0.28021(12) -0.05125(11) 0.13990(7) 0.0267(3) Uani 1 1 d . . . N4 N 0.23346(11) 0.22541(11) 0.15174(7) 0.0257(3) Uani 1 1 d . . . N5 N 0.42405(11) 0.18046(10) 0.21828(7) 0.0244(3) Uani 1 1 d . . . N6 N 0.63608(11) -0.03626(11) 0.16322(7) 0.0286(3) Uani 1 1 d . . . N7 N 0.62003(12) -0.14283(11) 0.32534(7) 0.0302(3) Uani 1 1 d . . . N8 N 0.39485(11) -0.01506(11) 0.28980(6) 0.0238(3) Uani 1 1 d . . . N9 N 0.36223(11) -0.25879(11) 0.25846(7) 0.0245(3) Uani 1 1 d . . . C1 C 0.17666(16) 0.28664(14) 0.36913(9) 0.0311(4) Uani 1 1 d . . . H1 H 0.2623(16) 0.3042(15) 0.3495(9) 0.037(4) Uiso 1 1 d . . . C2 C 0.09602(18) 0.35159(15) 0.43131(9) 0.0384(4) Uani 1 1 d . . . H2 H 0.1274(16) 0.4168(15) 0.4537(9) 0.040(5) Uiso 1 1 d . . . C3 C -0.03055(18) 0.32036(15) 0.45528(9) 0.0425(5) Uani 1 1 d . . . H3 H -0.0853(16) 0.3642(15) 0.4973(10) 0.041(5) Uiso 1 1 d . . . C4 C -0.07079(17) 0.22922(15) 0.41599(9) 0.0382(4) Uani 1 1 d . . . H4 H -0.1575(16) 0.2098(15) 0.4304(10) 0.042(5) Uiso 1 1 d . . . C5 C 0.01548(15) 0.16567(14) 0.35058(9) 0.0297(4) Uani 1 1 d . . . C6 C -0.01877(15) 0.07443(15) 0.30506(9) 0.0323(4) Uani 1 1 d . . . H6 H -0.1019(15) 0.0482(14) 0.3170(9) 0.034(4) Uiso 1 1 d . . . C7 C 0.06351(15) -0.07118(14) 0.20010(9) 0.0308(4) Uani 1 1 d . . . H7 H -0.0129(15) -0.1100(15) 0.2082(9) 0.037(4) Uiso 1 1 d . . . C8 C 0.17524(15) -0.11490(13) 0.14265(8) 0.0284(3) Uani 1 1 d . . . C9 C 0.18387(18) -0.21679(15) 0.09069(9) 0.0383(4) Uani 1 1 d . . . H9 H 0.1127(15) -0.2617(15) 0.0966(9) 0.036(4) Uiso 1 1 d . . . C10 C 0.29638(19) -0.25029(15) 0.03686(9) 0.0436(5) Uani 1 1 d . . . H10 H 0.3029(16) -0.3185(16) -0.0006(10) 0.047(5) Uiso 1 1 d . . . C11 C 0.40113(18) -0.18286(16) 0.03223(9) 0.0415(4) Uani 1 1 d . . . H11 H 0.4822(17) -0.1997(16) -0.0071(10) 0.051(5) Uiso 1 1 d . . . C12 C 0.38792(15) -0.08432(15) 0.08426(9) 0.0328(4) Uani 1 1 d . . . H12 H 0.4538(13) -0.0360(13) 0.0841(8) 0.021(4) Uiso 1 1 d . . . C13 C 0.12887(15) 0.24377(15) 0.11633(9) 0.0325(4) Uani 1 1 d . . . H13 H 0.0627(16) 0.1890(15) 0.1351(9) 0.041(5) Uiso 1 1 d . . . C14 C 0.11056(17) 0.33411(16) 0.06144(10) 0.0384(4) Uani 1 1 d . . . H14 H 0.0330(16) 0.3437(15) 0.0415(10) 0.043(5) Uiso 1 1 d . . . C15 C 0.20532(17) 0.41864(15) 0.04050(9) 0.0379(4) Uani 1 1 d . . . H15 H 