# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Simon J. Lancaster' _publ_contact_author_address ;Wolfson Materials and Catalysis Centre, School of Chemistry, University of East Anglia, Norwich, NR4 7TJ UK. ; _publ_contact_author_email S.Lancaster@uea.ac.uk _publ_contact_author_phone '+44 1603 592009' _publ_contact_author_fax '+44 1306 592003' loop_ _publ_author_name _publ_author_address A.-M.Fuller ;Wolfson Materials and Catalysis Centre, School of Chemistry, University of East Anglia, Norwich, NR4 7TJ UK. ; D.L.Hughes ;Wolfson Materials and Catalysis Centre, School of Chemistry, University of East Anglia, Norwich, NR4 7TJ UK. ; S.J.Lancaster ;Wolfson Materials and Catalysis Centre, School of Chemistry, University of East Anglia, Norwich, NR4 7TJ UK. ; _audit_creation_method 'SHELXL-97 and CrysAlis RED' data_2 _database_code_depnum_ccdc_archive 'CCDC 823223' #TrackingRef '- fuller et al cif.cif' _chemical_formula_structural HB(C3H3N2)3Ti(C2H6N)2NH2B(C6F5)3 _chemical_name_common HB(C3H3N2)3Ti(C2H6N)2NH2B(C6F5)3 _chemical_melting_point ? _chemical_formula_moiety 'C31 H24 B2 F15 N9 Ti' _chemical_formula_sum 'C31 H24 B2 F15 N9 Ti' _chemical_formula_weight 877.11 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 I2/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -y+1/2, z+1/2' _cell_length_a 27.3497(5) _cell_length_b 12.7238(2) _cell_length_c 21.1149(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.083(2) _cell_angle_gamma 90.00 _cell_volume 7318.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 13278 _cell_measurement_theta_min 3.2817 _cell_measurement_theta_max 29.9997 _exptl_crystal_description blocks _exptl_crystal_colour yellow _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3520 _exptl_absorpt_coefficient_mu 0.349 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.842 _exptl_absorpt_correction_T_max 0.939 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52275 _diffrn_reflns_av_R_equivalents 0.0544 _diffrn_reflns_av_sigmaI/netI 0.0629 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.32 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8377 _reflns_number_gt 4887 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0407P)^2^+0.0000P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8377 _refine_ls_number_parameters 619 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_restrained_S_all 0.937 _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 H1 H 0.2094(7) 1.2206(14) 0.1484(8) 0.025(5) Uiso 1 1 d . . . H3 H 0.2126(8) 1.1406(17) 0.0347(9) 0.038(6) Uiso 1 1 d . . . H4 H 0.1851(9) 0.9841(19) -0.0338(12) 0.063(8) Uiso 1 1 d . . . H5 H 0.1376(8) 0.8726(17) 0.0425(9) 0.034(6) Uiso 1 1 d . . . H13 H 0.2707(8) 1.1679(16) 0.2448(9) 0.036(6) Uiso 1 1 d . . . H14 H 0.2817(8) 1.0239(16) 0.3295(10) 0.039(6) Uiso 1 1 d . . . H15 H 0.2091(6) 0.9058(14) 0.3091(8) 0.018(5) Uiso 1 1 d . . . H23 H 0.1353(7) 1.3395(15) 0.1747(9) 0.024(5) Uiso 1 1 d . . . H24 H 0.0488(7) 1.3248(15) 0.2089(9) 0.031(6) Uiso 1 1 d . . . H25 H 0.0337(7) 1.1267(14) 0.2187(9) 0.027(5) Uiso 1 1 d . . . H32A H 0.0259(9) 0.960(2) 0.0534(12) 0.068(8) Uiso 1 1 d . . . H32B H 0.0068(10) 1.0415(19) 0.1012(11) 0.057(8) Uiso 1 1 d . . . H32C H 0.0644(7) 1.0528(15) 0.0795(9) 0.029(5) Uiso 1 1 d . . . H33A H -0.0029(8) 0.8253(18) 0.1210(11) 0.052(7) Uiso 1 1 d . . . H33B H -0.0137(9) 0.9139(19) 0.1741(11) 0.061(8) Uiso 1 1 d . . . H33C H 0.0214(8) 0.8140(17) 0.1911(10) 0.039(6) Uiso 1 1 d . . . H42A H 0.1217(8) 0.6984(16) 0.1008(11) 0.038(6) Uiso 1 1 d . . . H42B H 0.0755(11) 0.734(2) 0.1294(13) 0.074(9) Uiso 1 1 d . . . H42C H 0.1096(9) 0.650(2) 0.1650(12) 0.063(8) Uiso 1 1 d . . . H43A H 0.1892(9) 0.697(2) 0.2151(12) 0.060(8) Uiso 1 1 d . . . H43B H 0.2003(9) 0.7443(18) 0.1440(12) 0.059(7) Uiso 1 1 d . . . H43C H 0.2093(9) 0.8050(19) 0.2098(11) 0.059(8) Uiso 1 1 d . . . H51A H 0.0831(7) 0.9966(16) 0.2869(8) 0.018(5) Uiso 1 1 d . . . H51B H 0.0593(8) 0.9076(15) 0.2701(9) 0.031(6) Uiso 1 1 d . . . Ti1 Ti 0.116030(12) 0.93667(3) 0.188133(15) 0.02075(9) Uani 1 1 d . . . B1 B 0.18571(8) 1.14925(18) 0.15891(11) 0.0245(5) Uani 1 1 d . . . N1 N 0.15197(6) 0.98415(12) 0.10550(7) 0.0259(4) Uani 1 1 d . . . N2 N 0.17707(6) 1.07639(12) 0.10107(7) 0.0249(4) Uani 1 1 d . . . C3 C 0.19332(9) 1.08375(19) 0.04332(10) 0.0393(6) Uani 1 1 d . . . C4 C 0.17863(11) 0.9968(2) 0.00887(11) 0.0529(7) Uani 1 1 d . . . C5 C 0.15309(9) 0.93637(19) 0.04927(10) 0.0389(6) Uani 1 1 d . . . N11 N 0.18789(5) 0.99586(12) 0.23542(7) 0.0219(4) Uani 1 1 d . . . N12 N 0.20992(6) 1.08464(11) 0.21449(7) 0.0219(4) Uani 1 1 d . . . C13 C 0.25078(7) 1.10471(17) 0.25227(9) 0.0263(5) Uani 1 1 d . . . C14 C 0.25642(7) 1.02914(17) 0.29828(10) 0.0291(5) Uani 1 1 d . . . C15 C 0.21668(7) 0.96371(16) 0.28607(9) 0.0254(5) Uani 1 1 d . . . N21 N 0.10243(6) 1.11273(12) 0.19360(7) 0.0236(4) Uani 1 1 d . . . N22 N 0.13537(6) 1.18578(12) 0.17803(7) 0.0227(4) Uani 1 1 d . . . C23 C 0.11640(8) 1.28225(16) 0.18298(10) 0.0291(5) Uani 1 1 d . . . C24 C 0.07006(8) 1.27261(17) 0.20244(10) 0.0320(5) Uani 1 1 d . . . C25 C 0.06278(8) 1.16622(16) 0.20815(9) 0.0276(5) Uani 1 1 d . . . N31 N 0.05284(6) 0.93187(12) 0.14260(7) 0.0262(4) Uani 1 1 d . . . C32 C 0.03650(10) 1.0020(2) 0.08979(12) 0.0399(6) Uani 1 1 d . . . C33 C 0.01173(8) 0.8661(2) 0.15833(12) 0.0356(5) Uani 1 1 d . . . N41 N 0.13656(6) 0.79583(12) 0.17674(7) 0.0252(4) Uani 1 1 d . . . C42 C 0.10821(10) 0.7136(2) 0.14199(13) 0.0385(6) Uani 1 1 d . . . C43 C 0.18702(9) 0.7569(2) 0.18833(13) 0.0387(6) Uani 1 1 d . . . N51 N 0.08809(6) 0.93241(15) 0.28342(7) 0.0207(4) Uani 1 1 d . . . B52 B 0.10177(8) 0.88164(16) 0.35183(10) 0.0205(5) Uani 1 1 d . . . F62 F 0.13607(4) 1.11025(8) 0.33389(5) 0.0295(3) Uani 1 1 d . . . F63 F 0.18371(4) 1.22602(9) 0.42269(5) 0.0384(3) Uani 1 1 d . . . F64 F 0.20991(4) 1.14582(9) 0.54071(5) 0.0401(3) Uani 1 1 d . . . F65 F 0.18943(5) 0.94155(9) 0.56532(5) 0.0428(3) Uani 1 1 d . . . F66 F 0.14073(4) 0.82293(8) 0.47741(5) 0.0317(3) Uani 1 1 d . . . F72 F 0.20435(4) 0.77935(9) 0.39003(5) 0.0312(3) Uani 1 1 d . . . F73 F 0.22637(4) 0.58076(9) 0.36989(6) 0.0462(3) Uani 1 1 d . . . F74 F 0.15891(5) 0.44729(9) 0.30987(7) 0.0561(4) Uani 1 1 d . . . F75 F 0.06999(5) 0.52454(9) 0.26354(6) 0.0476(3) Uani 1 1 d . . . F76 F 0.04644(4) 0.72218(8) 0.28453(5) 0.0321(3) Uani 1 1 d . . . F82 F 0.03055(4) 1.05075(8) 0.36267(5) 0.0329(3) Uani 1 1 d . . . F83 F -0.04911(5) 1.05079(10) 0.42563(6) 0.0452(3) Uani 1 1 d . . . F84 F -0.07397(4) 0.87835(10) 0.49176(6) 0.0480(3) Uani 1 1 d . . . F85 F -0.01608(4) 0.70462(9) 0.49367(5) 0.0382(3) Uani 1 1 d . . . F86 F 0.06220(4) 0.69849(8) 0.43027(5) 0.0302(3) Uani 1 1 d . . . C61 C 0.13706(7) 0.95751(14) 0.39927(9) 0.0211(4) Uani 1 1 d . . . C62 C 0.14922(7) 1.06203(15) 0.39013(9) 0.0227(4) Uani 1 1 d . . . C63 C 0.17376(7) 1.12514(15) 0.43551(9) 0.0257(5) Uani 1 1 d . . . C64 C 0.18727(7) 1.08501(16) 0.49480(9) 0.0284(5) Uani 1 1 d . . . C65 C 0.17657(7) 0.98205(17) 0.50698(9) 0.0279(5) Uani 1 1 d . . . C66 C 0.15192(7) 0.92243(15) 0.46086(9) 0.0242(4) Uani 1 1 d . . . C71 C 0.12336(7) 0.76259(14) 0.33935(8) 0.0211(4) Uani 1 1 d . . . C72 C 0.16870(7) 0.72015(15) 0.35891(9) 0.0259(4) Uani 1 1 d . . . C73 C 0.18127(8) 0.61611(17) 0.34874(10) 0.0323(5) Uani 1 1 d . . . C74 C 0.14814(9) 0.54938(16) 0.31786(11) 0.0370(6) Uani 1 1 d . . . C75 C 0.10306(8) 0.58771(16) 0.29554(10) 0.0328(5) Uani 1 1 d . . . C76 C 0.09237(7) 0.69141(15) 0.30662(9) 0.0265(5) Uani 1 1 d . . . C81 C 0.05068(7) 0.87344(14) 0.39014(8) 0.0204(4) Uani 1 1 d . . . C82 C 0.01994(7) 0.96011(15) 0.39286(9) 0.0244(4) Uani 1 1 d . . . C83 C -0.02149(7) 0.96319(16) 0.42555(9) 0.0300(5) Uani 1 1 d . . . C84 C -0.03407(7) 0.87663(17) 0.45917(9) 0.0306(5) Uani 1 1 d . . . C85 C -0.00483(7) 0.78932(15) 0.45998(9) 0.0267(5) Uani 1 1 d . . . C86 C 0.03618(7) 0.78904(15) 0.42588(9) 0.0233(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ti1 0.02231(18) 0.02062(18) 0.01928(19) -0.00104(15) 0.00166(14) -0.00015(15) B1 0.0283(12) 0.0213(12) 0.0237(12) 0.0005(10) 0.0018(10) 0.0022(10) N1 0.0304(9) 0.0259(9) 0.0219(9) -0.0024(7) 0.0043(7) -0.0006(8) N2 0.0300(9) 0.0238(9) 0.0214(9) 0.0038(7) 0.0054(7) 0.0007(7) C3 0.0522(15) 0.0381(15) 0.0299(13) 0.0057(11) 0.0154(11) -0.0042(12) C4 0.085(2) 0.0535(17) 0.0236(13) -0.0075(12) 0.0220(13) -0.0095(15) C5 0.0565(15) 0.0352(13) 0.0261(12) -0.0086(11) 0.0097(11) -0.0072(12) N11 0.0220(8) 0.0226(9) 0.0216(9) 0.0018(7) 0.0049(7) 0.0023(7) N12 0.0214(8) 0.0204(9) 0.0241(9) 0.0007(7) 0.0042(7) -0.0005(7) C13 0.0214(10) 0.0270(11) 0.0302(12) -0.0028(9) 0.0005(9) -0.0019(9) C14 0.0230(11) 0.0344(12) 0.0286(12) 0.0014(10) -0.0049(9) 0.0035(9) C15 0.0302(11) 0.0259(12) 0.0206(11) 0.0053(9) 0.0045(9) 0.0028(9) N21 0.0245(9) 0.0229(9) 0.0231(9) -0.0005(7) -0.0004(7) 0.0020(7) N22 0.0263(9) 0.0184(9) 0.0228(9) 0.0031(7) -0.0013(7) -0.0007(7) C23 0.0325(12) 0.0201(11) 0.0340(12) 0.0007(10) -0.0020(9) 0.0021(10) C24 0.0277(12) 0.0263(12) 0.0415(14) -0.0048(10) 0.0006(10) 0.0105(10) C25 0.0258(11) 0.0298(12) 0.0270(11) -0.0004(9) 0.0007(9) 0.0058(10) N31 0.0274(9) 0.0290(9) 0.0216(9) -0.0016(7) -0.0010(7) -0.0016(8) C32 0.0409(14) 0.0446(15) 0.0319(14) 0.0060(12) -0.0110(11) -0.0001(13) C33 0.0309(13) 0.0429(15) 0.0322(14) -0.0016(12) -0.0005(11) -0.0046(11) N41 0.0291(9) 0.0235(9) 0.0236(9) -0.0029(7) 0.0064(7) -0.0019(7) C42 0.0412(15) 0.0290(14) 0.0461(16) -0.0127(12) 0.0090(13) -0.0037(11) C43 0.0360(13) 0.0289(14) 0.0507(17) -0.0062(13) 0.0010(12) 0.0065(11) N51 0.0206(9) 0.0187(9) 0.0225(9) -0.0025(8) -0.0009(7) -0.0008(8) B52 0.0212(11) 0.0196(11) 0.0207(12) 0.0001(9) 0.0026(9) 0.0003(9) F62 0.0393(7) 0.0229(6) 0.0253(6) 0.0021(5) -0.0020(5) -0.0023(5) F63 0.0494(8) 0.0230(6) 0.0416(7) -0.0038(5) -0.0028(6) -0.0084(6) F64 0.0453(8) 0.0421(7) 0.0312(7) -0.0130(6) -0.0064(6) -0.0105(6) F65 0.0542(8) 0.0504(8) 0.0216(7) 0.0031(6) -0.0095(6) -0.0115(7) F66 0.0389(7) 0.0299(7) 0.0259(6) 0.0050(5) 0.0002(5) -0.0060(5) F72 0.0241(6) 0.0357(7) 0.0337(7) 0.0079(5) 0.0014(5) 0.0039(5) F73 0.0399(8) 0.0426(8) 0.0586(9) 0.0184(6) 0.0182(6) 0.0211(6) F74 0.0701(10) 0.0225(7) 0.0814(11) 0.0023(6) 0.0383(8) 0.0110(6) F75 0.0596(9) 0.0285(7) 0.0569(9) -0.0166(6) 0.0171(7) -0.0160(6) F76 0.0277(6) 0.0309(7) 0.0372(7) -0.0048(5) 0.0009(5) -0.0042(5) F82 0.0399(7) 0.0246(6) 0.0355(7) 0.0048(5) 0.0112(5) 0.0097(5) F83 0.0427(7) 0.0482(8) 0.0463(8) 0.0043(6) 0.0137(6) 0.0257(6) F84 0.0343(7) 0.0629(9) 0.0503(8) 0.0010(7) 0.0241(6) 0.0063(6) F85 0.0423(7) 0.0379(7) 0.0369(7) 0.0031(6) 0.0177(6) -0.0058(6) F86 0.0351(6) 0.0227(6) 0.0342(7) 0.0044(5) 0.0109(5) 0.0035(5) C61 0.0205(9) 0.0244(11) 0.0188(10) -0.0019(8) 0.0039(8) 0.0029(8) C62 0.0231(10) 0.0261(11) 0.0187(10) 0.0002(9) 0.0008(8) 0.0016(9) C63 0.0254(11) 0.0226(11) 0.0292(12) -0.0038(9) 0.0035(9) -0.0017(9) C64 0.0248(10) 0.0352(13) 0.0251(12) -0.0124(9) 0.0012(9) -0.0038(9) C65 0.0286(11) 0.0370(12) 0.0176(11) 0.0012(9) -0.0014(8) -0.0012(9) C66 0.0238(10) 0.0227(11) 0.0264(11) 0.0024(9) 0.0033(8) -0.0022(8) C71 0.0248(10) 0.0210(10) 0.0186(10) 0.0025(8) 0.0070(8) 0.0005(8) C72 0.0276(11) 0.0261(11) 0.0250(11) 0.0059(9) 0.0079(9) -0.0006(9) C73 0.0320(12) 0.0317(12) 0.0354(12) 0.0125(10) 0.0160(10) 0.0147(10) C74 0.0511(15) 0.0191(12) 0.0450(14) 0.0028(10) 0.0275(12) 0.0056(11) C75 0.0406(13) 0.0255(12) 0.0345(13) -0.0032(9) 0.0163(10) -0.0063(10) C76 0.0279(11) 0.0251(11) 0.0279(11) 0.0011(9) 0.0094(9) 0.0015(9) C81 0.0220(10) 0.0205(10) 0.0181(10) -0.0026(8) -0.0015(8) -0.0007(8) C82 0.0297(11) 0.0230(11) 0.0202(10) -0.0001(8) 0.0010(8) 0.0015(9) C83 0.0284(11) 0.0340(13) 0.0279(11) -0.0039(9) 0.0042(9) 0.0104(9) C84 0.0216(10) 0.0435(14) 0.0275(12) -0.0063(10) 0.0071(9) 0.0015(10) C85 0.0285(11) 0.0281(11) 0.0239(11) 0.0020(9) 0.0051(9) -0.0042(9) C86 0.0222(10) 0.0232(11) 0.0244(11) -0.0046(9) 0.0011(8) 0.0014(9) _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 N41 1.8996(16) . ? Ti1 N31 1.9028(16) . ? Ti1 N1 2.1631(15) . ? Ti1 N51 2.2152(16) . ? Ti1 N11 2.2537(15) . ? Ti1 N21 2.2755(15) . ? B1 N12 1.534(3) . ? B1 N2 1.535(3) . ? B1 N22 1.541(3) . ? B1 H1 1.148(18) . ? N1 C5 1.337(3) . ? N1 N2 1.367(2) . ? N2 C3 1.338(3) . ? C3 C4 1.364(3) . ? C3 H3 0.92(2) . ? C4 C5 1.383(3) . ? C4 H4 0.95(2) . ? C5 H5 0.92(2) . ? N11 C15 1.335(2) . ? N11 N12 1.372(2) . ? N12 C13 1.339(2) . ? C13 C14 1.366(3) . ? C13 H13 0.99(2) . ? C14 C15 1.375(3) . ? C14 H14 0.91(2) . ? C15 H15 0.917(18) . ? N21 C25 1.339(2) . ? N21 N22 1.355(2) . ? N22 C23 1.340(2) . ? C23 C24 1.372(3) . ? C23 H23 0.919(19) . ? C24 C25 1.375(3) . ? C24 H24 0.90(2) . ? C25 H25 0.98(2) . ? N31 C33 1.463(3) . ? N31 C32 1.467(3) . ? C32 H32A 0.96(3) . ? C32 H32B 1.00(3) . ? C32 H32C 1.04(2) . ? C33 H33A 1.00(2) . ? C33 H33B 1.00(3) . ? C33 H33C 0.98(2) . ? N41 C42 1.461(3) . ? N41 C43 1.466(3) . ? C42 H42A 0.99(2) . ? C42 H42B 0.94(3) . ? C42 H42C 0.95(3) . ? C43 H43A 0.95(3) . ? C43 H43B 1.05(3) . ? C43 H43C 0.95(3) . ? N51 B52 1.596(3) . ? N51 H51A 0.83(2) . ? N51 H51B 0.87(2) . ? B52 C61 1.642(3) . ? B52 C71 1.655(3) . ? B52 C81 1.679(3) . ? F62 C62 1.356(2) . ? F63 C63 1.345(2) . ? F64 C64 1.347(2) . ? F65 C65 1.353(2) . ? F66 C66 1.355(2) . ? F72 C72 1.355(2) . ? F73 C73 1.351(2) . ? F74 C74 1.346(2) . ? F75 C75 1.346(2) . ? F76 C76 1.358(2) . ? F82 C82 1.361(2) . ? F83 C83 1.347(2) . ? F84 C84 1.341(2) . ? F85 C85 1.342(2) . ? F86 C86 1.353(2) . ? C61 C62 1.389(3) . ? C61 C66 1.401(3) . ? C62 C63 1.378(3) . ? C63 C64 1.372(3) . ? C64 C65 1.372(3) . ? C65 C66 1.365(3) . ? C71 C72 1.382(3) . ? C71 C76 1.383(3) . ? C72 C73 1.389(3) . ? C73 C74 1.365(3) . ? C74 C75 1.370(3) . ? C75 C76 1.376(3) . ? C81 C86 1.390(3) . ? C81 C82 1.391(3) . ? C82 C83 1.379(3) . ? C83 C84 1.371(3) . ? C84 C85 1.368(3) . ? C85 C86 1.385(3) . ? 