# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Swartz, Douglas' 'Staples, Richard' 'Odom, Aaron' _publ_contact_author_name 'Odom, Aaron' _publ_contact_author_email odom@chemistry.msu.edu _publ_section_title ; Synthesis and Hydroamination Catalysis with 3-Aryl Substituted Pyrrolyl and Dipyrrolylmethane Titanium(IV) Complexes ; _journal_name_full 'Private Communication' _journal_page_first ? _journal_page_last ? _journal_volume ? _journal_year 2011 # Attachment '- structures.cif' data_00108 _database_code_depnum_ccdc_archive 'CCDC 809525' #TrackingRef '- structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C33 H35 F12 N5 Ti, C7 H8' _chemical_formula_sum 'C40 H43 F12 N5 Ti' _chemical_melting_point ? _exptl_crystal_description plate _exptl_crystal_colour orange _diffrn_ambient_temperature 173(2) _chemical_formula_weight 869.69 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab ' _symmetry_int_tables_number 60 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 18.861(4) _cell_length_b 23.944(6) _cell_length_c 18.076(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8163(3) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6888 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.17 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3584 _exptl_absorpt_coefficient_mu 0.300 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.759214 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; Data was collected using a BRUKER SMART CCD (charge coupled device) based diffractometer equipped with an Oxford Cryostream low-temperature apparatus operating at 173 K. A suitable crystal was chosen and mounted on a glass fiber using grease. Ratio Observed / Unique Reflections is Low at 47 Percent. Data were measured using omega scans of 0.3\% per frame for 30 s , such that a hemisphere was collected. A total of 1818 frames were collected with a final resolution of 0.83 \%A. Cell parameters were retrieved using SMART software and refined using SAINT on all observed reflections. Data reduction was performed using the SAINT software which corrects for Lp and decay. Absorption corrections were applied using SADABS based on Blessing, (1995). The structures are solved by the direct method using the SHELX-90 program and refined by least squares method on F2 SHELXL-93, incorporated in SHELXTL V5.1. Disorder modelled. All H atoms were placed in calculated positions and refined using a riding model. C-H(aromatic) = 0.94 \%A and Uiso(H) = 1.2Ueq(C) C-H (alaphatic) = 0.99 \%A and Uiso(H) = 1.2Ueq(C) CH2 = 0.98 \%A and Uiso(H) = 1.2Ueq(C) CH3 = 0.97\%A and Uiso(H) = 1.5Ueq(C) N-H = 0.86 (0.92)\%A and Uiso(H) = 1.2 Ueq(N) O-H(alcohol) = 0.85\%Aand Uiso(H) = 1.2Ueq(O) O-H(acid) = 0.82\%A and Uiso(H) = 1.5Ueq(O) ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_reflns_number 52492 _diffrn_reflns_av_R_equivalents 0.1455 _diffrn_reflns_av_sigmaI/netI 0.0930 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7198 _reflns_number_gt 3373 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'ASTRO (BRUKER, V5.007, 1997)' _computing_cell_refinement 'SMART (BRUKER, V5.625, 2001)' _computing_data_reduction 'SAINT (BRUKER, V7.56A, 2008)' _computing_structure_solution 'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)' _computing_structure_refinement 'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)' _computing_molecular_graphics 'SHELXTL (Sheldrick, Acta Cryst. A64 2008, 112-122)' _computing_publication_material 'SHELXTL (Sheldrick, Acta Cryst. A64 2008, 112-122)' _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^)+(0.1226P)^2^+34.9044P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7198 _refine_ls_number_parameters 581 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1911 _refine_ls_R_factor_gt 0.0922 _refine_ls_wR_factor_ref 0.3095 _refine_ls_wR_factor_gt 0.2256 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.24858(7) 0.20976(5) 0.93772(7) 0.0483(4) Uani 1 1 d . . . N1A N 0.3308(12) 0.2619(9) 0.9176(12) 0.076(3) Uani 0.359(7) 1 d PD A 2 N1 N 0.3036(6) 0.2774(5) 0.9604(7) 0.076(3) Uani 0.641(7) 1 d PD A 1 N2 N 0.2739(6) 0.1849(5) 0.8463(6) 0.053(3) Uani 0.641(7) 1 d PD A 1 N2A N 0.2352(11) 0.1818(12) 0.8381(13) 0.053(3) Uani 0.359(7) 1 d PD A 2 N3 N 0.1617(5) 0.2653(3) 0.9127(6) 0.108(3) Uani 1 1 d . A . H3 H 0.1333 0.2420 0.8842 0.130 Uiso 1 1 calc R . . N4 N 0.1717(3) 0.1618(3) 0.9880(3) 0.0516(16) Uani 1 1 d . A . N5 N 0.3150(3) 0.1600(2) 1.0001(3) 0.0472(15) Uani 1 1 d . A . C1 C 0.2347(3) 0.1476(3) 1.1086(3) 0.0432(17) Uani 1 1 d . A . C2 C 0.2283(4) 0.1099(4) 1.1772(4) 0.058(2) Uani 1 1 d . . . H2A H 0.2281 0.0706 1.1618 0.088 Uiso 1 1 calc R . . H2B H 0.1840 0.1183 1.2033 0.088 Uiso 1 1 calc R . . H2C H 0.2685 0.1166 1.2103 0.088 Uiso 1 1 calc R . . C3 C 0.2334(4) 0.2083(4) 1.1349(5) 0.071(3) Uani 1 1 d . . . H3A H 0.2747 0.2154 1.1663 0.107 Uiso 1 1 calc R . . H3B H 0.1899 0.2151 1.1631 0.107 Uiso 1 1 calc R . . H3C H 0.2347 0.2332 1.0919 0.107 Uiso 1 1 calc R . . C11A C 0.376(2) 0.2811(15) 0.9765(17) 0.133(7) Uani 0.359(7) 1 d PD A 2 H11A H 0.4162 0.3014 0.9557 0.199 Uiso 0.359(7) 1 calc PR A 2 H11B H 0.3930 0.2490 1.0050 0.199 Uiso 0.359(7) 1 calc PR A 2 H11C H 0.3487 0.3060 1.0091 0.199 Uiso 0.359(7) 1 calc PR A 2 C11 C 0.2872(10) 0.3242(6) 1.0079(10) 0.133(7) Uani 0.641(7) 1 d PD A 1 H11D H 0.3138 0.3206 1.0543 0.199 Uiso 0.641(7) 1 calc PR A 1 H11E H 0.2363 0.3245 1.0185 0.199 Uiso 0.641(7) 1 calc PR A 1 H11F H 0.3006 0.3590 0.9831 0.199 Uiso 0.641(7) 1 calc PR A 1 C12A C 0.3404(16) 0.2962(14) 0.8531(14) 0.117(6) Uani 0.359(7) 1 d PD A 2 H12A H 0.3876 0.3134 0.8544 0.176 Uiso 0.359(7) 1 calc PR A 2 H12B H 0.3042 0.3256 0.8523 0.176 Uiso 0.359(7) 1 calc PR A 2 H12C H 0.3360 0.2732 0.8085 0.176 Uiso 0.359(7) 1 calc PR A 2 C12 C 0.3749(9) 0.2823(9) 0.9329(12) 0.117(6) Uani 0.641(7) 1 d PD A 1 H12D H 0.3828 0.3203 0.9146 0.176 Uiso 0.641(7) 1 calc PR A 1 H12E H 0.3820 0.2556 0.8925 0.176 Uiso 0.641(7) 1 calc PR A 1 H12F H 0.4084 0.2742 0.9729 0.176 Uiso 0.641(7) 1 calc PR A 1 C21 C 0.3181(10) 0.2077(7) 0.7875(8) 0.120(6) Uani 0.641(7) 1 d PD A 1 H21A H 0.3620 0.1859 0.7838 0.179 Uiso 0.641(7) 1 calc PR A 1 H21B H 0.3297 0.2467 0.7987 0.179 Uiso 0.641(7) 1 calc PR A 1 H21C H 0.2925 0.2058 0.7404 0.179 Uiso 0.641(7) 1 calc PR A 1 C21A C 0.1901(16) 0.1964(13) 0.7761(13) 0.120(6) Uani 0.359(7) 1 d PD A 2 H21D H 0.2195 0.2031 0.7322 0.179 Uiso 0.359(7) 1 calc PR A 2 H21E H 0.1633 0.2303 0.7879 0.179 Uiso 0.359(7) 1 calc PR A 2 H21F H 0.1571 0.1657 0.7662 0.179 Uiso 0.359(7) 1 calc PR A 2 C22 C 0.2502(15) 0.1305(8) 0.8206(14) 0.097(11) Uani 0.641(7) 1 d PD A 1 H22A H 0.2311 0.1339 0.7704 0.146 Uiso 0.641(7) 1 calc PR A 1 H22B H 0.2131 0.1164 0.8538 0.146 Uiso 0.641(7) 1 calc PR A 1 H22C H 0.2903 0.1045 0.8205 0.146 Uiso 0.641(7) 1 calc PR A 1 C22A C 0.262(3) 0.1285(15) 0.831(3) 0.086(18) Uani 0.359(7) 1 d PD A 2 H22D H 0.2232 0.1019 0.8259 0.130 Uiso 0.359(7) 1 calc PR A 2 H22E H 0.2899 0.1192 0.8755 0.130 Uiso 0.359(7) 1 calc PR A 2 H22F H 0.2929 0.1266 0.7875 0.130 Uiso 0.359(7) 1 calc PR A 2 C31 C 0.1735(8) 0.3104(6) 0.8613(10) 0.175(7) Uani 1 1 d . . . H31A H 0.1279 0.3264 0.8464 0.263 Uiso 1 1 calc R A . H31B H 0.1983 0.2962 0.8175 0.263 Uiso 1 1 calc R . . H31C H 0.2025 0.3393 0.8850 0.263 Uiso 1 1 calc R . . C32 C 0.1105(7) 0.2855(6) 0.9656(9) 0.163(7) Uani 1 1 d . . . H32A H 0.1318 0.3153 0.9954 0.244 Uiso 1 1 calc R A . H32B H 0.0960 0.2547 0.9980 0.244 Uiso 1 1 calc R . . H32C H 0.0690 0.3001 0.9394 0.244 Uiso 1 1 calc R . . C41 C 0.1719(3) 0.1381(3) 1.0583(4) 0.0422(16) Uani 1 1 d . . . C42 C 0.1112(4) 0.1080(3) 1.0687(4) 0.0434(17) Uani 1 1 d . A . H42 H 0.0984 0.0883 1.1122 0.052 Uiso 1 1 calc R . . C43 C 0.0702(3) 0.1118(3) 1.0019(4) 0.0389(16) Uani 1 1 d . . . C43' C -0.1519(4) 0.0207(4) 1.0874(4) 0.056(2) Uani 1 1 d . . . C44 C 0.1094(4) 0.1449(3) 0.9555(4) 0.055(2) Uani 1 1 d . A . H44 H 0.0952 0.1550 0.9069 0.065 Uiso 1 1 calc R . . C45' C -0.1050(4) 0.0424(4) 0.8177(4) 0.059(2) Uani 1 1 d . . . C51 C 0.3026(3) 0.1361(3) 1.0686(4) 0.0429(17) Uani 1 1 d . . . C52 C 0.3600(4) 0.1052(3) 1.0898(4) 0.0435(17) Uani 1 1 d . A . H52 H 0.3646 0.0852 1.1350 0.052 Uiso 1 1 calc R . . C53 C 0.4117(3) 0.1082(3) 1.0325(4) 0.0429(17) Uani 1 1 d . . . C53' C 0.6374(4) 0.0636(4) 0.9027(4) 0.057(2) Uani 1 1 d . . . C54 C 0.3813(4) 0.1428(3) 0.9788(4) 0.054(2) Uani 1 1 d . A . H54 H 0.4036 0.1530 0.9337 0.065 Uiso 1 1 calc R . . C55' C 0.6044(4) 0.0113(4) 1.1671(4) 0.060(2) Uani 1 1 d . . . C431 C 0.0015(3) 0.0853(3) 0.9858(3) 0.0390(15) Uani 1 1 d . A . C432 C -0.0418(4) 0.0650(3) 1.0419(4) 0.0430(17) Uani 1 1 d . . . H432 H -0.0270 0.0683 1.0919 0.052 Uiso 1 1 calc R A . C433 C -0.1069(4) 0.0396(3) 1.0257(4) 0.0441(17) Uani 1 1 d . A . C434 C -0.1284(4) 0.0336(3) 0.9534(4) 0.0465(18) Uani 1 1 d . . . H434 H -0.1724 0.0162 0.9422 0.056 Uiso 1 1 calc R A . C435 C -0.0855(4) 0.0529(3) 0.8974(4) 0.0458(17) Uani 1 1 d . A . C436 C -0.0209(4) 0.0780(3) 0.9123(4) 0.0444(17) Uani 1 1 d . . . H436 H 0.0084 0.0903 0.8727 0.053 Uiso 1 1 calc R A . C531 C 0.4828(3) 0.0837(3) 1.0320(4) 0.0429(17) Uani 1 1 d . A . C532 C 0.5255(4) 0.0837(3) 0.9693(4) 0.0441(17) Uani 1 1 d . . . H532 H 0.5079 0.0995 0.9247 0.053 Uiso 1 1 calc R A . C533 C 0.5934(4) 0.0610(3) 0.9705(4) 0.0446(17) Uani 1 1 d . A . C534 C 0.6202(4) 0.0372(3) 1.0345(4) 0.0488(18) Uani 1 1 d . . . H534 H 0.6664 0.0213 1.0353 0.059 Uiso 1 1 calc R A . C535 C 0.5787(4) 0.0370(3) 1.0967(4) 0.0467(17) Uani 1 1 d . A . C536 C 0.5106(4) 0.0591(3) 1.0961(4) 0.0462(17) Uani 1 1 d . . . H536 H 0.4825 0.0576 1.1397 0.055 Uiso 1 1 calc R A . F431 F -0.1846(4) 0.0622(2) 1.1208(4) 0.125(3) Uani 1 1 d . . . F432 F -0.2044(3) -0.0140(2) 1.0655(3) 0.0867(16) Uani 1 1 d . . . F433 F -0.1187(3) -0.0087(3) 1.1379(3) 0.0962(19) Uani 1 1 d . . . F451 F -0.0749(4) -0.0058(2) 0.7912(3) 0.0996(19) Uani 1 1 d . . . F452 F -0.0820(3) 0.0818(2) 0.7724(2) 0.0850(17) Uani 1 1 d . . . F453 F -0.1727(3) 0.0355(3) 0.8070(3) 0.0940(18) Uani 1 1 d . . . F531 F 0.6549(5) 0.1128(3) 0.8838(4) 0.161(4) Uani 1 1 d . . . F532 F 0.6953(3) 0.0352(3) 0.9052(3) 0.135(3) Uani 1 1 d . . . F533 F 0.6058(4) 0.0432(4) 0.8451(3) 0.149(3) Uani 1 1 d . . . F551 F 0.6717(3) 0.0028(3) 1.1702(3) 0.132(3) Uani 1 1 d . . . F552 F 0.5747(4) -0.0367(3) 1.1824(3) 0.116(2) Uani 1 1 d . . . F553 F 0.5894(4) 0.0421(3) 1.2265(3) 0.117(2) Uani 1 1 d . . . C1S C 0.5000 0.2980(6) 0.7500 0.080(4) Uani 1 2 d S . . C2S C 0.5266(5) 0.2683(5) 0.8112(6) 0.085(3) Uani 1 1 d . . . H2S H 0.5447 0.2880 0.8527 0.103 Uiso 1 1 calc R . . C3S C 0.5266(8) 0.2148(6) 0.8112(11) 0.153(7) Uani 1 1 d . . . H3S H 0.5449 0.1954 0.8529 0.183 Uiso 1 1 calc R . . C5S C 0.5000 0.1836(9) 0.7500 0.195(14) Uani 1 2 d S . . H5S H 0.5000 0.1439 0.7500 0.234 Uiso 1 2 calc SR . . C6S C 0.5000 0.3591(8) 0.7500 0.172(10) Uani 1 2 d S . . H6S1 H 0.4614 0.3728 0.7814 0.258 Uiso 0.50 1 calc PR . . H6S2 H 0.4932 0.3728 0.6994 0.258 Uiso 0.50 1 calc PR . . H6S3 H 0.5454 0.3728 0.7692 0.258 Uiso 0.50 1 calc PR . . C21S C -0.0309(11) 0.2485(5) 0.7950(12) 0.080(7) Uani 0.50 1 d PG . . C22S C -0.0104(14) 0.2087(5) 0.7432(16) 0.114(13) Uani 0.50 1 d PG . . H22G H -0.0245 0.1705 0.7488 0.137 Uiso 0.50 1 d PR . . C23S C 0.0302(12) 0.2244(6) 0.6825(13) 0.116(12) Uani 0.50 1 d PG . . H23A H 0.0447 0.1969 0.6470 0.139 Uiso 0.50 1 d PR . . C24S C 0.0502(9) 0.2799(7) 0.6735(9) 0.083(6) Uani 0.50 1 d PG . . H24A H 0.0781 0.2907 0.6316 0.099 Uiso 0.50 1 d PR . . C25S C 0.0296(13) 0.3196(5) 0.7253(10) 0.114(14) Uani 0.50 1 d PG . . H25A H 0.0433 0.3580 0.7190 0.137 Uiso 0.50 1 d PR . . C26S C -0.0109(12) 0.3039(5) 0.7861(9) 0.074(7) Uani 0.50 1 d PG . . H26A H -0.0252 0.3314 0.8218 0.089 Uiso 0.50 1 d PR . . C27S C -0.0671(12) 0.2313(11) 0.8622(14) 0.106(8) Uani 0.50 1 d P . . H27D H -0.0768 0.2637 0.8920 0.159 Uiso 0.50 1 d PR . . H27A H -0.1109 0.2129 0.8503 0.159 Uiso 0.50 1 d PR . . H27B H -0.0371 0.2062 0.8891 0.159 Uiso 0.50 1 d PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0485(8) 0.0475(7) 0.0489(8) 0.0115(6) 0.0049(7) -0.0009(6) N1A 0.056(8) 0.075(8) 0.098(10) 0.004(7) 0.000(6) -0.002(6) N1 0.056(8) 0.075(8) 0.098(10) 0.004(7) 0.000(6) -0.002(6) N2 0.049(7) 0.059(5) 0.051(5) 0.018(4) 0.002(7) 0.001(8) N2A 0.049(7) 0.059(5) 0.051(5) 0.018(4) 0.002(7) 0.001(8) N3 0.112(7) 0.050(5) 0.163(9) 0.021(5) 0.036(7) -0.011(5) N4 0.040(3) 0.072(4) 0.043(3) 0.020(3) -0.005(3) -0.004(3) N5 