0.1945(16) 0.4826(16) 0.0033(10) 0.043(5) Uiso 1 1 d . . . C16 C 0.30992(16) 0.40587(14) 0.07500(9) 0.0336(4) Uani 1 1 d . . . H16 H 0.3759(15) 0.4578(14) 0.0623(9) 0.033(4) Uiso 1 1 d . . . C17 C 0.32803(14) 0.30852(13) 0.13101(8) 0.0263(3) Uani 1 1 d . . . C18 C 0.43115(14) 0.28292(13) 0.16841(8) 0.0271(3) Uani 1 1 d . . . H18 H 0.5056(15) 0.3309(14) 0.1597(9) 0.034(4) Uiso 1 1 d . . . C19 C 0.53562(14) 0.13903(13) 0.25538(8) 0.0259(3) Uani 1 1 d . . . H19 H 0.5676(13) 0.2133(13) 0.2782(8) 0.024(4) Uiso 1 1 d . . . C20 C 0.64718(13) 0.07669(13) 0.19226(8) 0.0258(3) Uani 1 1 d . . . C21 C 0.75177(14) 0.14123(15) 0.16092(9) 0.0313(4) Uani 1 1 d . . . H21 H 0.7554(14) 0.2196(14) 0.1844(8) 0.025(4) Uiso 1 1 d . . . C22 C 0.84250(15) 0.09230(16) 0.09630(10) 0.0372(4) Uani 1 1 d . . . H22 H 0.9120(15) 0.1372(15) 0.0720(9) 0.037(4) Uiso 1 1 d . . . C23 C 0.82908(15) -0.02086(16) 0.06518(9) 0.0363(4) Uani 1 1 d . . . H23 H 0.8842(16) -0.0574(15) 0.0195(10) 0.044(5) Uiso 1 1 d . . . C24 C 0.72673(15) -0.08179(15) 0.10028(9) 0.0329(4) Uani 1 1 d . . . H24 H 0.7145(15) -0.1635(15) 0.0816(9) 0.038(4) Uiso 1 1 d . . . C25 C 0.47936(14) 0.05430(13) 0.32464(8) 0.0254(3) Uani 1 1 d . . . H25 H 0.4278(12) 0.1109(12) 0.3698(8) 0.018(3) Uiso 1 1 d . . . C26 C 0.58194(13) -0.02861(14) 0.35850(8) 0.0261(3) Uani 1 1 d . . . C27 C 0.63508(15) 0.01146(15) 0.41944(9) 0.0317(4) Uani 1 1 d . . . H27 H 0.6085(13) 0.0848(13) 0.4388(8) 0.024(4) Uiso 1 1 d . . . C28 C 0.73191(15) -0.06695(17) 0.44617(9) 0.0394(4) Uani 1 1 d . . . H28 H 0.7667(17) -0.0428(16) 0.4853(10) 0.050(5) Uiso 1 1 d . . . C29 C 0.77276(16) -0.18177(17) 0.41112(10) 0.0388(4) Uani 1 1 d . . . H29 H 0.8363(16) -0.2378(15) 0.4293(10) 0.042(5) Uiso 1 1 d . . . C30 C 0.71451(16) -0.21687(16) 0.35160(10) 0.0364(4) Uani 1 1 d . . . H30 H 0.7393(16) -0.2972(16) 0.3292(10) 0.043(5) Uiso 1 1 d . . . C31 C 0.28807(14) -0.06740(13) 0.33248(8) 0.0246(3) Uani 1 1 d . . . H31 H 0.2393(13) -0.0314(13) 0.3815(8) 0.025(4) Uiso 1 1 d . . . C32 C 0.26780(13) -0.19031(13) 0.31275(8) 0.0232(3) Uani 1 1 d . . . C33 C 0.15033(15) -0.23841(14) 0.34476(9) 0.0292(4) Uani 1 1 d . . . H33 H 0.0875(15) -0.1903(14) 0.3805(9) 0.034(4) Uiso 1 1 d . . . C34 C 0.12933(15) -0.35391(14) 0.32161(9) 0.0325(4) Uani 1 1 d . . . H34 