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 N41 Ti1 N31 99.86(7) . . ? N41 Ti1 N1 90.04(6) . . ? N31 Ti1 N1 93.37(6) . . ? N41 Ti1 N51 102.80(7) . . ? N31 Ti1 N51 95.00(6) . . ? N1 Ti1 N51 163.21(7) . . ? N41 Ti1 N11 96.62(6) . . ? N31 Ti1 N11 162.17(6) . . ? N1 Ti1 N11 79.82(6) . . ? N51 Ti1 N11 87.89(6) . . ? N41 Ti1 N21 170.63(6) . . ? N31 Ti1 N21 84.95(6) . . ? N1 Ti1 N21 81.61(6) . . ? N51 Ti1 N21 84.66(6) . . ? N11 Ti1 N21 77.80(6) . . ? N12 B1 N2 108.09(16) . . ? N12 B1 N22 107.24(16) . . ? N2 B1 N22 108.21(16) . . ? N12 B1 H1 111.1(9) . . ? N2 B1 H1 111.9(9) . . ? N22 B1 H1 110.2(9) . . ? C5 N1 N2 106.17(16) . . ? C5 N1 Ti1 129.58(15) . . ? N2 N1 Ti1 124.18(11) . . ? C3 N2 N1 109.38(17) . . ? C3 N2 B1 130.00(18) . . ? N1 N2 B1 120.47(15) . . ? N2 C3 C4 108.9(2) . . ? N2 C3 H3 118.4(13) . . ? C4 C3 H3 132.6(13) . . ? C3 C4 C5 105.2(2) . . ? C3 C4 H4 125.1(15) . . ? C5 C4 H4 129.7(15) . . ? N1 C5 C4 110.3(2) . . ? N1 C5 H5 119.5(13) . . ? C4 C5 H5 130.1(13) . . ? C15 N11 N12 105.41(15) . . ? C15 N11 Ti1 132.99(13) . . ? N12 N11 Ti1 121.55(11) . . ? C13 N12 N11 109.41(15) . . ? C13 N12 B1 129.38(17) . . ? N11 N12 B1 121.04(15) . . ? N12 C13 C14 108.97(18) . . ? N12 C13 H13 120.1(11) . . ? C14 C13 H13 130.9(11) . . ? C13 C14 C15 104.79(18) . . ? C13 C14 H14 126.5(13) . . ? C15 C14 H14 128.7(13) . . ? N11 C15 C14 111.40(18) . . ? N11 C15 H15 121.7(11) . . ? C14 C15 H15 126.8(11) . . ? C25 N21 N22 106.04(15) . . ? C25 N21 Ti1 130.66(14) . . ? N22 N21 Ti1 123.21(11) . . ? C23 N22 N21 109.81(16) . . ? C23 N22 B1 131.14(17) . . ? N21 N22 B1 119.05(15) . . ? N22 C23 C24 108.41(19) . . ? N22 C23 H23 118.9(12) . . ? C24 C23 H23 132.6(12) . . ? C23 C24 C25 105.01(19) . . ? C23 C24 H24 127.2(13) . . ? C25 C24 H24 127.8(13) . . ? N21 C25 C24 110.72(19) . . ? N21 C25 H25 118.7(11) . . ? C24 C25 H25 130.5(11) . . ? C33 N31 C32 109.40(18) . . ? C33 N31 Ti1 125.83(14) . . ? C32 N31 Ti1 124.52(14) . . ? N31 C32 H32A 108.7(15) . . ? N31 C32 H32B 108.7(14) . . ? H32A C32 H32B 106(2) . . ? N31 C32 H32C 111.0(11) . . ? H32A C32 H32C 110.7(19) . . ? H32B C32 H32C 111.4(17) . . ? N31 C33 H33A 112.4(13) . . ? N31 C33 H33B 107.4(14) . . ? H33A C33 H33B 109.6(19) . . ? N31 C33 H33C 112.5(12) . . ? H33A C33 H33C 105.8(18) . . ? H33B C33 H33C 109.1(18) . . ? C42 N41 C43 106.94(18) . . ? C42 N41 Ti1 126.13(15) . . ? C43 N41 Ti1 125.61(14) . . ? N41 C42 H42A 111.0(12) . . ? N41 C42 H42B 113.3(16) . . ? H42A C42 H42B 103(2) . . ? N41 C42 H42C 111.2(15) . . ? H42A C42 H42C 106.5(19) . . ? H42B C42 H42C 112(2) . . ? N41 C43 H43A 112.4(15) . . ? N41 C43 H43B 107.4(14) . . ? H43A C43 H43B 114(2) . . ? N41 C43 H43C 114.6(15) . . ? H43A C43 H43C 103(2) . . ? H43B C43 H43C 105(2) . . ? B52 N51 Ti1 139.44(12) . . ? B52 N51 H51A 110.2(12) . . ? Ti1 N51 H51A 97.4(12) . . ? B52 N51 H51B 106.1(13) . . ? Ti1 N51 H51B 95.2(13) . . ? H51A N51 H51B 103.4(18) . . ? N51 B52 C61 113.09(16) . . ? N51 B52 C71 106.53(15) . . ? C61 B52 C71 115.88(15) . . ? N51 B52 C81 108.83(15) . . ? C61 B52 C81 102.24(14) . . ? C71 B52 C81 110.11(15) . . ? C62 C61 C66 112.39(16) . . ? C62 C61 B52 127.84(17) . . ? C66 C61 B52 119.05(16) . . ? F62 C62 C63 114.84(17) . . ? F62 C62 C61 120.44(16) . . ? C63 C62 C61 124.70(18) . . ? F63 C63 C64 119.74(17) . . ? F63 C63 C62 120.73(17) . . ? C64 C63 C62 119.52(18) . . ? F64 C64 C65 120.37(18) . . ? F64 C64 C63 120.82(18) . . ? C65 C64 C63 118.81(17) . . ? F65 C65 C66 120.67(18) . . ? F65 C65 C64 119.48(17) . . ? C66 C65 C64 119.82(18) . . ? F66 C66 C65 116.35(17) . . ? F66 C66 C61 118.91(16) . . ? C65 C66 C61 124.73(18) . . ? C72 C71 C76 112.80(17) . . ? C72 C71 B52 129.30(17) . . ? C76 C71 B52 117.86(16) . . ? F72 C72 C71 121.05(17) . . ? F72 C72 C73 115.30(17) . . ? C71 C72 C73 123.65(19) . . ? F73 C73 C74 119.93(19) . . ? F73 C73 C72 119.8(2) . . ? C74 C73 C72 120.25(19) . . ? F74 C74 C73 121.1(2) . . ? F74 C74 C75 120.0(2) . . ? C73 C74 C75 118.83(19) . . ? F75 C75 C74 120.29(19) . . ? F75 C75 C76 121.0(2) . . ? C74 C75 C76 118.7(2) . . ? F76 C76 C75 114.95(18) . . ? F76 C76 C71 119.34(16) . . ? C75 C76 C71 125.67(19) . . ? C86 C81 C82 112.80(17) . . ? C86 C81 B52 126.80(16) . . ? C82 C81 B52 120.17(16) . . ? F82 C82 C83 115.40(16) . . ? F82 C82 C81 119.85(17) . . ? C83 C82 C81 124.74(18) . . ? F83 C83 C84 119.85(17) . . ? F83 C83 C82 120.69(18) . . ? C84 C83 C82 119.45(18) . . ? F84 C84 C85 120.55(19) . . ? F84 C84 C83 120.38(18) . . ? C85 C84 C83 119.05(18) . . ? F85 C85 C84 119.83(17) . . ? F85 C85 C86 120.50(17) . . ? C84 C85 C86 119.66(18) . . ? F86 C86 C85 114.31(16) . . ? F86 C86 C81 121.42(16) . . ? C85 C86 C81 124.27(18) . . ? 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 N41 Ti1 N1 C5 42.05(19) . . . . ? N31 Ti1 N1 C5 -57.82(19) . . . . ? N51 Ti1 N1 C5 -177.6(2) . . . . ? N11 Ti1 N1 C5 138.78(19) . . . . ? N21 Ti1 N1 C5 -142.21(19) . . . . ? N41 Ti1 N1 N2 -141.22(14) . . . . ? N31 Ti1 N1 N2 118.90(14) . . . . ? N51 Ti1 N1 N2 -0.9(3) . . . . ? N11 Ti1 N1 N2 -44.50(14) . . . . ? N21 Ti1 N1 N2 34.51(14) . . . . ? C5 N1 N2 C3 -0.4(2) . . . . ? Ti1 N1 N2 C3 -177.79(14) . . . . ? C5 N1 N2 B1 -176.48(18) . . . . ? Ti1 N1 N2 B1 6.1(2) . . . . ? N12 B1 N2 C3 -121.4(2) . . . . ? N22 B1 N2 C3 122.8(2) . . . . ? N12 B1 N2 N1 53.7(2) . . . . ? N22 B1 N2 N1 -62.1(2) . . . . ? N1 N2 C3 C4 0.6(3) . . . . ? B1 N2 C3 C4 176.2(2) . . . . ? N2 C3 C4 C5 -0.6(3) . . . . ? N2 N1 C5 C4 0.0(3) . . . . ? Ti1 N1 C5 C4 177.22(17) . . . . ? C3 C4 C5 N1 0.3(3) . . . . ? N41 Ti1 N11 C15 -54.07(17) . . . . ? N31 Ti1 N11 C15 148.4(2) . . . . ? N1 Ti1 N11 C15 -142.92(17) . . . . ? N51 Ti1 N11 C15 48.58(17) . . . . ? N21 Ti1 N11 C15 133.56(17) . . . . ? N41 Ti1 N11 N12 128.98(13) . . . . ? N31 Ti1 N11 N12 -28.6(3) . . . . ? N1 Ti1 N11 N12 40.13(12) . . . . ? N51 Ti1 N11 N12 -128.37(13) . . . . ? N21 Ti1 N11 N12 -43.39(12) . . . . ? C15 N11 N12 C13 -0.29(19) . . . . ? Ti1 N11 N12 C13 177.40(12) . . . . ? C15 N11 N12 B1 -176.00(16) . . . . ? Ti1 N11 N12 B1 1.7(2) . . . . ? N2 B1 N12 C13 128.14(19) . . . . ? N22 B1 N12 C13 -115.4(2) . . . . ? N2 B1 N12 N11 -57.1(2) . . . . ? N22 B1 N12 N11 59.4(2) . . . . ? N11 N12 C13 C14 0.4(2) . . . . ? B1 N12 C13 C14 175.65(18) . . . . ? N12 C13 C14 C15 -0.4(2) . . . . ? N12 N11 C15 C14 0.1(2) . . . . ? Ti1 N11 C15 C14 -177.24(13) . . . . ? C13 C14 C15 N11 0.2(2) . . . . ? N31 Ti1 N21 C25 45.65(17) . . . . ? N1 Ti1 N21 C25 139.82(17) . . . . ? N51 Ti1 N21 C25 -49.86(16) . . . . ? N11 Ti1 N21 C25 -138.86(17) . . . . ? N31 Ti1 N21 N22 -130.50(13) . . . . ? N1 Ti1 N21 N22 -36.34(13) . . . . ? N51 Ti1 N21 N22 133.98(13) . . . . ? N11 Ti1 N21 N22 44.98(13) . . . . ? C25 N21 N22 C23 0.08(19) . . . . ? Ti1 N21 N22 C23 177.05(12) . . . . ? C25 N21 N22 B1 179.77(16) . . . . ? Ti1 N21 N22 B1 -3.3(2) . . . . ? N12 B1 N22 C23 121.9(2) . . . . ? N2 B1 N22 C23 -121.7(2) . . . . ? N12 B1 N22 N21 -57.7(2) . . . . ? N2 B1 N22 N21 58.7(2) . . . . ? N21 N22 C23 C24 0.2(2) . . . . ? B1 N22 C23 C24 -179.42(18) . . . . ? N22 C23 C24 C25 -0.4(2) . . . . ? N22 N21 C25 C24 -0.4(2) . . . . ? Ti1 N21 C25 C24 -177.01(13) . . . . ? C23 C24 C25 N21 0.5(2) . . . . ? N41 Ti1 N31 C33 62.45(18) . . . . ? N1 Ti1 N31 C33 153.08(17) . . . . ? N51 Ti1 N31 C33 -41.49(18) . . . . ? N11 Ti1 N31 C33 -140.2(2) . . . . ? N21 Ti1 N31 C33 -125.66(17) . . . . ? N41 Ti1 N31 C32 -124.02(18) . . . . ? N1 Ti1 N31 C32 -33.39(18) . . . . ? N51 Ti1 N31 C32 132.04(18) . . . . ? N11 Ti1 N31 C32 33.3(3) . . . . ? N21 Ti1 N31 C32 47.87(18) . . . . ? N31 Ti1 N41 C42 -0.37(18) . . . . ? N1 Ti1 N41 C42 -93.79(18) . . . . ? N51 Ti1 N41 C42 97.12(18) . . . . ? N11 Ti1 N41 C42 -173.55(17) . . . . ? N31 Ti1 N41 C43 164.81(18) . . . . ? N1 Ti1 N41 C43 71.38(18) . . . . ? N51 Ti1 N41 C43 -97.71(18) . . . . ? N11 Ti1 N41 C43 -8.37(18) . . . . ? N41 Ti1 N51 B52 40.3(2) . . . . ? N31 Ti1 N51 B52 141.6(2) . . . . ? N1 Ti1 N51 B52 -98.8(3) . . . . ? N11 Ti1 N51 B52 -56.0(2) . . . . ? N21 Ti1 N51 B52 -134.0(2) . . . . ? Ti1 N51 B52 C61 91.0(2) . . . . ? Ti1 N51 B52 C71 -37.4(3) . . . . ? Ti1 N51 B52 C81 -156.12(15) . . . . ? N51 B52 C61 C62 10.6(3) . . . . ? C71 B52 C61 C62 133.97(19) . . . . ? C81 B52 C61 C62 -106.3(2) . . . . ? N51 B52 C61 C66 -179.91(16) . . . . ? C71 B52 C61 C66 -56.5(2) . . . . ? C81 B52 C61 C66 63.2(2) . . . . ? C66 C61 C62 F62 -177.66(16) . . . . ? B52 C61 C62 F62 -7.5(3) . . . . ? C66 C61 C62 C63 0.9(3) . . . . ? B52 C61 C62 C63 171.01(18) . . . . ? F62 C62 C63 F63 -0.8(3) . . . . ? C61 C62 C63 F63 -179.45(17) . . . . ? F62 C62 C63 C64 177.84(16) . . . . ? C61 C62 C63 C64 -0.8(3) . . . . ? F63 C63 C64 F64 0.8(3) . . . . ? C62 C63 C64 F64 -177.88(17) . . . . ? F63 C63 C64 C65 179.70(18) . . . . ? C62 C63 C64 C65 1.0(3) . . . . ? F64 C64 C65 F65 -0.7(3) . . . . ? C63 C64 C65 F65 -179.65(17) . . . . ? F64 C64 C65 C66 177.42(18) . . . . ? C63 C64 C65 C66 -1.5(3) . . . . ? F65 C65 C66 F66 1.1(3) . . . . ? C64 C65 C66 F66 -177.08(17) . . . . ? F65 C65 C66 C61 179.91(17) . . . . ? C64 C65 C66 C61 1.8(3) . . . . ? C62 C61 C66 F66 177.42(16) . . . . ? B52 C61 C66 F66 6.3(3) . . . . ? C62 C61 C66 C65 -1.4(3) . . . . ? B52 C61 C66 C65 -172.47(18) . . . . ? N51 B52 C71 C72 120.9(2) . . . . ? C61 B52 C71 C72 -5.9(3) . . . . ? C81 B52 C71 C72 -121.3(2) . . . . ? N51 B52 C71 C76 -61.5(2) . . . . ? C61 B52 C71 C76 171.72(16) . . . . ? C81 B52 C71 C76 56.3(2) . . . . ? C76 C71 C72 F72 177.99(16) . . . . ? B52 C71 C72 F72 -4.3(3) . . . . ? C76 C71 C72 C73 -2.1(3) . . . . ? B52 C71 C72 C73 175.63(18) . . . . ? F72 C72 C73 F73 0.4(3) . . . . ? C71 C72 C73 F73 -179.50(17) . . . . ? F72 C72 C73 C74 179.99(17) . . . . ? C71 C72 C73 C74 0.1(3) . . . . ? F73 C73 C74 F74 2.3(3) . . . . ? C72 C73 C74 F74 -177.22(18) . . . . ? F73 C73 C74 C75 -178.47(18) . . . . ? C72 C73 C74 C75 2.0(3) . . . . ? F74 C74 C75 F75 -2.4(3) . . . . ? C73 C74 C75 F75 178.40(18) . . . . ? F74 C74 C75 C76 177.44(18) . . . . ? C73 C74 C75 C76 -1.8(3) . . . . ? F75 C75 C76 F76 1.7(3) . . . . ? C74 C75 C76 F76 -178.17(17) . . . . ? F75 C75 C76 C71 179.34(18) . . . . ? C74 C75 C76 C71 -0.5(3) . . . . ? C72 C71 C76 F76 179.92(16) . . . . ? B52 C71 C76 F76 1.9(3) . . . . ? C72 C71 C76 C75 2.3(3) . . . . ? B52 C71 C76 C75 -175.67(18) . . . . ? N51 B52 C81 C86 137.11(19) . . . . ? C61 B52 C81 C86 -103.0(2) . . . . ? C71 B52 C81 C86 20.7(3) . . . . ? N51 B52 C81 C82 -48.7(2) . . . . ? C61 B52 C81 C82 71.1(2) . . . . ? C71 B52 C81 C82 -165.16(16) . . . . ? C86 C81 C82 F82 176.99(16) . . . . ? B52 C81 C82 F82 2.1(3) . . . . ? C86 C81 C82 C83 -1.8(3) . . . . ? B52 C81 C82 C83 -176.75(18) . . . . ? F82 C82 C83 F83 1.1(3) . . . . ? C81 C82 C83 F83 179.92(17) . . . . ? F82 C82 C83 C84 -177.79(17) . . . . ? C81 C82 C83 C84 1.1(3) . . . . ? F83 C83 C84 F84 0.5(3) . . . . ? C82 C83 C84 F84 179.38(18) . . . . ? F83 C83 C84 C85 -178.21(18) . . . . ? C82 C83 C84 C85 0.6(3) . . . . ? F84 C84 C85 F85 0.0(3) . . . . ? C83 C84 C85 F85 178.70(18) . . . . ? F84 C84 C85 C86 179.87(17) . . . . ? C83 C84 C85 C86 -1.4(3) . . . . ? F85 C85 C86 F86 -0.1(3) . . . . ? C84 C85 C86 F86 -179.96(17) . . . . ? F85 C85 C86 C81 -179.56(17) . . . . ? C84 C85 C86 C81 0.5(3) . . . . ? C82 C81 C86 F86 -178.46(16) . . . . ? B52 C81 C86 F86 -3.9(3) . . . . ? C82 C81 C86 C85 1.0(3) . . . . ? B52 C81 C86 C85 175.53(18) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N51 H51A F62 0.83(2) 2.220(19) 2.780(2) 124.9(16) . N51 H51A F82 0.83(2) 2.347(18) 2.830(2) 117.6(15) . N51 H51A N21 0.83(2) 2.555(18) 3.024(2) 117.0(15) . N51 H51B F76 0.87(2) 2.41(2) 2.908(2) 116.9(16) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.315 _refine_diff_density_min -0.347 _refine_diff_density_rms 0.052 #===END data_4.hexane _database_code_depnum_ccdc_archive 'CCDC 823224' #TrackingRef '- fuller et al cif.cif' _chemical_formula_structural 'HB(C3H3N2)3Zr(N(CH3)2)2NH2B(C6F5)3, C6 H14' _chemical_name_common 'HB(C3H3N2)3Zr(N(CH3)2)2NH2B(C6F5)3, c6 H14' _chemical_melting_point ? _chemical_formula_moiety 'C31 H24 B2 F15 N9 Zr, C6 H14' _chemical_formula_sum 'C37 H38 B2 F15 N9 Zr' _chemical_formula_weight 1006.60 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 -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.6960(4) _cell_length_b 24.1645(8) _cell_length_c 14.1775(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.824(3) _cell_angle_gamma 90.00 _cell_volume 4184.