0.040(3) 0.061(4) 0.041(3) 0.008(3) -0.002(3) 0.002(3) C1 0.041(4) 0.060(5) 0.029(3) -0.005(3) 0.000(3) -0.005(3) C2 0.046(4) 0.100(6) 0.028(4) 0.010(4) 0.000(3) -0.003(4) C3 0.060(6) 0.091(7) 0.063(5) -0.029(5) 0.007(4) -0.004(5) C11A 0.20(2) 0.069(11) 0.126(14) -0.021(10) -0.036(14) -0.056(11) C11 0.20(2) 0.069(11) 0.126(14) -0.021(10) -0.036(14) -0.056(11) C12A 0.085(12) 0.135(15) 0.131(15) 0.043(14) 0.046(11) -0.010(11) C12 0.085(12) 0.135(15) 0.131(15) 0.043(14) 0.046(11) -0.010(11) C21 0.173(17) 0.125(13) 0.061(8) 0.022(9) 0.018(10) -0.030(12) C21A 0.173(17) 0.125(13) 0.061(8) 0.022(9) 0.018(10) -0.030(12) C22 0.12(2) 0.10(2) 0.072(17) -0.004(14) 0.042(15) -0.038(16) C22A 0.12(3) 0.08(3) 0.06(2) -0.026(18) -0.06(3) 0.01(2) C31 0.145(13) 0.109(11) 0.27(2) 0.061(13) -0.044(14) -0.002(10) C32 0.105(10) 0.134(12) 0.250(19) -0.105(12) 0.004(11) 0.029(9) C41 0.039(4) 0.050(4) 0.037(4) 0.000(3) 0.004(3) 0.002(3) C42 0.045(4) 0.047(4) 0.038(4) 0.003(3) 0.008(3) -0.007(3) C43 0.035(4) 0.045(4) 0.036(4) 0.001(3) -0.003(3) -0.001(3) C43' 0.042(4) 0.077(6) 0.049(4) 0.008(4) 0.001(4) -0.002(4) C44 0.042(4) 0.074(5) 0.047(4) 0.017(4) -0.013(4) -0.003(4) C45' 0.056(5) 0.079(6) 0.042(4) 0.015(4) -0.006(4) -0.011(5) C51 0.035(4) 0.061(5) 0.032(3) 0.000(3) -0.003(3) -0.007(3) C52 0.044(4) 0.057(4) 0.030(3) -0.001(3) -0.001(3) -0.001(3) C53 0.033(4) 0.056(4) 0.040(4) -0.002(3) -0.006(3) -0.001(3) C53' 0.050(5) 0.078(6) 0.044(4) -0.003(4) 0.002(4) 0.001(4) C54 0.040(4) 0.080(6) 0.043(4) 0.009(4) 0.004(4) 0.003(4) C55' 0.050(5) 0.079(6) 0.050(5) 0.000(4) -0.005(4) 0.009(4) C431 0.035(4) 0.043(4) 0.039(4) 0.004(3) 0.004(3) 0.007(3) C432 0.043(4) 0.051(4) 0.035(4) 0.001(3) 0.002(3) 0.002(3) C433 0.042(4) 0.050(4) 0.040(4) 0.008(3) 0.005(3) 0.000(3) C434 0.036(4) 0.058(5) 0.046(4) 0.009(3) -0.005(3) 0.000(3) C435 0.047(4) 0.053(4) 0.037(4) 0.006(3) -0.004(3) -0.008(4) C436 0.048(4) 0.050(4) 0.035(4) 0.008(3) 0.000(3) -0.004(3) C531 0.036(4) 0.053(4) 0.040(4) -0.005(3) -0.003(3) -0.003(3) C532 0.044(4) 0.047(4) 0.042(4) 0.001(3) 0.000(3) 0.002(3) C533 0.046(4) 0.047(4) 0.041(4) -0.011(3) 0.003(3) -0.003(3) C534 0.048(4) 0.051(4) 0.047(4) -0.007(4) -0.001(4) 0.004(4) C535 0.045(4) 0.054(4) 0.042(4) 0.003(3) -0.012(3) 0.000(4) C536 0.041(4) 0.057(4) 0.041(4) -0.002(3) -0.005(3) 0.002(3) F431 0.160(6) 0.080(4) 0.137(5) -0.010(4) 0.114(5) 0.007(4) F432 0.066(3) 0.121(4) 0.073(3) 0.022(3) 0.012(3) -0.027(3) F433 0.065(3) 0.160(5) 0.064(3) 0.051(3) 0.007(3) -0.004(3) F451 0.150(5) 0.096(4) 0.053(3) -0.012(3) -0.009(3) 0.019(4) F452 0.112(4) 0.096(4) 0.047(3) 0.023(3) -0.014(3) -0.043(3) F453 0.063(3) 0.156(5) 0.063(3) 0.010(3) -0.020(3) -0.035(3) F531 0.243(9) 0.090(5) 0.150(6) 0.002(4) 0.148(7) -0.019(5) F532 0.091(4) 0.220(8) 0.096(4) 0.042(5) 0.047(4) 0.079(5) F533 0.115(5) 0.273(10) 0.058(4) -0.056(5) 0.024(4) -0.053(6) F551 0.063(4) 0.242(8) 0.089(4) 0.071(5) -0.006(3) 0.043(4) F552 0.156(6) 0.103(5) 0.088(4) 0.040(4) -0.050(4) -0.036(4) F553 0.168(6) 0.134(5) 0.048(3) -0.016(3) -0.037(3) 0.066(5) C1S 0.066(9) 0.082(10) 0.092(10) 0.000 0.013(8) 0.000 C2S 0.054(6) 0.108(9) 0.095(8) 0.028(7) 0.006(5) 0.003(6) C3S 0.120(12) 0.089(11) 0.25(2) 0.033(11) -0.032(12) -0.008(9) C5S 0.14(2) 0.072(15) 0.37(4) 0.000 -0.07(2) 0.000 C6S 0.28(3) 0.107(16) 0.124(16) 0.000 -0.093(18) 0.000 C21S 0.121(18) 0.040(14) 0.081(15) 0.002(12) 0.027(13) 0.056(14) C22S 0.13(2) 0.053(10) 0.16(2) 0.04(2) 0.10(2) 0.04(2) C23S 0.14(3) 0.037(16) 0.16(4) 0.003(16) 0.01(2) -0.057(16) C24S 0.102(17) 0.057(14) 0.089(16) -0.002(12) 0.001(13) -0.001(12) C25S 0.21(4) 0.072(15) 0.060(15) 0.002(12) -0.016(16) -0.068(19) C26S 0.108(18) 0.030(9) 0.084(16) 0.012(10) -0.016(16) 0.008(12) C27S 0.076(15) 0.108(19) 0.13(2) -0.015(16) 0.034(14) 0.028(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti N2 1.821(12) . ? Ti N2A 1.94(3) . ? Ti N1 1.967(11) . ? Ti N1A 2.02(2) . ? Ti N4 2.061(6) . ? Ti N5 2.064(6) . ? Ti N3 2.159(9) . ? N1A C11A 1.436(15) . ? N1A C12A 1.439(15) . ? N1 C12 1.439(12) . ? N1 C11 1.443(13) . ? N2 C22 1.453(15) . ? N2 C21 1.457(12) . ? N2A C22A 1.38(4) . ? N2A C21A 1.450(16) . ? N3 C32 1.442(14) . ? N3 C31 1.442(15) . ? N3 H3 0.9300 . ? N4 C44 1.374(9) . ? N4 C41 1.393(8) . ? N5 C54 1.373(9) . ? N5 C51 1.383(8) . ? C1 C51 1.498(9) . ? C1 C41 1.511(9) . ? C1 C3 1.527(11) . ? C1 C2 1.539(9) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C11A H11A 0.9800 . ? C11A H11B 0.9800 . ? C11A H11C 0.9800 . ? C11 H11D 0.9800 . ? C11 H11E 0.9800 . ? C11 H11F 0.9800 . ? C12A H12A 0.9800 . ? C12A H12B 0.9800 . ? C12A H12C 0.9800 . ? C12 H12D 0.9800 . ? C12 H12E 0.9800 . ? C12 H12F 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C41 C42 1.364(9) . ? C42 C43 1.437(9) . ? C42 H42 0.9500 . ? C43 C44 1.371(9) . ? C43 C431 1.473(9) . ? C43' F433 1.313(9) . ? C43' F431 1.316(9) . ? C43' F432 1.352(9) . ? C43' C433 1.471(10) . ? C44 H44 0.9500 . ? C45' F453 1.304(9) . ? C45' F452 1.322(8) . ? C45' F451 1.374(10) . ? C45' C435 1.506(10) . ? C51 C52 1.365(9) . ? C52 C53 1.424(9) . ? C52 H52 0.9500 . ? C53 C54 1.399(10) . ? C53 C531 1.463(9) . ? C53' F531 1.271(10) . ? C53' F532 1.288(9) . ? C53' F533 1.294(9) . ? C53' C533 1.482(10) . ? C54 H54 0.9500 . ? C55' F551 1.287(9) . ? C55' F552 1.309(9) . ? C55' F553 1.332(9) . ? C55' C535 1.494(10) . ? C431 C432 1.389(9) . ? C431 C436 1.405(9) . ? C432 C433 1.400(9) . ? C432 H432 0.9500 . ? C433 C434 1.377(9) . ? C434 C435 1.376(9) . ? C434 H434 0.9500 . ? C435 C436 1.386(9) . ? C436 H436 0.9500 . ? C531 C532 1.390(9) . ? C531 C536 1.402(9) . ? C532 C533 1.391(9) . ? C532 H532 0.9500 . ? C533 C534 1.386(10) . ? C534 C535 1.369(10) . ? C534 H534 0.9500 . ? C535 C536 1.391(9) . ? C536 H536 0.9500 . ? C1S C2S 1.407(11) . ? C1S C2S 1.407(11) 3_656 ? C1S C6S 1.46(2) . ? C2S C3S 1.281(16) . ? C2S H2S 0.9500 . ? C3S C5S 1.425(17) . ? C3S H3S 0.9500 . ? C5S C3S 1.425(17) 3_656 ? C5S H5S 0.9500 . ? C6S H6S1 0.9800 . ? C6S H6S2 0.9800 . ? C6S H6S3 0.9800 . ? C21S C23S 0.70(3) 3_556 ? C21S C24S 1.01(2) 3_556 ? C21S C22S 1.3900 . ? C21S C26S 1.3900 . ? C21S C22S 1.41(3) 3_556 ? C21S C27S 1.45(3) . ? C21S C25S 1.744(8) 3_556 ? C21S C21S 2.00(3) 3_556 ? C22S C22S 0.46(6) 3_556 ? C22S C23S 1.3900 . ? C22S C21S 1.41(3) 3_556 ? C22S C23S 1.44(4) 3_556 ? C22S H22G 0.9590 . ? C23S C21S 0.70(2) 3_556 ? C23S C27S 1.08(3) 3_556 ? C23S C24S 1.3900 . ? C23S C22S 1.44(5) 3_556 ? C23S C26S 2.019(12) 3_556 ? C23S H23A 0.9594 . ? C24S C21S 1.01(3) 3_556 ? C24S C26S 1.19(3) 3_556 ? C24S C27S 1.37(3) 3_556 ? C24S C25S 1.3900 . ? C24S H24A 0.9591 . ? C25S C26S 0.55(3) 3_556 ? C25S C26S 1.3900 . ? C25S C25S 1.43(4) 3_556 ? C25S C21S 1.744(14) 3_556 ? C25S H25A 0.9599 . ? C26S C25S 0.55(4) 3_556 ? C26S C24S 1.19(3) 3_556 ? C26S C26S 1.37(3) 3_556 ? C26S C23S 2.019(13) 3_556 ? C26S H26A 0.9609 . ? C27S C23S 1.08(3) 3_556 ? C27S C24S 1.37(3) 3_556 ? C27S H27D 0.9599 . ? C27S H27A 0.9601 . ? C27S H27B 0.9600 . ? 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 N2 Ti N2A 22.7(5) . . ? N2 Ti N1 108.7(5) . . ? N2A Ti N1 123.1(8) . . ? N2 Ti N1A 80.6(8) . . ? N2A Ti N1A 98.4(9) . . ? N1 Ti N1A 29.0(7) . . ? N2 Ti N4 113.7(4) . . ? N2A Ti N4 97.2(7) . . ? N1 Ti N4 137.6(4) . . ? N1A Ti N4 164.2(6) . . ? N2 Ti N5 98.6(4) . . ? N2A Ti N5 112.8(7) . . ? N1 Ti N5 92.4(4) . . ? N1A Ti N5 89.4(6) . . ? N4 Ti N5 82.2(2) . . ? N2 Ti N3 102.1(5) . . ? N2A Ti N3 85.4(7) . . ? N1 Ti N3 86.3(4) . . ? N1A Ti N3 99.4(7) . . ? N4 Ti N3 84.4(3) . . ? N5 Ti N3 158.6(3) . . ? C11A N1A C12A 110.1(17) . . ? C11A N1A Ti 121(2) . . ? C12A N1A Ti 126.5(16) . . ? C12 N1 C11 110.0(12) . . ? C12 N1 Ti 119.2(12) . . ? C11 N1 Ti 130.5(10) . . ? C22 N2 C21 106.2(12) . . ? C22 N2 Ti 120.1(12) . . ? C21 N2 Ti 133.6(10) . . ? C22A N2A C21A 112(2) . . ? C22A N2A Ti 110.8(19) . . ? C21A N2A Ti 135(2) . . ? C32 N3 C31 106.3(11) . . ? C32 N3 Ti 125.1(9) . . ? C31 N3 Ti 118.6(8) . . ? C32 N3 H3 100.5 . . ? C31 N3 H3 100.5 . . ? Ti N3 H3 100.5 . . ? C44 N4 C41 105.8(6) . . ? C44 N4 Ti 125.3(5) . . ? C41 N4 Ti 128.9(5) . . ? C54 N5 C51 106.3(6) . . ? C54 N5 Ti 125.0(5) . . ? C51 N5 Ti 128.7(5) . . ? C51 C1 C41 110.6(5) . . ? C51 C1 C3 109.8(6) . . ? C41 C1 C3 108.6(6) . . ? C51 C1 C2 110.4(6) . . ? C41 C1 C2 109.5(6) . . ? C3 C1 C2 107.9(6) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1A C11A H11A 109.5 . . ? N1A C11A H11B 109.5 . . ? H11A C11A H11B 109.5 . . ? N1A C11A H11C 109.5 . . ? H11A C11A H11C 109.5 . . ? H11B C11A H11C 109.5 . . ? N1A C12A H12A 109.5 . . ? N1A C12A H12B 109.5 . . ? H12A C12A H12B 109.5 . . ? N1A C12A H12C 109.5 . . ? H12A C12A H12C 109.5 . . ? H12B C12A H12C 109.5 . . ? N2A C21A H21D 109.5 . . ? N2A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? N2A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? N2A C22A H22D 109.5 . . ? N2A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? N2A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C42 C41 N4 109.8(6) . . ? C42 C41 C1 130.9(6) . . ? N4 C41 C1 119.3(6) . . ? C41 C42 C43 107.6(6) . . ? C41 C42 H42 126.2 . . ? C43 C42 H42 126.2 . . ? C44 C43 C42 105.0(6) . . ? C44 C43 C431 127.1(6) . . ? C42 C43 C431 127.8(6) . . ? F433 C43' F431 108.0(7) . . ? F433 C43' F432 102.9(7) . . ? F431 C43' F432 104.7(7) . . ? F433 C43' C433 114.7(6) . . ? F431 C43' C433 112.7(7) . . ? F432 C43' C433 113.0(7) . . ? C43 C44 N4 111.7(6) . . ? C43 C44 H44 124.1 . . ? N4 C44 H44 124.1 . . ? F453 C45' F452 108.6(7) . . ? F453 C45' F451 104.2(7) . . ? F452 C45' F451 104.3(7) . . ? F453 C45' C435 113.7(7) . . ? F452 C45' C435 113.3(7) . . ? F451 C45' C435 111.9(6) . . ? C52 C51 N5 110.0(6) . . ? C52 C51 C1 129.9(6) . . ? N5 C51 C1 120.1(6) . . ? C51 C52 C53 108.1(6) . . ? C51 C52 H52 125.9 . . ? C53 C52 H52 125.9 . . ? C54 C53 C52 104.7(6) . . ? C54 C53 C531 127.4(6) . . ? C52 C53 C531 127.8(6) . . ? F531 C53' F532 106.2(8) . . ? F531 C53' F533 104.7(8) . . ? F532 C53' F533 102.7(8) . . ? F531 C53' C533 114.0(7) . . ? F532 C53' C533 115.0(7) . . ? F533 C53' C533 113.1(7) . . ? N5 C54 C53 110.9(6) . . ? N5 C54 H54 124.6 . . ? C53 C54 H54 124.6 . . ? F551 C55' F552 106.0(8) . . ? F551 C55' F553 105.3(7) . . ? F552 C55' F553 103.0(7) . . ? F551 C55' C535 114.9(7) . . ? F552 C55' C535 113.7(7) . . ? F553 C55' C535 112.9(7) . . ? C432 C431 C436 118.1(6) . . ? C432 C431 C43 121.6(6) . . ? C436 C431 C43 120.3(6) . . ? C431 C432 C433 121.0(6) . . ? C431 C432 H432 119.5 . . ? C433 C432 H432 119.5 . . ? C434 C433 C432 120.1(6) . . ? C434 C433 C43' 121.1(7) . . ? C432 C433 C43' 118.8(6) . . ? C435 C434 C433 119.4(7) . . ? C435 C434 H434 120.3 . . ? C433 C434 H434 120.3 . . ? C434 C435 C436 121.3(6) . . ? C434 C435 C45' 120.3(6) . . ? C436 C435 C45' 118.2(6) . . ? C435 C436 C431 120.1(6) . . ? C435 C436 H436 119.9 . . ? C431 C436 H436 119.9 . . ? C532 C531 C536 117.2(6) . . ? C532 C531 C53 122.5(6) . . ? C536 C531 C53 120.3(6) . . ? C531 C532 C533 121.4(6) . . ? C531 C532 H532 119.3 . . ? C533 C532 H532 119.3 . . ? C534 C533 C532 120.7(6) . . ? C534 C533 C53' 120.3(7) . . ? C532 C533 C53' 119.0(7) . . ? C535 C534 C533 118.5(7) . . ? C535 C534 H534 120.7 . . ? C533 C534 H534 120.7 . . ? C534 C535 C536 121.4(6) . . ? C534 C535 C55' 121.0(7) . . ? C536 C535 C55' 117.6(7) . . ? C535 C536 C531 120.8(7) . . ? C535 C536 H536 119.6 . . ? C531 C536 H536 119.6 . . ? C2S C1S C2S 119.3(15) . 3_656 ? C2S C1S C6S 120.3(7) . . ? C2S C1S C6S 120.3(7) 3_656 . ? C3S C2S C1S 120.4(14) . . ? C3S C2S H2S 119.8 . . ? C1S C2S H2S 119.8 . . ? C2S C3S C5S 121.6(17) . . ? C2S C3S H3S 119.2 . . ? C5S C3S H3S 119.2 . . ? C3S C5S C3S 117(2) 3_656 . ? C3S C5S H5S 121.6 3_656 . ? C3S C5S H5S 121.6 . . ? C1S C6S H6S1 109.5 . . ? C1S C6S H6S2 109.5 . . ? H6S1 C6S H6S2 109.5 . . ? C1S C6S H6S3 109.5 . . ? H6S1 C6S H6S3 109.5 . . ? H6S2 C6S H6S3 109.5 . . ? C23S C21S C24S 107(4) 3_556 3_556 ? C23S C21S C22S 80(3) 3_556 . ? C24S C21S C22S 171(3) 3_556 . ? C23S C21S C26S 147(4) 3_556 . ? C24S C21S C26S 56.7(15) 3_556 . ? C22S C21S C26S 120.0 . . ? C23S C21S C22S 73.8(18) 3_556 3_556 ? C24S C21S C22S 168(4) 3_556 3_556 ? C22S C21S C22S 19(3) . 3_556 ? C26S C21S C22S 116.0(11) . 3_556 ? C23S C21S C27S 45(3) 3_556 . ? C24S C21S C27S 65(2) 3_556 . ? C22S C21S C27S 120.1(15) . . ? C26S C21S C27S 119.6(15) . . ? C22S C21S C27S 118.6(16) 3_556 . ? C23S C21S C25S 157(4) 3_556 3_556 ? C24S C21S C25S 52.8(7) 3_556 3_556 ? C22S C21S C25S 121.6(12) . 3_556 ? C26S C21S C25S 15.8(18) . 