# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Dr Simon J Lancaster' _publ_contact_author_address ; School of Chemical Sciences and Pharmacy University of East Anglia Earlham Road Norwich NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email S.LANCASTER@UEA.AC.UK _publ_section_title ; New Titanium and Zirconium Complexes with M-NH2 bonds formed by Facile Deprotonation of H3N*B(C6F5)3 ; loop_ _publ_author_name 'Simon J. Lancaster' 'William Clegg' 'Ross W. Harrington' 'Simon Humphrey' 'Andrew J. Mountford' data_ssd0056 _database_code_depnum_ccdc_archive 'CCDC 258171' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H27 B F15 N5 Zr' _chemical_formula_sum 'C26 H27 B F15 N5 Zr' _chemical_formula_weight 796.56 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' B B 0.0013 0.0007 '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' Zr Zr -7.1640 0.5320 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 10.7826(18) _cell_length_b 16.140(3) _cell_length_c 17.502(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3045.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 6294 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 28.70 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.737 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 0.481 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6892 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 15 _diffrn_reflns_number 20458 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.66 _diffrn_reflns_theta_max 29.47 _reflns_number_total 6128 _reflns_number_gt 4943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'SHELXL-97 (Sheldrick)' _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^)+(0.0531P)^2^+1.7023P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0088(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_number_reflns 6128 _refine_ls_number_parameters 454 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.1066 _refine_ls_wR_factor_gt 0.0957 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.76859(3) 0.25922(2) 0.57154(3) 0.01239(10) Uani 1 1 d . . . B1 B 0.4649(4) 0.2217(3) 0.6394(3) 0.0166(8) Uani 1 1 d . . . N1 N 0.6071(3) 0.1965(2) 0.6415(2) 0.0184(7) Uani 1 1 d . . . H1A H 0.627(4) 0.192(3) 0.694(4) 0.031(13) Uiso 1 1 d . . . H1B H 0.619(6) 0.144(4) 0.624(4) 0.056(19) Uiso 1 1 d . . . N2 N 0.7590(3) 0.1660(2) 0.4934(2) 0.0266(8) Uani 1 1 d . . . N3 N 0.8822(3) 0.2469(2) 0.6633(2) 0.0267(8) Uani 1 1 d . . . N4 N 0.6938(3) 0.3725(2) 0.5486(2) 0.0251(8) Uani 1 1 d . . . N5 N 0.9397(3) 0.3081(2) 0.4938(2) 0.0272(8) Uani 1 1 d . . . H5 H 0.905(5) 0.324(4) 0.445(4) 0.055(19) Uiso 1 1 d . . . F2 F 0.5028(2) 0.16072(15) 0.79156(15) 0.0255(5) Uani 1 1 d . . . F3 F 0.3821(3) 0.04129(18) 0.86549(17) 0.0383(7) Uani 1 1 d . . . F4 F 0.1877(3) -0.03847(16) 0.79697(19) 0.0396(7) Uani 1 1 d . . . F5 F 0.1149(2) 0.00777(16) 0.65488(18) 0.0341(7) Uani 1 1 d . . . F6 F 0.2317(2) 0.12654(14) 0.5803(2) 0.0287(6) Uani 1 1 d . . . F8 F 0.4746(2) 0.09147(14) 0.52818(15) 0.0248(5) Uani 1 1 d . . . F9 F 0.4153(2) 0.09705(17) 0.38086(16) 0.0317(6) Uani 1 1 d . . . F10 F 0.3373(2) 0.24202(16) 0.31575(17) 0.0327(6) Uani 1 1 d . . . F11 F 0.3316(2) 0.38294(17) 0.40242(17) 0.0329(6) Uani 1 1 d . . . F12 F 0.3910(2) 0.38005(14) 0.54820(14) 0.0237(5) Uani 1 1 d . . . F14 F 0.22938(19) 0.30445(15) 0.64667(15) 0.0233(5) Uani 1 1 d . . . F15 F 0.1656(2) 0.43567(15) 0.73079(16) 0.0281(6) Uani 1 1 d . . . F16 F 0.3339(2) 0.50808(15) 0.82580(17) 0.0343(6) Uani 1 1 d . . . F17 F 0.5640(2) 0.43988(17) 0.84042(16) 0.0322(6) Uani 1 1 d . . . F18 F 0.6319(2) 