H 0.0512(16) -0.3867(15) 0.3410(9) 0.040(5) Uiso 1 1 d . . . C35 C 0.22459(15) -0.42300(14) 0.26583(9) 0.0303(4) Uani 1 1 d . . . H35 H 0.2147(13) -0.5031(14) 0.2466(8) 0.025(4) Uiso 1 1 d . . . C36 C 0.33670(14) -0.37073(13) 0.23642(8) 0.0276(3) Uani 1 1 d . . . H36 H 0.4032(14) -0.4146(13) 0.1977(8) 0.025(4) Uiso 1 1 d . . . C1S C 0.82780(17) -0.41001(18) 0.16181(10) 0.0445(5) Uani 1 1 d . . . H1S H 0.8533(18) -0.3556(18) 0.1184(11) 0.061(6) Uiso 1 1 d . . . C2S C 0.69855(17) -0.42832(18) 0.18640(10) 0.0443(5) Uani 1 1 d . . . H2S H 0.6335(17) -0.3895(16) 0.1571(10) 0.050(5) Uiso 1 1 d . . . C3S C 0.66100(17) -0.50125(17) 0.25259(11) 0.0439(5) Uani 1 1 d . . . H3S H 0.5722(18) -0.5136(17) 0.2694(11) 0.055(5) Uiso 1 1 d . . . C4S C 0.75370(18) -0.55713(16) 0.29286(11) 0.0443(5) Uani 1 1 d . . . H4S H 0.7269(18) -0.6069(17) 0.3392(11) 0.057(6) Uiso 1 1 d . . . C5S C 0.88298(17) -0.54078(16) 0.26751(11) 0.0441(4) Uani 1 1 d . . . H5S H 0.9458(17) -0.5784(16) 0.2959(10) 0.048(5) Uiso 1 1 d . . . C6S C 0.91979(17) -0.46706(18) 0.20248(11) 0.0444(5) Uani 1 1 d . . . H6S H 1.0076(17) -0.4546(16) 0.1853(10) 0.045(5) Uiso 1 1 d . . . C7S C 0.4687(2) 0.6155(2) 0.46774(13) 0.0604(6) Uani 1 1 d . . . H7S H 0.4460(18) 0.6935(19) 0.4453(12) 0.063(6) Uiso 1 1 d . . . C8S C 0.41809(19) 0.5130(2) 0.44659(12) 0.0595(6) Uani 1 1 d . . . H8S H 0.3651(19) 0.5218(18) 0.4094(11) 0.059(6) Uiso 1 1 d . . . C9S C 0.4496(2) 0.3977(2) 0.47884(13) 0.0645(6) Uani 1 1 d . . . H9S H 0.419(2) 0.328(2) 0.4639(13) 0.082(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.02388(13) 0.02196(13) 0.02224(12) -0.00183(10) -0.00401(10) -0.00247(10) Li1 0.0305(13) 0.0281(13) 0.0311(12) -0.0033(10) -0.0051(10) -0.0050(11) N1 0.0300(6) 0.0220(6) 0.0250(6) 0.0013(5) -0.0044(5) 0.0003(5) N2 0.0280(6) 0.0260(6) 0.0261(6) 0.0035(5) -0.0068(5) -0.0039(5) N3 0.0327(6) 0.0241(6) 0.0238(6) 0.0012(5) -0.0086(5) -0.0013(5) N4 0.0282(6) 0.0233(6) 0.0252(6) -0.0020(5) -0.0043(5) -0.0029(5) N5 0.0251(6) 0.0217(6) 0.0264(6) -0.0013(5) -0.0045(5) -0.0029(5) N6 0.0269(6) 0.0295(7) 0.0285(6) -0.0010(5) -0.0039(5) -0.0020(5) N7 0.0306(6) 0.0303(7) 0.0304(6) 0.0016(5) -0.0092(5) -0.0020(5) N8 0.0251(6) 0.0238(6) 0.0233(6) -0.0010(5) -0.0053(5) -0.0054(5) N9 0.0275(6) 0.0224(6) 0.0241(6) 