3_556 ? C22S C21S C25S 123(2) 3_556 3_556 ? C27S C21S C25S 117.3(16) . 3_556 ? C23S C21S C21S 117(3) 3_556 3_556 ? C24S C21S C21S 131.8(15) 3_556 3_556 ? C22S C21S C21S 44.8(4) . 3_556 ? C26S C21S C21S 75.4(4) . 3_556 ? C22S C21S C21S 44.0(10) 3_556 3_556 ? C27S C21S C21S 162.5(13) . 3_556 ? C25S C21S C21S 79.7(11) 3_556 3_556 ? C22S C22S C23S 87(5) 3_556 . ? C22S C22S C21S 83(4) 3_556 . ? C23S C22S C21S 120.0 . . ? C22S C22S C21S 78(4) 3_556 3_556 ? C23S C22S C21S 29.1(11) . 3_556 ? C21S C22S C21S 91.3(10) . 3_556 ? C22S C22S C23S 74(6) 3_556 3_556 ? C23S C22S C23S 143.8(12) . 3_556 ? C21S C22S C23S 28.7(7) . 3_556 ? C21S C22S C23S 115.0(16) 3_556 3_556 ? C22S C22S H22G 100.4 3_556 . ? C23S C22S H22G 119.7 . . ? C21S C22S H22G 120.3 . . ? C21S C22S H22G 148.1 3_556 . ? C23S C22S H22G 94.5 3_556 . ? C21S C23S C27S 107(3) 3_556 3_556 ? C21S C23S C22S 77(3) 3_556 . ? C27S C23S C22S 171(2) 3_556 . ? C21S C23S C24S 44(3) 3_556 . ? C27S C23S C24S 65.9(17) 3_556 . ? C22S C23S C24S 120.0 . . ? C21S C23S C22S 71(3) 3_556 3_556 ? C27S C23S C22S 155(4) 3_556 3_556 ? C22S C23S C22S 19(2) . 3_556 ? C24S C23S C22S 115.3(9) . 3_556 ? C21S C23S C26S 22(3) 3_556 3_556 ? C27S C23S C26S 100.5(19) 3_556 3_556 ? C22S C23S C26S 86.2(10) . 3_556 ? C24S C23S C26S 35.0(10) . 3_556 ? C22S C23S C26S 86.4(12) 3_556 3_556 ? C21S C23S H23A 160.2 3_556 . ? C27S C23S H23A 54.7 3_556 . ? C22S C23S H23A 119.9 . . ? C24S C23S H23A 120.1 . . ? C22S C23S H23A 121.1 3_556 . ? C26S C23S H23A 152.5 3_556 . ? C21S C24S C26S 78(2) 3_556 3_556 ? C21S C24S C27S 73.5(15) 3_556 3_556 ? C26S C24S C27S 147.9(18) 3_556 3_556 ? C21S C24S C25S 91.8(15) 3_556 . ? C26S C24S C25S 23.2(15) 3_556 . ? C27S C24S C25S 164.8(14) 3_556 . ? C21S C24S C23S 29.0(16) 3_556 . ? C26S C24S C23S 102.8(9) 3_556 . ? C27S C24S C23S 46.1(13) 3_556 . ? C25S C24S C23S 120.0 . . ? C21S C24S H24A 147.5 3_556 . ? C26S C24S H24A 134.2 3_556 . ? C27S C24S H24A 74.2 3_556 . ? C25S C24S H24A 120.1 . . ? C23S C24S H24A 119.9 . . ? C26S C25S C26S 76(4) 3_556 . ? C26S C25S C24S 58(4) 3_556 . ? C26S C25S C24S 120.0 . . ? C26S C25S C25S 75(4) 3_556 3_556 ? C26S C25S C25S 22.6(15) . 3_556 ? C24S C25S C25S 129.7(10) . 3_556 ? C26S C25S C21S 43(3) 3_556 3_556 ? C26S C25S C21S 84.8(12) . 3_556 ? C24S C25S C21S 35.4(12) . 3_556 ? C25S C25S C21S 98.2(11) 3_556 3_556 ? C26S C25S H25A 140.8 3_556 . ? C26S C25S H25A 120.0 . . ? C24S C25S H25A 120.0 . . ? C25S C25S H25A 106.5 3_556 . ? C21S C25S H25A 154.9 3_556 . ? C25S C26S C24S 99(5) 3_556 3_556 ? C25S C26S C26S 81(4) 3_556 3_556 ? C24S C26S C26S 141(2) 3_556 3_556 ? C25S C26S C25S 83(4) 3_556 . ? C24S C26S C25S 163.6(15) 3_556 . ? C26S C26S C25S 23.2(12) 3_556 . ? C25S C26S C21S 121(4) 3_556 . ? C24S C26S C21S 45.3(8) 3_556 . ? C26S C26S C21S 101.1(4) 3_556 . ? C25S C26S C21S 120.0 . . ? C25S C26S C23S 129(4) 3_556 3_556 ? C24S C26S C23S 42.2(6) 3_556 3_556 ? C26S C26S C23S 108.8(12) 3_556 3_556 ? C25S C26S C23S 125.2(10) . 3_556 ? C21S C26S C23S 10.8(17) . 3_556 ? C25S C26S H26A 66.8 3_556 . ? C24S C26S H26A 75.2 3_556 . ? C26S C26S H26A 136.5 3_556 . ? C25S C26S H26A 119.9 . . ? C21S C26S H26A 120.1 . . ? C23S C26S H26A 114.0 3_556 . ? C23S C27S C24S 68.1(16) 3_556 3_556 ? C23S C27S C21S 27.6(14) 3_556 . ? C24S C27S C21S 41.9(10) 3_556 . ? C23S C27S H27D 131.7 3_556 . ? C24S C27S H27D 67.9 3_556 . ? C21S C27S H27D 109.3 . . ? C23S C27S H27A 108.5 3_556 . ? C24S C27S H27A 119.0 3_556 . ? C21S C27S H27A 110.3 . . ? H27D C27S H27A 109.5 . . ? C23S C27S H27B 84.4 3_556 . ? C24S C27S H27B 129.4 3_556 . ? C21S C27S H27B 108.9 . . ? H27D C27S H27B 109.5 . . ? H27A C27S H27B 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ti N1A C11A -147(3) . . . . ? N2A Ti N1A C11A -161(3) . . . . ? N1 Ti N1A C11A 48(3) . . . . ? N4 Ti N1A C11A 9(5) . . . . ? N5 Ti N1A C11A -48(3) . . . . ? N3 Ti N1A C11A 112(3) . . . . ? N2 Ti N1A C12A 52(3) . . . . ? N2A Ti N1A C12A 38(3) . . . . ? N1 Ti N1A C12A -113(3) . . . . ? N4 Ti N1A C12A -151(2) . . . . ? N5 Ti N1A C12A 151(3) . . . . ? N3 Ti N1A C12A -49(3) . . . . ? N2 Ti N1 C12 -33.7(15) . . . . ? N2A Ti N1 C12 -53.2(16) . . . . ? N1A Ti N1 C12 -18.2(16) . . . . ? N4 Ti N1 C12 147.2(12) . . . . ? N5 Ti N1 C12 66.1(14) . . . . ? N3 Ti N1 C12 -135.3(14) . . . . ? N2 Ti N1 C11 152.9(14) . . . . ? N2A Ti N1 C11 133.4(16) . . . . ? N1A Ti N1 C11 168(2) . . . . ? N4 Ti N1 C11 -26.1(17) . . . . ? N5 Ti N1 C11 -107.2(15) . . . . ? N3 Ti N1 C11 51.4(15) . . . . ? N2A Ti N2 C22 -57(3) . . . . ? N1 Ti N2 C22 169.8(17) . . . . ? N1A Ti N2 C22 162.3(18) . . . . ? N4 Ti N2 C22 -10.9(18) . . . . ? N5 Ti N2 C22 74.3(17) . . . . ? N3 Ti N2 C22 -100.0(17) . . . . ? N2A Ti N2 C21 126(3) . . . . ? N1 Ti N2 C21 -7.8(16) . . . . ? N1A Ti N2 C21 -15.3(16) . . . . ? N4 Ti N2 C21 171.5(14) . . . . ? N5 Ti N2 C21 -103.3(15) . . . . ? N3 Ti N2 C21 82.4(15) . . . . ? N2 Ti N2A C22A 65(3) . . . . ? N1 Ti N2A C22A 120(3) . . . . ? N1A Ti N2A C22A 104(3) . . . . ? N4 Ti N2A C22A -74(3) . . . . ? N5 Ti N2A C22A 11(3) . . . . ? N3 Ti N2A C22A -157(3) . . . . ? N2 Ti N2A C21A -134(5) . . . . ? N1 Ti N2A C21A -79(3) . . . . ? N1A Ti N2A C21A -95(3) . . . . ? N4 Ti N2A C21A 88(3) . . . . ? N5 Ti N2A C21A 172(3) . . . . ? N3 Ti N2A C21A 4(3) . . . . ? N2 Ti N3 C32 163.4(9) . . . . ? N2A Ti N3 C32 148.0(12) . . . . ? N1 Ti N3 C32 -88.3(10) . . . . ? N1A Ti N3 C32 -114.3(11) . . . . ? N4 Ti N3 C32 50.2(9) . . . . ? N5 Ti N3 C32 -1.2(15) . . . . ? N2 Ti N3 C31 -55.8(11) . . . . ? N2A Ti N3 C31 -71.2(13) . . . . ? N1 Ti N3 C31 52.5(11) . . . . ? N1A Ti N3 C31 26.5(13) . . . . ? N4 Ti N3 C31 -169.0(11) . . . . ? N5 Ti N3 C31 139.6(10) . . . . ? N2 Ti N4 C44 -48.9(8) . . . . ? N2A Ti N4 C44 -32.7(9) . . . . ? N1 Ti N4 C44 130.2(8) . . . . ? N1A Ti N4 C44 157(3) . . . . ? N5 Ti N4 C44 -144.8(7) . . . . ? N3 Ti N4 C44 51.9(7) . . . . ? N2 Ti N4 C41 128.4(7) . . . . ? N2A Ti N4 C41 144.6(9) . . . . ? N1 Ti N4 C41 -52.5(9) . . . . ? N1A Ti N4 C41 -26(3) . . . . ? N5 Ti N4 C41 32.4(6) . . . . ? N3 Ti N4 C41 -130.8(7) . . . . ? N2 Ti N5 C54 33.3(7) . . . . ? N2A Ti N5 C54 51.6(10) . . . . ? N1 Ti N5 C54 -76.0(7) . . . . ? N1A Ti N5 C54 -47.1(9) . . . . ? N4 Ti N5 C54 146.3(6) . . . . ? N3 Ti N5 C54 -162.0(8) . . . . ? N2 Ti N5 C51 -144.6(7) . . . . ? N2A Ti N5 C51 -126.2(9) . . . . ? N1 Ti N5 C51 106.2(7) . . . . ? N1A Ti N5 C51 135.0(9) . . . . ? N4 Ti N5 C51 -31.6(6) . . . . ? N3 Ti N5 C51 20.1(11) . . . . ? C44 N4 C41 C42 -0.5(8) . . . . ? Ti N4 C41 C42 -178.2(5) . . . . ? C44 N4 C41 C1 178.8(6) . . . . ? Ti N4 C41 C1 1.1(10) . . . . ? C51 C1 C41 C42 130.2(8) . . . . ? C3 C1 C41 C42 -109.2(9) . . . . ? C2 C1 C41 C42 8.3(10) . . . . ? C51 C1 C41 N4 -48.9(9) . . . . ? C3 C1 C41 N4 71.6(8) . . . . ? C2 C1 C41 N4 -170.8(6) . . . . ? N4 C41 C42 C43 0.8(8) . . . . ? C1 C41 C42 C43 -178.4(7) . . . . ? C41 C42 C43 C44 -0.7(8) . . . . ? C41 C42 C43 C431 178.5(6) . . . . ? C42 C43 C44 N4 0.4(9) . . . . ? C431 C43 C44 N4 -178.8(6) . . . . ? C41 N4 C44 C43 0.0(9) . . . . ? Ti N4 C44 C43 177.8(5) . . . . ? C54 N5 C51 C52 0.6(8) . . . . ? Ti N5 C51 C52 178.7(5) . . . . ? C54 N5 C51 C1 178.7(6) . . . . ? Ti N5 C51 C1 -3.1(9) . . . . ? C41 C1 C51 C52 -132.2(8) . . . . ? C3 C1 C51 C52 108.0(9) . . . . ? C2 C1 C51 C52 -10.8(10) . . . . ? C41 C1 C51 N5 50.1(9) . . . . ? C3 C1 C51 N5 -69.7(8) . . . . ? C2 C1 C51 N5 171.4(6) . . . . ? N5 C51 C52 C53 -0.9(8) . . . . ? C1 C51 C52 C53 -178.9(7) . . . . ? C51 C52 C53 C54 0.9(8) . . . . ? C51 C52 C53 C531 177.1(7) . . . . ? C51 N5 C54 C53 0.0(8) . . . . ? Ti N5 C54 C53 -178.2(5) . . . . ? C52 C53 C54 N5 -0.6(8) . . . . ? C531 C53 C54 N5 -176.8(6) . . . . ? C44 C43 C431 C432 -163.0(7) . . . . ? C42 C43 C431 C432 17.9(11) . . . . ? C44 C43 C431 C436 19.5(11) . . . . ? C42 C43 C431 C436 -159.6(7) . . . . ? C436 C431 C432 C433 -2.1(10) . . . . ? C43 C431 C432 C433 -179.7(6) . . . . ? C431 C432 C433 C434 1.2(11) . . . . ? C431 C432 C433 C43' -177.8(7) . . . . ? F433 C43' C433 C434 132.8(8) . . . . ? F431 C43' C433 C434 -103.1(9) . . . . ? F432 C43' C433 C434 15.4(10) . . . . ? F433 C43' C433 C432 -48.2(10) . . . . ? F431 C43' C433 C432 75.9(9) . . . . ? F432 C43' C433 C432 -165.6(6) . . . . ? C432 C433 C434 C435 -0.4(11) . . . . ? C43' C433 C434 C435 178.6(7) . . . . ? C433 C434 C435 C436 0.5(11) . . . . ? C433 C434 C435 C45' 174.9(7) . . . . ? F453 C45' C435 C434 25.7(11) . . . . ? F452 C45' C435 C434 150.3(7) . . . . ? F451 C45' C435 C434 -92.1(9) . . . . ? F453 C45' C435 C436 -159.7(7) . . . . ? F452 C45' C435 C436 -35.1(10) . . . . ? F451 C45' C435 C436 82.5(9) . . . . ? C434 C435 C436 C431 -1.4(11) . . . . ? C45' C435 C436 C431 -175.9(7) . . . . ? C432 C431 C436 C435 2.2(10) . . . . ? C43 C431 C436 C435 179.8(6) . . . . ? C54 C53 C531 C532 -12.6(11) . . . . ? C52 C53 C531 C532 172.1(7) . . . . ? C54 C53 C531 C536 167.3(7) . . . . ? C52 C53 C531 C536 -8.1(11) . . . . ? C536 C531 C532 C533 -1.0(10) . . . . ? C53 C531 C532 C533 178.9(6) . . . . ? C531 C532 C533 C534 0.6(11) . . . . ? C531 C532 C533 C53' -178.2(7) . . . . ? F531 C53' C533 C534 -112.8(9) . . . . ? F532 C53' C533 C534 10.2(12) . . . . ? F533 C53' C533 C534 127.8(9) . . . . ? F531 C53' C533 C532 66.0(10) . . . . ? F532 C53' C533 C532 -170.9(8) . . . . ? F533 C53' C533 C532 -53.4(11) . . . . ? C532 C533 C534 C535 -0.7(11) . . . . ? C53' C533 C534 C535 178.2(7) . . . . ? C533 C534 C535 C536 1.1(11) . . . . ? C533 C534 C535 C55' 179.3(7) . . . . ? F551 C55' C535 C534 16.6(12) . . . . ? F552 C55' C535 C534 -105.8(9) . . . . ? F553 C55' C535 C534 137.3(8) . . . . ? F551 C55' C535 C536 -165.2(8) . . . . ? F552 C55' C535 C536 72.4(10) . . . . ? F553 C55' C535 C536 -44.5(10) . . . . ? C534 C535 C536 C531 -1.6(11) . . . . ? C55' C535 C536 C531 -179.8(7) . . . . ? C532 C531 C536 C535 1.4(10) . . . . ? C53 C531 C536 C535 -178.4(6) . . . . ? C2S C1S C2S C3S 0.0(10) 3_656 . . . ? C6S C1S C2S C3S -180.0(10) . . . . ? C1S C2S C3S C5S -0.1(19) . . . . ? C2S C3S C5S C3S 0.0(10) . . . 3_656 ? C23S C21S C22S C22S -69(6) 3_556 . . 3_556 ? C24S C21S C22S C22S 148(15) 3_556 . . 3_556 ? C26S C21S C22S C22S 83(4) . . . 3_556 ? C27S C21S C22S C22S -91(4) . . . 3_556 ? C25S C21S C22S C22S 101(4) 3_556 . . 3_556 ? C21S C21S C22S C22S 78(3) 3_556 . . 3_556 ? C23S C21S C22S C23S -152(5) 3_556 . . . ? C24S C21S C22S C23S 65(14) 3_556 . . . ? C26S C21S C22S C23S 0.0 . . . . ? C22S C21S C22S C23S -83(4) 3_556 . . . ? C27S C21S C22S C23S -174(2) . . . . ? C25S C21S C22S C23S 18(2) 3_556 . . . ? C21S C21S C22S C23S -5.1(16) 3_556 . . . ? C23S C21S C22S C21S -147(6) 3_556 . . 3_556 ? C24S C21S C22S C21S 70(13) 3_556 . . 3_556 ? C26S C21S C22S C21S 5.1(16) . . . 3_556 ? C22S C21S C22S C21S -78(3) 3_556 . . 3_556 ? C27S C21S C22S C21S -169(3) . . . 3_556 ? C25S C21S C22S C21S 23(2) 3_556 . . 3_556 ? C24S C21S C22S C23S -143(17) 3_556 . . 3_556 ? C26S C21S C22S C23S 152(5) . . . 3_556 ? C22S C21S C22S C23S 69(6) 3_556 . . 3_556 ? C27S C21S C22S C23S -22(3) . . . 3_556 ? C25S C21S C22S C23S 170(5) 3_556 . . 3_556 ? C21S C21S C22S C23S 147(6) 3_556 . . 3_556 ? C22S C22S C23S C21S -70(4) 3_556 . . 3_556 ? C21S C22S C23S C21S 10(3) . . . 3_556 ? C23S C22S C23S C21S -11.9(15) 3_556 . . 3_556 ? C22S C22S C23S C27S 48(13) 3_556 . . 3_556 ? C21S C22S C23S C27S 129(13) . . . 3_556 ? C21S C22S C23S C27S 118(14) 3_556 . . 3_556 ? C23S C22S C23S C27S 107(14) 3_556 . . 3_556 ? C22S C22S C23S C24S -80.4(14) 3_556 . . . ? C21S C22S C23S C24S 0.0 . . . . ? C21S C22S C23S C24S -10(3) 3_556 . . . ? C23S C22S C23S C24S -22(4) 3_556 . . . ? C21S C22S C23S C22S 80.4(14) . . . 3_556 ? C21S C22S C23S C22S 70(4) 3_556 . . 3_556 ? C23S C22S C23S C22S 58(4) 3_556 . . 3_556 ? C22S C22S C23S C26S -90.0(18) 3_556 . . 3_556 ? C21S C22S C23S C26S -9.6(11) . . . 3_556 ? C21S C22S C23S C26S -20(3) 3_556 . . 3_556 ? C23S C22S C23S C26S -32(4) 3_556 . . 3_556 ? C27S C23S C24S C21S -158(6) 3_556 . . 3_556 ? C22S C23S C24S C21S 15(4) . . . 3_556 ? C22S C23S C24S C21S -6(2) 3_556 . . 3_556 ? C26S C23S C24S C21S 32(4) 3_556 . . 3_556 ? C21S C23S C24S C26S -32(4) 3_556 . . 3_556 ? C27S C23S C24S C26S 171(3) 3_556 . . 3_556 ? C22S C23S C24S C26S -16.9(18) . . . 3_556 ? C22S C23S C24S C26S -37(3) 3_556 . . 3_556 ? C21S C23S C24S C27S 158(6) 3_556 . . 3_556 ? C22S C23S C24S C27S 172(2) . . . 3_556 ? C22S C23S C24S C27S 152(4) 3_556 . . 3_556 ? C26S C23S C24S C27S -171(3) 3_556 . . 3_556 ? C21S C23S C24S C25S -15(4) 3_556 . . . ? C27S C23S C24S C25S -172(2) 3_556 . . . ? C22S C23S C24S C25S 0.0 . . . . ? C22S C23S C24S C25S -20(2) 3_556 . . . ? C26S C23S C24S C25S 16.9(18) 3_556 . . . ? C21S C24S C25S C26S -53(4) 3_556 . . 