0.31264(15) 0.75524(15) 0.0263(5) Uani 1 1 d . . . C1 C 0.3804(3) 0.1478(2) 0.6798(2) 0.0176(7) Uani 1 1 d . . . C2 C 0.4093(3) 0.1224(3) 0.7531(3) 0.0206(9) Uani 1 1 d . . . C3 C 0.3473(4) 0.0610(3) 0.7937(3) 0.0267(9) Uani 1 1 d . . . C4 C 0.2492(4) 0.0216(3) 0.7601(3) 0.0278(10) Uani 1 1 d . . . C5 C 0.2130(4) 0.0450(2) 0.6883(3) 0.0246(9) Uani 1 1 d . . . C6 C 0.2777(3) 0.1070(2) 0.6496(3) 0.0225(8) Uani 1 1 d . . . C7 C 0.4320(3) 0.2341(2) 0.5482(2) 0.0179(7) Uani 1 1 d . . . C8 C 0.4382(3) 0.1660(2) 0.4993(3) 0.0192(8) Uani 1 1 d . . . C9 C 0.4084(4) 0.1665(3) 0.4233(3) 0.0231(8) Uani 1 1 d . . . C10 C 0.3701(4) 0.2396(3) 0.3899(3) 0.0244(9) Uani 1 1 d . . . C11 C 0.3663(4) 0.3108(3) 0.4339(3) 0.0229(9) Uani 1 1 d . . . C12 C 0.3977(3) 0.3061(2) 0.5108(3) 0.0207(8) Uani 1 1 d . . . C13 C 0.4361(3) 0.3043(2) 0.6924(2) 0.0183(8) Uani 1 1 d . . . C14 C 0.3173(3) 0.3381(2) 0.6925(2) 0.0190(8) Uani 1 1 d . . . C15 C 0.2822(4) 0.4055(2) 0.7351(3) 0.0217(8) Uani 1 1 d . . . C16 C 0.3645(4) 0.4417(3) 0.7838(3) 0.0243(9) Uani 1 1 d . . . C17 C 0.4826(4) 0.4083(3) 0.7904(3) 0.0239(8) Uani 1 1 d . . . C18 C 0.5139(3) 0.3415(2) 0.7450(2) 0.0199(8) Uani 1 1 d . . . C19 C 0.7306(4) 0.1810(3) 0.4137(3) 0.0309(10) Uani 1 1 d . . . H19A H 0.8054 0.1726 0.3828 0.046 Uiso 1 1 calc R . . H19B H 0.7014 0.2381 0.4074 0.046 Uiso 1 1 calc R . . H19C H 0.6658 0.1425 0.3969 0.046 Uiso 1 1 calc R . . C20 C 0.7895(5) 0.0790(3) 0.5062(3) 0.0398(12) Uani 1 1 d . . . H20A H 0.7177 0.0445 0.4931 0.060 Uiso 1 1 calc R . . H20B H 0.8111 0.0706 0.5600 0.060 Uiso 1 1 calc R . . H20C H 0.8601 0.0634 0.4739 0.060 Uiso 1 1 calc R . . C21 C 0.9299(6) 0.1681(3) 0.6907(4) 0.0503(15) Uani 1 1 d . . . H21A H 1.0194 0.1728 0.6995 0.076 Uiso 1 1 calc R . . H21B H 0.9141 0.1250 0.6525 0.076 Uiso 1 1 calc R . . H21C H 0.8885 0.1535 0.7387 0.076 Uiso 1 1 calc R . . C22 C 0.9137(4) 0.3137(3) 0.7163(3) 0.0353(11) Uani 1 1 d . . . H22A H 0.8764 0.3023 0.7663 0.053 Uiso 1 1 calc R . . H22B H 0.8819 0.3663 0.6966 0.053 Uiso 1 1 calc R . . H22C H 1.0041 0.3171 0.7217 0.053 Uiso 1 1 calc R . . C23 C 0.6708(4) 0.4074(3) 0.4730(3) 0.0299(10) Uani 1 1 d . . . H23A H 0.5861 0.4293 0.4708 0.045 Uiso 1 1 calc R . . H23B H 0.6810 0.3641 0.4342 0.045 Uiso 1 1 calc R . . H23C H 0.7299 0.4523 0.4633 0.045 Uiso 1 1 calc R . . C24 C 0.6811(4) 0.4361(3) 0.6063(3) 0.0274(9) Uani 1 1 d . . . H24A H 0.7403 0.4809 0.5960 0.041 Uiso 1 1 calc R . . H24B H 0.6980 0.4123 0.6567 0.041 Uiso 1 1 calc R . . H24C H 0.5965 0.4583 0.6052 0.041 Uiso 1 1 calc R . . C25 C 0.9984(4) 0.3853(3) 0.5221(3) 0.0350(11) Uani 1 1 d . . . H25A H 1.0308 0.3762 0.5737 0.053 Uiso 1 1 calc R . . H25B H 0.9366 0.4299 0.5232 0.053 Uiso 1 1 calc R . . H25C H 1.0666 0.4010 0.4880 0.053 Uiso 1 1 calc R . . C26 C 1.0359(4) 0.2444(3) 0.4810(4) 0.0392(12) Uani 1 1 d . . . H26A H 1.0979 0.2656 0.4450 0.059 Uiso 1 1 calc R . . H26B H 0.9975 0.1944 0.4598 0.059 Uiso 1 1 calc R . . H26C H 1.0762 0.2309 0.5296 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.01281(15) 0.00964(18) 0.01471(19) 0.0002(3) 0.0007(2) -0.00087(13) B1 0.0172(17) 0.014(2) 0.019(2) 0.0021(17) 0.0017(16) -0.0008(14) N1 0.0195(15) 0.0179(18) 0.0178(18) -0.0002(14) 0.0005(13) 0.0008(11) N2 0.0317(18) 0.0214(18) 0.027(2) -0.0035(15) 0.0055(15) -0.0036(14) N3 0.0210(15) 0.032(2) 0.028(2) 0.0015(16) -0.0010(14) -0.0009(14) N4 0.0274(15) 0.0161(17) 0.032(2) 0.0052(14) -0.0005(14) -0.0006(12) N5 0.0239(17) 0.030(2) 0.028(2) 0.0005(17) -0.0008(15) -0.0032(13) F2 0.0261(11) 0.0281(13) 0.0223(13) 0.0047(11) -0.0029(10) -0.0015(9) F3 0.0474(15) 0.0386(17) 