0.0004(5) -0.0075(5) -0.0015(5) C1 0.0411(9) 0.0235(7) 0.0288(7) 0.0005(6) -0.0099(7) 0.0004(7) C2 0.0606(11) 0.0245(8) 0.0288(8) -0.0018(6) -0.0115(8) 0.0044(8) C3 0.0575(11) 0.0321(9) 0.0274(8) 0.0005(7) 0.0052(8) 0.0130(8) C4 0.0387(9) 0.0349(9) 0.0333(8) 0.0059(7) 0.0055(7) 0.0038(7) C5 0.0313(8) 0.0273(8) 0.0274(7) 0.0051(6) -0.0017(6) 0.0008(6) C6 0.0257(7) 0.0347(8) 0.0353(8) 0.0055(7) -0.0029(6) -0.0054(7) C7 0.0346(8) 0.0290(8) 0.0337(8) 0.0058(6) -0.0143(6) -0.0123(7) C8 0.0389(8) 0.0242(7) 0.0249(7) 0.0039(6) -0.0130(6) -0.0046(6) C9 0.0601(10) 0.0277(8) 0.0332(8) 0.0023(7) -0.0205(8) -0.0116(8) C10 0.0754(12) 0.0286(8) 0.0291(8) -0.0061(7) -0.0191(8) -0.0002(9) C11 0.0525(10) 0.0413(10) 0.0272(8) -0.0073(7) -0.0075(8) 0.0089(8) C12 0.0337(8) 0.0378(9) 0.0264(7) -0.0029(7) -0.0077(6) 0.0008(7) C13 0.0343(8) 0.0323(8) 0.0327(8) 0.0001(7) -0.0102(7) -0.0051(7) C14 0.0425(9) 0.0374(9) 0.0390(9) 0.0043(7) -0.0189(7) -0.0025(8) C15 0.0543(10) 0.0295(8) 0.0315(8) 0.0048(7) -0.0146(7) -0.0026(8) C16 0.0429(9) 0.0241(8) 0.0335(8) 0.0008(6) -0.0065(7) -0.0054(7) C17 0.0326(8) 0.0211(7) 0.0235(7) -0.0037(6) -0.0028(6) -0.0006(6) C18 0.0282(7) 0.0218(7) 0.0298(7) -0.0018(6) -0.0016(6) -0.0045(6) C19 0.0273(7) 0.0250(7) 0.0269(7) -0.0019(6) -0.0064(6) -0.0064(6) C20 0.0244(7) 0.0281(7) 0.0261(7) 0.0034(6) -0.0088(6) -0.0028(6) C21 0.0274(7) 0.0346(8) 0.0341(8) 0.0004(7) -0.0097(6) -0.0074(7) C22 0.0233(7) 0.0503(10) 0.0378(9) 0.0059(8) -0.0034(7) -0.0088(7) C23 0.0274(8) 0.0443(10) 0.0335(8) -0.0006(7) -0.0017(7) 0.0024(7) C24 0.0305(8) 0.0311(8) 0.0347(8) -0.0014(7) -0.0043(7) 0.0018(7) C25 0.0270(7) 0.0260(7) 0.0233(7) -0.0036(6) -0.0050(6) -0.0033(6) C26 0.0241(7) 0.0315(8) 0.0224(7) 0.0007(6) -0.0015(6) -0.0077(6) C27 0.0291(8) 0.0388(9) 0.0271(7) -0.0048(7) -0.0030(6) -0.0081(7) C28 0.0341(8) 0.0642(11) 0.0246(7) 0.0033(8) -0.0119(7) -0.0154(8) C29 0.0325(8) 0.0479(10) 0.0376(9) 0.0132(8) -0.0128(7) -0.0045(8) C30 0.0370(8) 0.0339(9) 0.0387(9) 0.0045(7) -0.0112(7) -0.0013(7) C31 0.0260(7) 0.0265(7) 0.0207(7) -0.0011(6) -0.0038(6) -0.0026(6) C32 0.0272(7) 0.0231(7) 0.0200(6) 0.0039(5) -0.0081(5) -0.0016(6) C33 0.0298(8) 0.0285(8) 0.0278(7) 0.0014(6) -0.0029(6) -0.0026(6) C34 0.0319(8) 0.0311(8) 0.0354(8) 0.0051(7) -0.0062(7) -0.0092(7) C35 