3_556 ? C27S C24S C25S C26S -67(7) 3_556 . . 3_556 ? C23S C24S C25S C26S -46(3) . . . 3_556 ? C21S C24S C25S C26S -7(2) 3_556 . . . ? C26S C24S C25S C26S 46(3) 3_556 . . . ? C27S C24S C25S C26S -22(6) 3_556 . . . ? C23S C24S C25S C26S 0.0 . . . . ? C21S C24S C25S C25S -32(3) 3_556 . . 3_556 ? C26S C24S C25S C25S 20.8(19) 3_556 . . 3_556 ? C27S C24S C25S C25S -47(7) 3_556 . . 3_556 ? C23S C24S C25S C25S -25(2) . . . 3_556 ? C26S C24S C25S C21S 53(4) 3_556 . . 3_556 ? C27S C24S C25S C21S -14(6) 3_556 . . 3_556 ? C23S C24S C25S C21S 7(2) . . . 3_556 ? C26S C25S C26S C25S -83(6) 3_556 . . 3_556 ? C24S C25S C26S C25S -122(4) . . . 3_556 ? C21S C25S C26S C25S -126(4) 3_556 . . 3_556 ? C26S C25S C26S C24S 15(6) 3_556 . . 3_556 ? C24S C25S C26S C24S -24(7) . . . 3_556 ? C25S C25S C26S C24S 98(10) 3_556 . . 3_556 ? C21S C25S C26S C24S -28(7) 3_556 . . 3_556 ? C24S C25S C26S C26S -39(3) . . . 3_556 ? C25S C25S C26S C26S 83(6) 3_556 . . 3_556 ? C21S C25S C26S C26S -43(3) 3_556 . . 3_556 ? C26S C25S C26S C21S 39(3) 3_556 . . . ? C24S C25S C26S C21S 0.0 . . . . ? C25S C25S C26S C21S 122(4) 3_556 . . . ? C21S C25S C26S C21S -4.1(13) 3_556 . . . ? C26S C25S C26S C23S 50(4) 3_556 . . 3_556 ? C24S C25S C26S C23S 11(2) . . . 3_556 ? C25S C25S C26S C23S 133(4) 3_556 . . 3_556 ? C21S C25S C26S C23S 7.2(11) 3_556 . . 3_556 ? C23S C21S C26S C25S -138(9) 3_556 . . 3_556 ? C24S C21S C26S C25S -70(5) 3_556 . . 3_556 ? C22S C21S C26S C25S 100(4) . . . 3_556 ? C22S C21S C26S C25S 121(5) 3_556 . . 3_556 ? C27S C21S C26S C25S -86(5) . . . 3_556 ? C21S C21S C26S C25S 104(4) 3_556 . . 3_556 ? C23S C21S C26S C24S -68(6) 3_556 . . 3_556 ? C22S C21S C26S C24S 171(3) . . . 3_556 ? C22S C21S C26S C24S -168(5) 3_556 . . 3_556 ? C27S C21S C26S C24S -15(3) . . . 3_556 ? C25S C21S C26S C24S 70(5) 3_556 . . 3_556 ? C21S C21S C26S C24S 174(4) 3_556 . . 3_556 ? C23S C21S C26S C26S 136(6) 3_556 . . 3_556 ? C24S C21S C26S C26S -156(4) 3_556 . . 3_556 ? C22S C21S C26S C26S 14.5(17) . . . 3_556 ? C22S C21S C26S C26S 35(4) 3_556 . . 3_556 ? C27S C21S C26S C26S -172(2) . . . 3_556 ? C25S C21S C26S C26S -86(4) 3_556 . . 3_556 ? C21S C21S C26S C26S 18.2(19) 3_556 . . 3_556 ? C23S C21S C26S C25S 122(6) 3_556 . . . ? C24S C21S C26S C25S -171(3) 3_556 . . . ? C22S C21S C26S C25S 0.0 . . . . ? C22S C21S C26S C25S 21(3) 3_556 . . . ? C27S C21S C26S C25S 173.9(19) . . . . ? C25S C21S C26S C25S -100(4) 3_556 . . . ? C21S C21S C26S C25S 3.7(11) 3_556 . . . ? C24S C21S C26S C23S 68(6) 3_556 . . 3_556 ? C22S C21S C26S C23S -122(6) . . . 3_556 ? C22S C21S C26S C23S -101(7) 3_556 . . 3_556 ? C27S C21S C26S C23S 52(5) . . . 3_556 ? C25S C21S C26S C23S 138(9) 3_556 . . 3_556 ? C21S C21S C26S C23S -118(7) 3_556 . . 3_556 ? C24S C21S C27S C23S -157(7) 3_556 . . 3_556 ? C22S C21S C27S C23S 31(5) . . . 3_556 ? C26S C21S C27S C23S -143(6) . . . 3_556 ? C22S C21S C27S C23S 9(3) 3_556 . . 3_556 ? C25S C21S C27S C23S -161(6) 3_556 . . 3_556 ? C21S C21S C27S C23S 4(5) 3_556 . . 3_556 ? C23S C21S C27S C24S 157(7) 3_556 . . 3_556 ? C22S C21S C27S C24S -172(3) . . . 3_556 ? C26S C21S C27S C24S 14(2) . . . 3_556 ? C22S C21S C27S C24S 166(5) 3_556 . . 3_556 ? C25S C21S C27S C24S -3.5(12) 3_556 . . 3_556 ? C21S C21S C27S C24S 161(10) 3_556 . . 3_556 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.604 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.084 #===END data_070118b _database_code_depnum_ccdc_archive 'CCDC 809526' #TrackingRef '- structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_formula_moiety 'C24 H23 F11 N4 Ti' _chemical_formula_sum 'C24 H23 F11 N4 Ti' _chemical_melting_point ? _exptl_crystal_description ? _exptl_crystal_colour yellow _diffrn_ambient_temperature 173(2) _chemical_formula_weight 624.36 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.1580(3) _cell_length_b 20.8436(3) _cell_length_c 13.8566(2) _cell_angle_alpha 90.00 _cell_angle_beta 107.6380(10) _cell_angle_gamma 90.00 _cell_volume 5548.37(14) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9981 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 25.14 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2528 _exptl_absorpt_coefficient_mu 0.403 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8577 _exptl_absorpt_correction_T_max 0.9623 _exptl_absorpt_process_details SADABS _exptl_special_details ; Data was collected using a BRUKER CCD (charge coupled device) based diffractometer equipped with an Oxford low-temperature apparatus operating at 173 K. A suitable crystal was chosen and mounted on a glass fiber or nylon loop using Paratone oil for Mo radiation and Mineral oil for Copper radiation. Data were measured using omega and Phi scans of 0.5\% per frame for 30 s. The total number of images were based on results from the program COSMO where redundancy was expected to be 4.0 and completeness to 0.83\%A to 100%. Cell parameters were retrieved using APEX II software and refined using SAINT on all observed reflections. Data reduction was performed using the SAINT software which corrects for Lp. Scaling and absorption corrections were applied using SADABS6 multi-scan technique, supplied by George Sheldrick. The structures are solved by the direct method using the SHELXS-97 program and refined by least squares method on F2, SHELXL-97, incorporated in SHELXTL-PC V 6.14. All H atoms were found by difference Fourier methods and refined isotrpically. ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w,and/f 0.5 deg' _diffrn_detector_area_resol_mean 836.6 _diffrn_reflns_number 56783 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0569 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9767 _reflns_number_gt 5949 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COSMO (BRUKER, V1.58, 2006)' _computing_cell_refinement 'APEX2 (BRUKER, V2008.5-0, 2006)' _computing_data_reduction 'SAINT (BRUKER, V7.34A, 2006)' _computing_structure_solution 'SHELXS (Sheldrick, Acta Cryst. A64 2008, 112-122)' _computing_structure_refinement 'SHELXL (Sheldrick, Acta Cryst. A64 2008, 112-122)' _computing_molecular_graphics 'SHELXTL (Sheldrick, Acta Cryst. A64 2008, 112-122)' _computing_publication_material 'SHELXTL (Sheldrick, Acta Cryst. A64 2008, 112-122)' _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^)+(0.1260P)^2^+1.6133P] 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 9767 _refine_ls_number_parameters 733 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1179 _refine_ls_R_factor_gt 0.0649 _refine_ls_wR_factor_ref 0.2234 _refine_ls_wR_factor_gt 0.1793 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.084 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.13045(4) 0.88256(4) 0.00960(6) 0.0400(3) Uani 1 1 d . . . N1 N 0.1811(2) 0.95867(17) 0.0411(3) 0.0505(11) Uani 1 1 d . . . N2 N 0.0567(2) 0.88995(19) 0.0634(3) 0.0521(11) Uani 1 1 d . . . N3 N 0.0938(2) 0.87796(19) -0.1311(3) 0.0535(11) Uani 1 1 d . . . N4 N 0.19695(18) 0.80948(16) 0.0812(3) 0.0368(9) Uani 1 1 d . . . F2' F 0.38302(13) 0.89423(12) 0.2317(2) 0.0577(8) Uani 1 1 d . . . F3' F 0.51598(15) 0.89896(14) 0.3376(2) 0.0669(9) Uani 1 1 d . . . F4' F 0.59298(13) 0.78975(15) 0.3857(2) 0.0599(8) Uani 1 1 d . . . F5' F 0.52964(14) 0.67450(14) 0.3284(2) 0.0582(8) Uani 1 1 d . . . F6' F 0.39704(13) 0.66786(12) 0.2226(2) 0.0500(7) Uani 1 1 d . . . F431 F 0.11507(19) 0.49220(14) 0.0350(3) 0.0823(10) Uani 1 1 d . . . F432 F 0.04215(17) 0.50674(15) -0.1099(3) 0.0867(11) Uani 1 1 d . . . F433 F 0.14919(18) 0.52625(14) -0.0874(3) 0.0828(11) Uani 1 1 d . . . F451 F -0.10389(18) 0.6606(2) -0.0104(4) 0.1241(18) Uani 1 1 d . . . F452 F -0.05480(17) 0.7312(2) 0.0987(3) 0.0970(13) Uani 1 1 d . . . F453 F -0.07853(17) 0.7510(2) -0.0552(3) 0.0970(12) Uani 1 1 d . . . C11 C 0.1787(3) 1.0128(2) 0.1066(4) 0.0660(16) Uani 1 1 d . . . H11A H 0.2228 1.0157 0.1612 0.099 Uiso 1 1 calc R . . H11B H 0.1405 1.0067 0.1357 0.099 Uiso 1 1 calc R . . H11C H 0.1711 1.0525 0.0668 0.099 Uiso 1 1 calc R . . C12 C 0.2356(3) 0.9667(3) -0.0068(5) 0.0685(17) Uani 1 1 d . . . H12A H 0.2806 0.9718 0.0454 0.103 Uiso 1 1 calc R . . H12B H 0.2259 1.0048 -0.0502 0.103 Uiso 1 1 calc R . . H12C H 0.2371 0.9287 -0.0479 0.103 Uiso 1 1 calc R . . C21 C 0.0734(4) 0.8882(3) 0.1730(5) 0.085(2) Uani 1 1 d . . . H21A H 0.0468 0.8540 0.1925 0.127 Uiso 1 1 calc R . . H21B H 0.0615 0.9295 0.1972 0.127 Uiso 1 1 calc R . . H21C H 0.1233 0.8801 0.2032 0.127 Uiso 1 1 calc R . . C22 C -0.0168(3) 0.9030(3) 0.0155(5) 0.0796(19) Uani 1 1 d . . . H22A H -0.0447 0.8690 0.0331 0.119 Uiso 1 1 calc R . . H22B H -0.0263 0.9044 -0.0582 0.119 Uiso 1 1 calc R . . H22C H -0.0288 0.9444 0.0392 0.119 Uiso 1 1 calc R . . C31 C 0.0969(4) 0.9216(4) -0.2127(5) 0.108(3) Uani 1 1 d . . . H31A H 0.0495 0.9326 -0.2539 0.162 Uiso 1 1 calc R . . H31B H 0.1214 0.9005 -0.2553 0.162 Uiso 1 1 calc R . . H31C H 0.1218 0.9607 -0.1834 0.162 Uiso 1 1 calc R . . C32 C 0.0567(3) 0.8197(3) -0.1741(4) 0.0731(17) Uani 1 1 d . . . H32A H 0.0111 0.8310 -0.2208 0.110 Uiso 1 1 calc R . . H32B H 0.0506 0.7927 -0.1196 0.110 Uiso 1 1 calc R . . H32C H 0.0836 0.7963 -0.2109 0.110 Uiso 1 1 calc R . . C41 C 0.1994(2) 0.74239(19) 0.0862(3) 0.0318(10) Uani 1 1 d . . . C42 C 0.2653(2) 0.72249(19) 0.1359(3) 0.0303(10) Uani 1 1 d . . . H42A H 0.2800 0.6792 0.1490 0.036 Uiso 1 1 calc R . . C43 C 0.3080(2) 0.77750(18) 0.1646(3) 0.0289(9) Uani 1 1 d . . . C43' C 0.0985(3) 0.5318(2) -0.0450(4) 0.0545(14) Uani 1 1 d . . . C44 C 0.2639(2) 0.8291(2) 0.1294(3) 0.0375(11) Uani 1 1 d . . . H44A H 0.2783 0.8727 0.1377 0.045 Uiso 1 1 calc R . . C45' C -0.0556(3) 0.7044(3) 0.0124(5) 0.0615(15) Uani 1 1 d . . . C411 C 0.1375(2) 0.7017(2) 0.0493(3) 0.0320(10) Uani 1 1 d . . . C412 C 0.1449(2) 0.6395(2) 0.0170(3) 0.0342(10) Uani 1 1 d . . . H41A H 0.1896 0.6249 0.0169 0.041 Uiso 1 1 calc R . . C413 C 0.0889(2) 0.5987(2) -0.0148(3) 0.0394(11) Uani 1 1 d . . . C414 C 0.0223(2) 0.6189(2) -0.0184(4) 0.0467(12) Uani 1 1 d . . . H41B H -0.0166 0.5911 -0.0423 0.056 Uiso 1 1 calc R . . C415 C 0.0144(2) 0.6807(2) 0.0137(4) 0.0418(11) Uani 1 1 d . . . C416 C 0.0713(2) 0.7217(2) 0.0473(3) 0.0403(11) Uani 1 1 d . . . H41C H 0.0649 0.7637 0.0692 0.048 Uiso 1 1 calc R . . C431 C 0.3820(2) 0.78075(19) 0.2209(3) 0.0303(10) Uani 1 1 d . . . C432 C 0.4173(2) 0.8378(2) 0.2537(3) 0.0367(11) Uani 1 1 d . . . C433 C 0.4870(2) 0.8410(2) 0.3093(4) 0.0435(12) Uani 1 1 d . . . C434 C 0.5249(2) 0.7864(3) 0.3333(3) 0.0425(12) Uani 1 1 d . . . C435 C 0.4932(2) 0.7287(2) 0.3034(3) 0.0401(11) Uani 1 1 d . . . C436 C 0.4240(2) 0.7267(2) 0.2489(3) 0.0335(10) Uani 1 1 d . . . Ti2 Ti 0.67372(4) 0.85082(4) 0.70251(6) 0.0382(3) Uani 1 1 d . . . N2A N 0.7567(2) 0.85179(17) 0.6679(3) 0.0465(10) Uani 1 1 d . . . N1A N 0.6959(2) 0.84288(17) 0.8427(3) 0.0455(10) Uani 1 1 d . . . N3A N 0.6316(2) 0.93024(17) 0.6642(3) 0.0449(10) Uani 1 1 d . . . N4A N 0.60509(19) 0.77936(16) 0.6277(3) 0.0382(9) Uani 1 1 d . . . F31 F 0.84976(19) 0.6388(4) 0.6153(3) 0.167(3) Uani 1 1 d . . . F32A F 0.40065(15) 0.64720(12) 0.4648(2) 0.0574(8) Uani 1 1 d . . . F32 F 0.89415(19) 0.6088(2) 0.7592(4) 0.136(2) Uani 1 1 d . . . F33A F 0.26716(14) 0.65949(13) 0.3639(2) 0.0586(8) Uani 1 1 d . . . F33 F 0.8695(2) 0.7019(2) 0.7291(5) 0.160(2) Uani 1 1 d . . . F34A F 0.20504(14) 0.77691(14) 0.3381(2) 0.0587(8) Uani 1 1 d . . . F35A F 0.28195(14) 0.88168(13) 0.4160(3) 0.0641(9) Uani 1 1 d . . . F36A F 0.41665(14) 0.87202(12) 0.5144(2) 0.0535(7) Uani 1 1 d . . . F51 F 0.7124(5) 0.4993(3) 0.8955(5) 0.212(4) Uani 1 1 d . . . F52 F 0.7012(4) 0.45607(19) 0.7684(6) 0.196(3) Uani 1 1 d . . . F53 F 0.6186(3) 0.4962(3) 0.7982(7) 0.225(4) Uani 1 1 d . . . C3' C 0.8453(3) 0.6454(3) 0.7048(4) 0.0532(13) Uani 1 1 d . . . C5' C 0.6781(4) 0.5040(3) 0.7955(6) 0.083(2) Uani 1 1 d . . . C1A C 0.7381(3) 0.7873(3) 0.8848(4) 0.0682(16) Uani 1 1 d . . . H1AA H 0.7794 0.8011 0.9390 0.102 Uiso 1 1 calc R . . H1AB H 0.7526 0.7659 0.8315 0.102 Uiso 1 1 calc R . . H1AC H 0.7109 0.7575 0.9123 0.102 Uiso 1 1 calc R . . C1A1 C 0.6559(2) 0.6689(2) 0.6778(3) 0.0351(10) Uani 1 1 d . . . C1A2 C 0.7231(2) 0.6796(2) 0.6754(3) 0.0381(11) Uani 1 1 d . . . H1AD H 0.7338 0.7185 0.6475 0.046 Uiso 1 1 calc R . . C1A3 C 0.7751(2) 0.6346(2) 0.7130(3) 0.0394(11) Uani 1 1 d . . . C1A4 C 0.7616(3) 0.5772(2) 0.7545(4) 0.0460(12) Uani 1 1 d . . . H1AE H 0.7975 0.5466 0.7813 