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 14054 _cell_measurement_theta_min 3.3157 _cell_measurement_theta_max 33.6205 _exptl_crystal_description plates _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.598 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 0.371 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9102 _exptl_absorpt_correction_T_max 1.0679 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44382 _diffrn_reflns_av_R_equivalents 0.0728 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7352 _reflns_number_gt 5407 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^ > 2\s(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^)+(0.0322P)^2^+4.4782P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7352 _refine_ls_number_parameters 669 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0818 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.0987 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.066 _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 H1 H 0.165(3) 0.1276(13) 0.234(2) 0.029(9) Uiso 1 1 d . . . H3 H 0.102(3) 0.2222(14) 0.294(3) 0.034(10) Uiso 1 1 d . . . H4 H 0.174(4) 0.3111(19) 0.362(3) 0.068(15) Uiso 1 1 d . . . H5 H 0.377(3) 0.3087(15) 0.378(3) 0.039(10) Uiso 1 1 d . . . H13 H 0.215(3) 0.0554(17) 0.372(3) 0.058(13) Uiso 1 1 d . . . H14 H 0.380(3) 0.0292(18) 0.510(3) 0.058(14) Uiso 1 1 d . . . H15 H 0.529(3) 0.0907(15) 0.495(3) 0.036(11) Uiso 1 1 d . . . H23 H 0.189(3) 0.1086(15) 0.059(3) 0.038(11) Uiso 1 1 d . . . H24 H 0.328(3) 0.1185(15) -0.037(3) 0.038(11) Uiso 1 1 d . . . H25 H 0.491(2) 0.1645(12) 0.077(2) 0.017(8) Uiso 1 1 d . . . H32A H 0.645(3) 0.3089(14) 0.386(3) 0.031(10) Uiso 1 1 d . . . H32B H 0.553(3) 0.3497(19) 0.330(3) 0.061(13) Uiso 1 1 d . . . H32C H 0.659(3) 0.3362(18) 0.292(3) 0.063(14) Uiso 1 1 d . . . H33A H 0.438(4) 0.322(2) 0.178(4) 0.082(17) Uiso 1 1 d . . . H33B H 0.446(3) 0.2626(17) 0.131(3) 0.045(11) Uiso 1 1 d . . . H33C H 0.544(4) 0.305(2) 0.137(4) 0.082(16) Uiso 1 1 d . . . H42A H 0.725(3) 0.1925(17) 0.566(3) 0.054(12) Uiso 1 1 d . . . H42B H 0.711(3) 0.2582(19) 0.539(3) 0.058(13) Uiso 1 1 d . . . H42C H 0.729(4) 0.2189(18) 0.463(3) 0.064(14) Uiso 1 1 d . . . H43A H 0.443(3) 0.2101(14) 0.526(3) 0.039(11) Uiso 1 1 d . . . H43B H 0.559(4) 0.1907(19) 0.606(4) 0.073(15) Uiso 1 1 d . . . H43C H 0.536(4) 0.252(2) 0.586(4) 0.082(17) Uiso 1 1 d . . . H51A H 0.627(3) 0.1083(19) 0.298(3) 0.055(15) Uiso 1 1 d . . . H51B H 0.617(3) 0.1408(16) 0.225(3) 0.039(12) Uiso 1 1 d . . . Zr1 Zr 0.51833(3) 0.198938(14) 0.32876(3) 0.02722(10) Uani 1 1 d . . . B1 B 0.2506(4) 0.14400(19) 0.2553(4) 0.0396(11) Uani 1 1 d . . . N1 N 0.3471(2) 0.23281(12) 0.3219(2) 0.0373(8) Uani 1 1 d . . . N2 N 0.2513(2) 0.20420(13) 0.2921(2) 0.0361(7) Uani 1 1 d . . . C3 C 0.1693(3) 0.23567(18) 0.3052(3) 0.0454(11) Uani 1 1 d . . . C4 C 0.2108(4) 0.28522(19) 0.3428(4) 0.0567(13) Uani 1 1 d . . . C5 C 0.3211(3) 0.28217(17) 0.3519(4) 0.0479(11) Uani 1 1 d . . . N11 N 0.4288(2) 0.12205(12) 0.3795(2) 0.0348(7) Uani 1 1 d . . . N12 N 0.3210(2) 0.10923(12) 0.3390(2) 0.0356(7) Uani 1 1 d . . . C13 C 0.2905(4) 0.06880(17) 0.3905(3) 0.0469(11) Uani 1 1 d . . . C14 C 0.3783(4) 0.0542(2) 0.4660(4) 0.0567(13) Uani 1 1 d . . . C15 C 0.4618(4) 0.08807(18) 0.4580(3) 0.0449(11) Uani 1 1 d . . . N21 N 0.4053(2) 0.16157(12) 0.1773(2) 0.0346(7) Uani 1 1 d . . . N22 N 0.3014(2) 0.14277(12) 0.1684(2) 0.0347(7) Uani 1 1 d . . . C23 C 0.2584(3) 0.12352(17) 0.0773(3) 0.0416(10) Uani 1 1 d . . . C24 C 0.3328(3) 0.12918(17) 0.0251(3) 0.0415(10) Uani 1 1 d . . . C25 C 0.4228(3) 0.15333(16) 0.0891(3) 0.0365(9) Uani 1 1 d . . . N31 N 0.5466(2) 0.27245(12) 0.2691(2) 0.0310(7) Uani 1 1 d . . . C32 C 0.6053(4) 0.31923(19) 0.3227(4) 0.0458(11) Uani 1 1 d . . . C33 C 0.4890(5) 0.2920(2) 0.1705(4) 0.0521(11) Uani 1 1 d . . . N41 N 0.5757(2) 0.21382(12) 0.4735(2) 0.0347(7) Uani 1 1 d . . . C42 C 0.6935(4) 0.2217(2) 0.5127(4) 0.0465(11) Uani 1 1 d . . . C43 C 0.5211(4) 0.2161(3) 0.5518(4) 0.0567(13) Uani 1 1 d . . . N51 N 0.6464(3) 0.14051(15) 0.2872(3) 0.0330(8) Uani 1 1 d . . . B52 B 0.7755(3) 0.14276(18) 0.2986(3) 0.0330(10) Uani 1 1 d . . . F62 F 0.70057(17) 0.09345(10) 0.46846(18) 0.0524(6) Uani 1 1 d . . . F63 F 0.8280(2) 0.04484(12) 0.6247(2) 0.0773(9) Uani 1 1 d . . . F64 F 1.0476(2) 0.03863(12) 0.6512(2) 0.0773(9) Uani 1 1 d . . . F65 F 1.13790(18) 0.08661(12) 0.51788(19) 0.0659(8) Uani 1 1 d . . . F66 F 1.01161(16) 0.13706(10) 0.36019(16) 0.0466(6) Uani 1 1 d . . . F72 F 0.92317(16) 0.23131(8) 0.42760(15) 0.0401(5) Uani 1 1 d . . . F73 F 0.96327(19) 0.33040(9) 0.36677(18) 0.0542(6) Uani 1 1 d . . . F74 F 0.8652(2) 0.36493(10) 0.1807(2) 0.0677(8) Uani 1 1 d . . . F75 F 0.7243(2) 0.29550(11) 0.05511(18) 0.0672(7) Uani 1 1 d . . . F76 F 0.68424(17) 0.19475(10) 0.11314(15) 0.0502(6) Uani 1 1 d . . . F82 F 0.71176(19) 0.02759(9) 0.28511(19) 0.0528(6) Uani 1 1 d . . . F83 F 0.7664(2) -0.05232(11) 0.1791(2) 0.0784(9) Uani 1 1 d . . . F84 F 0.9018(2) -0.03110(14) 0.0653(3) 0.1062(13) Uani 1 1 d . . . F85 F 0.9755(2) 0.07481(16) 0.0554(2) 0.1005(12) Uani 1 1 d . . . F86 F 0.91702(19) 0.15607(12) 0.15329(18) 0.0595(7) Uani 1 1 d . . . C61 C 0.8484(3) 0.11940(14) 0.4059(3) 0.0316(8) Uani 1 1 d . . . C62 C 0.8096(3) 0.09407(15) 0.4769(3) 0.0363(9) Uani 1 1 d . . . C63 C 0.8734(3) 0.06782(17) 0.5584(3) 0.0469(11) Uani 1 1 d . . . C64 C 0.9841(4) 0.06482(17) 0.5725(3) 0.0506(11) Uani 1 1 d . . . C65 C 1.0289(3) 0.08912(17) 0.5052(3) 0.0446(10) Uani 1 1 d . . . C66 C 0.9621(3) 0.11537(15) 0.4247(3) 0.0348(9) Uani 1 1 d . . . C71 C 0.8024(3) 0.20673(15) 0.2726(3) 0.0331(8) Uani 1 1 d . . . C72 C 0.8717(3) 0.24400(16) 0.3333(3) 0.0342(9) Uani 1 1 d . . . C73 C 0.8941(3) 0.29652(17) 0.3038(3) 0.0412(9) Uani 1 1 d . . . C74 C 0.8455(4) 0.31403(17) 0.2101(3) 0.0487(11) Uani 1 1 d . . . C75 C 0.7737(3) 0.27930(18) 0.1473(3) 0.0464(11) Uani 1 1 d . . . C76 C 0.7543(3) 0.22735(17) 0.1793(3) 0.0400(9) Uani 1 1 d . . . C81 C 0.8066(3) 0.09722(16) 0.2224(3) 0.0386(9) Uani 1 1 d . . . C82 C 0.7736(3) 0.04256(18) 0.2247(3) 0.0452(11) Uani 1 1 d . . . C83 C 0.8022(4) -0.00002(19) 0.1722(4) 0.0577(13) Uani 1 1 d . . . C84 C 0.8701(4) 0.0105(2) 0.1152(4) 0.0705(17) Uani 1 1 d . . . C85 C 0.9074(4) 0.0633(3) 0.1106(3) 0.0660(15) Uani 1 1 d . . . C86 C 0.8750(3) 0.1051(2) 0.1631(3) 0.0507(12) Uani 1 1 d . . . C91A C 0.6066(12) 0.0591(6) 0.9434(11) 0.156(5) Uiso 0.78 1 d P A 1 C91B C 0.535(4) 0.034(2) 0.961(4) 0.172(18) Uiso 0.22 1 d P A 2 C92A C 0.512(2) 0.0147(11) 0.866(2) 0.136(8) Uiso 0.35 1 d P A 3 C92B C 0.5453(11) -0.0084(6) 0.8042(11) 0.129(4) Uiso 0.65 1 d P A 4 C93 C 0.6289(9) 0.0304(5) 0.8662(14) 0.229(7) Uani 1 1 d . . . C94A C 0.779(2) 0.0212(11) 0.8373(19) 0.145(9) Uiso 0.41 1 d P A 5 C94B C 0.7001(19) 0.0429(9) 0.8269(13) 0.139(6) Uiso 0.59 1 d P A 6 C95 C 0.8032(18) 0.0674(7) 0.8383(11) 0.289(9) Uani 1 1 d . . . C96A C 0.6209(13) 0.0700(7) 0.7343(12) 0.148(5) Uiso 0.58 1 d P A 6 C96B C 0.5343(19) 0.0175(10) 0.7311(19) 0.157(8) Uiso 0.42 1 d P A 7 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 0.02540(17) 0.02723(18) 0.02902(19) -0.00115(17) 0.00742(13) -0.00038(16) B1 0.031(2) 0.038(3) 0.050(3) -0.001(2) 0.010(2) -0.003(2) N1 0.0293(17) 0.0329(18) 0.051(2) -0.0019(15) 0.0139(15) -0.0006(14) N2 0.0257(15) 0.0382(18) 0.0447(19) 0.0040(15) 0.0100(14) 0.0025(14) C3 0.030(2) 0.049(3) 0.062(3) 0.009(2) 0.019(2) 0.005(2) C4 0.047(3) 0.042(3) 0.090(4) -0.003(2) 0.033(3) 0.011(2) C5 0.037(2) 0.034(2) 0.076(3) -0.005(2) 0.020(2) 0.0015(19) N11 0.0306(17) 0.0365(18) 0.0377(19) 0.0060(15) 0.0102(14) -0.0020(14) N12 0.0335(18) 0.0343(18) 0.042(2) -0.0011(15) 0.0145(15) -0.0054(14) C13 0.044(3) 0.038(2) 0.064(3) 0.008(2) 0.023(2) -0.005(2) C14 0.055(3) 0.051(3) 0.072(4) 0.027(3) 0.032(3) 0.000(2) C15 0.038(2) 0.049(3) 0.049(3) 0.011(2) 0.014(2) 0.003(2) N21 0.0277(16) 0.0383(19) 0.0356(19) 0.0009(14) 0.0048(14) -0.0021(14) N22 0.0293(17) 0.0361(18) 0.0358(19) -0.0022(14) 0.0041(14) -0.0036(14) C23 0.034(2) 0.040(2) 0.042(3) -0.0029(19) -0.004(2) -0.0054(18) C24 0.044(2) 0.045(3) 0.031(2) -0.0049(19) 0.002(2) 0.0017(19) C25 0.036(2) 0.045(2) 0.029(2) -0.0026(17) 0.0092(18) 0.0008(18) N31 0.0302(16) 0.0320(17) 0.0295(17) -0.0017(13) 0.0058(13) -0.0001(13) C32 0.049(3) 0.039(3) 0.046(3) 0.002(2) 0.007(2) -0.010(2) C33 0.058(3) 0.041(3) 0.048(3) 0.010(2) 0.000(2) -0.006(3) N41 0.0316(17) 0.0388(19) 0.0355(18) -0.0045(14) 0.0119(14) -0.0032(13) C42 0.046(3) 0.041(3) 0.053(3) -0.008(2) 0.014(2) -0.009(2) C43 0.049(3) 0.086(4) 0.037(3) -0.010(3) 0.015(2) 0.001(3) N51 0.0282(17) 0.034(2) 0.036(2) -0.0022(16) 0.0073(16) 0.0029(15) B52 0.029(2) 0.034(2) 0.037(3) -0.0048(19) 0.0115(19) 0.0013(18) F62 0.0410(13) 0.0583(15) 0.0601(16) 0.0104(12) 0.0172(12) -0.0108(11) F63 0.085(2) 0.075(2) 0.0698(19) 0.0320(16) 0.0171(16) -0.0246(16) F64 0.0766(19) 0.0723(19) 0.0649(19) 0.0257(15) -0.0114(15) 0.0069(15) F65 0.0366(14) 0.090(2) 0.0627(18) 0.0002(15) -0.0003(12) 0.0159(13) F66 0.0305(12) 0.0665(16) 0.0454(14) -0.0007(11) 0.0145(10) 0.0018(11) F72 0.0407(12) 0.0402(13) 0.0388(14) -0.0054(10) 0.0099(10) -0.0048(10) F73 0.0575(15) 0.0425(14) 0.0712(17) -0.0094(12) 0.0319(13) -0.0140(12) F74 0.0828(19) 0.0468(16) 0.085(2) 0.0198(14) 0.0430(16) -0.0011(13) F75 0.0738(17) 0.0771(19) 0.0518(16) 0.0261(14) 0.0193(13) 0.0093(15) F76 0.0454(13) 0.0672(16) 0.0344(13) 0.0017(12) 0.0047(10) -0.0024(12) F82 0.0542(14) 0.0320(13) 0.0688(17) -0.0116(11) 0.0112(13) 0.0017(11) F83 0.0680(18) 0.0516(18) 0.095(2) -0.0372(15) -0.0131(16) 0.0150(14) F84 0.0721(19) 0.126(3) 0.113(3) -0.086(2) 0.0122(18) 0.0242(19) F85 0.0678(19) 0.160(3) 0.085(2) -0.063(2) 0.0402(18) -0.0020(19) F86 0.0491(15) 0.085(2) 0.0532(16) -0.0101(14) 0.0283(12) 0.0012(14) C61 0.0288(19) 0.0257(19) 0.040(2) -0.0062(16) 0.0096(17) 0.0002(15) C62 0.032(2) 0.030(2) 0.045(2) 0.0002(18) 0.0075(18) -0.0034(16) C63 0.052(3) 0.037(2) 0.048(3) 0.007(2) 0.008(2) -0.012(2) C64 0.059(3) 0.039(2) 0.043(3) 0.008(2) -0.006(2) 0.003(2) C65 0.034(2) 0.045(2) 0.049(3) -0.010(2) 0.001(2) 0.0033(19) C66 0.035(2) 0.033(2) 0.036(2) -0.0064(17) 0.0100(18) -0.0014(17) C71 0.0276(18) 0.037(2) 0.038(2) -0.0017(17) 0.0142(16) 0.0027(16) C72 0.030(2) 0.040(2) 0.037(2) -0.0027(18) 0.0147(18) 0.0032(17) C73 0.036(2) 0.038(2) 0.056(3) -0.007(2) 0.0249(19) -0.0045(19) C74 0.053(3) 0.040(3) 0.064(3) 0.010(2) 0.035(2) 0.002(2) C75 0.046(2) 0.055(3) 0.042(3) 0.017(2) 0.019(2) 0.009(2) C76 0.038(2) 0.050(3) 0.033(2) -0.0006(19) 0.0108(18) 0.0008(19) C81 0.029(2) 0.043(2) 0.039(2) -0.0098(19) 0.0024(18) 0.0065(17) C82 0.036(2) 0.050(3) 0.042(3) -0.014(2) -0.0008(19) 0.013(2) C83 0.043(3) 0.051(3) 0.063(3) -0.027(2) -0.012(2) 0.015(2) C84 0.047(3) 0.088(4) 0.067(4) -0.053(3) -0.001(3) 0.019(3) C85 0.037(3) 0.111(5) 0.050(3) -0.039(3) 0.012(2) 0.010(3) C86 0.036(2) 0.068(3) 0.045(3) -0.020(2) 0.007(2) 0.004(2) C93 0.116(8) 0.215(13) 0.36(2) -0.080(14) 0.065(11) -0.042(8) C95 0.39(3) 0.198(16) 0.229(16) -0.012(12) 0.007(15) -0.002(16) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N41 2.014(3) . ? Zr1 N31 2.041(3) . ? Zr1 N1 2.300(3) . ? Zr1 N51 2.347(3) . ? Zr1 N11 2.389(3) . ? Zr1 N21 2.409(3) . ? B1 N12 1.528(5) . ? B1 N22 1.539(6) . ? B1 N2 1.545(5) . ? B1 H1 1.12(3) . ? N1 C5 1.337(5) . ? N1 N2 1.361(4) . ? N2 C3 1.343(5) . ? C3 C4 1.358(6) . ? C3 H3 0.89(4) . ? C4 C5 1.373(6) . ? C4 H4 0.86(5) . ? C5 H5 0.95(4) . ? N11 C15 1.355(5) . ? N11 N12 1.367(4) . ? N12 C13 1.338(5) . ? C13 C14 1.365(6) . ? C13 H13 0.98(4) . ? C14 C15 1.369(6) . ? C14 H14 0.86(4) . ? C15 H15 0.88(3) . ? N21 C25 1.344(5) . ? N21 N22 1.369(4) . ? N22 C23 1.342(5) . ? C23 C24 1.356(6) . ? C23 H23 0.92(4) . ? C24 C25 1.380(5) . ? C24 H24 0.91(4) . ? C25 H25 0.96(3) . ? N31 C32 1.450(5) . ? N31 C33 1.469(5) . ? C32 H32A 0.94(4) . ? C32 H32B 1.01(4) . ? C32 H32C 0.99(5) . ? C33 H33A 0.99(5) . ? C33 H33B 0.97(4) . ? C33 H33C 1.00(5) . ? N41 C42 1.460(5) . ? N41 C43 1.460(5) . ? C42 H42A 1.03(4) . ? C42 H42B 0.96(5) . ? C42 H42C 0.94(5) . ? C43 H43A 0.97(4) . ? C43 H43B 1.00(5) . ? C43 H43C 0.99(5) . ? N51 B52 1.603(5) . ? N51 H51A 0.84(4) . ? N51 H51B 0.86(4) . ? B52 C71 1.647(5) . ? B52 C61 1.650(6) . ? B52 C81 1.664(5) . ? F62 C62 1.357(4) . ? F63 C63 1.350(5) . ? F64 C64 1.343(4) . ? F65 C65 1.348(4) . ? F66 C66 1.349(4) . ? F72 C72 1.354(4) . ? F73 C73 1.345(4) . ? F74 C74 1.344(4) . ? F75 C75 1.345(4) . ? F76 C76 1.355(4) . ? F82 C82 1.360(5) . ? F83 C83 1.356(5) . ? F84 C84 1.351(5) . ? F85 C85 1.344(6) . ? F86 C86 1.363(5) . ? C61 C62 1.378(5) . ? C61 C66 1.399(5) . ? C62 C63 1.372(5) . ? C63 C64 1.366(6) . ? C64 C65 1.370(6) . ? C65 C66 1.376(5) . ? C71 C72 1.382(5) . ? C71 C76 1.390(5) . ? C72 C73 1.390(5) . ? C73 C74 1.370(6) . ? C74 C75 1.373(6) . ? C75 C76 1.380(6) . ? C81 C86 1.377(6) . ? C81 C82 1.389(6) . ? C82 C83 1.376(6) . ? C83 C84 1.357(7) . ? C84 C85 1.370(7) . ? C85 C86 1.383(6) . ? C91A C93 1.389(16) . ? C91B C93 2.03(5) . ? C92A C93 1.52(3) . ? C92B C93 1.506(16) . ? C93 C94B 1.222(19) . ? C93 C96B 1.99(3) . ? C94A C95 1.16(3) . ? C94B C95 1.41(2) . ? C94B C96A 1.56(2) . ? 