0.0288(16) 0.0179(13) 0.0021(13) 0.0003(12) F4 0.0485(15) 0.0217(13) 0.049(2) 0.0095(13) 0.0163(14) -0.0089(11) F5 0.0295(12) 0.0252(13) 0.0477(19) -0.0068(13) 0.0047(12) -0.0130(10) F6 0.0247(9) 0.0295(11) 0.0320(16) 0.0034(13) -0.0037(12) -0.0074(8) F8 0.0313(12) 0.0161(12) 0.0269(14) 0.0002(10) -0.0026(10) 0.0025(9) F9 0.0397(14) 0.0296(15) 0.0258(15) -0.0133(12) -0.0035(12) 0.0015(11) F10 0.0369(15) 0.0427(15) 0.0186(13) 0.0002(12) -0.0061(10) 0.0019(11) F11 0.0403(14) 0.0281(14) 0.0303(16) 0.0077(12) -0.0065(12) 0.0076(11) F12 0.0332(11) 0.0159(12) 0.0220(13) -0.0003(9) 0.0004(9) 0.0023(9) F14 0.0178(10) 0.0243(12) 0.0279(14) -0.0029(10) -0.0032(10) -0.0012(9) F15 0.0244(11) 0.0260(13) 0.0339(16) -0.0008(11) 0.0042(10) 0.0067(9) F16 0.0428(14) 0.0263(13) 0.0339(16) -0.0164(13) 0.0113(12) -0.0006(11) F17 0.0359(14) 0.0354(14) 0.0254(15) -0.0090(11) -0.0047(11) -0.0115(11) F18 0.0199(10) 0.0302(13) 0.0288(15) -0.0006(11) -0.0055(10) 0.0002(9) C1 0.0183(15) 0.0124(17) 0.022(2) -0.0003(16) 0.0036(15) 0.0005(13) C2 0.0184(16) 0.017(2) 0.026(2) -0.0011(18) 0.0011(15) 0.0018(14) C3 0.035(2) 0.019(2) 0.026(2) 0.0071(18) 0.0069(18) 0.0021(16) C4 0.030(2) 0.017(2) 0.036(3) 0.0010(18) 0.0120(18) -0.0003(15) C5 0.0262(19) 0.0138(18) 0.034(3) -0.0026(17) 0.0056(17) -0.0029(14) C6 0.0225(17) 0.0188(19) 0.026(2) 0.0004(16) 0.0009(17) 0.0014(14) C7 0.0168(14) 0.0187(18) 0.0181(19) -0.0001(15) 0.0005(13) -0.0016(13) C8 0.0187(16) 0.0158(19) 0.023(2) 0.0008(16) 0.0001(15) 0.0016(13) C9 0.0254(18) 0.022(2) 0.022(2) -0.0067(18) 0.0004(16) -0.0015(15) C10 0.0227(17) 0.029(2) 0.022(2) 0.0012(18) -0.0014(15) -0.0005(15) C11 0.0207(17) 0.023(2) 0.025(2) 0.0041(17) 0.0024(16) 0.0021(15) C12 0.0185(16) 0.019(2) 0.024(2) 0.0006(16) 0.0021(15) -0.0007(13) C13 0.0167(16) 0.0175(19) 0.021(2) 0.0013(15) 0.0030(15) -0.0001(13) C14 0.0230(17) 0.0177(19) 0.016(2) -0.0012(16) 0.0021(15) -0.0044(14) C15 0.0225(18) 0.0175(19) 0.025(2) 0.0017(16) 0.0065(16) 0.0030(14) C16 0.032(2) 0.0163(19) 0.025(2) -0.0035(17) 0.0059(17) -0.0007(15) C17 0.0268(18) 0.026(2) 0.019(2) -0.0024(18) -0.0004(16) -0.0089(15) C18 0.0175(16) 0.020(2) 0.022(2) 0.0031(17) 0.0002(15) -0.0015(13) C19 0.034(2) 0.031(2) 0.028(2) -0.0041(19) 0.0030(19) 0.0024(18) C20 0.053(3) 0.030(3) 0.036(3) -0.002(2) -0.003(2) -0.006(2) C21 0.060(3) 0.038(3) 0.053(4) 0.003(3) -0.026(3) -0.003(2) C22 0.029(2) 0.038(3) 0.039(3) -0.005(2) -0.007(2) 0.0042(18) C23 0.035(2) 0.027(2) 0.028(2) 0.001(2) 0.0001(19) 0.0007(17) C24 0.030(2) 0.026(2) 0.027(2) 0.0026(18) 0.0033(18) -0.0007(16) C25 0.029(2) 0.029(2) 0.047(3) 0.006(2) 0.000(2) -0.0130(18) C26 0.027(2) 0.043(3) 0.048(3) -0.007(3) 0.008(2) -0.0015(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N3 2.030(4) . ? Zr1 N2 2.035(4) . ? Zr1 N4 2.039(3) . ? Zr1 N1 2.356(3) . ? Zr1 N5 2.424(4) . ? B1 N1 1.587(5) . ? B1 C7 1.648(6) . ? B1 C13 1.653(6) . ? B1 C1 1.660(6) . ? N1 F18 2.747(5) . y N1 F2 2.916(4) . y N1 F8 2.975(4) . y N1 H1A 0.95(6) . ? N1 H1B 0.91(7) . ? N2 C19 1.450(6) . ? N2 C20 1.460(6) . ? N3 C21 1.453(6) . ? N3 C22 1.463(6) . ? N4 C24 1.447(6) . ? N4 C23 1.459(6) . ? N5 C26 1.478(6) . ? N5 C25 1.484(6) . ? N5 H5 0.96(7) . ? F2 C2 1.361(5) . ? F2 H1A 2.22(5) . y F3 C3 1.349(6) . ? F4 C4 1.341(5) . ? F5 C5 1.350(5) . ? F6 C6 1.349(6) . ? F8 C8 1.363(4) . ? F8 H1B 2.44(7) . y F9 C9 1.348(5) . ? F10 C10 1.346(5) . ? F11 C11 1.341(5) . ? F12 C12 1.364(5) . ? F14 C14 1.355(4) . ? F15 C15 1.350(4) . ? F16 C16 1.340(5) . ? F17 C17 1.340(5) . ? F18 C18 1.367(4) . ? F18 C24 3.324(5) . y F18 H1A 2.22(5) . y F18 H24B 2.464 . y C1 C2 1.382(6) . ? C1 