0.055 Uiso 1 1 calc R . . C1A5 C 0.6945(3) 0.5661(2) 0.7555(4) 0.0478(12) Uani 1 1 d . . . C1A6 C 0.6427(3) 0.6113(2) 0.7190(4) 0.0460(12) Uani 1 1 d . . . H1AF H 0.5971 0.6028 0.7221 0.055 Uiso 1 1 calc R . . C21A C 0.8294(3) 0.8558(3) 0.7273(5) 0.0687(17) Uani 1 1 d . . . H21D H 0.8554 0.8211 0.7076 0.103 Uiso 1 1 calc R . . H21E H 0.8336 0.8518 0.7994 0.103 Uiso 1 1 calc R . . H21F H 0.8484 0.8973 0.7151 0.103 Uiso 1 1 calc R . . C22A C 0.7479(3) 0.8555(3) 0.5590(4) 0.0672(16) Uani 1 1 d . . . H22D H 0.7731 0.8201 0.5394 0.101 Uiso 1 1 calc R . . H22E H 0.7665 0.8965 0.5438 0.101 Uiso 1 1 calc R . . H22F H 0.6984 0.8526 0.5211 0.101 Uiso 1 1 calc R . . C3A1 C 0.4170(2) 0.7590(2) 0.4953(3) 0.0329(10) Uani 1 1 d . . . C31A C 0.6530(4) 0.9839(2) 0.6122(5) 0.0759(18) Uani 1 1 d . . . H31D H 0.6151 0.9947 0.5510 0.114 Uiso 1 1 calc R . . H31E H 0.6944 0.9718 0.5936 0.114 Uiso 1 1 calc R . . H31F H 0.6636 1.0213 0.6573 0.114 Uiso 1 1 calc R . . C3A2 C 0.3742(2) 0.7064(2) 0.4550(3) 0.0382(11) Uani 1 1 d . . . C32A C 0.5682(3) 0.9461(2) 0.6902(4) 0.0599(15) Uani 1 1 d . . . H32D H 0.5760 0.9851 0.7315 0.090 Uiso 1 1 calc R . . H32E H 0.5565 0.9105 0.7283 0.090 Uiso 1 1 calc R . . H32F H 0.5298 0.9532 0.6279 0.090 Uiso 1 1 calc R . . C3A3 C 0.3046(2) 0.7118(2) 0.4018(3) 0.0421(12) Uani 1 1 d . . . C3A4 C 0.2730(2) 0.7709(2) 0.3881(4) 0.0430(12) Uani 1 1 d . . . C3A5 C 0.3123(2) 0.8241(2) 0.4276(4) 0.0416(12) Uani 1 1 d . . . C3A6 C 0.3816(2) 0.8177(2) 0.4791(3) 0.0373(11) Uani 1 1 d . . . C41A C 0.5977(2) 0.71296(19) 0.6335(3) 0.0326(10) Uani 1 1 d . . . C42A C 0.5301(2) 0.6958(2) 0.5875(3) 0.0358(10) Uani 1 1 d . . . H42B H 0.5122 0.6534 0.5812 0.043 Uiso 1 1 calc R . . C2A C 0.6775(3) 0.8793(3) 0.9202(4) 0.0585(14) Uani 1 1 d . . . H2AA H 0.6551 0.8509 0.9574 0.088 Uiso 1 1 calc R . . H2AB H 0.6453 0.9139 0.8883 0.088 Uiso 1 1 calc R . . H2AC H 0.7196 0.8979 0.9673 0.088 Uiso 1 1 calc R . . C43A C 0.4911(2) 0.7525(2) 0.5504(3) 0.0318(10) Uani 1 1 d . . . C45A C 0.5396(2) 0.8012(2) 0.5768(3) 0.0364(10) Uani 1 1 d . . . H45A H 0.5288 0.8451 0.5615 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0359(5) 0.0373(5) 0.0416(6) -0.0002(4) 0.0036(4) 0.0073(4) N1 0.047(2) 0.036(2) 0.061(3) -0.003(2) 0.005(2) 0.0087(19) N2 0.043(2) 0.054(3) 0.057(3) -0.001(2) 0.012(2) 0.010(2) N3 0.059(3) 0.050(2) 0.044(3) 0.003(2) 0.004(2) 0.006(2) N4 0.030(2) 0.035(2) 0.041(2) -0.0042(17) 0.0045(18) 0.0003(16) F2' 0.0392(16) 0.0394(15) 0.085(2) -0.0090(14) 0.0040(15) -0.0035(12) F3' 0.0444(17) 0.0655(19) 0.083(2) -0.0179(17) 0.0082(17) -0.0200(15) F4' 0.0253(15) 0.099(2) 0.0487(18) -0.0115(16) 0.0015(13) -0.0038(14) F5' 0.0414(16) 0.0695(19) 0.0553(19) -0.0001(15) 0.0021(14) 0.0211(14) F6' 0.0424(16) 0.0400(15) 0.0569(18) -0.0034(13) -0.0011(14) 0.0071(12) F431 0.093(3) 0.0448(18) 0.094(3) 0.0143(18) 0.005(2) -0.0043(17) F432 0.070(2) 0.065(2) 0.106(3) -0.029(2) -0.003(2) -0.0212(18) F433 0.084(2) 0.0518(18) 0.126(3) -0.0270(19) 0.053(2) -0.0122(17) F451 0.043(2) 0.103(3) 0.238(6) -0.025(3) 0.060(3) -0.021(2) F452 0.055(2) 0.156(4) 0.086(3) -0.008(3) 0.030(2) 0.025(2) F453 0.048(2) 0.126(3) 0.108(3) 0.028(3) 0.010(2) 0.032(2) C11 0.069(4) 0.049(3) 0.067(4) -0.013(3) 0.002(3) -0.001(3) C12 0.074(4) 0.044(3) 0.089(5) -0.001(3) 0.027(4) -0.005(3) C21 0.092(5) 0.093(5) 0.078(5) -0.001(4) 0.039(4) 0.022(4) C22 0.046(4) 0.086(4) 0.106(5) 0.000(4) 0.022(4) 0.021(3) C31 0.155(8) 0.094(5) 0.053(4) 0.024(4) 0.000(5) -0.017(5) C32 0.083(4) 0.076(4) 0.045(4) 0.003(3) -0.005(3) -0.005(3) C41 0.035(3) 0.030(2) 0.032(3) 0.0004(19) 0.013(2) 0.0013(19) C42 0.029(2) 0.031(2) 0.030(3) 0.0006(19) 0.008(2) 0.0021(18) C43 0.029(2) 0.034(2) 0.023(2) -0.0010(18) 0.0075(19) 0.0023(18) C43' 0.042(3) 0.046(3) 0.066(4) 0.000(3) 0.002(3) -0.012(2) C44 0.035(3) 0.032(2) 0.041(3) -0.001(2) 0.006(2) 0.000(2) C45' 0.036(3) 0.080(4) 0.070(4) -0.004(4) 0.019(3) -0.005(3) C411 0.028(2) 0.042(2) 0.023(2) 0.003(2) 0.0036(19) -0.0032(19) C412 0.029(2) 0.040(2) 0.030(3) 0.000(2) 0.003(2) -0.0027(19) C413 0.037(3) 0.041(3) 0.036(3) 0.004(2) 0.005(2) -0.007(2) C414 0.036(3) 0.059(3) 0.040(3) 0.004(2) 0.005(2) -0.010(2) C415 0.029(3) 0.053(3) 0.042(3) 0.008(2) 0.007(2) -0.004(2) C416 0.037(3) 0.043(3) 0.042(3) 0.001(2) 0.012(2) 0.000(2) C431 0.029(2) 0.038(2) 0.025(2) -0.0010(19) 0.0102(19) 0.0018(19) C432 0.034(3) 0.041(3) 0.034(3) -0.006(2) 0.009(2) 0.000(2) C433 0.038(3) 0.054(3) 0.039(3) -0.010(2) 0.012(2) -0.014(2) C434 0.031(3) 0.069(3) 0.028(3) -0.005(2) 0.009(2) 0.001(2) C435 0.036(3) 0.053(3) 0.031(3) 0.000(2) 0.010(2) 0.012(2) C436 0.033(2) 0.040(2) 0.027(3) -0.009(2) 0.008(2) -0.004(2) Ti2 0.0418(5) 0.0306(4) 0.0385(5) 0.0007(4) 0.0069(4) -0.0055(4) N2A 0.045(2) 0.041(2) 0.051(3) -0.0104(19) 0.011(2) -0.0109(18) N1A 0.048(2) 0.043(2) 0.039(2) -0.0013(19) 0.004(2) -0.0147(19) N3A 0.058(3) 0.031(2) 0.045(2) -0.0001(18) 0.015(2) -0.0078(18) N4A 0.045(2) 0.0312(19) 0.036(2) 0.0041(17) 0.0087(19) -0.0002(17) F31 0.046(2) 0.396(9) 0.067(3) -0.033(4) 0.028(2) -0.034(4) F32A 0.0576(19) 0.0377(15) 0.064(2) -0.0045(13) -0.0015(16) -0.0044(13) F32 0.049(2) 0.163(4) 0.188(5) 0.093(4) 0.025(3) 0.027(3) F33A 0.0485(17) 0.0599(18) 0.058(2) -0.0028(15) 0.0018(15) -0.0172(14) F33 0.089(3) 0.102(3) 0.321(8) -0.042(4) 0.111(4) -0.032(3) F34A 0.0360(16) 0.080(2) 0.0573(19) 0.0124(15) 0.0099(15) -0.0025(14) F35A 0.0443(17) 0.0529(18) 0.097(3) 0.0144(16) 0.0251(17) 0.0116(14) F36A 0.0423(16) 0.0391(15) 0.077(2) 0.0011(14) 0.0146(15) 0.0019(12) F51 0.361(11) 0.140(5) 0.129(5) 0.064(4) 0.067(6) -0.060(6) F52 0.336(9) 0.035(2) 0.315(9) 0.023(3) 0.249(8) 0.009(3) F53 0.109(4) 0.126(4) 0.468(12) 0.196(6) 0.130(6) 0.040(3) C3' 0.043(3) 0.052(3) 0.061(4) 0.002(3) 0.011(3) 0.002(3) C5' 0.084(5) 0.062(4) 0.111(6) 0.053(4) 0.044(4) 0.026(4) C1A 0.072(4) 0.056(3) 0.058(4) 0.010(3) -0.008(3) -0.007(3) C1A1 0.043(3) 0.034(2) 0.027(3) -0.0037(19) 0.008(2) 0.002(2) C1A2 0.042(3) 0.035(2) 0.035(3) 0.000(2) 0.009(2) -0.001(2) C1A3 0.042(3) 0.043(3) 0.033(3) -0.004(2) 0.011(2) 0.001(2) C1A4 0.053(3) 0.042(3) 0.040(3) 0.003(2) 0.011(2) 0.010(2) C1A5 0.056(3) 0.042(3) 0.047(3) 0.008(2) 0.018(3) 0.006(2) C1A6 0.049(3) 0.042(3) 0.052(3) 0.007(2) 0.023(3) 0.003(2) C21A 0.047(3) 0.069(4) 0.087(5) -0.019(3) 0.016(3) -0.011(3) C22A 0.063(4) 0.073(4) 0.069(4) -0.017(3) 0.024(3) -0.025(3) C3A1 0.041(3) 0.037(2) 0.022(2) 0.0021(19) 0.013(2) -0.006(2) C31A 0.109(5) 0.041(3) 0.087(5) 0.015(3) 0.044(4) -0.007(3) C3A2 0.042(3) 0.043(3) 0.031(3) 0.008(2) 0.012(2) 0.002(2) C32A 0.069(4) 0.038(3) 0.073(4) 0.000(3) 0.022(3) 0.001(3) C3A3 0.045(3) 0.051(3) 0.030(3) 0.002(2) 0.010(2) -0.014(2) C3A4 0.030(3) 0.065(3) 0.036(3) 0.011(2) 0.012(2) 0.001(2) C3A5 0.040(3) 0.047(3) 0.043(3) 0.011(2) 0.021(2) 0.006(2) C3A6 0.040(3) 0.037(3) 0.039(3) 0.002(2) 0.019(2) -0.005(2) C41A 0.037(3) 0.035(2) 0.028(3) -0.0019(19) 0.012(2) -0.002(2) C42A 0.042(3) 0.031(2) 0.037(3) 0.002(2) 0.017(2) -0.004(2) C2A 0.059(3) 0.074(4) 0.039(3) -0.011(3) 0.010(3) -0.021(3) C43A 0.034(2) 0.037(2) 0.026(2) -0.0008(19) 0.012(2) -0.001(2) C45A 0.043(3) 0.031(2) 0.032(3) 0.003(2) 0.007(2) 0.003(2) _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 N2 1.860(4) . ? Ti1 N1 1.865(4) . ? Ti1 N3 1.866(4) . ? Ti1 N4 2.073(4) . ? N1 C11 1.458(6) . ? N1 C12 1.456(6) . ? N2 C21 1.453(7) . ? N2 C22 1.454(7) . ? N3 C32 1.455(7) . ? N3 C31 1.467(7) . ? N4 C44 1.375(5) . ? N4 C41 1.400(5) . ? F2' C432 1.352(5) . ? F3' C433 1.347(5) . ? F4' C434 1.346(5) . ? F5' C435 1.335(5) . ? F6' C436 1.347(5) . ? F431 C43' 1.341(6) . ? F432 C43' 1.324(6) . ? F433 C43' 1.329(6) . ? F451 C45' 1.302(6) . ? F452 C45' 1.315(7) . ? F453 C45' 1.331(7) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C41 C42 1.363(6) . ? C41 C411 1.465(6) . ? C42 C43 1.417(6) . ? C42 H42A 0.9500 . ? C43 C44 1.385(6) . ? C43 C431 1.460(6) . ? C43' C413 1.486(7) . ? C44 H44A 0.9500 . ? C45' C415 1.492(7) . ? C411 C416 1.390(6) . ? C411 C412 1.395(6) . ? C412 C413 1.375(6) . ? C412 H41A 0.9500 . ? C413 C414 1.392(6) . ? C414 C415 1.387(7) . ? C414 H41B 0.9500 . ? C415 C416 1.393(6) . ? C416 H41C 0.9500 . ? C431 C432 1.389(6) . ? C431 C436 1.392(6) . ? C432 C433 1.384(7) . ? C433 C434 1.356(7) . ? C434 C435 1.366(6) . ? C435 C436 1.370(6) . ? Ti2 N3A 1.862(4) . ? Ti2 N1A 1.864(4) . ? Ti2 N2A 1.874(4) . ? Ti2 N4A 2.083(4) . ? N2A C21A 1.451(7) . ? N2A C22A 1.467(7) . ? N1A C2A 1.453(6) . ? N1A C1A 1.451(6) . ? N3A C31A 1.465(6) . ? N3A C32A 1.466(6) . ? N4A C45A 1.372(5) . ? N4A C41A 1.397(5) . ? F31 C3' 1.278(6) . ? F32A C3A2 1.335(5) . ? F32 C3' 1.292(6) . ? F33A C3A3 1.339(5) . ? F33 C3' 1.279(6) . ? F34A C3A4 1.341(5) . ? F35A C3A5 1.335(5) . ? F36A C3A6 1.346(5) . ? F51 C5' 1.351(9) . ? F52 C5' 1.208(7) . ? F53 C5' 1.224(7) . ? C3' C1A3 1.471(7) . ? C5' C1A5 1.485(7) . ? C1A H1AA 0.9800 . ? C1A H1AB 0.9800 . ? C1A H1AC 0.9800 . ? C1A1 C1A2 1.383(6) . ? C1A1 C1A6 1.389(6) . ? C1A1 C41A 1.470(6) . ? C1A2 C1A3 1.386(6) . ? C1A2 H1AD 0.9500 . ? C1A3 C1A4 1.390(6) . ? C1A4 C1A5 1.377(7) . ? C1A4 H1AE 0.9500 . ? C1A5 C1A6 1.383(6) . ? C1A6 H1AF 0.9500 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C3A1 C3A6 1.400(6) . ? C3A1 C3A2 1.402(6) . ? C3A1 C43A 1.463(6) . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? C3A2 C3A3 1.378(6) . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C3A3 C3A4 1.374(7) . ? C3A4 C3A5 1.375(7) . ? C3A5 C3A6 1.369(6) . ? C41A C42A 1.365(6) . ? C42A C43A 1.425(6) . ? C42A H42B 0.9500 . ? C2A H2AA 0.9800 . ? C2A H2AB 0.9800 . ? C2A H2AC 0.9800 . ? C43A C45A 1.380(6) . ? C45A H45A 0.9500 . ? 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 N2 Ti1 N1 106.42(18) . . ? N2 Ti1 N3 108.18(19) . . ? N1 Ti1 N3 107.66(19) . . ? N2 Ti1 N4 110.39(16) . . ? N1 Ti1 N4 106.53(16) . . ? N3 Ti1 N4 117.13(16) . . ? C11 N1 C12 111.5(4) . . ? C11 N1 Ti1 133.2(4) . . ? C12 N1 Ti1 115.2(3) . . ? C21 N2 C22 111.3(5) . . ? C21 N2 Ti1 117.2(4) . . ? C22 N2 Ti1 131.3(4) . . ? C32 N3 C31 109.7(5) . . ? C32 N3 Ti1 117.5(3) . . ? C31 N3 Ti1 132.7(4) . . ? C44 N4 C41 105.0(3) . . ? C44 N4 Ti1 114.3(3) . . ? C41 N4 Ti1 139.9(3) . . ? N1 C11 H11A 109.5 . . ? N1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N1 C12 H12A 109.5 . . ? N1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C42 C41 N4 110.0(4) . . ? C42 C41 C411 126.6(4) . . ? N4 C41 C411 123.2(4) . . ? C41 C42 C43 108.2(4) . . ? C41 C42 H42A 125.9 . . ? C43 C42 H42A 125.9 . . ? C44 C43 C42 105.0(4) . . ? C44 C43 C431 126.4(4) . . ? C42 C43 C431 128.5(4) . . ? F432 C43' F433 106.4(5) . . ? F432 C43' F431 105.5(4) . . ? F433 C43' F431 106.3(4) . . ? F432 C43' C413 113.8(4) . . ? F433 C43' C413 113.0(4) . . ? F431 C43' C413 111.4(5) . . ? N4 C44 C43 111.8(4) . . ? N4 C44 H44A 124.1 . . ? C43 C44 H44A 124.1 . . ? F451 C45' F452 108.8(5) . . ? F451 C45' F453 105.5(5) . . ? F452 C45' F453 103.7(5) . . ? F451 C45' C415 113.9(5) . . ? F452 C45' C415 112.3(5) . . ? F453 C45' C415 112.0(4) . . ? C416 C411 C412 117.8(4) . . ? C416 C411 C41 122.9(4) . . ? C412 C411 C41 119.2(4) . . ? C413 C412 C411 121.4(4) . . ? C413 C412 H41A 119.3 . . ? C411 C412 H41A 119.3 . . ? C412 C413 C414 120.9(4) . . ? C412 C413 C43' 120.4(4) . . ? C414 C413 C43' 118.7(4) . . ? C415 C414 C413 118.2(4) . . ? C415 C414 H41B 120.9 . . ? C413 C414 H41B 120.9 . . ? C414 C415 C416 120.9(4) . . ? C414 C415 C45' 120.3(4) . . ? C416 C415 C45' 118.7(5) . . ? C411 C416 C415 120.7(4) . . ? C411 C416 H41C 119.6 . . ? C415 C416 H41C 119.6 . . ? C432 C431 C436 113.1(4) . . ? C432 C431 C43 123.6(4) . . ? C436 C431 C43 123.3(4) . . ? F2' C432 C433 116.5(4) . . ? F2' C432 C431 119.6(4) . . ? C433 C432 C431 123.9(4) . . ? F3' C433 C434 121.2(4) . . ? F3' C433 C432 119.0(4) . . ? C434 C433 C432 119.8(4) . . ? F4' C434 C433 119.7(4) . . ? F4' C434 C435 121.1(4) . . ? C433 C434 C435 119.2(4) . . ? F5' C435 C434 119.7(4) . . ? F5' C435 C436 120.4(4) . . ? C434 C435 C436 119.9(4) . . ? F6' C436 C435 115.9(4) . . ? F6' C436 C431 120.0(4) . . ? C435 C436 C431 124.1(4) . . ? N3A Ti2 N1A 108.69(17) . . ? N3A Ti2 N2A 106.40(17) . . ? N1A Ti2 N2A 108.47(18) . . ? N3A Ti2 N4A 108.50(16) . . ? N1A Ti2 N4A 111.64(15) . . ? N2A Ti2 N4A 112.94(15) . . ? C21A N2A C22A 111.5(4) . . ? C21A N2A Ti2 133.0(4) . . ? C22A N2A Ti2 115.2(3) . . ? C2A N1A C1A 111.8(4) . . ? C2A N1A Ti2 133.6(3) . . ? C1A N1A Ti2 114.6(3) . . ? C31A N3A C32A 110.9(4) . . ? C31A N3A Ti2 130.0(4) . . ? C32A N3A Ti2 119.1(3) . . ? C45A N4A C41A 