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 N41 Zr1 N31 102.19(12) . . ? N41 Zr1 N1 93.12(12) . . ? N31 Zr1 N1 86.76(11) . . ? N41 Zr1 N51 106.31(12) . . ? N31 Zr1 N51 101.99(12) . . ? N1 Zr1 N51 156.21(11) . . ? N41 Zr1 N11 84.36(11) . . ? N31 Zr1 N11 162.45(10) . . ? N1 Zr1 N11 76.56(10) . . ? N51 Zr1 N11 91.54(12) . . ? N41 Zr1 N21 159.55(11) . . ? N31 Zr1 N21 94.96(11) . . ? N1 Zr1 N21 76.66(11) . . ? N51 Zr1 N21 80.54(11) . . ? N11 Zr1 N21 76.11(10) . . ? N12 B1 N22 109.1(3) . . ? N12 B1 N2 107.9(3) . . ? N22 B1 N2 108.9(3) . . ? N12 B1 H1 109.6(17) . . ? N22 B1 H1 111.4(17) . . ? N2 B1 H1 110.0(17) . . ? C5 N1 N2 106.0(3) . . ? C5 N1 Zr1 128.0(3) . . ? N2 N1 Zr1 125.9(2) . . ? C3 N2 N1 109.3(3) . . ? C3 N2 B1 130.3(3) . . ? N1 N2 B1 120.4(3) . . ? N2 C3 C4 108.7(4) . . ? N2 C3 H3 121(2) . . ? C4 C3 H3 130(2) . . ? C3 C4 C5 105.4(4) . . ? C3 C4 H4 125(3) . . ? C5 C4 H4 129(3) . . ? N1 C5 C4 110.6(4) . . ? N1 C5 H5 120(2) . . ? C4 C5 H5 129(2) . . ? C15 N11 N12 104.9(3) . . ? C15 N11 Zr1 130.7(3) . . ? N12 N11 Zr1 123.6(2) . . ? C13 N12 N11 110.0(3) . . ? C13 N12 B1 129.0(3) . . ? N11 N12 B1 120.5(3) . . ? N12 C13 C14 108.7(4) . . ? N12 C13 H13 120(2) . . ? C14 C13 H13 131(2) . . ? C13 C14 C15 105.4(4) . . ? C13 C14 H14 127(3) . . ? C15 C14 H14 127(3) . . ? N11 C15 C14 111.0(4) . . ? N11 C15 H15 119(2) . . ? C14 C15 H15 130(2) . . ? C25 N21 N22 105.4(3) . . ? C25 N21 Zr1 132.5(2) . . ? N22 N21 Zr1 122.1(2) . . ? C23 N22 N21 109.4(3) . . ? C23 N22 B1 128.9(3) . . ? N21 N22 B1 121.6(3) . . ? N22 C23 C24 109.2(4) . . ? N22 C23 H23 120(2) . . ? C24 C23 H23 130(2) . . ? C23 C24 C25 105.0(4) . . ? C23 C24 H24 129(2) . . ? C25 C24 H24 125(2) . . ? N21 C25 C24 110.9(4) . . ? N21 C25 H25 120.5(18) . . ? C24 C25 H25 128.6(18) . . ? C32 N31 C33 107.5(3) . . ? C32 N31 Zr1 125.8(3) . . ? C33 N31 Zr1 125.2(3) . . ? N31 C32 H32A 111(2) . . ? N31 C32 H32B 111(2) . . ? H32A C32 H32B 107(3) . . ? N31 C32 H32C 114(3) . . ? H32A C32 H32C 106(3) . . ? H32B C32 H32C 107(3) . . ? N31 C33 H33A 107(3) . . ? N31 C33 H33B 111(2) . . ? H33A C33 H33B 108(4) . . ? N31 C33 H33C 109(3) . . ? H33A C33 H33C 112(4) . . ? H33B C33 H33C 109(4) . . ? C42 N41 C43 110.8(4) . . ? C42 N41 Zr1 117.3(3) . . ? C43 N41 Zr1 131.8(3) . . ? N41 C42 H42A 110(2) . . ? N41 C42 H42B 112(2) . . ? H42A C42 H42B 110(3) . . ? N41 C42 H42C 111(3) . . ? H42A C42 H42C 109(4) . . ? H42B C42 H42C 105(4) . . ? N41 C43 H43A 111(2) . . ? N41 C43 H43B 110(3) . . ? H43A C43 H43B 115(3) . . ? N41 C43 H43C 110(3) . . ? H43A C43 H43C 111(4) . . ? H43B C43 H43C 100(4) . . ? B52 N51 Zr1 135.5(2) . . ? B52 N51 H51A 111(3) . . ? Zr1 N51 H51A 105(3) . . ? B52 N51 H51B 104(3) . . ? Zr1 N51 H51B 97(3) . . ? H51A N51 H51B 97(4) . . ? N51 B52 C71 106.2(3) . . ? N51 B52 C61 112.5(3) . . ? C71 B52 C61 115.4(3) . . ? N51 B52 C81 109.2(3) . . ? C71 B52 C81 112.0(3) . . ? C61 B52 C81 101.5(3) . . ? C62 C61 C66 112.7(3) . . ? C62 C61 B52 127.1(3) . . ? C66 C61 B52 119.3(3) . . ? F62 C62 C63 115.0(3) . . ? F62 C62 C61 120.0(3) . . ? C63 C62 C61 125.0(4) . . ? F63 C63 C64 119.6(4) . . ? F63 C63 C62 120.7(4) . . ? C64 C63 C62 119.7(4) . . ? F64 C64 C63 120.5(4) . . ? F64 C64 C65 120.8(4) . . ? C63 C64 C65 118.7(4) . . ? F65 C65 C64 119.6(4) . . ? F65 C65 C66 120.6(4) . . ? C64 C65 C66 119.8(4) . . ? F66 C66 C65 116.5(3) . . ? F66 C66 C61 119.4(3) . . ? C65 C66 C61 124.1(4) . . ? C72 C71 C76 113.5(3) . . ? C72 C71 B52 127.5(3) . . ? C76 C71 B52 119.0(3) . . ? F72 C72 C71 121.4(3) . . ? F72 C72 C73 114.9(3) . . ? C71 C72 C73 123.8(4) . . ? F73 C73 C74 119.7(4) . . ? F73 C73 C72 120.4(4) . . ? C74 C73 C72 119.9(4) . . ? F74 C74 C73 120.7(4) . . ? F74 C74 C75 120.3(4) . . ? C73 C74 C75 118.9(4) . . ? F75 C75 C74 120.2(4) . . ? F75 C75 C76 120.5(4) . . ? C74 C75 C76 119.3(4) . . ? F76 C76 C75 116.3(4) . . ? F76 C76 C71 119.1(4) . . ? C75 C76 C71 124.6(4) . . ? C86 C81 C82 113.0(4) . . ? C86 C81 B52 127.3(4) . . ? C82 C81 B52 119.1(4) . . ? F82 C82 C83 115.1(4) . . ? F82 C82 C81 119.9(3) . . ? C83 C82 C81 125.0(5) . . ? F83 C83 C84 119.8(4) . . ? F83 C83 C82 121.0(5) . . ? C84 C83 C82 119.1(5) . . ? F84 C84 C83 120.1(5) . . ? F84 C84 C85 120.8(5) . . ? C83 C84 C85 119.1(4) . . ? F85 C85 C84 120.4(4) . . ? F85 C85 C86 119.7(5) . . ? C84 C85 C86 119.9(5) . . ? F86 C86 C81 121.1(4) . . ? F86 C86 C85 115.0(4) . . ? C81 C86 C85 123.8(5) . . ? C94B C93 C91A 124.7(16) . . ? C94B C93 C92B 112.3(19) . . ? C91A C93 C92B 120.6(13) . . ? C94B C93 C92A 154(2) . . ? C91A C93 C92A 74.0(14) . . ? C92B C93 C92A 46.6(11) . . ? C94B C93 C96B 85.9(17) . . ? C91A C93 C96B 129.6(12) . . ? C92A C93 C96B 68.0(14) . . ? C94B C93 C91B 159(2) . . ? C92B C93 C91B 87.9(16) . . ? C96B C93 C91B 109.6(17) . . ? C93 C94B C95 147(2) . . ? C93 C94B C96A 95.7(18) . . ? C95 C94B C96A 106.6(17) . . ? C94A C95 C94B 49.9(16) . . ? 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 N41 Zr1 N1 C5 53.8(4) . . . . ? N31 Zr1 N1 C5 -48.2(4) . . . . ? N51 Zr1 N1 C5 -161.0(4) . . . . ? N11 Zr1 N1 C5 137.2(4) . . . . ? N21 Zr1 N1 C5 -144.1(4) . . . . ? N41 Zr1 N1 N2 -121.2(3) . . . . ? N31 Zr1 N1 N2 136.8(3) . . . . ? N51 Zr1 N1 N2 24.0(5) . . . . ? N11 Zr1 N1 N2 -37.7(3) . . . . ? N21 Zr1 N1 N2 40.9(3) . . . . ? C5 N1 N2 C3 -0.8(4) . . . . ? Zr1 N1 N2 C3 175.1(3) . . . . ? C5 N1 N2 B1 -178.1(4) . . . . ? Zr1 N1 N2 B1 -2.2(5) . . . . ? N12 B1 N2 C3 -116.0(4) . . . . ? N22 B1 N2 C3 125.8(4) . . . . ? N12 B1 N2 N1 60.8(4) . . . . ? N22 B1 N2 N1 -57.4(4) . . . . ? N1 N2 C3 C4 0.5(5) . . . . ? B1 N2 C3 C4 177.5(4) . . . . ? N2 C3 C4 C5 0.0(6) . . . . ? N2 N1 C5 C4 0.7(5) . . . . ? Zr1 N1 C5 C4 -175.0(3) . . . . ? C3 C4 C5 N1 -0.5(6) . . . . ? N41 Zr1 N11 C15 -36.0(3) . . . . ? N31 Zr1 N11 C15 -149.0(4) . . . . ? N1 Zr1 N11 C15 -130.6(4) . . . . ? N51 Zr1 N11 C15 70.2(4) . . . . ? N21 Zr1 N11 C15 150.1(4) . . . . ? N41 Zr1 N11 N12 133.0(3) . . . . ? N31 Zr1 N11 N12 20.0(5) . . . . ? N1 Zr1 N11 N12 38.4(3) . . . . ? N51 Zr1 N11 N12 -120.8(3) . . . . ? N21 Zr1 N11 N12 -40.9(3) . . . . ? C15 N11 N12 C13 -0.6(4) . . . . ? Zr1 N11 N12 C13 -171.9(3) . . . . ? C15 N11 N12 B1 172.5(4) . . . . ? Zr1 N11 N12 B1 1.1(4) . . . . ? N22 B1 N12 C13 -129.2(4) . . . . ? N2 B1 N12 C13 112.7(4) . . . . ? N22 B1 N12 N11 59.3(4) . . . . ? N2 B1 N12 N11 -58.8(4) . . . . ? N11 N12 C13 C14 -0.1(5) . . . . ? B1 N12 C13 C14 -172.4(4) . . . . ? N12 C13 C14 C15 0.7(5) . . . . ? N12 N11 C15 C14 1.0(5) . . . . ? Zr1 N11 C15 C14 171.6(3) . . . . ? C13 C14 C15 N11 -1.1(6) . . . . ? N41 Zr1 N21 C25 -156.6(3) . . . . ? N31 Zr1 N21 C25 56.3(3) . . . . ? N1 Zr1 N21 C25 141.8(3) . . . . ? N51 Zr1 N21 C25 -45.1(3) . . . . ? N11 Zr1 N21 C25 -139.0(3) . . . . ? N41 Zr1 N21 N22 22.5(5) . . . . ? N31 Zr1 N21 N22 -124.6(3) . . . . ? N1 Zr1 N21 N22 -39.1(2) . . . . ? N51 Zr1 N21 N22 134.1(3) . . . . ? N11 Zr1 N21 N22 40.1(2) . . . . ? C25 N21 N22 C23 0.4(4) . . . . ? Zr1 N21 N22 C23 -179.0(2) . . . . ? C25 N21 N22 B1 178.9(3) . . . . ? Zr1 N21 N22 B1 -0.5(4) . . . . ? N12 B1 N22 C23 118.5(4) . . . . ? N2 B1 N22 C23 -124.1(4) . . . . ? N12 B1 N22 N21 -59.7(4) . . . . ? N2 B1 N22 N21 57.7(4) . . . . ? N21 N22 C23 C24 0.1(4) . . . . ? B1 N22 C23 C24 -178.3(4) . . . . ? N22 C23 C24 C25 -0.5(5) . . . . ? N22 N21 C25 C24 -0.7(4) . . . . ? Zr1 N21 C25 C24 178.5(3) . . . . ? C23 C24 C25 N21 0.8(5) . . . . ? N41 Zr1 N31 C32 6.3(3) . . . . ? N1 Zr1 N31 C32 98.7(3) . . . . ? N51 Zr1 N31 C32 -103.6(3) . . . . ? N11 Zr1 N31 C32 116.7(4) . . . . ? N21 Zr1 N31 C32 175.0(3) . . . . ? N41 Zr1 N31 C33 -157.8(4) . . . . ? N1 Zr1 N31 C33 -65.3(4) . . . . ? N51 Zr1 N31 C33 92.4(4) . . . . ? N11 Zr1 N31 C33 -47.3(6) . . . . ? N21 Zr1 N31 C33 11.0(4) . . . . ? N31 Zr1 N41 C42 -67.6(3) . . . . ? N1 Zr1 N41 C42 -155.0(3) . . . . ? N51 Zr1 N41 C42 38.9(3) . . . . ? N11 Zr1 N41 C42 128.9(3) . . . . ? N21 Zr1 N41 C42 146.0(3) . . . . ? N31 Zr1 N41 C43 115.6(4) . . . . ? N1 Zr1 N41 C43 28.2(4) . . . . ? N51 Zr1 N41 C43 -137.9(4) . . . . ? N11 Zr1 N41 C43 -47.9(4) . . . . ? N21 Zr1 N41 C43 -30.8(6) . . . . ? N41 Zr1 N51 B52 -55.1(4) . . . . ? N31 Zr1 N51 B52 51.6(4) . . . . ? N1 Zr1 N51 B52 161.4(3) . . . . ? N11 Zr1 N51 B52 -139.7(4) . . . . ? N21 Zr1 N51 B52 144.7(4) . . . . ? Zr1 N51 B52 C71 -41.2(5) . . . . ? Zr1 N51 B52 C61 85.9(4) . . . . ? Zr1 N51 B52 C81 -162.1(3) . . . . ? N51 B52 C61 C62 7.6(5) . . . . ? C71 B52 C61 C62 129.6(4) . . . . ? C81 B52 C61 C62 -109.1(4) . . . . ? N51 B52 C61 C66 175.9(3) . . . . ? C71 B52 C61 C66 -62.1(4) . . . . ? C81 B52 C61 C66 59.3(4) . . . . ? C66 C61 C62 F62 -178.8(3) . . . . ? B52 C61 C62 F62 -9.8(6) . . . . ? C66 C61 C62 C63 0.5(6) . . . . ? B52 C61 C62 C63 169.5(4) . . . . ? F62 C62 C63 F63 -1.6(6) . . . . ? C61 C62 C63 F63 179.0(4) . . . . ? F62 C62 C63 C64 178.3(4) . . . . ? C61 C62 C63 C64 -1.0(6) . . . . ? F63 C63 C64 F64 0.8(6) . . . . ? C62 C63 C64 F64 -179.1(4) . . . . ? F63 C63 C64 C65 -179.0(4) . . . . ? C62 C63 C64 C65 1.0(6) . . . . ? F64 C64 C65 F65 0.1(6) . . . . ? C63 C64 C65 F65 180.0(4) . . . . ? F64 C64 C65 C66 179.5(4) . . . . ? C63 C64 C65 C66 -0.6(6) . . . . ? F65 C65 C66 F66 1.1(5) . . . . ? C64 C65 C66 F66 -178.3(4) . . . . ? F65 C65 C66 C61 179.5(3) . . . . ? C64 C65 C66 C61 0.2(6) . . . . ? C62 C61 C66 F66 178.3(3) . . . . ? B52 C61 C66 F66 8.4(5) . . . . ? C62 C61 C66 C65 -0.1(5) . . . . ? B52 C61 C66 C65 -170.0(4) . . . . ? N51 B52 C71 C72 119.5(4) . . . . ? C61 B52 C71 C72 -5.9(5) . . . . ? C81 B52 C71 C72 -121.4(4) . . . . ? N51 B52 C71 C76 -62.2(4) . . . . ? C61 B52 C71 C76 172.4(3) . . . . ? C81 B52 C71 C76 56.9(4) . . . . ? C76 C71 C72 F72 178.1(3) . . . . ? B52 C71 C72 F72 -3.5(5) . . . . ? C76 C71 C72 C73 -1.8(5) . . . . ? B52 C71 C72 C73 176.6(3) . . . . ? F72 C72 C73 F73 0.7(5) . . . . ? C71 C72 C73 F73 -179.4(3) . . . . ? F72 C72 C73 C74 -179.3(3) . . . . ? C71 C72 C73 C74 0.6(6) . . . . ? F73 C73 C74 F74 -0.8(6) . . . . ? C72 C73 C74 F74 179.2(3) . . . . ? F73 C73 C74 C75 -178.9(3) . . . . ? C72 C73 C74 C75 1.1(6) . . . . ? F74 C74 C75 F75 1.5(6) . . . . ? C73 C74 C75 F75 179.7(3) . . . . ? F74 C74 C75 C76 -179.6(4) . . . . ? C73 C74 C75 C76 -1.5(6) . . . . ? F75 C75 C76 F76 0.2(5) . . . . ? C74 C75 C76 F76 -178.7(3) . . . . ? F75 C75 C76 C71 179.1(3) . . . . ? C74 C75 C76 C71 0.3(6) . . . . ? C72 C71 C76 F76 -179.8(3) . . . . ? B52 C71 C76 F76 1.7(5) . . . . ? C72 C71 C76 C75 1.3(5) . . . . ? B52 C71 C76 C75 -177.2(4) . . . . ? N51 B52 C81 C86 136.0(4) . . . . ? C71 B52 C81 C86 18.7(5) . . . . ? C61 B52 C81 C86 -104.9(4) . . . . ? N51 B52 C81 C82 -53.0(5) . . . . ? C71 B52 C81 C82 -170.3(3) . . . . ? C61 B52 C81 C82 66.0(4) . . . . ? C86 C81 C82 F82 175.7(3) . . . . ? B52 C81 C82 F82 3.4(5) . . . . ? C86 C81 C82 C83 -1.7(6) . . . . ? B52 C81 C82 C83 -173.9(4) . . . . ? F82 C82 C83 F83 2.3(5) . . . . ? C81 C82 C83 F83 179.8(4) . . . . ? F82 C82 C83 C84 -175.5(4) . . . . ? C81 C82 C83 C84 2.0(7) . . . . ? F83 C83 C84 F84 0.2(7) . . . . ? C82 C83 C84 F84 178.0(4) . . . . ? F83 C83 C84 C85 -178.6(4) . . . . ? C82 C83 C84 C85 -0.8(7) . . . . ? F84 C84 C85 F85 0.6(7) . . . . ? C83 C84 C85 F85 179.5(4) . . . . ? F84 C84 C85 C86 -179.3(4) . . . . ? C83 C84 C85 C86 -0.4(7) . . . . ? C82 C81 C86 F86 -178.8(3) . . . . ? B52 C81 C86 F86 -7.4(6) . . . . ? C82 C81 C86 C85 0.3(6) . . . . ? B52 C81 C86 C85 171.8(4) . . . . ? F85 C85 C86 F86 0.0(6) . . . . ? C84 C85 C86 F86 179.9(4) . . . . ? F85 C85 C86 C81 -179.2(4) . . . . ? C84 