C6 1.391(5) . ? C2 C3 1.391(6) . ? C3 C4 1.367(6) . ? C4 C5 1.369(7) . ? C5 C6 1.395(6) . ? C7 C12 1.383(6) . ? C7 C8 1.394(6) . ? C8 C9 1.368(6) . ? C9 C10 1.379(6) . ? C10 C11 1.384(6) . ? C11 C12 1.390(6) . ? C13 C18 1.382(6) . ? C13 C14 1.392(5) . ? C14 C15 1.373(5) . ? C15 C16 1.362(6) . ? C16 C17 1.387(6) . ? C17 C18 1.382(6) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 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 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 Zr1 N2 119.30(15) . . ? N3 Zr1 N4 118.88(15) . . ? N2 Zr1 N4 120.69(16) . . ? N3 Zr1 N1 89.59(13) . . ? N2 Zr1 N1 89.67(14) . . ? N4 Zr1 N1 101.25(13) . . ? N3 Zr1 N5 90.97(14) . . ? N2 Zr1 N5 84.37(14) . . ? N4 Zr1 N5 84.18(14) . . ? N1 Zr1 N5 173.45(13) . . ? N1 B1 C7 105.1(3) . . ? N1 B1 C13 112.0(3) . . ? C7 B1 C13 113.9(3) . . ? N1 B1 C1 109.7(3) . . ? C7 B1 C1 112.4(3) . . ? C13 B1 C1 103.8(3) . . ? B1 N1 Zr1 126.3(2) . . ? B1 N1 F18 86.3(2) . . ? Zr1 N1 F18 90.67(12) . . ? B1 N1 F2 72.4(2) . . ? Zr1 N1 F2 146.95(16) . . ? F18 N1 F2 61.30(11) . . ? B1 N1 F8 70.5(2) . . ? Zr1 N1 F8 104.68(14) . . ? F18 N1 F8 156.75(14) . . ? F2 N1 F8 107.59(12) . . ? B1 N1 H1A 105(3) . . ? Zr1 N1 H1A 112(3) . . ? F18 N1 H1A 48(3) . . ? F2 N1 H1A 37(3) . . ? F8 N1 H1A 136(3) . . ? B1 N1 H1B 112(4) . . ? Zr1 N1 H1B 97(4) . . ? F18 N1 H1B 150(4) . . ? F2 N1 H1B 100(4) . . ? F8 N1 H1B 47(4) . . ? H1A N1 H1B 103(5) . . ? C19 N2 C20 110.8(4) . . ? C19 N2 Zr1 122.3(3) . . ? C20 N2 Zr1 126.7(3) . . ? C21 N3 C22 110.6(4) . . ? C21 N3 Zr1 124.2(3) . . ? C22 N3 Zr1 124.8(3) . . ? C24 N4 C23 110.1(3) . . ? C24 N4 Zr1 122.4(3) . . ? C23 N4 Zr1 126.3(3) . . ? C26 N5 C25 109.6(4) . . ? C26 N5 Zr1 113.2(3) . . ? C25 N5 Zr1 114.3(3) . . ? C26 N5 H5 109(4) . . ? C25 N5 H5 103(4) . . ? Zr1 N5 H5 107(4) . . ? C2 F2 N1 86.0(2) . . ? C8 F8 N1 83.2(2) . . ? C18 F18 N1 92.7(2) . . ? C2 C1 C6 113.0(4) . . ? C2 C1 B1 119.0(3) . . ? C6 C1 B1 128.0(4) . . ? F2 C2 C1 119.5(4) . . ? F2 C2 C3 115.3(4) . . ? C1 C2 C3 125.2(4) . . ? F3 C3 C4 120.4(4) . . ? F3 C3 C2 120.7(4) . . ? C4 C3 C2 118.9(4) . . ? F4 C4 C3 120.8(4) . . ? F4 C4 C5 120.0(4) . . ? C3 C4 C5 119.2(4) . . ? F5 C5 C4 119.9(4) . . ? F5 C5 C6 120.1(4) . . ? C4 C5 C6 120.0(4) . . ? F6 C6 C1 121.6(4) . . ? F6 C6 C5 114.8(3) . . ? C1 C6 C5 123.6(4) . . ? C12 C7 C8 112.6(4) . . ? C12 C7 B1 128.2(4) . . ? C8 C7 B1 119.2(3) . . ? F8 C8 C9 115.7(4) . . ? F8 C8 C7 118.8(4) . . ? C9 C8 C7 125.5(4) . . ? F9 C9 C8 121.2(4) . . ? F9 C9 C10 119.6(4) . . ? C8 C9 C10 119.2(4) . . ? F10 C10 C9 120.9(4) . . ? F10 C10 C11 120.3(4) . . ? C9 C10 C11 118.8(4) . . ? F11 C11 C10 120.1(4) . . ? F11 C11 C12 120.9(4) . . ? C10 C11 C12 119.1(4) . . ? F12 C12 C7 121.5(4) . . ? F12 C12 C11 113.8(4) . . ? C7 C12 C11 124.7(4) . . ? C18 C13 C14 112.8(4) . . ? C18 C13 B1 127.6(3) . . ? C14 C13 B1 119.2(3) . . ? F14 C14 C15 116.5(3) . . ? F14 C14 C13 119.1(3) . . ? C15 C14 C13 124.4(4) . . ? F15 C15 C16 119.1(4) . . ? F15 C15 C14 120.8(4) . . ? C16 C15 C14 120.1(4) . . ? F16 C16 C15 121.7(4) . . ? F16 C16 C17 119.4(4) . . ? C15 C16 C17 118.9(4) . . ? F17 C17 C18 120.8(4) . . ? F17 C17 C16 120.6(4) . . ? C18 C17 C16 118.6(4) . . ? F18 C18 C13 120.2(3) . . ? F18 C18 C17 114.7(3) . . ? C13 C18 C17 125.1(3) . . ? N2 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 H21A 109.5 . . ? N3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 H22A 109.5 . . ? N3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 H25A 109.5 . . ? N5 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N5 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N5 