0.0371(8) 0.0213(7) 0.0353(8) 0.0002(6) -0.0123(7) -0.0060(6) C36 0.0298(7) 0.0241(7) 0.0294(7) -0.0017(6) -0.0094(6) 0.0011(6) C1S 0.0426(10) 0.0541(11) 0.0353(9) 0.0034(8) -0.0068(8) -0.0020(9) C2S 0.0383(9) 0.0539(11) 0.0421(9) -0.0014(8) -0.0170(8) 0.0029(8) C3S 0.0370(9) 0.0454(10) 0.0514(10) -0.0012(8) -0.0125(8) -0.0068(8) C4S 0.0506(10) 0.0347(9) 0.0512(10) 0.0066(8) -0.0174(8) -0.0088(8) C5S 0.0460(10) 0.0373(9) 0.0530(10) 0.0027(8) -0.0236(8) 0.0015(8) C6S 0.0339(9) 0.0516(11) 0.0474(10) -0.0035(8) -0.0100(8) -0.0010(8) C7S 0.0577(12) 0.0662(13) 0.0569(12) 0.0197(10) -0.0079(10) -0.0151(11) C8S 0.0489(11) 0.0906(16) 0.0435(10) 0.0075(11) -0.0136(9) -0.0204(11) C9S 0.0678(13) 0.0720(14) 0.0602(13) 0.0006(11) -0.0127(11) -0.0335(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 N8 1.9722(12) . ? Ti1 N5 2.0231(12) . ? Ti1 N4 2.1120(12) . ? Ti1 N3 2.1678(12) . ? Ti1 N1 2.1693(11) . ? Ti1 N2 2.1956(12) . ? Ti1 C31 2.3260(14) . ? Ti1 Li1 3.445(2) . ? Li1 N8 2.005(3) . ? Li1 N9 2.056(3) . ? Li1 N7 2.095(3) . ? Li1 N6 2.106(3) . ? Li1 C25 2.728(3) . ? Li1 C31 2.744(3) . ? Li1 C32 2.778(3) . ? N1 C1 1.3447(19) . ? N1 C5 1.3812(19) . ? N2 C7 1.3234(19) . ? N2 C6 1.3437(18) . ? N3 C12 1.3447(18) . ? N3 C8 1.3668(19) . ? N4 C13 1.3553(19) . ? N4 C17 1.4105(18) . ? N5 C18 1.3789(18) . ? N5 C19 1.4656(18) . ? N6 C24 1.3460(18) . ? N6 C20 1.3503(18) . ? N7 C30 1.341(2) . ? N7 C26 1.3453(18) . ? N8 C31 1.3903(17) . ? N8 C25 1.4528(18) . ? N9 C36 1.3444(18) . ? N9 C32 1.3700(17) . ? C1 C2 1.367(2) . ? C2 C3 1.398(3) . ? C3 C4 1.358(3) . ? C4 C5 1.422(2) . ? C5 C6 1.392(2) . ? C7 C8 1.414(2) . ? C8 C9 1.410(2) . ? C9 C10 1.364(2) . ? C10 C11 1.385(3) . ? C11 C12 1.376(2) . ? C13 C14 1.360(2) . ? C14 C15 1.423(2) . ? C15 C16 1.345(2) . ? C16 C17 1.425(2) . ? C17 C18 1.367(2) . ? C19 C20 1.5269(19) . ? C19 C25 1.5472(19) . ? C20 C21 1.388(2) . ? C21 C22 1.377(2) . ? C22 C23 1.374(2) . ? C23 C24 1.363(2) . ? C25 C26 1.514(2) . ? C26 C27 1.381(2) . ? C27 C28 1.386(2) . ? C28 C29 1.367(2) . ? C29 C30 1.374(2) . ? C31 C32 1.424(2) . ? C32 C33 1.408(2) . ? C33 C34 1.370(2) . ? C34 C35 1.392(2) . ? C35 C36 1.373(2) . ? C1S C6S 1.382(3) . ? C1S C2S 1.383(2) . ? C2S C3S 1.384(3) . ? C3S C4S 1.379(3) . ? C4S C5S 1.380(3) . ? C5S C6S 1.372(3) . ? C7S