C85 C86 C81 0.7(7) . . . . ? C91A C93 C94B C95 30(5) . . . . ? C92B C93 C94B C95 -168(4) . . . . ? C92A C93 C94B C95 160(4) . . . . ? C96B C93 C94B C95 167(4) . . . . ? C91B C93 C94B C95 27(9) . . . . ? C91A C93 C94B C96A -102(2) . . . . ? C92B C93 C94B C96A 60.3(18) . . . . ? C92A C93 C94B C96A 28(5) . . . . ? C96B C93 C94B C96A 34.5(13) . . . . ? C91B C93 C94B C96A -105(6) . . . . ? C93 C94B C95 C94A 101(5) . . . . ? C96A C94B C95 C94A -130(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N51 H51A F62 0.84(4) 2.37(4) 2.722(5) 106(3) . N51 H51B F76 0.86(4) 2.38(4) 2.947(5) 124(3) . N51 H51A F82 0.84(4) 2.26(4) 2.855(4) 128(4) . _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.569 _refine_diff_density_min -0.416 _refine_diff_density_rms 0.063 #===END data_4.CH2Cl2 _database_code_depnum_ccdc_archive 'CCDC 823225' #TrackingRef '- fuller et al cif.cif' _chemical_formula_structural 'HB(C3H3N2)3Zr(N(CH3)2)2NH2B(C6F5)3 CH2Cl2' _chemical_name_common 'HB(C3H3N2)3Zr(N(CH3)2)2NH2B(C6F5)3 CH2Cl2' _chemical_melting_point ? _chemical_formula_moiety 'C31 H24 B2 F15 N9 Zr, C H2 Cl2' _chemical_formula_sum 'C32 H26 B2 Cl2 F15 N9 Zr' _chemical_formula_weight 1005.36 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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.9240(2) _cell_length_b 23.2383(3) _cell_length_c 13.4537(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.201(2) _cell_angle_gamma 90.00 _cell_volume 3933.80(12) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 74665 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 33.98 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2000 _exptl_absorpt_coefficient_mu 0.526 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8215 _exptl_absorpt_correction_T_max 1.1167 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 53224 _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9024 _reflns_number_gt 6101 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0409P)^2^+0.0000P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9024 _refine_ls_number_parameters 654 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0590 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0698 _refine_ls_goodness_of_fit_ref 0.956 _refine_ls_restrained_S_all 0.956 _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 0.017971(16) 0.700393(8) 0.365099(16) 0.01880(6) Uani 1 1 d . . . B1 B -0.2441(2) 0.64560(12) 0.2993(2) 0.0266(6) Uani 1 1 d . . . N1 N -0.14756(15) 0.73754(8) 0.36224(14) 0.0262(4) Uani 1 1 d . . . N2 N -0.24119(14) 0.70812(8) 0.33622(14) 0.0256(4) Uani 1 1 d . . . C3 C -0.3204(2) 0.74218(11) 0.35038(19) 0.0321(6) Uani 1 1 d . . . C4 C -0.2794(2) 0.79444(12) 0.3857(2) 0.0374(6) Uani 1 1 d . . . C5 C -0.1718(2) 0.79010(10) 0.39169(19) 0.0314(6) Uani 1 1 d . . . N11 N -0.07190(14) 0.62177(7) 0.42426(14) 0.0231(4) Uani 1 1 d . . . N12 N -0.17602(14) 0.60911(8) 0.38558(14) 0.0246(4) Uani 1 1 d . . . C13 C -0.2057(2) 0.56536(10) 0.43722(19) 0.0300(5) Uani 1 1 d . . . C14 C -0.1209(2) 0.54843(11) 0.5113(2) 0.0329(6) Uani 1 1 d . . . C15 C -0.0394(2) 0.58440(10) 0.50158(19) 0.0296(5) Uani 1 1 d . . . N21 N -0.09250(14) 0.66038(7) 0.21072(13) 0.0226(4) Uani 1 1 d . . . N22 N -0.19357(14) 0.64176(8) 0.20634(14) 0.0240(4) Uani 1 1 d . . . C23 C -0.2339(2) 0.61829(10) 0.11480(18) 0.0287(5) Uani 1 1 d . . . C24 C -0.1599(2) 0.62187(10) 0.05675(19) 0.0308(6) Uani 1 1 d . . . C25 C -0.0734(2) 0.64860(10) 0.11884(17) 0.0269(5) Uani 1 1 d . . . N31 N 0.04691(15) 0.77630(8) 0.30068(14) 0.0251(4) Uani 1 1 d . . . C32 C -0.0105(2) 0.79542(12) 0.2002(2) 0.0401(6) Uani 1 1 d . . . C33 C 0.1046(2) 0.82548(12) 0.3542(2) 0.0371(6) Uani 1 1 d . . . N41 N 0.07798(15) 0.71657(8) 0.51447(14) 0.0249(4) Uani 1 1 d . . . C42 C 0.1915(2) 0.72592(13) 0.5517(2) 0.0348(6) Uani 1 1 d . . . C43 C 0.0237(2) 0.71850(14) 0.5975(2) 0.0382(6) Uani 1 1 d . . . N51 N 0.14201(15) 0.64015(9) 0.31395(16) 0.0216(4) Uani 1 1 d . . . B52 B 0.2673(2) 0.64188(11) 0.3228(2) 0.0228(5) Uani 1 1 d . . . F62 F 0.18874(10) 0.59804(6) 0.50593(10) 0.0328(3) Uani 1 1 d . . . F63 F 0.30537(12) 0.55091(6) 0.67248(11) 0.0444(4) Uani 1 1 d . . . F64 F 0.51722(13) 0.53453(7) 0.69182(12) 0.0571(5) Uani 1 1 d . . . F65 F 0.61065(11) 0.57196(7) 0.54264(13) 0.0563(4) Uani 1 1 d . . . F66 F 0.49649(10) 0.62475(6) 0.37743(11) 0.0403(4) Uani 1 1 d . . . F72 F 0.42362(10) 0.72744(5) 0.45464(10) 0.0327(3) Uani 1 1 d . . . F73 F 0.46950(11) 0.83094(6) 0.39439(11) 0.0401(4) Uani 1 1 d . . . F74 F 0.36874(13) 0.87291(6) 0.20974(12) 0.0459(4) Uani 1 1 d . . . F75 F 0.22024(13) 0.80759(6) 0.08276(11) 0.0452(4) Uani 1 1 d . . . F76 F 0.17524(11) 0.70197(5) 0.13861(10) 0.0325(3) Uani 1 1 d . . . F82 F 0.20010(10) 0.52263(5) 0.29525(10) 0.0282(3) Uani 1 1 d . . . F83 F 0.24795(11) 0.44508(5) 0.16896(11) 0.0366(3) Uani 1 1 d . . . F84 F 0.37568(12) 0.47281(6) 0.04044(11) 0.0452(4) Uani 1 1 d . . . F85 F 0.45240(13) 0.58206(6) 0.04147(12) 0.0510(4) Uani 1 1 d . . . F86 F 0.40654(12) 0.66031(6) 0.16548(12) 0.0431(4) Uani 1 1 d . . . C61 C 0.33551(17) 0.61477(9) 0.43146(17) 0.0226(5) Uani 1 1 d . . . C62 C 0.29429(17) 0.59386(9) 0.51078(17) 0.0245(5) Uani 1 1 d . . . C63 C 0.35226(19) 0.56781(9) 0.59764(18) 0.0293(5) Uani 1 1 d . . . C64 C 0.4584(2) 0.55980(10) 0.60818(19) 0.0346(6) Uani 1 1 d . . . C65 C 0.50552(19) 0.57927(11) 0.5323(2) 0.0354(6) Uani 1 1 d . . . C66 C 0.44471(18) 0.60587(10) 0.44825(19) 0.0288(5) Uani 1 1 d . . . C71 C 0.29681(17) 0.70856(9) 0.29928(17) 0.0234(5) Uani 1 1 d . . . C72 C 0.37054(18) 0.74447(10) 0.36050(17) 0.0256(5) Uani 1 1 d . . . C73 C 0.39535(18) 0.79859(10) 0.33177(18) 0.0283(5) Uani 1 1 d . . . C74 C 0.3453(2) 0.82040(10) 0.2384(2) 0.0322(6) Uani 1 1 d . . . C75 C 0.2696(2) 0.78707(10) 0.17460(18) 0.0319(6) Uani 1 1 d . . . C76 C 0.24852(19) 0.73333(10) 0.20673(17) 0.0283(5) Uani 1 1 d . . . C81 C 0.29593(17) 0.59697(9) 0.23558(17) 0.0232(5) Uani 1 1 d . . . C82 C 0.26121(17) 0.54029(9) 0.23103(17) 0.0231(5) Uani 1 1 d . . . C83 C 0.28557(18) 0.49893(9) 0.16733(17) 0.0254(5) Uani 1 1 d . . . C84 C 0.35021(19) 0.51266(10) 0.10291(17) 0.0301(6) Uani 1 1 d . . . C85 C 0.38856(19) 0.56781(10) 0.10384(18) 0.0313(6) Uani 1 1 d . . . C86 C 0.36185(18) 0.60788(10) 0.16870(18) 0.0297(5) Uani 1 1 d . . . C91 C 0.5209(3) 0.98043(16) 0.3470(2) 0.0521(8) Uani 1 1 d . . . Cl92 Cl 0.60931(7) 0.95172(3) 0.45415(6) 0.0615(2) Uani 1 1 d . . . Cl93 Cl 0.57961(8) 0.99793(4) 0.24670(7) 0.0779(3) Uani 1 1 d . . . H1 H -0.3224(17) 0.6287(8) 0.2799(16) 0.021(6) Uiso 1 1 d . . . H3 H -0.3881(19) 0.7282(9) 0.3348(17) 0.023(6) Uiso 1 1 d . . . H4 H -0.317(2) 0.8238(11) 0.402(2) 0.044(8) Uiso 1 1 d . . . H5 H -0.121(2) 0.8162(10) 0.4111(19) 0.033(7) Uiso 1 1 d . . . H13 H -0.2762(18) 0.5529(9) 0.4185(17) 0.025(6) Uiso 1 1 d . . . H14 H -0.1169(18) 0.5210(10) 0.5598(18) 0.032(7) Uiso 1 1 d . . . H15 H 0.0280(18) 0.5860(9) 0.5356(17) 0.022(6) Uiso 1 1 d . . . H23 H -0.3016(18) 0.6015(9) 0.1024(16) 0.021(6) Uiso 1 1 d . . . H24 H -0.1652(19) 0.6111(10) -0.0064(19) 0.031(7) Uiso 1 1 d . . . H25 H -0.0095(19) 0.6607(9) 0.1032(17) 0.025(6) Uiso 1 1 d . . . H32A H 0.035(2) 0.8115(11) 0.158(2) 0.049(8) Uiso 1 1 d . . . H32B H -0.059(2) 0.8269(11) 0.2096(19) 0.038(7) Uiso 1 1 d . . . H32C H -0.048(2) 0.7608(12) 0.160(2) 0.053(8) Uiso 1 1 d . . . H33A H 0.138(2) 0.8161(12) 0.418(3) 0.061(10) Uiso 1 1 d . . . H33B H 0.156(2) 0.8424(12) 0.315(2) 0.059(9) Uiso 1 1 d . . . H33C H 0.054(2) 0.8579(12) 0.357(2) 0.049(8) Uiso 1 1 d . . . H42A H 0.2037(18) 0.7659(11) 0.5809(18) 0.030(6) Uiso 1 1 d . . . H42B H 0.221(2) 0.6996(10) 0.600(2) 0.034(7) Uiso 1 1 d . . . H42C H 0.227(2) 0.7238(10) 0.498(2) 0.036(7) Uiso 1 1 d . . . H43A H 0.051(2) 0.6897(11) 0.648(2) 0.042(8) Uiso 1 1 d . . . H43B H 0.036(2) 0.7555(11) 0.633(2) 0.041(7) Uiso 1 1 d . . . H43C H -0.050(2) 0.7104(9) 0.5728(18) 0.030(7) Uiso 1 1 d . . . H51A H 0.1206(17) 0.6104(10) 0.3283(17) 0.017(7) Uiso 1 1 d . . . H51B H 0.118(2) 0.6380(11) 0.248(2) 0.045(8) Uiso 1 1 d . . . H91A H 0.494(4) 1.018(2) 0.374(4) 0.16(2) Uiso 1 1 d . . . H91B H 0.460(3) 0.9520(14) 0.320(3) 0.081(11) 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 Zr1 0.01865(11) 0.01815(11) 0.01991(10) -0.00060(9) 0.00505(8) 0.00000(9) B1 0.0194(14) 0.0316(15) 0.0292(14) -0.0037(12) 0.0062(11) -0.0039(11) N1 0.0235(10) 0.0243(10) 0.0309(11) -0.0012(8) 0.0069(9) 0.0016(8) N2 0.0189(9) 0.0313(11) 0.0267(10) 0.0003(8) 0.0057(8) 0.0005(8) C3 0.0226(14) 0.0419(16) 0.0328(14) 0.0029(11) 0.0082(11) 0.0083(12) C4 0.0364(15) 0.0360(15) 0.0418(15) -0.0024(12) 0.0130(12) 0.0138(13) C5 0.0325(14) 0.0252(14) 0.0376(14) -0.0037(11) 0.0102(12) 0.0043(11) N11 0.0217(10) 0.0244(10) 0.0243(10) 0.0036(8) 0.0077(8) -0.0021(8) N12 0.0226(10) 0.0246(10) 0.0279(10) -0.0015(8) 0.0087(8) -0.0031(8) C13 0.0311(14) 0.0277(13) 0.0344(14) -0.0013(11) 0.0142(12) -0.0079(11) C14 0.0399(16) 0.0283(13) 0.0354(14) 0.0077(11) 0.0186(12) -0.0028(11) C15 0.0302(14) 0.0314(14) 0.0297(13) 0.0037(10) 0.0118(12) 0.0021(11) N21 0.0206(10) 0.0238(10) 0.0234(10) -0.0013(8) 0.0049(8) -0.0020(8) N22 0.0202(10) 0.0251(10) 0.0254(10) -0.0014(8) 0.0022(8) -0.0035(8) C23 0.0269(13) 0.0287(13) 0.0273(13) -0.0051(10) -0.0009(11) -0.0036(11) C24 0.0370(15) 0.0319(14) 0.0209(12) -0.0057(11) 0.0011(11) 0.0013(11) C25 0.0282(14) 0.0301(13) 0.0230(12) 0.0024(10) 0.0067(10) 0.0011(11) N31 0.0255(10) 0.0208(9) 0.0287(10) -0.0008(8) 0.0055(8) -0.0003(8) C32 0.0510(17) 0.0282(15) 0.0376(15) 0.0088(13) 0.0025(13) -0.0029(14) C33 0.0443(17) 0.0264(14) 0.0411(17) 0.0002(12) 0.0109(14) -0.0079(13) N41 0.0269(10) 0.0266(10) 0.0223(10) -0.0028(8) 0.0078(8) -0.0006(8) C42 0.0342(15) 0.0350(16) 0.0361(15) -0.0078(13) 0.0096(13) -0.0050(12) C43 0.0364(16) 0.0550(19) 0.0245(13) -0.0051(13) 0.0094(12) 0.0056(14) N51 0.0223(10) 0.0198(11) 0.0235(11) 0.0003(8) 0.0066(9) -0.0020(8) B52 0.0215(13) 0.0211(13) 0.0273(13) -0.0011(11) 0.0089(11) -0.0038(10) F62 0.0238(7) 0.0423(8) 0.0340(8) 0.0087(6) 0.0102(6) -0.0006(6) F63 0.0511(10) 0.0490(9) 0.0323(8) 0.0122(7) 0.0081(7) -0.0059(7) F64 0.0507(10) 0.0614(11) 0.0479(10) 0.0128(8) -0.0120(8) 0.0143(8) F65 0.0235(8) 0.0800(12) 0.0612(11) -0.0055(9) 0.0009(8) 0.0139(8) F66 0.0254(8) 0.0548(9) 0.0441(9) -0.0053(7) 0.0152(7) -0.0025(7) F72 0.0329(8) 0.0318(7) 0.0318(7) -0.0037(6) 0.0043(6) -0.0075(6) F73 0.0408(9) 0.0346(8) 0.0498(9) -0.0146(7) 0.0202(8) -0.0168(7) F74 0.0693(11) 0.0246(8) 0.0533(10) 0.0005(7) 0.0337(9) -0.0111(7) F75 0.0681(11) 0.0353(8) 0.0334(8) 0.0102(6) 0.0143(8) 0.0006(7) F76 0.0401(8) 0.0293(7) 0.0260(7) 0.0007(6) 0.0032(6) -0.0041(6) F82 0.0314(7) 0.0233(7) 0.0330(7) 0.0002(6) 0.0140(6) -0.0034(6) F83 0.0427(9) 0.0233(7) 0.0440(9) -0.0087(6) 0.0103(7) -0.0016(6) F84 0.0532(10) 0.0420(9) 0.0449(9) -0.0192(7) 0.0204(8) 0.0067(7) F85 0.0620(11) 0.0501(10) 0.0559(10) -0.0034(8) 0.0450(9) 0.0018(8) F86 0.0520(10) 0.0301(8) 0.0605(10) -0.0035(7) 0.0407(8) -0.0074(7) C61 0.0214(11) 0.0190(11) 0.0273(12) -0.0063(9) 0.0053(10) -0.0008(9) C62 0.0207(12) 0.0222(12) 0.0311(13) -0.0033(10) 0.0070(10) -0.0006(9) C63 0.0337(14) 0.0233(12) 0.0309(13) -0.0001(10) 0.0074(11) -0.0030(10) C64 0.0348(15) 0.0292(13) 0.0332(14) 0.0000(11) -0.0058(11) 0.0067(11) C65 0.0187(12) 0.0385(15) 0.0465(16) -0.0087(12) 0.0021(12) 0.0066(11) C66 0.0225(12) 0.0296(13) 0.0361(14) -0.0066(11) 0.0102(11) -0.0018(10) C71 0.0252(12) 0.0220(12) 0.0264(12) -0.0027(9) 0.0128(10) 0.0004(10) C72 0.0239(12) 0.0268(12) 0.0296(13) -0.0024(10) 0.0135(10) -0.0010(10) C73 0.0284(12) 0.0264(12) 0.0351(13) -0.0102(11) 0.0178(11) -0.0089(11) C74 0.0434(16) 0.0201(12) 0.0426(15) -0.0020(11) 0.0293(13) -0.0044(11) C75 0.0424(15) 0.0292(13) 0.0291(13) 0.0036(10) 0.0188(12) 0.0027(11) C76 0.0331(14) 0.0255(13) 0.0285(13) -0.0055(10) 0.0119(11) -0.0033(10) C81 0.0210(12) 0.0248(12) 0.0247(12) 0.0006(9) 0.0072(10) 0.0006(9) C82 0.0186(11) 0.0269(12) 0.0241(12) 0.0013(9) 0.0052(9) 0.0018(9) C83 0.0240(12) 0.0211(12) 0.0284(12) -0.0034(9) 0.0002(10) 0.0018(9) C84 0.0317(13) 0.0335(14) 0.0245(12) -0.0101(10) 0.0051(11) 0.0102(11) C85 0.0322(14) 0.0355(14) 0.0316(13) -0.0011(11) 0.0186(11) 0.0047(11) C86 0.0300(13) 0.0249(13) 0.0370(14) -0.0020(10) 0.0133(11) -0.0010(10) C91 0.0465(18) 0.062(2) 0.0418(18) 0.0046(15) -0.0021(15) -0.0074(17) Cl92 0.0600(5) 0.0582(5) 0.0543(5) -0.0032(4) -0.0118(4) 0.0015(4) Cl93 0.0816(7) 0.1047(7) 0.0513(5) -0.0115(5) 0.0232(5) -0.0407(5) _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 N41 2.0173(18) . ? Zr1 N31 2.0372(18) . ? Zr1 N1 2.2991(18) . ? Zr1 N51 2.3467(19) . ? Zr1 N11 2.3964(17) . ? Zr1 N21 2.4213(18) . ? B1 N2 1.533(3) . ? B1 N22 1.540(3) . ? B1 N12 