C26 H26A 109.5 . . ? N5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 29.47 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.689 _refine_diff_density_min -0.694 _refine_diff_density_rms 0.085 data_ua0427 _database_code_depnum_ccdc_archive 'CCDC 258172' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H20 B F15 N4 Ti' _chemical_formula_sum 'C24 H20 B F15 N4 Ti' _chemical_formula_weight 708.15 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' B B 0.0013 0.0007 '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 13.5564(2) _cell_length_b 13.1607(2) _cell_length_c 15.8983(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.2522(7) _cell_angle_gamma 90.00 _cell_volume 2807.07(8) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 19829 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.854 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_reflns_number 16178 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 27.47 _reflns_number_total 6417 _reflns_number_gt 4391 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; HKL Denzo and Scalepack (Otwinowski & Minor 1997) ; _computing_structure_solution 'SIR-92 (Altomare et al. 1994)' _computing_structure_refinement 'SHELXL-97 (Sheldrick 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick 1997)' _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^)+(0.0645P)^2^+2.2472P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6417 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.1467 _refine_ls_wR_factor_gt 0.1277 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.081 _refine_ls_shift/su_mean 0.010 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 0.14418(4) 0.50854(4) 0.17033(3) 0.03251(15) Uani 1 1 d . . . B1 B 0.2466(2) 0.5387(3) 0.37729(19) 0.0317(7) Uani 1 1 d . . . F2 F 0.42667(13) 0.59582(15) 0.48408(11) 0.0520(5) Uani 1 1 d . . . F3 F 0.52071(15) 0.77431(19) 0.49151(14) 0.0709(7) Uani 1 1 d . . . F4 F 0.44347(17) 0.93219(17) 0.39388(15) 0.0723(6) Uani 1 1 d . . . F5 F 0.26922(14) 0.90667(15) 0.28661(13) 0.0551(5) Uani 1 1 d . . . F6 F 0.17546(12) 0.73127(14) 0.27616(11) 0.0453(4) Uani 1 1 d . . . F8 F 0.18619(13) 0.33150(13) 0.38757(11) 0.0446(4) Uani 1 1 d . . . F9 F 0.28212(17) 0.16323(16) 0.35609(15) 0.0676(6) Uani 1 1 d . . . F10 F 0.46510(19) 0.1748(2) 0.30542(18) 0.0961(9) Uani 1 1 d . . . F11 F 0.55322(16) 0.3606(2) 0.29609(16) 0.0912(9) Uani 1 1 d . . . F12 F 0.45835(13) 0.52968(18) 0.32586(13) 0.0604(6) Uani 1 1 d . . . F14 F 0.33587(13) 0.41706(13) 0.53525(10) 0.0445(4) Uani 1 1 d . . . F15 F 0.26328(16) 0.40598(15) 0.68027(11) 0.0567(5) Uani 1 1 d . . . F16 F 0.09127(16) 0.50443(17) 0.70103(12) 0.0634(6) Uani 1 1 d . . . F17 F 0.00181(13) 0.62582(17) 0.57477(13) 0.0596(6) Uani 1 1 d . . . F18 F 0.07586(13) 0.64499(14) 0.43008(11) 0.0465(4) Uani 1 1 d . . . N1 N 0.15113(17) 0.5286(2) 0.30535(15) 0.0330(5) Uani 1 1 d . . . H1A H 0.124(3) 0.480(3) 0.317(2) 0.040 Uiso 1 1 d . . . H1B H 0.110(2) 0.583(3) 0.308(2) 0.040 Uiso 1 1 d . . . N2 N 0.1730(2) 0.3750(2) 0.14233(16) 0.0439(6) Uani 1 1 d . . . N3 N 0.22482(18) 0.5989(2) 0.12140(16) 0.0416(6) Uani 1 1 d . . . N4 N 0.00983(17) 0.5338(2) 0.13036(15) 0.0387(6) Uani 1 1 d . . . C1 C 0.2986(2) 0.6505(2) 0.37675(17) 0.0347(6) Uani 1 1 d . . . C2 C 0.3860(2) 0.6703(2) 0.43229(18) 0.0406(7) Uani 1 1 d . . . C3 C 0.4355(2) 0.7617(3) 0.4378(2) 0.0493(8) Uani 1 1 d . . . C4 C 0.3967(3) 0.8421(3) 0.3887(2) 0.0498(8) Uani 1 1 d . . . C5 C 0.3090(2) 0.8288(2) 0.33488(19) 0.0424(7) Uani 1 1 d . . . C6 C 0.2634(2) 0.7357(2) 0.33009(17) 0.0365(6) Uani 1 1 d . . . C7 C 0.3161(2) 