C8S 1.370(3) . ? C7S C9S 1.372(3) 2_666 ? C8S C9S 1.375(3) . ? C9S C7S 1.372(3) 2_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Ti1 N5 74.94(5) . . ? N8 Ti1 N4 148.08(5) . . ? N5 Ti1 N4 74.29(5) . . ? N8 Ti1 N3 96.95(5) . . ? N5 Ti1 N3 113.15(5) . . ? N4 Ti1 N3 87.47(4) . . ? N8 Ti1 N1 102.80(5) . . ? N5 Ti1 N1 98.99(5) . . ? N4 Ti1 N1 90.18(4) . . ? N3 Ti1 N1 145.73(5) . . ? N8 Ti1 N2 117.99(5) . . ? N5 Ti1 N2 165.87(5) . . ? N4 Ti1 N2 93.56(5) . . ? N3 Ti1 N2 72.63(4) . . ? N1 Ti1 N2 73.41(4) . . ? N8 Ti1 C31 36.59(5) . . ? N5 Ti1 C31 109.12(5) . . ? N4 Ti1 C31 174.39(5) . . ? N3 Ti1 C31 95.07(5) . . ? N1 Ti1 C31 84.90(5) . . ? N2 Ti1 C31 82.46(5) . . ? N8 Ti1 Li1 30.26(5) . . ? N5 Ti1 Li1 79.40(5) . . ? N4 Ti1 Li1 133.03(5) . . ? N3 Ti1 Li1 68.12(5) . . ? N1 Ti1 Li1 132.38(5) . . ? N2 Ti1 Li1 114.59(5) . . ? C31 Ti1 Li1 52.55(5) . . ? N8 Li1 N9 85.79(10) . . ? N8 Li1 N7 84.76(10) . . ? N9 Li1 N7 116.45(12) . . ? N8 Li1 N6 93.07(11) . . ? N9 Li1 N6 153.60(14) . . ? N7 Li1 N6 89.64(11) . . ? N8 Li1 C25 31.25(6) . . ? N9 Li1 C25 112.33(10) . . ? N7 Li1 C25 58.85(7) . . ? N6 Li1 C25 76.61(9) . . ? N8 Li1 C31 29.07(6) . . ? N9 Li1 C31 57.97(7) . . ? N7 Li1 C31 90.85(9) . . ? N6 Li1 C31 121.58(11) . . ? C25 Li1 C31 54.88(6) . . ? N8 Li1 C32 58.36(7) . . ? N9 Li1 C32 28.19(5) . . ? N7 Li1 C32 104.16(10) . . ? N6 Li1 C32 146.03(12) . . ? C25 Li1 C32 84.21(8) . . ? C31 Li1 C32 29.87(5) . . ? N8 Li1 Ti1 29.72(5) . . ? N9 Li1 Ti1 80.80(8) . . ? N7 Li1 Ti1 113.30(9) . . ? N6 Li1 Ti1 85.21(8) . . ? C25 Li1 Ti1 55.31(5) . . ? C31 Li1 Ti1 42.29(4) . . ? C32 Li1 Ti1 60.84(5) . . ? C1 N1 C5 118.41(12) . . ? C1 N1 Ti1 125.20(10) . . ? C5 N1 Ti1 116.39(9) . . ? C7 N2 C6 125.07(13) . . ? C7 N2 Ti1 117.57(9) . . ? C6 N2 Ti1 117.03(10) . . ? C12 N3 C8 118.39(12) . . ? C12 N3 Ti1 124.02(10) . . ? C8 N3 Ti1 117.23(9) . . ? C13 N4 C17 117.00(12) . . ? C13 N4 Ti1 126.11(10) . . ? C17 N4 Ti1 116.89(9) . . ? C18 N5 C19 118.19(12) . . ? C18 N5 Ti1 121.00(10) . . ? C19 N5 Ti1 120.69(9) . . ? C24 N6 C20 117.73(13) . . ? C24 N6 Li1 120.02(12) . . ? C20 N6 Li1 119.78(11) . . ? C30 N7 C26 118.13(13) . . ? C30 N7 Li1 134.19(12) . . ? C26 N7 Li1 107.52(11) . . ? C31 N8 C25 124.99(11) . . ? C31 N8 Ti1 85.69(8) . . ? C25 N8 Ti1 117.10(9) . . ? C31 N8 Li1 