1.541(3) . ? B1 H1 1.06(2) . ? N1 C5 1.343(3) . ? N1 N2 1.364(3) . ? N2 C3 1.342(3) . ? C3 C4 1.366(4) . ? C3 H3 0.91(2) . ? C4 C5 1.378(4) . ? C4 H4 0.89(3) . ? C5 H5 0.89(2) . ? N11 C15 1.347(3) . ? N11 N12 1.360(2) . ? N12 C13 1.336(3) . ? C13 C14 1.361(4) . ? C13 H13 0.93(2) . ? C14 C15 1.375(3) . ? C14 H14 0.90(2) . ? C15 H15 0.89(2) . ? N21 C25 1.343(3) . ? N21 N22 1.365(2) . ? N22 C23 1.339(3) . ? C23 C24 1.369(3) . ? C23 H23 0.94(2) . ? C24 C25 1.381(3) . ? C24 H24 0.87(2) . ? C25 H25 0.94(2) . ? N31 C32 1.456(3) . ? N31 C33 1.461(3) . ? C32 H32A 0.98(3) . ? C32 H32B 0.99(3) . ? C32 H32C 1.03(3) . ? C33 H33A 0.90(3) . ? C33 H33B 1.02(3) . ? C33 H33C 1.01(3) . ? N41 C43 1.450(3) . ? N41 C42 1.454(3) . ? C42 H42A 1.01(2) . ? C42 H42B 0.91(3) . ? C42 H42C 0.94(3) . ? C43 H43A 0.96(3) . ? C43 H43B 0.98(3) . ? C43 H43C 0.95(3) . ? N51 B52 1.596(3) . ? N51 H51A 0.79(2) . ? N51 H51B 0.87(3) . ? B52 C71 1.644(3) . ? B52 C61 1.650(3) . ? B52 C81 1.674(3) . ? F62 C62 1.354(2) . ? F63 C63 1.347(3) . ? F64 C64 1.341(3) . ? F65 C65 1.345(3) . ? F66 C66 1.356(3) . ? F72 C72 1.354(3) . ? F73 C73 1.351(3) . ? F74 C74 1.335(3) . ? F75 C75 1.342(3) . ? F76 C76 1.368(3) . ? F82 C82 1.360(2) . ? F83 C83 1.344(2) . ? F84 C84 1.341(2) . ? F85 C85 1.346(3) . ? F86 C86 1.353(3) . ? C61 C62 1.385(3) . ? C61 C66 1.393(3) . ? C62 C63 1.376(3) . ? C63 C64 1.360(3) . ? C64 C65 1.378(4) . ? C65 C66 1.369(3) . ? C71 C76 1.384(3) . ? C71 C72 1.387(3) . ? C72 C73 1.375(3) . ? C73 C74 1.372(3) . ? C74 C75 1.382(4) . ? C75 C76 1.369(3) . ? C81 C82 1.388(3) . ? C81 C86 1.396(3) . ? C82 C83 1.371(3) . ? C83 C84 1.372(3) . ? C84 C85 1.373(3) . ? C85 C86 1.373(3) . ? C91 Cl93 1.741(3) . ? C91 Cl92 1.754(3) . ? C91 H91A 1.04(5) . ? C91 H91B 1.03(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 N41 Zr1 N31 101.32(7) . . ? N41 Zr1 N1 95.24(7) . . ? N31 Zr1 N1 85.89(7) . . ? N41 Zr1 N51 105.68(7) . . ? N31 Zr1 N51 100.82(7) . . ? N1 Zr1 N51 156.12(7) . . ? N41 Zr1 N11 85.21(7) . . ? N31 Zr1 N11 162.06(7) . . ? N1 Zr1 N11 76.82(6) . . ? N51 Zr1 N11 93.32(7) . . ? N41 Zr1 N21 160.62(7) . . ? N31 Zr1 N21 95.58(7) . . ? N1 Zr1 N21 76.45(6) . . ? N51 Zr1 N21 80.09(6) . . ? N11 Zr1 N21 75.91(6) . . ? N2 B1 N22 109.54(19) . . ? N2 B1 N12 108.06(19) . . ? N22 B1 N12 107.73(19) . . ? N2 B1 H1 112.5(11) . . ? N22 B1 H1 109.6(11) . . ? N12 B1 H1 109.3(11) . . ? C5 N1 N2 106.17(18) . . ? C5 N1 Zr1 127.97(16) . . ? N2 N1 Zr1 125.71(13) . . ? C3 N2 N1 109.21(19) . . ? C3 N2 B1 129.9(2) . . ? N1 N2 B1 120.85(18) . . ? N2 C3 C4 109.0(2) . . ? N2 C3 H3 118.7(14) . . ? C4 C3 H3 132.3(14) . . ? C3 C4 C5 105.2(2) . . ? C3 C4 H4 124.9(17) . . ? C5 C4 H4 129.9(18) . . ? N1 C5 C4 110.5(2) . . ? N1 C5 H5 120.0(16) . . ? C4 C5 H5 129.5(16) . . ? C15 N11 N12 105.27(18) . . ? C15 N11 Zr1 131.20(16) . . ? N12 N11 Zr1 123.39(13) . . ? C13 N12 N11 110.02(19) . . ? C13 N12 B1 128.9(2) . . ? N11 N12 B1 120.95(17) . . ? N12 C13 C14 108.8(2) . . ? N12 C13 H13 118.2(14) . . ? C14 C13 H13 133.0(14) . . ? C13 C14 C15 105.1(2) . . ? C13 C14 H14 129.5(16) . . ? C15 C14 H14 125.3(16) . . ? N11 C15 C14 110.8(2) . . ? N11 C15 H15 117.9(14) . . ? C14 C15 H15 131.3(14) . . ? C25 N21 N22 105.71(18) . . ? C25 N21 Zr1 132.20(15) . . ? N22 N21 Zr1 122.00(13) . . ? C23 N22 N21 109.69(18) . . ? C23 N22 B1 128.5(2) . . ? N21 N22 B1 121.73(17) . . ? N22 C23 C24 108.9(2) . . ? N22 C23 H23 119.0(13) . . ? C24 C23 H23 132.0(13) . . ? C23 C24 C25 104.9(2) . . ? C23 C24 H24 128.9(16) . . ? C25 C24 H24 126.2(16) . . ? N21 C25 C24 110.8(2) . . ? N21 C25 H25 120.0(14) . . ? C24 C25 H25 129.0(14) . . ? C32 N31 C33 108.3(2) . . ? C32 N31 Zr1 123.74(16) . . ? C33 N31 Zr1 126.16(17) . . ? N31 C32 H32A 114.0(17) . . ? N31 C32 H32B 108.0(15) . . ? H32A C32 H32B 106(2) . . ? N31 C32 H32C 109.4(15) . . ? H32A C32 H32C 105(2) . . ? H32B C32 H32C 114(2) . . ? N31 C33 H33A 111.2(19) . . ? N31 C33 H33B 111.4(16) . . ? H33A C33 H33B 111(3) . . ? N31 C33 H33C 109.8(16) . . ? H33A C33 H33C 109(2) . . ? H33B C33 H33C 104(2) . . ? C43 N41 C42 110.9(2) . . ? C43 N41 Zr1 129.06(17) . . ? C42 N41 Zr1 119.96(16) . . ? N41 C42 H42A 109.2(13) . . ? N41 C42 H42B 111.5(16) . . ? H42A C42 H42B 110(2) . . ? N41 C42 H42C 111.3(15) . . ? H42A C42 H42C 106(2) . . ? H42B C42 H42C 109(2) . . ? N41 C43 H43A 110.8(16) . . ? N41 C43 H43B 110.4(15) . . ? H43A C43 H43B 106(2) . . ? N41 C43 H43C 110.2(14) . . ? H43A C43 H43C 107(2) . . ? H43B C43 H43C 113(2) . . ? B52 N51 Zr1 135.41(14) . . ? B52 N51 H51A 114.4(16) . . ? Zr1 N51 H51A 98.6(16) . . ? B52 N51 H51B 101.7(18) . . ? Zr1 N51 H51B 102.6(18) . . ? H51A N51 H51B 98(2) . . ? N51 B52 C71 106.60(18) . . ? N51 B52 C61 112.59(18) . . ? C71 B52 C61 115.45(18) . . ? N51 B52 C81 108.37(18) . . ? C71 B52 C81 110.76(18) . . ? C61 B52 C81 102.93(17) . . ? C62 C61 C66 112.1(2) . . ? C62 C61 B52 126.49(19) . . ? C66 C61 B52 121.1(2) . . ? F62 C62 C63 114.8(2) . . ? F62 C62 C61 119.89(19) . . ? C63 C62 C61 125.3(2) . . ? F63 C63 C64 119.9(2) . . ? F63 C63 C62 120.8(2) . . ? C64 C63 C62 119.3(2) . . ? F64 C64 C63 120.8(2) . . ? F64 C64 C65 120.2(2) . . ? C63 C64 C65 118.9(2) . . ? F65 C65 C66 121.2(2) . . ? F65 C65 C64 119.3(2) . . ? C66 C65 C64 119.5(2) . . ? F66 C66 C65 116.4(2) . . ? F66 C66 C61 118.8(2) . . ? C65 C66 C61 124.8(2) . . ? C76 C71 C72 113.0(2) . . ? C76 C71 B52 119.2(2) . . ? C72 C71 B52 127.7(2) . . ? F72 C72 C73 115.4(2) . . ? F72 C72 C71 120.80(19) . . ? C73 C72 C71 123.8(2) . . ? F73 C73 C74 119.0(2) . . ? F73 C73 C72 120.8(2) . . ? C74 C73 C72 120.2(2) . . ? F74 C74 C73 120.8(2) . . ? F74 C74 C75 120.5(2) . . ? C73 C74 C75 118.7(2) . . ? F75 C75 C76 121.9(2) . . ? F75 C75 C74 119.5(2) . . ? C76 C75 C74 118.6(2) . . ? F76 C76 C75 115.6(2) . . ? F76 C76 C71 118.81(19) . . ? C75 C76 C71 125.6(2) . . ? C82 C81 C86 112.5(2) . . ? C82 C81 B52 120.09(18) . . ? C86 C81 B52 127.15(19) . . ? F82 C82 C83 115.77(19) . . ? F82 C82 C81 119.14(19) . . ? C83 C82 C81 125.1(2) . . ? F83 C83 C82 120.4(2) . . ? F83 C83 C84 120.1(2) . . ? C82 C83 C84 119.4(2) . . ? F84 C84 C83 120.5(2) . . ? F84 C84 C85 120.7(2) . . ? C83 C84 C85 118.8(2) . . ? F85 C85 C84 119.7(2) . . ? F85 C85 C86 120.5(2) . . ? C84 C85 C86 119.7(2) . . ? F86 C86 C85 114.8(2) . . ? F86 C86 C81 120.8(2) . . ? C85 C86 C81 124.4(2) . . ? Cl93 C91 Cl92 114.10(19) . . ? Cl93 C91 H91A 108(3) . . ? Cl92 C91 H91A 104(3) . . ? Cl93 C91 H91B 108.0(19) . . ? Cl92 C91 H91B 110.5(19) . . ? H91A C91 H91B 112(3) . . ? 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 N41 Zr1 N1 C5 54.4(2) . . . . ? N31 Zr1 N1 C5 -46.6(2) . . . . ? N51 Zr1 N1 C5 -154.2(2) . . . . ? N11 Zr1 N1 C5 138.2(2) . . . . ? N21 Zr1 N1 C5 -143.4(2) . . . . ? N41 Zr1 N1 N2 -120.68(17) . . . . ? N31 Zr1 N1 N2 138.31(17) . . . . ? N51 Zr1 N1 N2 30.7(3) . . . . ? N11 Zr1 N1 N2 -36.85(16) . . . . ? N21 Zr1 N1 N2 41.56(16) . . . . ? C5 N1 N2 C3 -0.4(2) . . . . ? Zr1 N1 N2 C3 175.53(15) . . . . ? C5 N1 N2 B1 -179.5(2) . . . . ? Zr1 N1 N2 B1 -3.5(3) . . . . ? N22 B1 N2 C3 124.9(2) . . . . ? N12 B1 N2 C3 -118.0(2) . . . . ? N22 B1 N2 N1 -56.2(3) . . . . ? N12 B1 N2 N1 60.9(3) . . . . ? N1 N2 C3 C4 0.1(3) . . . . ? B1 N2 C3 C4 179.1(2) . . . . ? N2 C3 C4 C5 0.2(3) . . . . ? N2 N1 C5 C4 0.6(3) . . . . ? Zr1 N1 C5 C4 -175.27(16) . . . . ? C3 C4 C5 N1 -0.5(3) . . . . ? N41 Zr1 N11 C15 -39.9(2) . . . . ? N31 Zr1 N11 C15 -152.2(2) . . . . ? N1 Zr1 N11 C15 -136.4(2) . . . . ? N51 Zr1 N11 C15 65.6(2) . . . . ? N21 Zr1 N11 C15 144.5(2) . . . . ? N41 Zr1 N11 N12 135.10(16) . . . . ? N31 Zr1 N11 N12 22.7(3) . . . . ? N1 Zr1 N11 N12 38.57(15) . . . . ? N51 Zr1 N11 N12 -119.42(16) . . . . ? N21 Zr1 N11 N12 -40.52(15) . . . . ? C15 N11 N12 C13 -0.3(2) . . . . ? Zr1 N11 N12 C13 -176.37(14) . . . . ? C15 N11 N12 B1 176.0(2) . . . . ? Zr1 N11 N12 B1 -0.1(3) . . . . ? N2 B1 N12 C13 117.9(2) . . . . ? N22 B1 N12 C13 -123.8(2) . . . . ? N2 B1 N12 N11 -57.6(3) . . . . ? N22 B1 N12 N11 60.7(3) . . . . ? N11 N12 C13 C14 0.0(3) . . . . ? B1 N12 C13 C14 -175.9(2) . . . . ? N12 C13 C14 C15 0.3(3) . . . . ? N12 N11 C15 C14 0.5(3) . . . . ? Zr1 N11 C15 C14 176.10(15) . . . . ? C13 C14 C15 N11 -0.5(3) . . . . ? N41 Zr1 N21 C25 -149.5(2) . . . . ? N31 Zr1 N21 C25 59.8(2) . . . . ? N1 Zr1 N21 C25 144.2(2) . . . . ? N51 Zr1 N21 C25 -40.2(2) . . . . ? N11 Zr1 N21 C25 -136.2(2) . . . . ? N41 Zr1 N21 N22 26.7(3) . . . . ? N31 Zr1 N21 N22 -123.97(15) . . . . ? N1 Zr1 N21 N22 -39.57(14) . . . . ? N51 Zr1 N21 N22 135.98(16) . . . . ? N11 Zr1 N21 N22 39.98(14) . . . . ? C25 N21 N22 C23 1.2(2) . . . . ? Zr1 N21 N22 C23 -175.93(14) . . . . ? C25 N21 N22 B1 177.7(2) . . . . ? Zr1 N21 N22 B1 0.6(3) . . . . ? N2 B1 N22 C23 -127.7(2) . . . . ? N12 B1 N22 C23 115.0(2) . . . . ? N2 B1 N22 N21 56.5(3) . . . . ? N12 B1 N22 N21 -60.9(3) . . . . ? N21 N22 C23 C24 -0.8(3) . . . . ? B1 N22 C23 C24 -177.0(2) . . . . ? N22 C23 C24 C25 0.1(3) . . . . ? N22 N21 C25 C24 -1.1(3) . . . . ? Zr1 N21 C25 C24 175.56(15) . . . . ? C23 C24 C25 N21 0.6(3) . . . . ? N41 Zr1 N31 C32 -158.4(2) . . . . ? N1 Zr1 N31 C32 -63.9(2) . . . . ? N51 Zr1 N31 C32 93.0(2) . . . . ? N11 Zr1 N31 C32 -48.4(3) . . . . ? N21 Zr1 N31 C32 12.1(2) . . . . ? N41 Zr1 N31 C33 4.4(2) . . . . ? N1 Zr1 N31 C33 98.9(2) . . . . ? N51 Zr1 N31 C33 -104.2(2) . . . . ? N11 Zr1 N31 C33 114.4(3) . . . . ? N21 Zr1 N31 C33 174.9(2) . . . . ? N31 Zr1 N41 C43 117.0(2) . . . . ? N1 Zr1 N41 C43 30.2(2) . . . . ? N51 Zr1 N41 C43 -138.2(2) . . . . ? N11 Zr1 N41 C43 -46.1(2) . . . . ? N21 Zr1 N41 C43 -33.2(3) . . . . ? N31 Zr1 N41 C42 -65.71(19) . . . . ? N1 Zr1 N41 C42 -152.56(18) . . . . ? N51 Zr1 N41 C42 39.06(19) . . . . ? N11 Zr1 N41 C42 131.17(18) . . . . ? N21 Zr1 N41 C42 144.1(2) . . . . ? N41 Zr1 N51 B52 -51.1(2) . . . . ? N31 Zr1 N51 B52 54.0(2) . . . . ? N1 Zr1 N51 B52 158.56(18) . . . . ? N11 Zr1 N51 B52 -137.1(2) . . . . ? N21 Zr1 N51 B52 147.8(2) . . . . ? Zr1 N51 B52 C71 -41.4(3) . . . . ? Zr1 N51 B52 C61 86.2(2) . . . . ? Zr1 N51 B52 C81 -160.61(16) . . . . ? N51 B52 C61 C62 -2.0(3) . . . . ? C71 B52 C61 C62 120.7(2) . . . . ? C81 B52 C61 C62 -118.5(2) . . . . ? N51 B52 C61 C66 171.93(19) . . . . ? C71 B52 C61 C66 -65.3(3) . . . . ? C81 B52 C61 C66 55.5(2) . . . . ? C66 C61 C62 F62 -178.79(19) . . . . ? B52 C61 C62 F62 -4.4(3) . . . . ? C66 C61 C62 C63 0.8(3) . . . . ? B52 C61 C62 C63 175.2(2) . . . . ? F62 C62 C63 F63 -3.0(3) . . . . ? C61 C62 C63 F63 177.4(2) . . . . ? F62 C62 C63 C64 177.8(2) . . . . ? C61 C62 C63 C64 -1.8(4) . . . . ? F63 C63 C64 F64 0.9(4) . . . . ? C62 C63 C64 F64 -180.0(2) . . . . ? F63 C63 C64 C65 -177.7(2) . . . . ? C62 C63 C64 C65 1.5(4) . . . . ? F64 C64 C65 F65 0.8(4) . . . . ? C63 C64 C65 F65 179.4(2) . . . . ? F64 C64 C65 C66 -178.9(2) . . . . ? C63 C64 C65 C66 -0.3(4) . . . . ? F65 C65 C66 F66 -0.7(3) . . . . ? C64 C65 C66 F66 179.0(2) . . . . ? F65 C65 C66 C61 179.6(2) . . . . ? C64 C65 C66 C61 -0.7(4) . . . . ? C62 C61 C66 F66 -179.22(18) . . . . ? B52 C61 C66 F66 6.0(3) . . . . ? C62 C61 C66 C65 0.5(3) . . . . ? B52 C61 C66 C65 -174.3(2) . . . . ? N51 B52 C71 C76 -58.5(3) . . . . ? C61 B52 C71 C76 175.66(19) . . . . ? C81 B52 C71 C76 59.2(3) . . . . ? N51 B52 C71 C72 124.7(2) . . . . ? C61 B52 C71 C72 -1.1(3) . . . . ? C81 B52 C71 C72 -117.6(2) . . . . ? C76 C71 C72 F72 178.63(19) . . . . ? B52 C71 C72 F72 -4.4(3) . . . . ? C76 C71 C72 C73 -1.5(3) . . . . ? B52 C71 C72 C73 175.5(2) . . . . ? F72 C72 C73 F73 1.2(3) . . . . ? C71 C72 C73 F73 -178.7(2) . . . . ? F72 C72 C73 C74 -179.17(19) . . . . ? C71 C72 C73 C74 0.9(3) . . . . ? F73 C73 C74 F74 -0.4(3) . . . . ? C72 C73 C74 F74 -180.0(2) . . . . ? F73 C73 C74 C75 179.9(2) . . . . ? C72 C73 C74 C75 0.2(3) . . . . ? F74 C74 C75 F75 0.6(3) . . . . ? C73 C74 C75 F75 -179.6(2) . . . . ? F74 C74 C75 C76 179.5(2) . . . . ? C73 C74 C75 C76 -0.7(3) . . . . ? F75 C75 C76 F76 0.8(3) . . . . ? C74 C75 C76 F76 -178.0(2) . . . . ? F75 C75 C76 C71 178.9(2) . . . . ? C74 C75 C76 C71 0.0(4) . . . . ? C72 C71 C76 F76 179.02(18) . . . . ? B52 C71 C76 F76 1.8(3) . . . . ? C72 C71 C76 C75 1.0(3) . . . . ? B52 C71 C76 C75 -176.3(2) . . . . ? N51 B52 C81 C82 -52.7(3) . . . . ? C71 B52 C81 C82 -169.3(2) . . . . ? C61 B52 C81 C82 66.7(2) . . . . ? N51 B52 C81 C86 133.8(2) . . . . ? C71 B52 C81 C86 17.2(3) . . . . ? C61 B52 C81 C86 -106.7(2) . . . . ? C86 C81 C82 F82 177.12(19) . . . . ? B52 C81 C82 F82 2.8(3) . . . . ? C86 C81 C82 C83 -1.3(3) . . . . ? B52 C81 C82 C83 -175.7(2) . . . . ? F82 C82 C83 F83 1.4(3) . . . . ? C81 C82 C83 F83 179.9(2) . . . . ? F82 C82 C83 C84 -177.54(19) . . . . ? C81 C82 C83 C84 1.0(3) . . . . ? F83 C83 C84 F84 0.6(3) . . . . ? C82 C83 C84 F84 179.5(2) . . . . ? F83 C83 C84 C85 -179.2(2) . . . . ? C82 