0.4407(3) 0.35911(17) 0.0374(7) Uani 1 1 d . . . C8 C 0.2781(2) 0.3435(2) 0.36404(18) 0.0410(7) Uani 1 1 d . . . C9 C 0.3250(3) 0.2539(3) 0.3473(2) 0.0508(9) Uani 1 1 d . . . C10 C 0.4165(3) 0.2598(3) 0.3227(2) 0.0599(10) Uani 1 1 d . . . C11 C 0.4602(2) 0.3517(4) 0.3173(2) 0.0614(11) Uani 1 1 d . . . C12 C 0.4108(2) 0.4415(3) 0.33518(19) 0.0472(8) Uani 1 1 d . . . C13 C 0.20807(19) 0.5288(2) 0.47185(17) 0.0306(6) Uani 1 1 d . . . C14 C 0.2530(2) 0.4712(2) 0.54048(17) 0.0338(6) Uani 1 1 d . . . C15 C 0.2160(2) 0.4637(2) 0.61722(18) 0.0403(7) Uani 1 1 d . . . C16 C 0.1306(2) 0.5140(3) 0.62805(19) 0.0444(8) Uani 1 1 d . . . C17 C 0.0846(2) 0.5736(2) 0.5643(2) 0.0415(7) Uani 1 1 d . . . C18 C 0.1246(2) 0.5809(2) 0.48924(18) 0.0347(6) Uani 1 1 d . . . C19 C 0.2442(4) 0.3306(4) 0.0923(3) 0.0672(11) Uani 1 1 d . . . H19C H 0.305(3) 0.291(3) 0.131(3) 0.081 Uiso 1 1 d . . . H19B H 0.284(3) 0.390(3) 0.067(3) 0.081 Uiso 1 1 d . . . H19A H 0.205(3) 0.286(4) 0.051(3) 0.081 Uiso 1 1 d . . . C20 C 0.1113(3) 0.2981(3) 0.1763(3) 0.0544(9) Uani 1 1 d . . . H20C H 0.064(3) 0.331(3) 0.211(3) 0.065 Uiso 1 1 d . . . H20B H 0.072(3) 0.263(3) 0.127(3) 0.065 Uiso 1 1 d . . . H20A H 0.152(3) 0.249(3) 0.216(3) 0.065 Uiso 1 1 d . . . C21 C 0.3303(3) 0.5780(4) 0.1434(3) 0.0697(12) Uani 1 1 d . . . H21C H 0.372(3) 0.639(3) 0.180(3) 0.084 Uiso 1 1 d . . . H21B H 0.340(3) 0.508(4) 0.176(3) 0.084 Uiso 1 1 d . . . H21A H 0.358(3) 0.560(3) 0.089(3) 0.084 Uiso 1 1 d . . . C22 C 0.2070(3) 0.6902(3) 0.0702(3) 0.0592(10) Uani 1 1 d . . . H22C H 0.240(3) 0.742(3) 0.095(3) 0.071 Uiso 1 1 d . . . H22B H 0.235(3) 0.682(3) 0.018(3) 0.071 Uiso 1 1 d . . . H22A H 0.125(3) 0.704(3) 0.053(3) 0.071 Uiso 1 1 d . . . C23 C -0.0702(3) 0.4700(4) 0.0885(2) 0.0561(9) Uani 1 1 d . . . H23C H -0.099(3) 0.498(3) 0.029(3) 0.067 Uiso 1 1 d . . . H23B H -0.122(3) 0.464(3) 0.124(3) 0.067 Uiso 1 1 d . . . H23A H -0.044(3) 0.403(3) 0.078(3) 0.067 Uiso 1 1 d . . . C24 C -0.0245(3) 0.6375(3) 0.1423(3) 0.0518(8) Uani 1 1 d . . . H24C H 0.036(3) 0.685(3) 0.173(2) 0.062 Uiso 1 1 d . . . H24B H -0.079(3) 0.636(3) 0.181(2) 0.062 Uiso 1 1 d . . . H24A H -0.050(3) 0.675(3) 0.088(3) 0.062 Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.0309(3) 0.0401(3) 0.0265(3) 0.0009(2) 0.00407(18) -0.0014(2) B1 0.0268(14) 0.0450(18) 0.0232(14) 0.0034(13) 0.0034(11) 0.0031(13) F2 0.0422(9) 0.0669(12) 0.0424(10) 0.0177(9) -0.0093(8) -0.0047(9) F3 0.0578(12) 0.0847(16) 0.0614(13) 0.0142(11) -0.0217(10) -0.0281(12) F4 0.0741(14) 0.0616(13) 0.0772(16) 0.0101(11) -0.0032(12) -0.0267(12) F5 0.0569(11) 0.0502(11) 0.0578(12) 0.0152(9) 0.0066(9) 0.0029(9) F6 0.0403(9) 0.0505(10) 0.0417(10) 0.0055(8) -0.0062(7) 0.0041(8) F8 0.0418(9) 0.0444(10) 0.0492(10) -0.0059(8) 0.0120(8) 0.0031(8) F9 0.0762(14) 0.0516(13) 0.0708(14) -0.0144(10) -0.0042(11) 0.0201(11) F10 0.0777(16) 0.110(2) 0.0984(19) -0.0313(16) 0.0055(14) 0.0603(16) F11 0.0461(12) 0.155(3) 0.0785(16) -0.0006(16) 0.0299(11) 0.0384(15) F12 0.0340(9) 0.1004(17) 0.0492(11) 0.0106(11) 0.0148(8) 0.0049(10) F14 0.0490(10) 0.0518(11) 0.0324(9) 0.0060(8) 0.0048(7) 0.0168(9) F15 0.0857(14) 0.0558(11) 0.0281(9) 0.0096(8) 0.0062(9) -0.0079(10) F16 0.0704(13) 0.0897(15) 0.0370(10) -0.0124(10) 0.0305(9) -0.0278(12) F17 0.0420(10) 0.0753(14) 0.0670(13) -0.0268(11) 0.0263(9) 0.0004(10) F18 0.0421(9) 0.0525(11) 0.0451(10) -0.0030(8) 0.0072(8) 0.0155(8) N1 0.0284(12) 0.0410(14) 0.0300(12) 0.0020(11) 0.0050(9) 0.0024(11) N2 0.0536(15) 0.0456(15) 0.0324(13) -0.0011(11) 0.0067(11) 0.0028(13) N3 0.0405(13) 0.0507(15) 0.0341(13) 0.0032(11) 0.0072(10) -0.0082(12) N4 0.0318(12) 