104.8(3) . . ? C45A N4A Ti2 114.1(3) . . ? C41A N4A Ti2 138.2(3) . . ? F31 C3' F33 102.8(6) . . ? F31 C3' F32 103.8(5) . . ? F33 C3' F32 103.2(5) . . ? F31 C3' C1A3 114.2(5) . . ? F33 C3' C1A3 114.9(4) . . ? F32 C3' C1A3 116.4(5) . . ? F52 C5' F53 111.9(8) . . ? F52 C5' F51 97.7(6) . . ? F53 C5' F51 99.3(7) . . ? F52 C5' C1A5 117.1(6) . . ? F53 C5' C1A5 117.3(5) . . ? F51 C5' C1A5 110.1(7) . . ? N1A C1A H1AA 109.5 . . ? N1A C1A H1AB 109.5 . . ? H1AA C1A H1AB 109.5 . . ? N1A C1A H1AC 109.5 . . ? H1AA C1A H1AC 109.5 . . ? H1AB C1A H1AC 109.5 . . ? C1A2 C1A1 C1A6 117.4(4) . . ? C1A2 C1A1 C41A 123.6(4) . . ? C1A6 C1A1 C41A 118.9(4) . . ? C1A1 C1A2 C1A3 121.1(4) . . ? C1A1 C1A2 H1AD 119.4 . . ? C1A3 C1A2 H1AD 119.4 . . ? C1A4 C1A3 C1A2 121.2(4) . . ? C1A4 C1A3 C3' 118.6(4) . . ? C1A2 C1A3 C3' 120.2(4) . . ? C1A5 C1A4 C1A3 117.7(4) . . ? C1A5 C1A4 H1AE 121.2 . . ? C1A3 C1A4 H1AE 121.2 . . ? C1A4 C1A5 C1A6 121.2(4) . . ? C1A4 C1A5 C5' 118.6(5) . . ? C1A6 C1A5 C5' 120.2(5) . . ? C1A5 C1A6 C1A1 121.5(4) . . ? C1A5 C1A6 H1AF 119.3 . . ? C1A1 C1A6 H1AF 119.3 . . ? N2A C21A H21D 109.5 . . ? N2A C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? N2A C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? N2A C22A H22D 109.5 . . ? N2A C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? N2A C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C3A6 C3A1 C3A2 113.4(4) . . ? C3A6 C3A1 C43A 123.8(4) . . ? C3A2 C3A1 C43A 122.9(4) . . ? N3A C31A H31D 109.5 . . ? N3A C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? N3A C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? F32A C3A2 C3A3 116.1(4) . . ? F32A C3A2 C3A1 120.3(4) . . ? C3A3 C3A2 C3A1 123.6(4) . . ? N3A C32A H32D 109.5 . . ? N3A C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? N3A C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? F33A C3A3 C3A4 119.6(4) . . ? F33A C3A3 C3A2 120.4(4) . . ? C3A4 C3A3 C3A2 120.0(4) . . ? F34A C3A4 C3A5 120.4(4) . . ? F34A C3A4 C3A3 120.9(4) . . ? C3A5 C3A4 C3A3 118.8(4) . . ? F35A C3A5 C3A4 119.3(4) . . ? F35A C3A5 C3A6 120.5(4) . . ? C3A4 C3A5 C3A6 120.2(4) . . ? F36A C3A6 C3A5 116.7(4) . . ? F36A C3A6 C3A1 119.3(4) . . ? C3A5 C3A6 C3A1 124.0(4) . . ? C42A C41A N4A 109.9(4) . . ? C42A C41A C1A1 126.1(4) . . ? N4A C41A C1A1 123.9(4) . . ? C41A C42A C43A 108.4(4) . . ? C41A C42A H42B 125.8 . . ? C43A C42A H42B 125.8 . . ? N1A C2A H2AA 109.5 . . ? N1A C2A H2AB 109.5 . . ? H2AA C2A H2AB 109.5 . . ? N1A C2A H2AC 109.5 . . ? H2AA C2A H2AC 109.5 . . ? H2AB C2A H2AC 109.5 . . ? C45A C43A C42A 104.2(4) . . ? C45A C43A C3A1 126.8(4) . . ? C42A C43A C3A1 129.0(4) . . ? N4A C45A C43A 112.7(4) . . ? N4A C45A H45A 123.6 . . ? C43A C45A H45A 123.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Ti1 N1 C11 9.9(5) . . . . ? N3 Ti1 N1 C11 125.7(5) . . . . ? N4 Ti1 N1 C11 -107.9(5) . . . . ? N2 Ti1 N1 C12 -171.5(4) . . . . ? N3 Ti1 N1 C12 -55.8(4) . . . . ? N4 Ti1 N1 C12 70.7(4) . . . . ? N1 Ti1 N2 C21 -70.1(4) . . . . ? N3 Ti1 N2 C21 174.4(4) . . . . ? N4 Ti1 N2 C21 45.1(4) . . . . ? N1 Ti1 N2 C22 103.7(5) . . . . ? N3 Ti1 N2 C22 -11.7(5) . . . . ? N4 Ti1 N2 C22 -141.1(5) . . . . ? N2 Ti1 N3 C32 -70.2(4) . . . . ? N1 Ti1 N3 C32 175.1(4) . . . . ? N4 Ti1 N3 C32 55.2(4) . . . . ? N2 Ti1 N3 C31 112.9(6) . . . . ? N1 Ti1 N3 C31 -1.7(6) . . . . ? N4 Ti1 N3 C31 -121.6(6) . . . . ? N2 Ti1 N4 C44 -119.7(3) . . . . ? N1 Ti1 N4 C44 -4.6(3) . . . . ? N3 Ti1 N4 C44 116.0(3) . . . . ? N2 Ti1 N4 C41 72.3(5) . . . . ? N1 Ti1 N4 C41 -172.6(4) . . . . ? N3 Ti1 N4 C41 -52.1(5) . . . . ? C44 N4 C41 C42 0.2(5) . . . . ? Ti1 N4 C41 C42 169.0(3) . . . . ? C44 N4 C41 C411 175.8(4) . . . . ? Ti1 N4 C41 C411 -15.4(7) . . . . ? N4 C41 C42 C43 -0.2(5) . . . . ? C411 C41 C42 C43 -175.6(4) . . . . ? C41 C42 C43 C44 0.0(4) . . . . ? C41 C42 C43 C431 178.8(4) . . . . ? C41 N4 C44 C43 -0.2(5) . . . . ? Ti1 N4 C44 C43 -172.3(3) . . . . ? C42 C43 C44 N4 0.1(5) . . . . ? C431 C43 C44 N4 -178.7(4) . . . . ? C42 C41 C411 C416 146.2(4) . . . . ? N4 C41 C411 C416 -28.7(6) . . . . ? C42 C41 C411 C412 -32.0(6) . . . . ? N4 C41 C411 C412 153.1(4) . . . . ? C416 C411 C412 C413 -0.7(6) . . . . ? C41 C411 C412 C413 177.6(4) . . . . ? C411 C412 C413 C414 1.8(7) . . . . ? C411 C412 C413 C43' -177.6(4) . . . . ? F432 C43' C413 C412 -154.0(5) . . . . ? F433 C43' C413 C412 -32.6(7) . . . . ? F431 C43' C413 C412 86.9(5) . . . . ? F432 C43' C413 C414 26.5(7) . . . . ? F433 C43' C413 C414 147.9(5) . . . . ? F431 C43' C413 C414 -92.6(5) . . . . ? C412 C413 C414 C415 -1.9(7) . . . . ? C43' C413 C414 C415 177.6(4) . . . . ? C413 C414 C415 C416 0.8(7) . . . . ? C413 C414 C415 C45' -179.3(5) . . . . ? F451 C45' C415 C414 6.8(8) . . . . ? F452 C45' C415 C414 130.9(5) . . . . ? F453 C45' C415 C414 -112.9(6) . . . . ? F451 C45' C415 C416 -173.4(5) . . . . ? F452 C45' C415 C416 -49.2(7) . . . . ? F453 C45' C415 C416 67.0(7) . . . . ? C412 C411 C416 C415 -0.3(6) . . . . ? C41 C411 C416 C415 -178.6(4) . . . . ? C414 C415 C416 C411 0.2(7) . . . . ? C45' C415 C416 C411 -179.7(5) . . . . ? C44 C43 C431 C432 5.1(7) . . . . ? C42 C43 C431 C432 -173.3(4) . . . . ? C44 C43 C431 C436 -176.2(4) . . . . ? C42 C43 C431 C436 5.3(7) . . . . ? C436 C431 C432 F2' 179.8(4) . . . . ? C43 C431 C432 F2' -1.5(6) . . . . ? C436 C431 C432 C433 -0.5(6) . . . . ? C43 C431 C432 C433 178.3(4) . . . . ? F2' C432 C433 F3' 0.1(6) . . . . ? C431 C432 C433 F3' -179.7(4) . . . . ? F2' C432 C433 C434 -179.3(4) . . . . ? C431 C432 C433 C434 1.0(7) . . . . ? F3' C433 C434 F4' -0.5(7) . . . . ? C432 C433 C434 F4' 178.8(4) . . . . ? F3' C433 C434 C435 179.6(4) . . . . ? C432 C433 C434 C435 -1.0(7) . . . . ? F4' C434 C435 F5' 1.6(6) . . . . ? C433 C434 C435 F5' -178.6(4) . . . . ? F4' C434 C435 C436 -179.1(4) . . . . ? C433 C434 C435 C436 0.7(7) . . . . ? F5' C435 C436 F6' -0.7(6) . . . . ? C434 C435 C436 F6' 180.0(4) . . . . ? F5' C435 C436 C431 179.1(4) . . . . ? C434 C435 C436 C431 -0.3(7) . . . . ? C432 C431 C436 F6' 179.9(4) . . . . ? C43 C431 C436 F6' 1.1(6) . . . . ? C432 C431 C436 C435 0.1(6) . . . . ? C43 C431 C436 C435 -178.7(4) . . . . ? N3A Ti2 N2A C21A 107.6(5) . . . . ? N1A Ti2 N2A C21A -9.1(5) . . . . ? N4A Ti2 N2A C21A -133.4(4) . . . . ? N3A Ti2 N2A C22A -65.3(4) . . . . ? N1A Ti2 N2A C22A 177.9(3) . . . . ? N4A Ti2 N2A C22A 53.6(4) . . . . ? N3A Ti2 N1A C2A 11.6(5) . . . . ? N2A Ti2 N1A C2A 126.9(4) . . . . ? N4A Ti2 N1A C2A -108.0(4) . . . . ? N3A Ti2 N1A C1A -171.4(3) . . . . ? N2A Ti2 N1A C1A -56.1(4) . . . . ? N4A Ti2 N1A C1A 68.9(4) . . . . ? N1A Ti2 N3A C31A 119.9(5) . . . . ? N2A Ti2 N3A C31A 3.2(5) . . . . ? N4A Ti2 N3A C31A -118.6(5) . . . . ? N1A Ti2 N3A C32A -57.9(4) . . . . ? N2A Ti2 N3A C32A -174.6(3) . . . . ? N4A Ti2 N3A C32A 63.6(4) . . . . ? N3A Ti2 N4A C45A -8.8(3) . . . . ? N1A Ti2 N4A C45A 111.0(3) . . . . ? N2A Ti2 N4A C45A -126.5(3) . . . . ? N3A Ti2 N4A C41A -166.1(4) . . . . ? N1A Ti2 N4A C41A -46.3(4) . . . . ? N2A Ti2 N4A C41A 76.2(4) . . . . ? C1A6 C1A1 C1A2 C1A3 -0.2(6) . . . . ? C41A C1A1 C1A2 C1A3 -176.1(4) . . . . ? C1A1 C1A2 C1A3 C1A4 -0.1(7) . . . . ? C1A1 C1A2 C1A3 C3' 176.8(4) . . . . ? F31 C3' C1A3 C1A4 104.0(6) . . . . ? F33 C3' C1A3 C1A4 -137.6(6) . . . . ? F32 C3' C1A3 C1A4 -16.9(7) . . . . ? F31 C3' C1A3 C1A2 -73.0(7) . . . . ? F33 C3' C1A3 C1A2 45.4(7) . . . . ? F32 C3' C1A3 C1A2 166.1(5) . . . . ? C1A2 C1A3 C1A4 C1A5 1.1(7) . . . . ? C3' C1A3 C1A4 C1A5 -175.9(5) . . . . ? C1A3 C1A4 C1A5 C1A6 -1.7(7) . . . . ? C1A3 C1A4 C1A5 C5' 177.4(5) . . . . ? F52 C5' C1A5 C1A4 -44.8(11) . . . . ? F53 C5' C1A5 C1A4 178.0(8) . . . . ? F51 C5' C1A5 C1A4 65.5(8) . . . . ? F52 C5' C1A5 C1A6 134.4(8) . . . . ? F53 C5' C1A5 C1A6 -2.9(12) . . . . ? F51 C5' C1A5 C1A6 -115.3(7) . . . . ? C1A4 C1A5 C1A6 C1A1 1.5(8) . . . . ? C5' C1A5 C1A6 C1A1 -177.7(6) . . . . ? C1A2 C1A1 C1A6 C1A5 -0.5(7) . . . . ? C41A C1A1 C1A6 C1A5 175.6(4) . . . . ? C3A6 C3A1 C3A2 F32A -179.9(4) . . . . ? C43A C3A1 C3A2 F32A -1.0(6) . . . . ? C3A6 C3A1 C3A2 C3A3 2.0(6) . . . . ? C43A C3A1 C3A2 C3A3 -179.0(4) . . . . ? F32A C3A2 C3A3 F33A 0.6(6) . . . . ? C3A1 C3A2 C3A3 F33A 178.8(4) . . . . ? F32A C3A2 C3A3 C3A4 180.0(4) . . . . ? C3A1 C3A2 C3A3 C3A4 -1.9(7) . . . . ? F33A C3A3 C3A4 F34A 0.6(6) . . . . ? C3A2 C3A3 C3A4 F34A -178.7(4) . . . . ? F33A C3A3 C3A4 C3A5 179.9(4) . . . . ? C3A2 C3A3 C3A4 C3A5 0.5(6) . . . . ? F34A C3A4 C3A5 F35A 0.1(6) . . . . ? C3A3 C3A4 C3A5 F35A -179.1(4) . . . . ? F34A C3A4 C3A5 C3A6 179.7(4) . . . . ? C3A3 C3A4 C3A5 C3A6 0.4(7) . . . . ? F35A C3A5 C3A6 F36A -1.3(6) . . . . ? C3A4 C3A5 C3A6 F36A 179.2(4) . . . . ? F35A C3A5 C3A6 C3A1 179.4(4) . . . . ? C3A4 C3A5 C3A6 C3A1 -0.1(7) . . . . ? C3A2 C3A1 C3A6 F36A 179.7(4) . . . . ? C43A C3A1 C3A6 F36A 0.7(6) . . . . ? C3A2 C3A1 C3A6 C3A5 -1.1(6) . . . . ? C43A C3A1 C3A6 C3A5 -180.0(4) . . . . ? C45A N4A C41A C42A 0.2(4) . . . . ? Ti2 N4A C41A C42A 158.8(3) . . . . ? C45A N4A C41A C1A1 176.8(4) . . . . ? Ti2 N4A C41A C1A1 -24.6(6) . . . . ? C1A2 C1A1 C41A C42A 144.9(5) . . . . ? C1A6 C1A1 C41A C42A -30.9(6) . . . . ? C1A2 C1A1 C41A N4A -31.1(6) . . . . ? C1A6 C1A1 C41A N4A 153.0(4) . . . . ? N4A C41A C42A C43A -0.4(5) . . . . ? C1A1 C41A C42A C43A -176.9(4) . . . . ? C41A C42A C43A C45A 0.5(5) . . . . ? C41A C42A C43A C3A1 179.6(4) . . . . ? C3A6 C3A1 C43A C45A -13.5(7) . . . . ? C3A2 C3A1 C43A C45A 167.7(4) . . . . ? C3A6 C3A1 C43A C42A 167.6(4) . . . . ? C3A2 C3A1 C43A C42A -11.3(7) . . . . ? C41A N4A C45A C43A 0.2(5) . . . . ? Ti2 N4A C45A C43A -164.4(3) . . . . ? C42A C43A C45A N4A -0.4(5) . . . . ? C3A1 C43A C45A N4A -179.6(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.933 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.093 #===END data_07001 _database_code_depnum_ccdc_archive 'CCDC 809527' #TrackingRef '- structures.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34.50 H46.50 F12 N7 Ti' _chemical_formula_weight 835.19 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.809(3) _cell_length_b 17.337(3) _cell_length_c 14.513(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.545(3) _cell_angle_gamma 90.00 _cell_volume 3952.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 446(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cube _exptl_crystal_colour orange _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1730 _exptl_absorpt_coefficient_mu 0.308 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7087 _exptl_absorpt_correction_T_max 0.8010 _exptl_absorpt_process_details SADABS _exptl_special_details ; Data was collected using a BRUKER CCD (charge coupled device) based diffractometer equipped with an Oxford low-temperature apparatus operating at 173 K. A suitable crystal was chosen and mounted on a glass fiber or nylon loop using Paratone oil for Mo radiation and Mineral oil for Copper radiation. Data were measured using omega and phi scans of 0.5\% per frame for 30 s. The total number of images were based on results from the program COSMO where redundancy was expected to be 4 and completeness to 100% out to 0.83\%A. Cell parameters were retrieved using APEX II software and refined using SAINT on all observed reflections.Data reduction was performed using the SAINT software which corrects for Lp. Scaling and absorption corrections were applied using SADABS multi-scan technique, supplied by George Sheldrick. The structures are solved by the direct method using the SHELXS-97 program and refined by least squares method on F2, SHELXL-97, incorporated in SHELXTL-PC V 6.14. All H atoms were placed in calculated positions and refined using a riding model. C-H(aromatic) = 0.94 \%A and Uiso(H) = 1.2Ueq(C) C-H (alaphatic) = 0.99 \%A and Uiso(H) = 1.2Ueq(C) CH2 = 0.98 \%A and Uiso(H) = 1.2Ueq(C) CH3 = 0.97\%A and Uiso(H) = 1.5Ueq(C) N-H = 0.86 (0.92)\%A and Uiso(H) = 1.2 Ueq(N) O-H(alcohol) = 0.85\%Aand Uiso(H) = 1.2Ueq(O) O-H(acid) = 0.82\%A and Uiso(H) = 1.5Ueq(O) ; _diffrn_ambient_temperature 446(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 'CCD area detector' _diffrn_measurement_method '\w,and/f 0.5 deg' _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33477 _diffrn_reflns_av_R_equivalents 0.0787 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 23.30 _reflns_number_total 5700 _reflns_number_gt 3676 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COSMO (BRUKER, V1.56, 2007)' _computing_cell_refinement 'APEX2 (BRUKER, V2.1-0, 2007)' _computing_data_reduction 'SAINT (BRUKER, V7.34A, 2007)' _computing_structure_solution 