C83 C84 C85 -0.2(3) . . . . ? F84 C84 C85 F85 0.0(4) . . . . ? C83 C84 C85 F85 179.8(2) . . . . ? F84 C84 C85 C86 -179.7(2) . . . . ? C83 C84 C85 C86 0.0(4) . . . . ? F85 C85 C86 F86 -1.6(3) . . . . ? C84 C85 C86 F86 178.1(2) . . . . ? F85 C85 C86 C81 179.7(2) . . . . ? C84 C85 C86 C81 -0.6(4) . . . . ? C82 C81 C86 F86 -177.5(2) . . . . ? B52 C81 C86 F86 -3.6(4) . . . . ? C82 C81 C86 C85 1.1(3) . . . . ? B52 C81 C86 C85 175.0(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N51 H51A F82 0.79(2) 2.37(2) 2.859(2) 121(2) . N51 H51A F62 0.79(2) 2.37(2) 2.698(2) 106.5(18) . N51 H51B F76 0.87(3) 2.33(3) 2.877(3) 121(2) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.747 _refine_diff_density_min -0.824 _refine_diff_density_rms 0.062 #===END data_6.pentane _database_code_depnum_ccdc_archive 'CCDC 823226' #TrackingRef '- fuller et al cif.cif' _chemical_formula_structural HB(C5H7N2)3Zr(NC2H6)2NH2B(C6F5)3.C5H12 _chemical_name_common HB(C5H7N2)3Zr(NC2H6)2NH2B(C6F5)3.C5H12 _chemical_melting_point ? _chemical_formula_moiety 'C37 H36 B2 F15 N9 Zr, C5 H12' _chemical_formula_sum 'C42 H48 B2 F15 N9 Zr' _chemical_formula_weight 1076.73 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 -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2726(5) _cell_length_b 11.8733(6) _cell_length_c 17.9169(8) _cell_angle_alpha 80.540(4) _cell_angle_beta 89.161(4) _cell_angle_gamma 81.252(4) _cell_volume 2337.79(19) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used 3863 _cell_measurement_theta_min 3.4452 _cell_measurement_theta_max 29.9999 _exptl_crystal_description needles _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1096 _exptl_absorpt_coefficient_mu 0.338 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8336 _exptl_absorpt_correction_T_max 1.2973 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.9 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18358 _diffrn_reflns_av_R_equivalents 0.1587 _diffrn_reflns_av_sigmaI/netI 0.1774 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6062 _reflns_number_gt 3533 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _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^)+(0.0382P)^2^+3.3737P] 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 6062 _refine_ls_number_parameters 644 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1710 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.1462 _refine_ls_wR_factor_gt 0.1182 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Zr1 Zr 0.61053(8) 0.79352(8) 0.73364(5) 0.0236(3) Uani 1 1 d . . . B1 B 0.3220(9) 0.7885(10) 0.6849(7) 0.037(3) Uani 1 1 d . . . N1 N 0.4592(6) 0.9395(6) 0.6848(4) 0.0317(19) Uani 1 1 d . . . N2 N 0.3471(5) 0.9152(6) 0.6672(4) 0.0249(18) Uani 1 1 d . . . C3 C 0.2767(7) 1.0103(8) 0.6341(5) 0.030(2) Uani 1 1 d . . . C4 C 0.3410(8) 1.1008(8) 0.6284(5) 0.034(2) Uani 1 1 d . . . H4 H 0.3147 1.1774 0.6074 0.041 Uiso 1 1 calc R . . C5 C 0.4514(8) 1.0558(8) 0.6599(5) 0.032(2) Uani 1 1 d . . . C6 C 0.5537(7) 1.1210(8) 0.6696(5) 0.041(3) Uani 1 1 d . . . H6A H 0.5579 1.1789 0.6258 0.061 Uiso 1 1 calc R . . H6B H 0.6277 1.0683 0.6754 0.061 Uiso 1 1 calc R . . H6C H 0.5405 1.1573 0.7137 0.061 Uiso 1 1 calc R . . C7 C 0.1517(7) 1.0090(8) 0.6064(5) 0.040(3) Uani 1 1 d . . . H7A H 0.1552 0.9626 0.5671 0.060 Uiso 1 1 calc R . . H7B H 0.1150 1.0864 0.5869 0.060 Uiso 1 1 calc R . . H7C H 0.1051 0.9771 0.6476 0.060 Uiso 1 1 calc R . . N11 N 0.4427(6) 0.7498(6) 0.8063(4) 0.0299(19) Uani 1 1 d . . . N12 N 0.3380(6) 0.7423(6) 0.7690(4) 0.0312(19) Uani 1 1 d . . . C13 C 0.2567(8) 0.7043(8) 0.8192(6) 0.036(3) Uani 1 1 d . . . C14 C 0.3070(8) 0.6866(8) 0.8888(6) 0.042(3) Uani 1 1 d . . . H14 H 0.2716 0.6599 0.9342 0.050 Uiso 1 1 calc R . . C15 C 0.4223(8) 0.7161(8) 0.8798(6) 0.036(3) Uani 1 1 d . . . C16 C 0.5125(8) 0.7132(9) 0.9422(5) 0.049(3) Uani 1 1 d . . . H16A H 0.5919 0.7074 0.9216 0.073 Uiso 1 1 calc R . . H16B H 0.5076 0.6476 0.9807 0.073 Uiso 1 1 calc R . . H16C H 0.4952 0.7827 0.9637 0.073 Uiso 1 1 calc R . . C17 C 0.1353(7) 0.6863(8) 0.7964(6) 0.051(3) Uani 1 1 d . . . H17A H 0.0878 0.7597 0.7783 0.076 Uiso 1 1 calc R . . H17B H 0.0970 0.6476 0.8393 0.076 Uiso 1 1 calc R . . H17C H 0.1429 0.6399 0.7570 0.076 Uiso 1 1 calc R . . N21 N 0.5299(6) 0.7086(6) 0.6394(4) 0.0241(18) Uani 1 1 d . . . N22 N 0.4058(6) 0.7169(6) 0.6349(4) 0.0258(18) Uani 1 1 d . . . C23 C 0.3764(8) 0.6841(7) 0.5690(6) 0.032(2) Uani 1 1 d . . . C24 C 0.4799(8) 0.6495(7) 0.5330(5) 0.033(2) Uani 1 1 d . . . H24 H 0.4869 0.6205 0.4878 0.040 Uiso 1 1 calc R . . C25 C 0.5721(7) 0.6667(7) 0.5780(5) 0.024(2) Uani 1 1 d . . . C26 C 0.7033(7) 0.6432(7) 0.5610(5) 0.031(2) Uani 1 1 d . . . H26A H 0.7481 0.6742 0.5958 0.047 Uiso 1 1 calc R . . H26B H 0.7173 0.6790 0.5102 0.047 Uiso 1 1 calc R . . H26C H 0.7286 0.5614 0.5660 0.047 Uiso 1 1 calc R . . C27 C 0.2502(8) 0.6842(9) 0.5448(6) 0.058(3) Uani 1 1 d . . . H27A H 0.2137 0.7619 0.5260 0.087 Uiso 1 1 calc R . . H27B H 0.2058 0.6528 0.5873 0.087 Uiso 1 1 calc R . . H27C H 0.2501 0.6379 0.5057 0.087 Uiso 1 1 calc R . . N31 N 0.7202(6) 0.8638(6) 0.6523(4) 0.033(2) Uani 1 1 d . . . C32 C 0.6877(8) 0.9106(8) 0.5735(5) 0.040(3) Uani 1 1 d . . . H32A H 0.6859 0.9929 0.5651 0.060 Uiso 1 1 calc R . . H32B H 0.6100 0.8933 0.5626 0.060 Uiso 1 1 calc R . . H32C H 0.7460 0.8765 0.5409 0.060 Uiso 1 1 calc R . . C33 C 0.8436(7) 0.8832(9) 0.6656(5) 0.051(3) Uani 1 1 d . . . H33A H 0.8972 0.8456 0.6320 0.076 Uiso 1 1 calc R . . H33B H 0.8669 0.8521 0.7170 0.076 Uiso 1 1 calc R . . H33C H 0.8471 0.9646 0.6563 0.076 Uiso 1 1 calc R . . N41 N 0.7047(6) 0.8214(6) 0.8211(4) 0.0282(19) Uani 1 1 d . . . C42 C 0.8038(8) 0.7819(9) 0.8757(5) 0.051(3) Uani 1 1 d . . . H42A H 0.8630 0.8326 0.8663 0.077 Uiso 1 1 calc R . . H42B H 0.8397 0.7049 0.8706 0.077 Uiso 1 1 calc R . . H42C H 0.7738 0.7822 0.9261 0.077 Uiso 1 1 calc R . . C43 C 0.6532(8) 0.9383(9) 0.8307(6) 0.053(3) Uani 1 1 d . . . H43A H 0.6305 0.9389 0.8825 0.080 Uiso 1 1 calc R . . H43B H 0.5837 0.9639 0.7985 0.080 Uiso 1 1 calc R . . H43C H 0.7115 0.9891 0.8173 0.080 Uiso 1 1 calc R . . N51 N 0.7000(6) 0.6016(6) 0.7850(4) 0.0293(18) Uani 1 1 d . . . H51A H 0.7779 0.6103 0.7855 0.035 Uiso 1 1 calc R . . H51B H 0.6777 0.5984 0.8337 0.035 Uiso 1 1 calc R . . B52 B 0.7115(9) 0.4686(9) 0.7767(6) 0.031(3) Uani 1 1 d . . . F62 F 0.9058(4) 0.5997(4) 0.6982(3) 0.0453(15) Uani 1 1 d . . . F63 F 1.0612(4) 0.5253(5) 0.5997(3) 0.069(2) Uani 1 1 d . . . F64 F 1.0606(5) 0.3156(5) 0.5560(3) 0.068(2) Uani 1 1 d . . . F65 F 0.8973(4) 0.1819(5) 0.6168(3) 0.0505(16) Uani 1 1 d . . . F66 F 0.7417(4) 0.2526(4) 0.7183(2) 0.0309(13) Uani 1 1 d . . . F72 F 0.5880(4) 0.4204(4) 0.6339(2) 0.0270(12) Uani 1 1 d . . . F73 F 0.3597(4) 0.3966(4) 0.6243(3) 0.0389(14) Uani 1 1 d . . . F74 F 0.2132(4) 0.4019(5) 0.7463(3) 0.0517(16) Uani 1 1 d . . . F75 F 0.3043(4) 0.4312(5) 0.8804(3) 0.0504(16) Uani 1 1 d . . . F76 F 0.5316(4) 0.4661(4) 0.8910(3) 0.0394(14) Uani 1 1 d . . . F82 F 0.9274(4) 0.4983(4) 0.8558(3) 0.0462(15) Uani 1 1 d . . . F83 F 1.0432(5) 0.3581(5) 0.9708(3) 0.0653(18) Uani 1 1 d . . . F84 F 0.9654(5) 0.1551(5) 1.0310(3) 0.0699(19) Uani 1 1 d . . . F85 F 0.7633(5) 0.1024(5) 0.9723(3) 0.0619(18) Uani 1 1 d . . . F86 F 0.6421(4) 0.2401(4) 0.8622(3) 0.0401(14) Uani 1 1 d . . . C61 C 0.8077(7) 0.4331(7) 0.7118(5) 0.023(2) Uani 1 1 d . . . C62 C 0.8975(7) 0.4939(7) 0.6798(5) 0.030(2) Uani 1 1 d . . . C63 C 0.9797(8) 0.4581(9) 0.6291(6) 0.039(3) Uani 1 1 d . . . C64 C 0.9827(8) 0.3536(10) 0.6067(5) 0.042(3) Uani 1 1 d . . . C65 C 0.8972(7) 0.2852(8) 0.6379(5) 0.029(2) Uani 1 1 d . . . C66 C 0.8176(7) 0.3267(8) 0.6882(5) 0.022(2) Uani 1 1 d . . . C71 C 0.5715(7) 0.4473(7) 0.7632(5) 0.023(2) Uani 1 1 d . . . C72 C 0.5217(7) 0.4271(7) 0.6984(5) 0.023(2) Uani 1 1 d . . . C73 C 0.4016(8) 0.4143(7) 0.6908(5) 0.028(2) Uani 1 1 d . . . C74 C 0.3297(7) 0.4175(8) 0.7531(6) 0.033(2) Uani 1 1 d . . . C75 C 0.3735(8) 0.4329(7) 0.8195(5) 0.031(2) Uani 1 1 d . . . C76 C 0.4922(7) 0.4501(7) 0.8227(5) 0.026(2) Uani 1 1 d . . . C81 C 0.7740(7) 0.3812(8) 0.8537(5) 0.027(2) Uani 1 1 d . . . C82 C 0.8801(8) 0.4016(8) 0.8861(5) 0.033(2) Uani 1 1 d . . . C83 C 0.9433(8) 0.3292(9) 0.9441(5) 0.042(3) Uani 1 1 d . . . C84 C 0.9039(9) 0.2291(9) 0.9737(5) 0.041(3) Uani 1 1 d . . . C85 C 0.8014(9) 0.2007(8) 0.9448(5) 0.041(3) Uani 1 1 d . . . C86 C 0.7409(8) 0.2771(8) 0.8868(5) 0.033(2) Uani 1 1 d . . . C91 C 0.0116(10) 0.9354(11) 0.1917(6) 0.080(4) Uani 1 1 d D . . C92A C -0.1214(14) 0.9454(19) 0.1981(10) 0.060(5) Uani 0.607(18) 1 d PDU A 1 C92B C -0.083(2) 0.861(2) 0.1990(14) 0.060(5) Uani 0.393(18) 1 d PDU A 2 C93 C -0.1841(11) 0.8986(13) 0.1375(6) 0.098(5) Uani 1 1 d D . . C94A C -0.3157(14) 0.9148(19) 0.1454(8) 0.087(7) Uani 0.81(2) 1 d PD A 3 C94B C -0.274(4) 0.826(3) 0.127(4) 0.087(7) Uani 0.19(2) 1 d PD A 4 C95 C -0.3838(10) 0.8861(13) 0.0792(7) 0.094(5) Uani 1 1 d D A 4 H1 H 0.222(6) 0.784(6) 0.670(4) 0.03(2) 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 Zr1 0.0239(5) 0.0226(6) 0.0262(6) -0.0028(4) -0.0015(4) -0.0109(4) B1 0.019(6) 0.043(8) 0.051(8) -0.002(7) 0.003(6) -0.021(6) N1 0.024(4) 0.029(5) 0.046(5) -0.014(4) -0.007(4) -0.006(4) N2 0.019(4) 0.028(5) 0.024(4) 0.010(4) 0.000(3) -0.006(4) C3 0.026(5) 0.024(6) 0.036(6) 0.001(5) 0.002(5) 0.003(5) C4 0.037(6) 0.023(6) 0.041(6) 0.006(5) 0.000(5) -0.010(5) C5 0.031(6) 0.028(6) 0.041(6) -0.009(5) -0.006(5) -0.009(5) C6 0.040(6) 0.034(7) 0.052(7) -0.011(5) 0.003(5) -0.015(5) C7 0.021(5) 0.050(7) 0.042(6) 0.010(5) -0.007(5) 0.001(5) N11 0.021(4) 0.030(5) 0.038(5) 0.002(4) 0.006(4) -0.007(4) N12 0.022(4) 0.035(5) 0.036(5) -0.003(4) 0.004(4) -0.005(4) C13 0.030(6) 0.029(6) 0.046(7) 0.003(5) 0.012(5) -0.004(5) C14 0.034(6) 0.051(8) 0.040(7) -0.003(6) 0.023(5) -0.013(5) C15 0.032(6) 0.030(6) 0.044(7) -0.003(5) 0.003(5) -0.001(5) C16 0.074(7) 0.046(7) 0.027(6) 0.001(5) -0.003(6) -0.021(6) C17 0.026(6) 0.051(8) 0.077(8) -0.001(6) 0.019(6) -0.017(5) N21 0.022(4) 0.032(5) 0.020(5) -0.011(4) -0.005(4) -0.006(3) N22 0.020(4) 0.026(5) 0.031(5) 0.003(4) -0.001(4) -0.010(3) C23 0.035(6) 0.014(6) 0.044(7) 0.005(5) -0.010(5) -0.008(4) C24 0.052(7) 0.021(6) 0.029(6) -0.004(5) -0.009(5) -0.011(5) C25 0.040(6) 0.012(5) 0.021(5) -0.005(4) -0.009(5) -0.010(4) C26 0.034(6) 0.030(6) 0.031(6) -0.003(5) 0.001(5) -0.008(4) C27 0.048(7) 0.063(8) 0.070(8) -0.019(7) -0.025(6) -0.019(6) N31 0.028(4) 0.043(5) 0.032(5) 0.000(4) -0.004(4) -0.022(4) C32 0.051(6) 0.036(7) 0.034(6) 0.005(5) -0.011(5) -0.021(5) C33 0.026(6) 0.063(8) 0.063(8) 0.006(6) 0.005(5) -0.025(5) N41 0.041(5) 0.022(5) 0.022(4) 0.001(4) -0.007(4) -0.009(4) C42 0.043(6) 0.065(8) 0.053(7) -0.022(6) -0.020(6) -0.015(6) C43 0.054(7) 0.045(8) 0.060(8) -0.005(6) -0.028(6) -0.004(6) N51 0.030(4) 0.028(5) 0.034(5) -0.008(4) 0.000(4) -0.016(4) B52 0.032(6) 0.024(7) 0.036(7) 0.003(6) -0.009(6) -0.005(5) F62 0.036(3) 0.037(4) 0.065(4) 0.004(3) 0.003(3) -0.026(3) F63 0.039(3) 0.068(5) 0.094(5) 0.020(4) 0.022(3) -0.027(3) F64 0.051(4) 0.070(5) 0.074(4) 0.006(4) 0.037(4) 0.000(3) F65 0.047(3) 0.044(4) 0.059(4) -0.007(3) 0.013(3) -0.002(3) F66 0.025(3) 0.028(3) 0.040(3) 0.001(3) 0.006(2) -0.013(2) F72 0.028(3) 0.028(3) 0.027(3) -0.002(2) -0.004(2) -0.012(2) F73 0.028(3) 0.044(4) 0.050(4) -0.010(3) -0.008(3) -0.016(3) F74 0.022(3) 0.071(4) 0.066(4) -0.011(3) -0.002(3) -0.019(3) F75 0.041(3) 0.064(4) 0.049(4) -0.012(3) 0.016(3) -0.018(3) F76 0.041(3) 0.045(4) 0.034(3) -0.007(3) 0.004(3) -0.011(3) F82 0.036(3) 0.040(4) 0.062(4) 0.006(3) -0.020(3) -0.014(3) F83 0.054(4) 0.075(5) 0.066(4) 0.001(4) -0.036(3) -0.017(3) F84 0.080(4) 0.070(5) 0.051(4) 0.020(4) -0.031(3) -0.014(4) F85 0.069(4) 0.050(4) 0.056(4) 0.028(3) -0.009(3) -0.015(3) F86 0.041(3) 0.033(3) 0.043(3) 0.012(3) -0.006(3) -0.016(3) C61 0.019(5) 0.019(6) 0.031(6) 0.003(5) -0.002(4) -0.009(4) C62 0.028(5) 0.013(6) 0.045(7) 0.011(5) -0.009(5) -0.013(4) C63 0.022(5) 0.042(7) 0.049(7) 0.006(6) 0.018(5) -0.011(5) C64 0.024(6) 0.053(8) 0.040(7) 0.003(6) 0.007(5) 0.005(5) C65 0.031(6) 0.016(6) 0.039(6) -0.004(5) 0.004(5) 0.003(4) C66 0.010(5) 0.033(6) 0.021(5) 0.001(5) 0.000(4) 0.000(4) C71 0.027(5) 0.019(6) 0.022(5) 0.008(4) -0.005(5) -0.013(4) C72 0.032(5) 0.017(5) 0.020(5) 0.004(4) 0.004(5) -0.011(4) C73 0.034(6) 0.020(6) 0.033(6) -0.011(5) -0.007(5) -0.005(4) C74 0.023(5) 0.033(6) 0.046(7) -0.008(5) 0.003(5) -0.012(5) C75 0.030(6) 0.027(6) 0.034(6) -0.002(5) 0.008(5) -0.006(5) C76 0.026(5) 0.034(6) 0.018(5) -0.003(5) -0.004(5) -0.012(4) C81 0.020(5) 0.029(6) 0.030(6) 0.001(5) 0.002(4) -0.007(4) C82 0.034(6) 0.027(6) 0.039(6) -0.001(5) 0.001(5) -0.013(5) C83 0.030(6) 0.050(8) 0.040(7) 