0.0563(16) 0.0276(12) 0.0020(11) 0.0027(9) -0.0005(11) C1 0.0300(13) 0.0483(17) 0.0265(13) 0.0032(12) 0.0072(10) 0.0009(13) C2 0.0363(15) 0.0537(19) 0.0311(14) 0.0115(13) 0.0024(11) -0.0038(14) C3 0.0413(17) 0.065(2) 0.0391(17) 0.0040(15) -0.0042(13) -0.0125(16) C4 0.0500(19) 0.054(2) 0.0455(18) 0.0025(15) 0.0086(14) -0.0150(16) C5 0.0436(17) 0.0480(18) 0.0369(16) 0.0096(14) 0.0104(13) 0.0031(15) C6 0.0311(14) 0.0514(18) 0.0268(14) 0.0033(12) 0.0031(11) 0.0047(13) C7 0.0287(13) 0.060(2) 0.0237(13) -0.0028(13) 0.0039(10) 0.0110(14) C8 0.0428(16) 0.0520(19) 0.0274(14) -0.0056(13) 0.0022(12) 0.0126(15) C9 0.0502(19) 0.063(2) 0.0365(17) -0.0102(15) -0.0040(14) 0.0192(17) C10 0.056(2) 0.074(3) 0.048(2) -0.0116(18) 0.0016(16) 0.029(2) C11 0.0341(16) 0.115(4) 0.0365(17) -0.003(2) 0.0108(13) 0.032(2) C12 0.0326(15) 0.076(2) 0.0330(16) 0.0053(15) 0.0064(12) 0.0060(16) C13 0.0304(13) 0.0351(14) 0.0270(13) -0.0025(11) 0.0070(10) -0.0037(11) C14 0.0390(15) 0.0345(15) 0.0283(14) -0.0030(11) 0.0061(11) -0.0028(12) C15 0.0545(18) 0.0410(16) 0.0258(14) 0.0002(12) 0.0076(12) -0.0129(14) C16 0.0528(18) 0.056(2) 0.0284(15) -0.0113(14) 0.0190(13) -0.0196(16) C17 0.0351(15) 0.0492(18) 0.0433(17) -0.0183(14) 0.0159(13) -0.0073(14) C18 0.0333(14) 0.0368(15) 0.0344(15) -0.0056(12) 0.0065(11) -0.0021(12) C19 0.086(3) 0.063(3) 0.058(2) -0.005(2) 0.025(2) 0.021(2) C20 0.066(2) 0.047(2) 0.048(2) -0.0038(16) 0.0027(18) -0.0051(18) C21 0.043(2) 0.103(4) 0.062(3) 0.019(2) 0.0023(17) -0.009(2) C22 0.068(3) 0.055(2) 0.056(2) 0.0106(18) 0.0166(19) -0.013(2) C23 0.0419(18) 0.083(3) 0.0418(19) -0.0043(19) -0.0008(15) -0.0127(19) C24 0.0434(18) 0.060(2) 0.051(2) 0.0042(17) 0.0008(15) 0.0077(17) _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 N3 1.860(2) . ? Ti1 N2 1.868(3) . ? Ti1 N4 1.871(2) . ? Ti1 N1 2.152(2) . ? B1 N1 1.605(4) . ? B1 C1 1.632(4) . ? B1 C7 1.647(4) . ? B1 C13 1.666(4) . ? F2 C2 1.346(3) . ? F3 C3 1.345(4) . ? F4 C4 1.342(4) . ? F5 C5 1.346(3) . ? F6 C6 1.366(3) . ? F6 N1 2.735(3) . y F6 C24 3.427(4) . y F6 H1B 2.23(3) . y F6 H24C 2.40(4) . y F8 C8 1.361(3) . ? F8 N1 2.913(3) . y F8 H1A 2.35(3) . y F9 C9 1.343(4) . ? F10 C10 1.346(4) . ? F10 C21 3.055(5) 2_655 y F10 H21C 2.23(5) 2_655 y F11 C11 1.357(4) . ? F12 C12 1.346(4) . ? F14 C14 1.342(3) . ? F15 C15 1.345(3) . ? F16 C16 1.350(3) . ? F17 C17 1.346(3) . ? F18 C18 1.361(3) . ? F18 N1 2.811(3) . y F18 H1B 2.22(3) . y N1 H1A 0.77(3) . ? N1 H1B 0.90(3) . ? N2 C19 1.459(5) . ? N2 C20 1.464(5) . ? N3 C21 1.449(5) . ? N3 C22 1.452(5) . ? N4 C23 1.455(4) . ? N4 C24 1.463(5) . ? C1 C6 1.391(4) . ? C1 C2 1.398(4) . ? C2 C3 1.374(5) . ? C3 C4 1.374(5) . ? C4 C5 1.373(5) . ? C5 C6 1.370(4) . ? C7 C8 1.385(5) . ? C7 C12 1.390(4) . ? C8 C9 1.384(4) . ? C9 C10 1.356(5) . ? C10 C11 1.355(6) . ? C11 C12 1.407(5) . ? C13 C18 1.385(4) . ? C13 C14 1.395(4) . ? C14 C15 1.388(4) . ? C15 C16 1.366(5) . ? C16 C17 1.360(5) . ? C17 C18 1.383(4) . ? C19 H19C 1.09(5) . ? C19 H19B 1.06(5) . ? C19 H19A 0.98(5) . ? C20 H20C 1.00(4) . ? C20 H20B 0.99(4) . ? C20 H20A 1.02(4) . ? C21 H21C 1.10(5) . ? C21 H21B 1.05(5) . ? C21 H21A 1.01(5) . ? C22 H22C 0.88(5) . ? C22 H22B 0.97(4) . ? C22 H22A 1.13(4) . ? C23 H23C 1.04(4) . ? C23 H23B 0.96(4) . ? C23 H23A 0.98(4) . ? C24 H24C 1.09(4) . ? C24 H24B 1.03(4) . ? C24 H24A 1.01(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ti1 N2 110.28(12) . . ? N3 Ti1 N4 110.26(11) . . ? N2 Ti1 N4 108.24(12) . . ? N3 Ti1 N1 113.23(11) . . ? N2 Ti1 N1 111.88(11) . . ? N4 Ti1 N1 102.60(10) . . ? N1 B1 C1 112.0(2) . . ? N1 B1 C7 103.5(2) . . ? C1 B1 C7 116.6(2) . . ? N1 B1 C13 