'BRUKER, SHELXS-90, V6.14)' _computing_structure_refinement 'BRUKER, SHELXL-97, V6.14)' _computing_molecular_graphics 'SHELXTL (BRUKER, 2000, V6.14)' _computing_publication_material 'XCIF (Sheldrick and BRUKER, V6.14, 2001,)' _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^)+(0.1640P)^2^+5.5268P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0001(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5700 _refine_ls_number_parameters 521 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.1220 _refine_ls_R_factor_gt 0.0790 _refine_ls_wR_factor_ref 0.2671 _refine_ls_wR_factor_gt 0.2293 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 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 Ti Ti 0.72295(6) 0.69483(6) 1.06153(6) 0.0318(4) Uani 1 1 d . . . N1 N 0.7535(3) 0.6615(3) 0.9304(3) 0.0358(11) Uani 1 1 d . . . N2 N 0.7643(3) 0.8037(3) 1.0337(3) 0.0355(11) Uani 1 1 d . . . N3 N 0.7991(3) 0.6322(3) 1.1348(3) 0.0407(12) Uani 1 1 d . . . N4 N 0.6147(3) 0.6501(3) 1.0400(3) 0.0409(12) Uani 1 1 d . . . N5 N 0.6848(3) 0.7553(3) 1.1874(3) 0.0389(11) Uani 1 1 d . . . H5A H 0.7313 0.7812 1.2140 0.047 Uiso 1 1 calc R . . F21' F 0.9503(17) 1.0792(14) 0.737(2) 0.126(12) Uani 0.50 1 d P A 2 F22' F 0.889(2) 1.1866(14) 0.729(2) 0.137(14) Uani 0.50 1 d P A 2 F23' F 0.9605(12) 1.1494(15) 0.8504(16) 0.105(9) Uani 0.50 1 d P A 2 F131 F 0.5327(5) 0.4276(6) 0.5699(7) 0.197(4) Uani 1 1 d . . . F132 F 0.5740(4) 0.3208(5) 0.6118(9) 0.228(6) Uani 1 1 d . . . F133 F 0.5258(4) 0.3973(6) 0.6988(6) 0.197(4) Uani 1 1 d . . . F151 F 0.9286(3) 0.3386(3) 0.6736(3) 0.1072(19) Uani 1 1 d . . . F152 F 0.9406(3) 0.4347(3) 0.5857(4) 0.0920(16) Uani 1 1 d . . . F153 F 0.8663(3) 0.3415(3) 0.5359(3) 0.1004(17) Uani 1 1 d . . . F231 F 0.5537(5) 1.0635(5) 0.7293(8) 0.197(5) Uani 1 1 d . . . F232 F 0.5490(5) 1.1019(7) 0.8551(6) 0.229(6) Uani 1 1 d . . . F233 F 0.5897(4) 1.1726(4) 0.7588(7) 0.187(4) Uani 1 1 d . . . F251 F 0.9780(14) 1.0784(15) 0.777(3) 0.147(16) Uani 0.50 1 d P A 1 F252 F 0.9427(19) 1.1847(15) 0.8310(16) 0.140(12) Uani 0.50 1 d P A 1 F253 F 0.8975(16) 1.1495(15) 0.6993(15) 0.101(8) Uani 0.50 1 d P A 1 C11' C 0.7544(4) 0.5156(3) 0.7452(4) 0.0393(14) Uani 1 1 d . . . C11 C 0.7199(4) 0.5990(3) 0.8804(4) 0.0386(14) Uani 1 1 d . . . H11A H 0.6709 0.5728 0.8921 0.046 Uiso 1 1 calc R . . C12' C 0.6734(4) 0.4847(4) 0.7213(4) 0.0504(16) Uani 1 1 d . . . H12A H 0.6267 0.5060 0.7458 0.060 Uiso 1 1 calc R . . C12 C 0.7684(4) 0.5804(3) 0.8105(4) 0.0377(14) Uani 1 1 d . . . C13 C 0.8356(4) 0.6352(3) 0.8169(4) 0.0393(14) Uani 1 1 d . . . H13A H 0.8791 0.6381 0.7789 0.047 Uiso 1 1 calc R . . C13' C 0.6621(4) 0.4221(4) 0.6609(5) 0.0607(19) Uani 1 1 d . . . C14 C 0.8240(3) 0.6829(3) 0.8893(4) 0.0381(14) Uani 1 1 d . . . H14A H 0.8591 0.7243 0.9083 0.046 Uiso 1 1 calc R . . C14' C 0.7302(5) 0.3893(4) 0.6233(5) 0.0570(18) Uani 1 1 d . . . H14B H 0.7223 0.3472 0.5835 0.068 Uiso 1 1 calc R . . C15' C 0.8111(4) 0.4209(3) 0.6465(4) 0.0476(16) Uani 1 1 d . . . C16' C 0.8228(4) 0.4825(3) 0.7057(4) 0.0416(14) Uani 1 1 d . . . H16A H 0.8772 0.5028 0.7201 0.050 Uiso 1 1 calc R . . C21 C 0.7291(4) 0.8621(3) 0.9778(4) 0.0399(14) Uani 1 1 d . . . H21A H 0.6720 0.8648 0.9541 0.048 Uiso 1 1 calc R . . C21' C 0.7776(3) 0.9854(3) 0.9030(4) 0.0385(14) Uani 1 1 d . . . C22' C 0.6968(4) 1.0142(4) 0.8764(4) 0.0488(16) Uani 1 1 d . . . H22A H 0.6498 0.9899 0.8965 0.059 Uiso 1 1 calc R . . C22 C 0.7897(3) 0.9163(3) 0.9616(4) 0.0362(13) Uani 1 1 d . . . C23 C 0.8665(3) 0.8896(3) 1.0110(4) 0.0393(14) Uani 1 1 d . . . H23A H 0.9194 0.9135 1.0137 0.047 Uiso 1 1 calc R . . C23' C 0.6850(4) 1.0790(4) 0.8199(5) 0.0586(18) Uani 1 1 d . . . C24 C 0.8488(4) 0.8227(3) 1.0541(4) 0.0384(14) Uani 1 1 d . . . H24A H 0.8884 0.7938 1.0919 0.046 Uiso 1 1 calc R . . C24' C 0.7540(4) 1.1158(4) 0.7896(5) 0.0560(18) Uani 1 1 d . . . H24B H 0.7462 1.1592 0.7519 0.067 Uiso 1 1 calc R . . C25' C 0.8355(4) 1.0872(3) 0.8160(4) 0.0412(14) Uani 1 1 d . A . C26' C 0.8465(3) 1.0225(3) 0.8721(4) 0.0384(14) Uani 1 1 d . . . H26A H 0.9011 1.0036 0.8892 0.046 Uiso 1 1 calc R . . C31 C 0.8632(4) 0.6559(4) 1.2123(4) 0.0521(16) Uani 1 1 d . . . H31A H 0.8934 0.6112 1.2376 0.078 Uiso 1 1 calc R . . H31B H 0.8351 0.6805 1.2597 0.078 Uiso 1 1 calc R . . H31C H 0.9027 0.6913 1.1897 0.078 Uiso 1 1 calc R . . C32 C 0.8035(5) 0.5490(4) 1.1135(5) 0.066(2) Uani 1 1 d . . . H32A H 0.8454 0.5248 1.1571 0.099 Uiso 1 1 calc R . . H32B H 0.8189 0.5425 1.0519 0.099 Uiso 1 1 calc R . . H32C H 0.7489 0.5258 1.1175 0.099 Uiso 1 1 calc R . . C41 C 0.5800(4) 0.5768(4) 1.0678(5) 0.063(2) Uani 1 1 d . . . H41A H 0.5209 0.5735 1.0441 0.095 Uiso 1 1 calc R . . H41B H 0.5856 0.5736 1.1343 0.095 Uiso 1 1 calc R . . H41C H 0.6106 0.5350 1.0435 0.095 Uiso 1 1 calc R . . C42 C 0.5549(4) 0.6929(4) 0.9760(4) 0.0537(17) Uani 1 1 d . . . H42A H 0.5011 0.6667 0.9687 0.080 Uiso 1 1 calc R . . H42B H 0.5765 0.6966 0.9169 0.080 Uiso 1 1 calc R . . H42C H 0.5476 0.7438 1.0000 0.080 Uiso 1 1 calc R . . C51 C 0.6588(5) 0.7008(4) 1.2579(4) 0.0582(18) Uani 1 1 d . . . H51A H 0.6434 0.7293 1.3102 0.087 Uiso 1 1 calc R . . H51B H 0.7053 0.6669 1.2777 0.087 Uiso 1 1 calc R . . H51C H 0.6109 0.6710 1.2314 0.087 Uiso 1 1 calc R . . C52 C 0.6167(4) 0.8127(4) 1.1650(5) 0.0585(18) Uani 1 1 d . . . H52A H 0.6032 0.8368 1.2210 0.088 Uiso 1 1 calc R . . H52B H 0.5669 0.7875 1.1350 0.088 Uiso 1 1 calc R . . H52C H 0.6356 0.8511 1.1243 0.088 Uiso 1 1 calc R . . C131 C 0.5758(6) 0.3903(6) 0.6386(7) 0.085(3) Uani 1 1 d . . . C151 C 0.8859(5) 0.3842(4) 0.6118(5) 0.0557(17) Uani 1 1 d . . . C231 C 0.5986(6) 1.1074(6) 0.7924(9) 0.095(3) Uani 1 1 d . . . C251 C 0.9103(5) 1.1255(5) 0.7826(5) 0.0614(19) Uani 1 1 d . . . N2SC N 0.7307(18) 0.371(2) 0.9442(18) 0.114(11) Uiso 0.25 1 d PD B 1 H2SC H 0.6956 0.3746 0.8946 0.136 Uiso 0.25 1 calc PR B 1 C1SC C 0.7046(11) 0.3577(11) 1.0398(11) 0.070(5) Uiso 0.50 1 d PD B 1 H1S1 H 0.6436 0.3568 1.0364 0.105 Uiso 0.50 1 calc PR B 1 H1S2 H 0.7265 0.3986 1.0802 0.105 Uiso 0.50 1 calc PR B 1 H1S3 H 0.7271 0.3093 1.0636 0.105 Uiso 0.50 1 calc PR B 1 C2SC C 0.8239(16) 0.376(2) 0.947(2) 0.126(12) Uiso 0.33 1 d PD B 1 H2S1 H 0.8384 0.3882 0.8860 0.189 Uiso 0.33 1 calc PR B 1 H2S2 H 0.8492 0.3279 0.9670 0.189 Uiso 0.33 1 calc PR B 1 H2S3 H 0.8448 0.4162 0.9893 0.189 Uiso 0.33 1 calc PR B 1 N2SD N 0.664(2) 0.357(2) 0.9328(17) 0.132(13) Uiso 0.25 1 d PD C 2 H2SD H 0.6274 0.3809 0.8938 0.158 Uiso 0.25 1 calc PR C 2 C1SD C 0.6774(11) 0.3816(10) 1.0270(11) 0.065(5) Uiso 0.50 1 d PD C 2 H1S4 H 0.6236 0.3928 1.0489 0.097 Uiso 0.50 1 calc PR C 2 H1S5 H 0.7123 0.4270 1.0317 0.097 Uiso 0.50 1 calc PR C 2 H1S6 H 0.7055 0.3412 1.0640 0.097 Uiso 0.50 1 calc PR C 2 C2SD C 0.713(4) 0.291(3) 0.903(3) 0.23(3) Uiso 0.33 1 d PD C 2 H2S4 H 0.6975 0.2813 0.8383 0.340 Uiso 0.33 1 calc PR C 2 H2S5 H 0.7006 0.2459 0.9381 0.340 Uiso 0.33 1 calc PR C 2 H2S6 H 0.7727 0.3021 0.9142 0.340 Uiso 0.33 1 calc PR C 2 N2SB N 0.7606(13) 0.3224(16) 0.8981(18) 0.174(10) Uiso 0.50 1 d PD D 3 H2SB H 0.8019 0.3161 0.8649 0.209 Uiso 0.50 1 calc PR D 3 C2SB C 0.6654(11) 0.3021(11) 0.8687(13) 0.087(5) Uiso 0.50 1 d PD D 3 H2S7 H 0.6602 0.2753 0.8104 0.130 Uiso 0.50 1 calc PR D 3 H2S8 H 0.6324 0.3487 0.8625 0.130 Uiso 0.50 1 calc PR D 3 H2S9 H 0.6449 0.2698 0.9151 0.130 Uiso 0.50 1 calc PR D 3 C1SB C 0.768(2) 0.355(3) 0.995(2) 0.171(18) Uiso 0.33 1 d PD D 3 H1S7 H 0.8266 0.3623 1.0172 0.257 Uiso 0.33 1 calc PR D 3 H1S8 H 0.7422 0.3199 1.0345 0.257 Uiso 0.33 1 calc PR D 3 H1S9 H 0.7386 0.4037 0.9936 0.257 Uiso 0.33 1 calc PR D 3 C1S C 0.9686(8) 0.3152(7) 0.9801(9) 0.036(3) Uiso 0.50 1 d PD E 5 H1SX H 0.9415 0.2656 0.9756 0.055 Uiso 0.50 1 calc PR E 5 H1SY H 0.9824 0.3286 1.0442 0.055 Uiso 0.50 1 calc PR E 5 H1SZ H 1.0198 0.3135 0.9504 0.055 Uiso 0.50 1 calc PR E 5 C2S C 0.9423(11) 0.4544(9) 0.9257(12) 0.075(5) Uiso 0.50 1 d PD E 5 H2SX H 0.9003 0.4853 0.8897 0.113 Uiso 0.50 1 calc PR E 5 H2SY H 0.9934 0.4532 0.8957 0.113 Uiso 0.50 1 calc PR E 5 H2SZ H 0.9546 0.4763 0.9865 0.113 Uiso 0.50 1 calc PR E 5 N1S N 0.9094(18) 0.3745(13) 0.933(2) 0.265(18) Uiso 0.50 1 d PD E 5 H1S H 0.8581 0.3628 0.9120 0.318 Uiso 0.50 1 calc PR E 5 C2SA C 0.9576(7) 0.4836(7) 0.9392(8) 0.033(3) Uiso 0.50 1 d PD F 4 H2SA H 0.9771 0.5300 0.9709 0.049 Uiso 0.50 1 calc PR F 4 H2SE H 0.8965 0.4821 0.9329 0.049 Uiso 0.50 1 calc PR F 4 H2SF H 0.9768 0.4827 0.8788 0.049 Uiso 0.50 1 calc PR F 4 C1SA C 0.966(2) 0.3376(10) 0.954(2) 0.135(11) Uiso 0.50 1 d PD F 4 H1SA H 0.9905 0.2966 0.9926 0.203 Uiso 0.50 1 calc PR F 4 H1SB H 0.9849 0.3334 0.8934 0.203 Uiso 0.50 1 calc PR F 4 H1SC H 0.9051 0.3341 0.9484 0.203 Uiso 0.50 1 calc PR F 4 N1SA N 0.9935(15) 0.4128(11) 0.9955(15) 0.161(8) Uiso 0.50 1 d PD F 4 H1SD H 1.0266 0.4167 1.0466 0.194 Uiso 0.50 1 calc PR F 4 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti 0.0317(6) 0.0380(6) 0.0260(6) -0.0004(4) 0.0047(4) -0.0009(4) N1 0.040(3) 0.042(3) 0.027(2) 0.000(2) 0.009(2) -0.005(2) N2 0.034(3) 0.039(3) 0.033(3) 0.000(2) 0.004(2) -0.002(2) N3 0.044(3) 0.042(3) 0.036(3) 0.002(2) 0.005(2) 0.003(2) N4 0.042(3) 0.044(3) 0.038(3) -0.008(2) 0.008(2) -0.006(2) N5 0.034(3) 0.049(3) 0.034(3) -0.005(2) 0.005(2) -0.001(2) F21' 0.11(2) 0.109(19) 0.17(2) -0.044(18) 0.101(18) -0.043(15) F22' 0.087(11) 0.101(14) 0.21(4) 0.110(17) -0.015(17) -0.022(12) F23' 0.064(8) 0.15(2) 0.095(10) 0.044(14) -0.015(7) -0.068(11) F131 0.093(5) 0.285(12) 0.199(8) 0.039(8) -0.053(5) -0.062(6) F132 0.090(5) 0.144(7) 0.444(16) -0.166(9) -0.001(7) -0.041(4) F133 0.104(5) 0.293(11) 0.206(8) -0.122(8) 0.070(6) -0.121(6) F151 0.119(4) 0.118(4) 0.090(3) 0.028(3) 0.034(3) 0.068(4) F152 0.085(3) 0.075(3) 0.127(4) -0.007(3) 0.063(3) 0.004(3) F153 0.105(4) 0.112(4) 0.089(3) -0.049(3) 0.032(3) 0.019(3) F231 0.089(5) 0.179(8) 0.301(12) -0.034(8) -0.077(7) 0.051(5) F232 0.136(6) 0.370(14) 0.198(8) 0.158(10) 0.090(6) 0.177(8) F233 0.076(4) 0.126(5) 0.352(12) 0.126(7) -0.004(5) 0.030(4) F251 0.051(9) 0.13(2) 0.27(3) 0.13(2) 0.078(13) 0.035(11) F252 0.19(2) 0.121(17) 0.112(19) -0.030(13) 0.042(16) -0.111(17) F253 0.072(10) 0.16(2) 0.075(9) 0.074(13) 0.000(6) -0.031(16) C11' 0.043(4) 0.043(3) 0.033(3) -0.001(3) 0.008(3) 0.001(3) C11 0.038(3) 0.047(4) 0.031(3) 0.001(3) 0.006(3) -0.009(3) C12' 0.044(4) 0.058(4) 0.050(4) -0.009(3) 0.009(3) -0.002(3) C12 0.040(3) 0.042(3) 0.032(3) -0.002(3) 0.008(3) 0.001(3) C13 0.040(3) 0.041(3) 0.039(3) -0.003(3) 0.013(3) 0.002(3) C13' 0.057(4) 0.059(4) 0.066(5) -0.017(4) 0.007(4) -0.012(3) C14 0.035(3) 0.042(3) 0.038(3) -0.004(3) 0.006(3) -0.006(3) C14' 0.068(5) 0.051(4) 0.053(4) -0.015(3) 0.012(3) -0.004(4) C15' 0.063(4) 0.044(4) 0.038(3) -0.003(3) 0.016(3) 0.001(3) C16' 0.045(3) 0.040(3) 0.041(3) -0.002(3) 0.009(3) -0.003(3) C21 0.034(3) 0.046(4) 0.040(3) -0.001(3) 0.008(3) 0.001(3) C21' 0.039(3) 0.040(3) 0.037(3) 0.000(3) 0.006(3) 0.001(3) C22' 0.040(4) 0.050(4) 0.058(4) 0.006(3) 0.015(3) 0.003(3) C22 0.038(3) 0.040(3) 0.031(3) -0.001(2) 0.009(2) 0.000(3) C23 0.029(3) 0.047(4) 0.042(3) 0.000(3) 0.002(3) -0.008(3) C23' 0.047(4) 0.058(4) 0.072(5) 0.019(4) 0.010(3) 0.014(3) C24 0.037(3) 0.040(3) 0.038(3) 0.003(3) 0.003(3) 0.000(3) C24' 0.062(5) 0.047(4) 0.059(4) 0.018(3) 0.005(3) 0.010(3) C25' 0.046(4) 0.042(3) 0.035(3) 0.000(3) 0.004(3) -0.005(3) C26' 0.033(3) 0.046(3) 0.036(3) 0.003(3) 0.001(2) -0.004(3) C31 0.047(4) 0.067(4) 0.041(4) 0.009(3) 0.002(3) 0.005(3) C32 0.079(5) 0.050(4) 0.067(5) -0.003(4) -0.004(4) 0.008(4) C41 0.059(4) 0.064(5) 0.071(5) -0.005(4) 0.023(4) -0.023(4) C42 0.036(3) 0.083(5) 0.041(4) 0.000(3) 0.000(3) -0.009(3) C51 0.072(5) 0.068(5) 0.039(4) 0.002(3) 0.026(3) 0.002(4) C52 0.051(4) 0.074(5) 0.051(4) -0.019(3) 0.008(3) 0.017(3) C131 0.066(6) 0.093(7) 0.098(7) -0.048(6) 0.015(5) -0.020(5) C151 0.067(5) 0.047(4) 0.055(4) -0.002(3) 0.014(4) 0.008(4) C231 0.059(6) 0.097(7) 0.133(9) 0.050(7) 0.026(6) 0.026(5) C251 0.062(5) 0.066(5) 0.055(5) 0.010(4) 0.001(4) -0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti N3 1.862(5) . ? Ti N4 1.873(5) . ? Ti N2 2.053(5) . ? Ti N1 2.098(4) . ? Ti N5 2.248(4) . ? N1 C11 1.376(7) . ? N1 C14 1.373(7) . ? N2 C21 1.374(7) . ? N2 C24 1.375(7) . ? N3 C32 1.478(8) . ? N3 C31 1.484(7) . ? N4 C41 1.460(8) . ? N4 C42 1.451(8) . ? N5 C52 1.476(7) . ? N5 C51 1.484(7) . ? N5 H5A 0.9100 . ? F21' C251 1.26(2) . ? F22' C251 1.34(2) . ? F23' C251 1.26(2) . ? F131 C131 1.312(12) . ? F132 C131 1.265(10) . ? F133 C131 1.249(10) . ? F151 C151 1.322(8) . ? F152 