106.46(11) . . ? C25 N8 Li1 103.04(11) . . ? Ti1 N8 Li1 120.03(9) . . ? C36 N9 C32 117.48(12) . . ? C36 N9 Li1 135.82(11) . . ? C32 N9 Li1 106.67(11) . . ? N1 C1 C2 123.96(15) . . ? C1 C2 C3 118.20(16) . . ? C4 C3 C2 119.84(15) . . ? C3 C4 C5 120.14(16) . . ? N1 C5 C6 116.57(13) . . ? N1 C5 C4 119.34(14) . . ? C6 C5 C4 124.09(15) . . ? N2 C6 C5 116.44(14) . . ? N2 C7 C8 116.30(13) . . ? N3 C8 C9 119.98(13) . . ? N3 C8 C7 115.25(13) . . ? C9 C8 C7 124.77(15) . . ? C10 C9 C8 119.87(16) . . ? C9 C10 C11 120.06(15) . . ? C12 C11 C10 117.84(15) . . ? N3 C12 C11 123.76(16) . . ? N4 C13 C14 124.77(15) . . ? C13 C14 C15 118.51(15) . . ? C16 C15 C14 119.07(15) . . ? C15 C16 C17 121.18(15) . . ? C18 C17 N4 113.48(13) . . ? C18 C17 C16 127.08(14) . . ? N4 C17 C16 119.43(13) . . ? C17 C18 N5 114.32(13) . . ? N5 C19 C20 109.08(11) . . ? N5 C19 C25 103.71(11) . . ? C20 C19 C25 116.20(11) . . ? N6 C20 C21 121.31(12) . . ? N6 C20 C19 118.71(12) . . ? C21 C20 C19 119.73(13) . . ? C22 C21 C20 119.42(15) . . ? C23 C22 C21 119.24(15) . . ? C24 C23 C22 118.59(14) . . ? N6 C24 C23 123.63(15) . . ? N8 C25 C26 113.63(11) . . ? N8 C25 C19 103.12(11) . . ? C26 C25 C19 113.97(11) . . ? N8 C25 Li1 45.71(8) . . ? C26 C25 Li1 77.12(9) . . ? C19 C25 Li1 94.86(9) . . ? N7 C26 C27 121.69(14) . . ? N7 C26 C25 116.49(12) . . ? C27 C26 C25 121.81(13) . . ? C26 C27 C28 119.24(15) . . ? C29 C28 C27 119.02(15) . . ? C28 C29 C30 118.89(15) . . ? N7 C30 C29 123.00(15) . . ? N8 C31 C32 119.25(12) . . ? N8 C31 Ti1 57.73(7) . . ? C32 C31 Ti1 115.21(9) . . ? N8 C31 Li1 44.47(8) . . ? C32 C31 Li1 76.39(9) . . ? Ti1 C31 Li1 85.17(7) . . ? N9 C32 C33 120.32(13) . . ? N9 C32 C31 118.64(12) . . ? C33 C32 C31 120.95(12) . . ? N9 C32 Li1 45.14(8) . . ? C33 C32 Li1 165.25(11) . . ? C31 C32 Li1 73.74(9) . . ? C34 C33 C32 120.23(13) . . ? C33 C34 C35 119.51(14) . . ? C36 C35 C34 117.53(14) . . ? N9 C36 C35 124.91(13) . . ? C6S C1S C2S 119.80(17) . . ? C1S C2S C3S 120.12(17) . . ? C4S C3S C2S 119.47(17) . . ? C3S C4S C5S 120.44(17) . . ? C6S C5S C4S 120.00(17) . . ? C5S C6S C1S 120.15(17) . . ? C8S C7S C9S 119.7(2) . 2_666 ? C7S C8S C9S 119.9(2) . . ? C7S C9S C8S 120.5(2) 2_666 . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.238 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.047