108.1(2) . . ? C1 B1 C13 105.5(2) . . ? C7 B1 C13 111.0(2) . . ? C6 F6 N1 92.90(16) . . ? C6 F6 C24 161.14(18) . . ? N1 F6 C24 69.53(9) . . ? C8 F8 N1 82.52(16) . . ? C18 F18 N1 87.75(15) . . ? B1 N1 Ti1 129.52(17) . . ? B1 N1 F6 86.33(17) . . ? Ti1 N1 F6 86.54(9) . . ? B1 N1 F18 77.87(15) . . ? Ti1 N1 F18 143.38(12) . . ? F6 N1 F18 69.72(9) . . ? B1 N1 F8 71.98(16) . . ? Ti1 N1 F8 108.61(11) . . ? F6 N1 F8 158.22(11) . . ? F18 N1 F8 102.77(9) . . ? B1 N1 H1A 105(3) . . ? Ti1 N1 H1A 101(3) . . ? F6 N1 H1A 157(2) . . ? F18 N1 H1A 92(3) . . ? F8 N1 H1A 38(3) . . ? B1 N1 H1B 110(2) . . ? Ti1 N1 H1B 102(2) . . ? F6 N1 H1B 48.0(19) . . ? F18 N1 H1B 42(2) . . ? F8 N1 H1B 138(2) . . ? H1A N1 H1B 109(3) . . ? C19 N2 C20 112.4(3) . . ? C19 N2 Ti1 133.2(3) . . ? C20 N2 Ti1 114.4(2) . . ? C21 N3 C22 111.8(3) . . ? C21 N3 Ti1 113.3(2) . . ? C22 N3 Ti1 134.7(2) . . ? C23 N4 C24 111.6(3) . . ? C23 N4 Ti1 132.7(3) . . ? C24 N4 Ti1 115.7(2) . . ? C6 C1 C2 112.4(3) . . ? C6 C1 B1 127.9(2) . . ? C2 C1 B1 119.5(2) . . ? F2 C2 C3 116.4(3) . . ? F2 C2 C1 119.1(3) . . ? C3 C2 C1 124.4(3) . . ? F3 C3 C4 119.3(3) . . ? F3 C3 C2 121.0(3) . . ? C4 C3 C2 119.6(3) . . ? F4 C4 C5 120.6(3) . . ? F4 C4 C3 120.5(3) . . ? C5 C4 C3 118.9(3) . . ? F5 C5 C6 120.5(3) . . ? F5 C5 C4 119.9(3) . . ? C6 C5 C4 119.5(3) . . ? F6 C6 C5 114.8(3) . . ? F6 C6 C1 120.1(3) . . ? C5 C6 C1 125.0(3) . . ? C8 C7 C12 112.8(3) . . ? C8 C7 B1 119.1(2) . . ? C12 C7 B1 128.0(3) . . ? F8 C8 C9 114.7(3) . . ? F8 C8 C7 119.1(2) . . ? C9 C8 C7 126.3(3) . . ? F9 C9 C10 120.6(3) . . ? F9 C9 C8 121.3(3) . . ? C10 C9 C8 118.1(4) . . ? F10 C10 C11 119.9(4) . . ? F10 C10 C9 120.4(4) . . ? C11 C10 C9 119.7(3) . . ? C10 C11 F11 121.5(4) . . ? C10 C11 C12 120.8(3) . . ? F11 C11 C12 117.6(4) . . ? F12 C12 C7 120.8(3) . . ? F12 C12 C11 116.9(3) . . ? C7 C12 C11 122.2(4) . . ? C18 C13 C14 113.0(2) . . ? C18 C13 B1 120.9(2) . . ? C14 C13 B1 126.1(2) . . ? F14 C14 C15 115.3(3) . . ? F14 C14 C13 121.0(2) . . ? C15 C14 C13 123.6(3) . . ? F15 C15 C16 120.1(3) . . ? F15 C15 C14 120.1(3) . . ? C16 C15 C14 119.8(3) . . ? F16 C16 C17 119.9(3) . . ? F16 C16 C15 120.6(3) . . ? C17 C16 C15 119.5(3) . . ? F17 C17 C16 120.2(3) . . ? F17 C17 C18 120.5(3) . . ? C16 C17 C18 119.2(3) . . ? F18 C18 C17 115.3(3) . . ? F18 C18 C13 119.9(2) . . ? C17 C18 C13 124.8(3) . . ? N2 C19 H19C 113(2) . . ? N2 C19 H19B 109(2) . . ? H19C C19 H19B 100(3) . . ? N2 C19 H19A 105(3) . . ? H19C C19 H19A 113(4) . . ? H19B C19 H19A 117(4) . . ? N2 C20 H20C 111(2) . . ? N2 C20 H20B 107(2) . . ? H20C C20 H20B 109(3) . . ? N2 C20 H20A 113(2) . . ? H20C C20 H20A 106(3) . . ? H20B C20 H20A 112(3) . . ? N3 C21 F10 144.3(4) . 2_655 ? N3 C21 H21C 114(2) . . ? F10 C21 H21C 34(2) 2_655 . ? N3 C21 H21B 110(2) . . ? F10 C21 H21B 101(2) 2_655 . ? H21C C21 H21B 111(4) . . ? N3 C21 H21A 108(3) . . ? F10 C21 H21A 84(3) 2_655 . ? H21C C21 H21A 113(3) . . ? H21B C21 H21A 100(4) . . ? N3 C22 H22C 111(3) . . ? N3 C22 H22B 109(3) . . ? H22C C22 H22B 104(4) . . ? N3 C22 H22A 110(2) . . ? H22C C22 H22A 114(4) . . ? H22B C22 H22A 108(3) . . ? N4 C23 H23C 111(2) . . ? N4 C23 H23B 109(2) . . ? H23C C23 H23B 111(3) . . ? N4 C23 H23A 110(2) . . ? H23C C23 H23A 105(3) . . ? H23B C23 H23A 110(3) . . ? N4 C24 F6 100.28(18) . . ? N4 C24 H24C 111.4(19) . . ? F6 C24 H24C 16(2) . . ? N4 C24 H24B 109(2) . . ? F6 C24 H24B 102(2) . . ? H24C C24 H24B 107(3) . . ? N4 C24 H24A 115(2) . . ? F6 C24 H24A 120(2) . . ? H24C C24 H24A 104(3) . . ? H24B C24 H24A 109(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.468 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.095