C151 1.316(8) . ? F153 C151 1.334(8) . ? F231 C231 1.332(13) . ? F232 C231 1.270(11) . ? F233 C231 1.234(10) . ? F251 C251 1.36(2) . ? F252 C251 1.31(2) . ? F253 C251 1.27(2) . ? C11' C12' 1.395(8) . ? C11' C16' 1.403(8) . ? C11' C12 1.471(8) . ? C11 C12 1.377(7) . ? C11 H11A 0.9300 . ? C12' C13' 1.394(9) . ? C12' H12A 0.9300 . ? C12 C13 1.420(8) . ? C13 C14 1.366(8) . ? C13 H13A 0.9300 . ? C13' C14' 1.383(9) . ? C13' C131 1.473(11) . ? C14 H14A 0.9300 . ? C14' C15' 1.397(9) . ? C14' H14B 0.9300 . ? C15' C16' 1.371(8) . ? C15' C151 1.482(9) . ? C16' H16A 0.9300 . ? C21 C22 1.381(8) . ? C21 H21A 0.9300 . ? C21' C22' 1.384(8) . ? C21' C26' 1.383(8) . ? C21' C22 1.470(8) . ? C22' C23' 1.390(9) . ? C22' H22A 0.9300 . ? C22 C23 1.414(8) . ? C23 C24 1.362(8) . ? C23 H23A 0.9300 . ? C23' C24' 1.377(9) . ? C23' C231 1.464(11) . ? C24 H24A 0.9300 . ? C24' C25' 1.393(9) . ? C24' H24B 0.9300 . ? C25' C26' 1.387(8) . ? C25' C251 1.484(9) . ? C26' H26A 0.9300 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? N2SC C1SC 1.509(19) . ? N2SC C2SC 1.473(19) . ? N2SC H2SC 0.8600 . ? C1SC H1S1 0.9600 . ? C1SC H1S2 0.9600 . ? C1SC H1S3 0.9600 . ? C2SC H2S1 0.9600 . ? C2SC H2S2 0.9600 . ? C2SC H2S3 0.9600 . ? N2SD C1SD 1.422(19) . ? N2SD C2SD 1.49(2) . ? N2SD H2SD 0.8600 . ? C1SD H1S4 0.9600 . ? C1SD H1S5 0.9600 . ? C1SD H1S6 0.9600 . ? C2SD H2S4 0.9600 . ? C2SD H2S5 0.9600 . ? C2SD H2S6 0.9600 . ? N2SB C2SB 1.558(18) . ? N2SB C1SB 1.502(19) . ? N2SB H2SB 0.8600 . ? C2SB H2S7 0.9600 . ? C2SB H2S8 0.9600 . ? C2SB H2S9 0.9600 . ? C1SB H1S7 0.9600 . ? C1SB H1S8 0.9600 . ? C1SB H1S9 0.9600 . ? C1S N1S 1.499(19) . ? C1S H1SX 0.9600 . ? C1S H1SY 0.9600 . ? C1S H1SZ 0.9600 . ? C2S N1S 1.489(18) . ? C2S H2SX 0.9600 . ? C2S H2SY 0.9600 . ? C2S H2SZ 0.9600 . ? N1S H1S 0.8600 . ? C2SA N1SA 1.547(16) . ? C2SA H2SA 0.9600 . ? C2SA H2SE 0.9600 . ? C2SA H2SF 0.9600 . ? C1SA N1SA 1.481(17) . ? C1SA H1SA 0.9600 . ? C1SA H1SB 0.9600 . ? C1SA H1SC 0.9600 . ? N1SA H1SD 0.8600 . ? 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 N3 Ti N4 111.9(2) . . ? N3 Ti N2 116.7(2) . . ? N4 Ti N2 130.8(2) . . ? N3 Ti N1 99.03(19) . . ? N4 Ti N1 92.01(19) . . ? N2 Ti N1 87.89(18) . . ? N3 Ti N5 91.33(18) . . ? N4 Ti N5 90.21(18) . . ? N2 Ti N5 81.54(17) . . ? N1 Ti N5 167.72(18) . . ? C11 N1 C14 105.6(4) . . ? C11 N1 Ti 125.5(3) . . ? C14 N1 Ti 126.9(4) . . ? C21 N2 C24 105.6(4) . . ? C21 N2 Ti 132.6(4) . . ? C24 N2 Ti 120.1(4) . . ? C32 N3 C31 112.6(5) . . ? C32 N3 Ti 119.4(4) . . ? C31 N3 Ti 127.8(4) . . ? C41 N4 C42 112.6(5) . . ? C41 N4 Ti 132.8(4) . . ? C42 N4 Ti 114.3(4) . . ? C52 N5 C51 109.2(5) . . ? C52 N5 Ti 113.1(3) . . ? C51 N5 Ti 112.6(4) . . ? C52 N5 H5A 107.2 . . ? C51 N5 H5A 107.2 . . ? Ti N5 H5A 107.2 . . ? C12' C11' C16' 118.1(5) . . ? C12' C11' C12 121.3(5) . . ? C16' C11' C12 120.6(5) . . ? N1 C11 C12 111.0(5) . . ? N1 C11 H11A 124.5 . . ? C12 C11 H11A 124.5 . . ? C13' C12' C11' 120.2(6) . . ? C13' C12' H12A 119.9 . . ? C11' C12' H12A 119.9 . . ? C11 C12 C13 105.7(5) . . ? C11 C12 C11' 126.7(5) . . ? C13 C12 C11' 127.6(5) . . ? C14 C13 C12 106.8(5) . . ? C14 C13 H13A 126.6 . . ? C12 C13 H13A 126.6 . . ? C14' C13' C12' 121.3(6) . . ? C14' C13' C131 120.1(6) . . ? C12' C13' C131 118.6(7) . . ? C13 C14 N1 110.9(5) . . ? C13 C14 H14A 124.5 . . ? N1 C14 H14A 124.5 . . ? C13' C14' C15' 118.4(6) . . ? C13' C14' H14B 120.8 . . ? C15' C14' H14B 120.8 . . ? C16' C15' C14' 120.8(6) . . ? C16' C15' C151 119.4(6) . . ? C14' C15' C151 119.7(6) . . ? C15' C16' C11' 121.2(6) . . ? C15' C16' H16A 119.4 . . ? C11' C16' H16A 119.4 . . ? N2 C21 C22 111.0(5) . . ? N2 C21 H21A 124.5 . . ? C22 C21 H21A 124.5 . . ? C22' C21' C26' 118.5(5) . . ? C22' C21' C22 120.8(5) . . ? C26' C21' C22 120.7(5) . . ? C21' C22' C23' 120.9(6) . . ? C21' C22' H22A 119.6 . . ? C23' C22' H22A 119.6 . . ? C21 C22 C23 105.3(5) . . ? C21 C22 C21' 127.3(5) . . ? C23 C22 C21' 127.4(5) . . ? C24 C23 C22 107.6(5) . . ? C24 C23 H23A 126.2 . . ? C22 C23 H23A 126.2 . . ? C24' C23' C22' 120.3(6) . . ? C24' C23' C231 120.4(7) . . ? C22' C23' C231 119.4(7) . . ? C23 C24 N2 110.4(5) . . ? C23 C24 H24A 124.8 . . ? N2 C24 H24A 124.8 . . ? C23' C24' C25' 119.3(6) . . ? C23' C24' H24B 120.3 . . ? C25' C24' H24B 120.3 . . ? C26' C25' C24' 119.9(6) . . ? C26' C25' C251 120.2(6) . . ? C24' C25' C251 119.9(6) . . ? C21' C26' C25' 121.1(5) . . ? C21' C26' H26A 119.5 . . ? C25' C26' H26A 119.5 . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N4 C42 H42A 109.5 . . ? N4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N5 C51 H51A 109.5 . . ? N5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N5 C52 H52A 109.5 . . ? N5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? F133 C131 F132 108.3(10) . . ? F133 C131 F131 99.7(10) . . ? F132 C131 F131 104.1(9) . . ? F133 C131 C13' 116.9(8) . . ? F132 C131 C13' 114.4(8) . . ? F131 C131 C13' 111.7(9) . . ? F152 C151 F151 107.0(6) . . ? F152 C151 F153 103.3(6) . . ? F151 C151 F153 106.3(6) . . ? F152 C151 C15' 112.9(6) . . ? F151 C151 C15' 113.0(6) . . ? F153 C151 C15' 113.6(6) . . ? F233 C231 F232 107.5(10) . . ? F233 C231 F231 103.0(10) . . ? F232 C231 F231 97.3(10) . . ? F233 C231 C23' 118.4(9) . . ? F232 C231 C23' 114.3(9) . . ? F231 C231 C23' 113.8(9) . . ? F253 C251 F23' 130.7(14) . . ? F253 C251 F21' 75.1(18) . . ? F23' C251 F21' 108.1(18) . . ? F253 C251 F22' 35.3(15) . . ? F23' C251 F22' 106.9(17) . . ? F21' C251 F22' 107.9(19) . . ? F253 C251 F252 105.3(14) . . ? F23' C251 F252 32.3(14) . . ? F21' C251 F252 126.2(18) . . ? F22' C251 F252 75.6(17) . . ? F253 C251 F251 100.4(17) . . ? F23' C251 F251 79.3(18) . . ? F21' C251 F251 30.1(19) . . ? F22' C251 F251 126.2(17) . . ? F252 C251 F251 103.9(18) . . ? F253 C251 C25' 114.2(13) . . ? F23' C251 C25' 110.3(11) . . ? F21' C251 C25' 110.7(12) . . ? F22' C251 C25' 112.8(15) . . ? F252 C251 C25' 116.9(13) . . ? F251 C251 C25' 114.4(12) . . ? C1SC N2SC C2SC 111.3(18) . . ? C1SC N2SC H2SC 124.4 . . ? C2SC N2SC H2SC 124.4 . . ? N2SC C1SC H1S1 109.5 . . ? N2SC C1SC H1S2 109.5 . . ? H1S1 C1SC H1S2 109.5 . . ? N2SC C1SC H1S3 109.5 . . ? H1S1 C1SC H1S3 109.5 . . ? H1S2 C1SC H1S3 109.5 . . ? N2SC C2SC H2S1 109.5 . . ? N2SC C2SC H2S2 109.5 . . ? H2S1 C2SC H2S2 109.5 . . ? N2SC C2SC H2S3 109.5 . . ? H2S1 C2SC H2S3 109.5 . . ? H2S2 C2SC H2S3 109.5 . . ? C1SD N2SD C2SD 119(2) . . ? C1SD N2SD H2SD 120.7 . . ? C2SD N2SD H2SD 120.7 . . ? N2SD C1SD H1S4 109.5 . . ? N2SD C1SD H1S5 109.5 . . ? H1S4 C1SD H1S5 109.5 . . ? N2SD C1SD H1S6 109.5 . . ? H1S4 C1SD H1S6 109.5 . . ? H1S5 C1SD H1S6 109.5 . . ? N2SD C2SD H2S4 109.5 . . ? N2SD C2SD H2S5 109.5 . . ? H2S4 C2SD H2S5 109.5 . . ? N2SD C2SD H2S6 109.5 . . ? H2S4 C2SD H2S6 109.5 . . ? H2S5 C2SD H2S6 109.5 . . ? C2SB N2SB C1SB 107.8(17) . . ? C2SB N2SB H2SB 126.1 . . ? C1SB N2SB H2SB 126.1 . . ? N2SB C2SB H2S7 109.5 . . ? N2SB C2SB H2S8 109.5 . . ? H2S7 C2SB H2S8 109.5 . . ? N2SB C2SB H2S9 109.5 . . ? H2S7 C2SB H2S9 109.5 . . ? H2S8 C2SB H2S9 109.5 . . ? N2SB C1SB H1S7 109.5 . . ? N2SB C1SB H1S8 109.5 . . ? H1S7 C1SB H1S8 109.5 . . ? N2SB C1SB H1S9 109.5 . . ? H1S7 C1SB H1S9 109.5 . . ? H1S8 C1SB H1S9 109.5 . . ? N1S C1S H1SX 109.5 . . ? N1S C1S H1SY 109.5 . . ? H1SX C1S H1SY 109.5 . . ? N1S C1S H1SZ 109.5 . . ? H1SX C1S H1SZ 109.5 . . ? H1SY C1S H1SZ 109.5 . . ? N1S C2S H2SX 109.5 . . ? N1S C2S H2SY 109.5 . . ? H2SX C2S H2SY 109.5 . . ? N1S C2S H2SZ 109.5 . . ? H2SX C2S H2SZ 109.5 . . ? H2SY C2S H2SZ 109.5 . . ? C1S N1S C2S 117.8(19) . . ? C1S N1S H1S 121.1 . . ? C2S N1S H1S 121.1 . . ? N1SA C2SA H2SA 109.5 . . ? N1SA C2SA H2SE 109.5 . . ? H2SA C2SA H2SE 109.5 . . ? N1SA C2SA H2SF 109.5 . . ? H2SA C2SA H2SF 109.5 . . ? H2SE C2SA H2SF 109.5 . . ? N1SA C1SA H1SA 109.5 . . ? N1SA C1SA H1SB 109.5 . . ? H1SA C1SA H1SB 109.5 . . ? N1SA C1SA H1SC 109.5 . . ? H1SA C1SA H1SC 109.5 . . ? H1SB C1SA H1SC 109.5 . . ? C1SA N1SA C2SA 114.2(16) . . ? C1SA N1SA H1SD 122.9 . . ? C2SA N1SA H1SD 122.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ti N1 C11 85.5(5) . . . . ? N4 Ti N1 C11 -27.0(5) . . . . ? N2 Ti N1 C11 -157.8(5) . . . . ? N5 Ti N1 C11 -127.3(8) . . . . ? N3 Ti N1 C14 -75.9(5) . . . . ? N4 Ti N1 C14 171.5(5) . . . . ? N2 Ti N1 C14 40.8(5) . . . . ? N5 Ti N1 C14 71.3(10) . . . . ? N3 Ti N2 C21 174.3(5) . . . . ? N4 Ti N2 C21 -15.6(6) . . . . ? N1 Ti N2 C21 75.2(5) . . . . ? N5 Ti N2 C21 -98.5(5) . . . . ? N3 Ti N2 C24 11.6(5) . . . . ? N4 Ti N2 C24 -178.3(4) . . . . ? N1 Ti N2 C24 -87.4(4) . . . . ? N5 Ti N2 C24 98.8(4) . . . . ? N4 Ti N3 C32 46.3(5) . . . . ? N2 Ti N3 C32 -141.7(5) . . . . ? N1 Ti N3 C32 -49.5(5) . . . . ? N5 Ti N3 C32 137.1(5) . . . . ? N4 Ti N3 C31 -138.1(5) . . . . ? N2 Ti N3 C31 33.8(5) . . . . ? N1 Ti N3 C31 126.0(5) . . . . ? N5 Ti N3 C31 -47.4(5) . . . . ? N3 Ti N4 C41 -1.2(6) . . . . ? N2 Ti N4 C41 -171.6(5) . . . . ? N1 Ti N4 C41 99.4(5) . . . . ? N5 Ti N4 C41 -92.7(5) . . . . ? N3 Ti N4 C42 -174.4(4) . . . . ? N2 Ti N4 C42 15.1(5) . . . . ? N1 Ti N4 C42 -73.8(4) . . . . ? N5 Ti N4 C42 94.1(4) . . . . ? N3 Ti N5 C52 -176.9(4) . . . . ? N4 Ti N5 C52 -65.0(4) . . . . ? N2 Ti N5 C52 66.3(4) . . . . ? N1 Ti N5 C52 35.5(10) . . . . ? N3 Ti N5 C51 -52.5(4) . . . . ? N4 Ti N5 C51 59.5(4) . . . . ? N2 Ti N5 C51 -169.2(4) . . . . ? N1 Ti N5 C51 159.9(8) . . . . ? C14 N1 C11 C12 1.0(6) . . . . ? Ti N1 C11 C12 -163.7(4) . . . . ? C16' C11' C12' C13' 0.8(9) . . . . ? C12 C11' C12' C13' -178.5(6) . . . . ? N1 C11 C12 C13 -0.7(6) . . . . ? N1 C11 C12 C11' 177.5(5) . . . . ? C12' C11' C12 C11 26.9(9) . . . . ? C16' C11' C12 C11 -152.4(6) . . . . ? C12' C11' C12 C13 -155.2(6) . . . . ? C16' C11' C12 C13 25.5(9) . . . . ? C11 C12 C13 C14 0.2(6) . . . . ? C11' C12 C13 C14 -178.1(5) . . . . ? C11' C12' C13' C14' -0.1(11) . . . . ? C11' C12' C13' C131 179.0(8) . . . . ? C12 C13 C14 N1 0.4(7) . . . . ? C11 N1 C14 C13 -0.9(6) . . . . ? Ti N1 C14 C13 163.5(4) . . . . ? C12' C13' C14' C15' -0.6(11) . . . . ? C131 C13' C14' C15' -179.7(8) . . . . ? C13' C14' C15' C16' 0.5(10) . . . . ? C13' C14' C15' C151 176.4(6) . . . . ? C14' C15' C16' C11' 0.3(9) . . . . ? C151 C15' C16' C11' -175.7(6) . . . . ? C12' C11' C16' C15' -1.0(9) . . . . ? C12 C11' C16' C15' 178.3(5) . . . . ? C24 N2 C21 C22 1.0(6) . . . . ? Ti N2 C21 C22 -163.5(4) . . . . ? C26' C21' C22' C23' -0.1(9) . . . . ? C22 C21' C22' C23' -179.1(6) . . . . ? N2 C21 C22 C23 -0.4(6) . . . . ? N2 C21 C22 C21' 177.8(5) . . . . ? C22' C21' C22 C21 17.3(9) . . . . ? C26' C21' C22 C21 -161.7(6) . . . . ? C22' C21' C22 C23 -164.9(6) . . . . ? C26' C21' C22 C23 16.1(9) . . . . ? C21 C22 C23 C24 -0.4(6) . . . . ? C21' C22 C23 C24 -178.5(5) . . . . ? C21' C22' C23' C24' -0.1(11) . . . . ? C21' C22' C23' C231 179.4(8) . . . . ? C22 C23 C24 N2 1.0(6) . . . . ? C21 N2 C24 C23 -1.2(6) . . . . ? Ti N2 C24 C23 165.6(4) . . . . ? C22' C23' C24' C25' 0.1(11) . . . . ? C231 C23' C24' C25' -179.4(8) . . . . ? C23' C24' C25' C26' 0.0(10) . . . . ? C23' C24' C25' C251 179.1(7) . . . . ? C22' C21' C26' C25' 0.2(9) . . . . ? C22 C21' C26' C25' 179.3(5) . . . . ? C24' C25' C26' C21' -0.2(9) . . . . ? C251 C25' C26' C21' -179.2(6) . . . . ? C14' C13' C131 F133 150.5(10) . . . . ? C12' C13' C131 F133 -28.5(14) . . . . ? C14' C13' C131 F132 22.5(15) . . . . ? C12' C13' C131 F132 -156.6(10) . . . . ? C14' C13' C131 F131 -95.5(11) . . . . ? C12' C13' C131 F131 85.4(11) . . . . ? C16' C15' C151 F152 -44.1(9) . . . . ? C14' C15' C151 F152 139.9(6) . . . . ? C16' C15' C151 F151 77.5(8) . . . . ? C14' C15' C151 F151 -98.5(8) . . . . ? C16' C15' C151 F153 -161.2(6) . . . . ? C14' C15' C151 F153 22.8(9) . . . . ? C24' C23' C231 F233 -15.0(16) . . . . ? C22' C23' C231 F233 165.5(10) . . . . ? C24' C23' C231 F232 -143.3(11) . . . . ? C22' C23' C231 F232 37.2(15) . . . . ? C24' C23' C231 F231 106.2(11) . . . . ? C22' C23' C231 F231 -73.3(12) . . . . ? C26' C25' C251 F253 140.9(15) . . . . ? C24' C25' C251 F253 -38.1(17) . . . . ? C26' C25' C251 F23' -61.1(17) . . . . ? C24' C25' C251 F23' 119.9(16) . . . . ? C26' C25' C251 F21' 58.5(19) . . . . ? C24' C25' C251 F21' -120.5(18) . . . . ? C26' C25' C251 F22' 179.5(16) . . . . ? C24' C25' C251 F22' 0.5(18) . . . . ? C26' C25' C251 F252 -95.6(18) . . . . ? C24' C25' C251 F252 85.4(18) . . . . ? C26' C25' C251 F251 26(2) . . . . ? C24' C25' C251 F251 -153(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.30 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.650 _refine_diff_density_min -0.549 _refine_diff_density_rms 0.082