0.006(6) -0.016(5) -0.004(5) C84 0.059(7) 0.040(7) 0.016(6) 0.013(5) -0.016(5) 0.000(6) C85 0.057(7) 0.026(6) 0.038(6) 0.016(5) -0.002(6) -0.018(5) C86 0.030(6) 0.037(7) 0.034(6) -0.009(5) 0.002(5) -0.003(5) C91 0.080(9) 0.101(11) 0.059(8) -0.005(8) -0.004(7) -0.022(8) C92A 0.065(7) 0.065(8) 0.057(7) -0.022(6) -0.001(5) -0.020(6) C92B 0.065(7) 0.065(8) 0.057(7) -0.022(6) -0.001(5) -0.020(6) C93 0.073(9) 0.168(16) 0.047(8) 0.019(9) -0.018(7) -0.037(9) C94A 0.073(11) 0.14(2) 0.060(11) -0.031(11) 0.021(9) -0.041(12) C94B 0.073(11) 0.14(2) 0.060(11) -0.031(11) 0.021(9) -0.041(12) C95 0.065(9) 0.128(14) 0.086(10) -0.001(9) -0.020(8) -0.016(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 N41 2.004(7) . ? Zr1 N31 2.052(6) . ? Zr1 N1 2.308(7) . ? Zr1 N11 2.356(6) . ? Zr1 N21 2.362(7) . ? Zr1 N51 2.386(7) . ? B1 N12 1.521(12) . ? B1 N22 1.549(13) . ? B1 N2 1.554(12) . ? B1 H1 1.18(6) . ? N1 C5 1.369(10) . ? N1 N2 1.389(8) . ? N2 C3 1.334(10) . ? C3 C4 1.375(11) . ? C3 C7 1.504(10) . ? C4 C5 1.368(11) . ? C4 H4 0.9300 . ? C5 C6 1.510(11) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? N11 C15 1.339(10) . ? N11 N12 1.386(9) . ? N12 C13 1.350(9) . ? C13 C14 1.349(12) . ? C13 C17 1.490(11) . ? C14 C15 1.397(11) . ? C14 H14 0.9300 . ? C15 C16 1.514(12) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? N21 C25 1.333(9) . ? N21 N22 1.390(8) . ? N22 C23 1.362(10) . ? C23 C24 1.365(11) . ? C23 C27 1.492(11) . ? C24 C25 1.384(10) . ? C24 H24 0.9300 . ? C25 C26 1.499(10) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? N31 C32 1.460(9) . ? N31 C33 1.473(9) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? N41 C43 1.457(11) . ? N41 C42 1.466(10) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? N51 B52 1.596(12) . ? N51 H51A 0.9000 . ? N51 H51B 0.9000 . ? B52 C61 1.641(13) . ? B52 C71 1.664(12) . ? B52 C81 1.677(13) . ? F62 C62 1.367(9) . ? F63 C63 1.353(9) . ? F64 C64 1.338(10) . ? F65 C65 1.341(9) . ? F66 C66 1.363(8) . ? F72 C72 1.373(8) . ? F73 C73 1.347(9) . ? F74 C74 1.363(9) . ? F75 C75 1.330(9) . ? F76 C76 1.360(9) . ? F82 C82 1.367(9) . ? F83 C83 1.342(9) . ? F84 C84 1.359(9) . ? F85 C85 1.322(9) . ? F86 C86 1.362(9) . ? C61 C66 1.386(11) . ? C61 C62 1.394(10) . ? C62 C63 1.359(12) . ? C63 C64 1.361(13) . ? C64 C65 1.407(12) . ? C65 C66 1.358(11) . ? C71 C72 1.368(10) . ? C71 C76 1.382(10) . ? C72 C73 1.396(11) . ? C73 C74 1.372(11) . ? C74 C75 1.345(11) . ? C75 C76 1.387(11) . ? C81 C86 1.382(11) . ? C81 C82 1.407(11) . ? C82 C83 1.368(12) . ? C83 C84 1.355(12) . ? C84 C85 1.382(12) . ? C85 C86 1.374(12) . ? C91 C92B 1.474(19) . ? C91 C92A 1.490(16) . ? C92A C93 1.525(17) . ? C92B C93 1.56(2) . ? C93 C94B 1.46(2) . ? C93 C94A 1.474(16) . ? C94A C95 1.532(17) . ? C94B C95 1.53(2) . ? 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 N41 Zr1 N31 95.0(3) . . ? N41 Zr1 N1 116.6(3) . . ? N31 Zr1 N1 87.5(3) . . ? N41 Zr1 N11 94.9(3) . . ? N31 Zr1 N11 163.7(3) . . ? N1 Zr1 N11 76.6(2) . . ? N41 Zr1 N21 164.0(3) . . ? N31 Zr1 N21 87.8(2) . . ? N1 Zr1 N21 79.2(2) . . ? N11 Zr1 N21 86.2(2) . . ? N41 Zr1 N51 78.6(3) . . ? N31 Zr1 N51 109.5(3) . . ? N1 Zr1 N51 156.9(2) . . ? N11 Zr1 N51 85.1(2) . . ? N21 Zr1 N51 85.6(2) . . ? N12 B1 N22 113.2(8) . . ? N12 B1 N2 110.5(8) . . ? N22 B1 N2 107.7(7) . . ? N12 B1 H1 106(3) . . ? N22 B1 H1 109(3) . . ? N2 B1 H1 111(3) . . ? C5 N1 N2 103.7(6) . . ? C5 N1 Zr1 135.1(5) . . ? N2 N1 Zr1 120.9(5) . . ? C3 N2 N1 111.0(7) . . ? C3 N2 B1 129.7(7) . . ? N1 N2 B1 119.2(7) . . ? N2 C3 C4 107.9(8) . . ? N2 C3 C7 122.7(8) . . ? C4 C3 C7 129.4(8) . . ? C5 C4 C3 106.3(8) . . ? C5 C4 H4 126.9 . . ? C3 C4 H4 126.9 . . ? C4 C5 N1 111.0(7) . . ? C4 C5 C6 126.9(9) . . ? N1 C5 C6 122.1(8) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C3 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C15 N11 N12 105.5(6) . . ? C15 N11 Zr1 135.5(6) . . ? N12 N11 Zr1 118.6(5) . . ? C13 N12 N11 110.1(7) . . ? C13 N12 B1 129.0(8) . . ? N11 N12 B1 120.4(7) . . ? C14 C13 N12 107.7(8) . . ? C14 C13 C17 129.3(8) . . ? N12 C13 C17 122.9(9) . . ? C13 C14 C15 107.0(8) . . ? C13 C14 H14 126.5 . . ? C15 C14 H14 126.5 . . ? N11 C15 C14 109.7(8) . . ? N11 C15 C16 123.7(8) . . ? C14 C15 C16 126.6(9) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 H17A 109.5 . . ? C13 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C13 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C25 N21 N22 105.7(6) . . ? C25 N21 Zr1 135.5(5) . . ? N22 N21 Zr1 117.8(5) . . ? C23 N22 N21 108.8(7) . . ? C23 N22 B1 127.1(8) . . ? N21 N22 B1 121.4(7) . . ? N22 C23 C24 108.5(8) . . ? N22 C23 C27 123.4(9) . . ? C24 C23 C27 128.1(9) . . ? C23 C24 C25 105.7(8) . . ? C23 C24 H24 127.2 . . ? C25 C24 H24 127.2 . . ? N21 C25 C24 111.3(8) . . ? N21 C25 C26 123.3(7) . . ? C24 C25 C26 125.5(8) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C32 N31 C33 108.3(6) . . ? C32 N31 Zr1 126.5(5) . . ? C33 N31 Zr1 125.1(6) . . ? N31 C32 H32A 109.5 . . ? N31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N31 C33 H33A 109.5 . . ? N31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C43 N41 C42 107.7(7) . . ? C43 N41 Zr1 103.1(5) . . ? C42 N41 Zr1 149.0(6) . . ? N41 C42 H42A 109.5 . . ? N41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N41 C43 H43A 109.5 . . ? N41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? B52 N51 Zr1 145.1(5) . . ? B52 N51 H51A 100.6 . . ? Zr1 N51 H51A 100.6 . . ? B52 N51 H51B 100.6 . . ? Zr1 N51 H51B 100.6 . . ? H51A N51 H51B 104.3 . . ? N51 B52 C61 112.9(7) . . ? N51 B52 C71 104.8(7) . . ? C61 B52 C71 115.5(8) . . ? N51 B52 C81 112.0(7) . . ? C61 B52 C81 100.6(7) . . ? C71 B52 C81 111.3(7) . . ? C66 C61 C62 110.5(8) . . ? C66 C61 B52 121.7(7) . . ? C62 C61 B52 127.4(8) . . ? C63 C62 F62 115.0(8) . . ? C63 C62 C61 125.4(9) . . ? F62 C62 C61 119.6(8) . . ? F63 C63 C62 120.9(10) . . ? F63 C63 C64 118.1(9) . . ? C62 C63 C64 121.1(8) . . ? F64 C64 C63 123.2(9) . . ? F64 C64 C65 119.6(10) . . ? C63 C64 C65 117.1(9) . . ? F65 C65 C66 122.8(8) . . ? F65 C65 C64 118.7(9) . . ? C66 C65 C64 118.5(9) . . ? C65 C66 F66 114.6(8) . . ? C65 C66 C61 127.2(8) . . ? F66 C66 C61 118.2(7) . . ? C72 C71 C76 113.6(7) . . ? C72 C71 B52 127.8(8) . . ? C76 C71 B52 118.6(8) . . ? C71 C72 F72 121.4(7) . . ? C71 C72 C73 124.2(8) . . ? F72 C72 C73 114.4(8) . . ? F73 C73 C74 121.6(8) . . ? F73 C73 C72 120.2(8) . . ? C74 C73 C72 118.1(8) . . ? C75 C74 F74 120.9(8) . . ? C75 C74 C73 121.0(8) . . ? F74 C74 C73 118.1(9) . . ? F75 C75 C74 120.5(8) . . ? F75 C75 C76 121.2(9) . . ? C74 C75 C76 118.2(8) . . ? F76 C76 C71 119.4(7) . . ? F76 C76 C75 115.8(8) . . ? C71 C76 C75 124.8(8) . . ? C86 C81 C82 112.0(8) . . ? C86 C81 B52 126.6(8) . . ? C82 C81 B52 121.0(8) . . ? F82 C82 C83 116.7(8) . . ? F82 C82 C81 118.3(8) . . ? C83 C82 C81 124.9(8) . . ? F83 C83 C84 121.1(9) . . ? F83 C83 C82 119.6(9) . . ? C84 C83 C82 119.2(9) . . ? C83 C84 F84 120.5(9) . . ? C83 C84 C85 120.1(9) . . ? F84 C84 C85 119.4(9) . . ? F85 C85 C86 121.3(9) . . ? F85 C85 C84 120.5(9) . . ? C86 C85 C84 118.2(9) . . ? F86 C86 C85 113.3(8) . . ? F86 C86 C81 121.0(8) . . ? C85 C86 C81 125.6(9) . . ? C92B C91 C92A 40.3(12) . . ? C91 C92A C93 115.4(12) . . ? C91 C92B C93 114.4(15) . . ? C94B C93 C94A 48(2) . . ? C94B C93 C92A 142(3) . . ? C94A C93 C92A 112.7(13) . . ? C94B C93 C92B 122.3(18) . . ? C94A C93 C92B 130.2(14) . . ? C92A C93 C92B 38.7(11) . . ? C93 C94A C95 114.6(12) . . ? C93 C94B C95 115(2) . . ? C94A C95 C94B 46(2) . . ? 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 N41 Zr1 N1 C5 51.7(9) . . . . ? N31 Zr1 N1 C5 -42.6(8) . . . . ? N11 Zr1 N1 C5 140.5(9) . . . . ? N21 Zr1 N1 C5 -130.9(8) . . . . ? N51 Zr1 N1 C5 179.2(7) . . . . ? N41 Zr1 N1 N2 -135.6(5) . . . . ? N31 Zr1 N1 N2 130.1(6) . . . . ? N11 Zr1 N1 N2 -46.7(6) . . . . ? N21 Zr1 N1 N2 41.9(5) . . . . ? N51 Zr1 N1 N2 -8.1(10) . . . . ? C5 N1 N2 C3 -0.1(9) . . . . ? Zr1 N1 N2 C3 -174.8(5) . . . . ? C5 N1 N2 B1 178.1(8) . . . . ? Zr1 N1 N2 B1 3.3(9) . . . . ? N12 B1 N2 C3 -122.9(9) . . . . ? N22 B1 N2 C3 113.0(9) . . . . ? N12 B1 N2 N1 59.4(10) . . . . ? N22 B1 N2 N1 -64.7(10) . . . . ? N1 N2 C3 C4 0.3(10) . . . . ? B1 N2 C3 C4 -177.6(8) . . . . ? N1 N2 C3 C7 177.8(7) . . . . ? B1 N2 C3 C7 0.0(14) . . . . ? N2 C3 C4 C5 -0.4(10) . . . . ? C7 C3 C4 C5 -177.7(9) . . . . ? C3 C4 C5 N1 0.4(10) . . . . ? C3 C4 C5 C6 -178.0(9) . . . . ? N2 N1 C5 C4 -0.2(9) . . . . ? Zr1 N1 C5 C4 173.4(6) . . . . ? N2 N1 C5 C6 178.3(8) . . . . ? Zr1 N1 C5 C6 -8.1(13) . . . . ? N41 Zr1 N11 C15 -20.0(9) . . . . ? N31 Zr1 N11 C15 -147.5(10) . . . . ? N1 Zr1 N11 C15 -136.2(9) . . . . ? N21 Zr1 N11 C15 144.0(9) . . . . ? N51 Zr1 N11 C15 58.1(9) . . . . ? N41 Zr1 N11 N12 168.9(6) . . . . ? N31 Zr1 N11 N12 41.5(13) . . . . ? N1 Zr1 N11 N12 52.8(6) . . . . ? N21 Zr1 N11 N12 -27.0(6) . . . . ? N51 Zr1 N11 N12 -113.0(6) . . . . ? C15 N11 N12 C13 -0.3(10) . . . . ? Zr1 N11 N12 C13 173.3(6) . . . . ? C15 N11 N12 B1 172.2(8) . . . . ? Zr1 N11 N12 B1 -14.3(10) . . . . ? N22 B1 N12 C13 -120.3(9) . . . . ? N2 B1 N12 C13 118.8(9) . . . . ? N22 B1 N12 N11 68.8(10) . . . . ? N2 B1 N12 N11 -52.1(11) . . . . ? N11 N12 C13 C14 -0.2(11) . . . . ? B1 N12 C13 C14 -171.8(9) . . . . ? N11 N12 C13 C17 -179.5(8) . . . . ? B1 N12 C13 C17 8.9(15) . . . . ? N12 C13 C14 C15 0.5(11) . . . . ? C17 C13 C14 C15 179.7(9) . . . . ? N12 N11 C15 C14 0.6(10) . . . . ? Zr1 N11 C15 C14 -171.3(6) . . . . ? N12 N11 C15 C16 -178.7(8) . . . . ? Zr1 N11 C15 C16 9.5(15) . . . . ? C13 C14 C15 N11 -0.7(11) . . . . ? C13 C14 C15 C16 178.5(9) . . . . ? N41 Zr1 N21 C25 -67.4(13) . . . . ? N31 Zr1 N21 C25 33.0(8) . . . . ? N1 Zr1 N21 C25 120.9(8) . . . . ? N11 Zr1 N21 C25 -162.1(8) . . . . ? N51 Zr1 N21 C25 -76.7(8) . . . . ? N41 Zr1 N21 N22 125.8(9) . . . . ? N31 Zr1 N21 N22 -133.8(6) . . . . ? N1 Zr1 N21 N22 -46.0(5) . . . . ? N11 Zr1 N21 N22 31.1(5) . . . . ? N51 Zr1 N21 N22 116.5(5) . . . . ? C25 N21 N22 C23 -2.5(9) . . . . ? Zr1 N21 N22 C23 168.0(5) . . . . ? C25 N21 N22 B1 -165.1(7) . . . . ? Zr1 N21 N22 B1 5.3(9) . . . . ? N12 B1 N22 C23 137.4(8) . . . . ? N2 B1 N22 C23 -100.2(9) . . . . ? N12 B1 N22 N21 -63.3(10) . . . . ? N2 B1 N22 N21 59.1(10) . . . . ? N21 N22 C23 C24 3.0(9) . . . . ? B1 N22 C23 C24 164.4(8) . . . . ? N21 N22 C23 C27 -179.0(8) . . . . ? B1 N22 C23 C27 -17.6(13) . . . . ? N22 C23 C24 C25 -2.2(9) . . . . ? C27 C23 C24 C25 179.9(9) . . . . ? N22 N21 C25 C24 1.1(9) . . . . ? Zr1 N21 C25 C24 -166.8(6) . . . . ? N22 N21 C25 C26 -179.4(7) . . . . ? Zr1 N21 C25 C26 12.7(13) . . . . ? C23 C24 C25 N21 0.7(10) . . . . ? C23 C24 C25 C26 -178.8(8) . . . . ? N41 Zr1 N31 C32 -157.1(7) . . . . ? N1 Zr1 N31 C32 -40.7(7) . . . . ? N11 Zr1 N31 C32 -29.7(15) . . . . ? N21 Zr1 N31 C32 38.6(7) . . . . ? N51 Zr1 N31 C32 123.2(7) . . . . ? N41 Zr1 N31 C33 18.1(7) . . . . ? N1 Zr1 N31 C33 134.6(7) . . . . ? N11 Zr1 N31 C33 145.5(9) . . . . ? N21 Zr1 N31 C33 -146.2(7) . . . . ? N51 Zr1 N31 C33 -61.6(7) . . . . ? N31 Zr1 N41 C43 87.1(6) . . . . ? N1 Zr1 N41 C43 -2.5(6) . . . . ? N11 Zr1 N41 C43 -80.0(6) . . . . ? N21 Zr1 N41 C43 -173.4(8) . . . . ? N51 Zr1 N41 C43 -164.0(6) . . . . ? N31 Zr1 N41 C42 -87.0(11) . . . . ? N1 Zr1 N41 C42 -176.6(10) . . . . ? N11 Zr1 N41 C42 105.9(11) . . . . ? N21 Zr1 N41 C42 12.4(17) . . . . ? N51 Zr1 N41 C42 21.9(10) . . . . ? N41 Zr1 N51 B52 179.5(9) . . . . ? N31 Zr1 N51 B52 -89.2(9) . . . . ? N1 Zr1 N51 B52 45.8(12) . . . . ? N11 Zr1 N51 B52 83.4(9) . . . . ? N21 Zr1 N51 B52 -3.1(9) . . . . ? Zr1 N51 B52 C61 80.7(10) . . . . ? Zr1 N51 B52 C71 -45.8(12) . . . . ? Zr1 N51 B52 C81 -166.6(6) . . . . ? N51 B52 C61 C66 -170.3(7) . . . . ? C71 B52 C61 C66 -49.7(11) . . . . ? C81 B52 C61 C66 70.1(9) . . . . ? N51 B52 C61 C62 17.8(12) . . . . ? C71 B52 C61 C62 138.3(8) . . . . ? C81 B52 C61 C62 -101.8(9) . . . . ? C66 C61 C62 C63 3.5(12) . . . . ? B52 C61 C62 C63 176.2(9) . . . . ? C66 C61 C62 F62 -177.8(7) . . . . ? B52 C61 C62 F62 -5.1(13) . . . . ? F62 C62 C63 F63 -0.7(12) . . . . ? C61 C62 C63 F63 178.1(8) . . . . ? F62 C62 C63 C64 179.0(8) . . . . ? C61 C62 C63 C64 -2.2(15) . . . . ? F63 C63 C64 F64 -1.4(14) . . . . ? C62 C63 C64 F64 178.9(8) . . . . ? F63 C63 C64 C65 180.0(7) . . . . ? C62 C63 C64 C65 0.3(14) . . . . ? F64 C64 C65 F65 1.1(13) . . . . ? C63 C64 C65 F65 179.7(8) . . . . ? F64 C64 C65 C66 -178.8(8) . . . . ? C63 C64 C65 C66 -0.1(13) . . . . ? F65 C65 C66 F66 3.1(11) . . . . ? C64 C65 C66 F66 -177.0(7) . . . . ? F65 C65 C66 C61 -177.9(8) . . . . ? C64 C65 C66 C61 2.0(13) . . . . ? C62 C61 C66 C65 -3.4(12) . . . . ? B52 C61 C66 C65 -176.6(8) . . . . ? C62 C61 C66 F66 175.5(6) . . . . ? B52 C61 C66 F66 2.4(11) . . . . ? N51 B52 C71 C72 110.1(9) . . . . ? C61 B52 C71 C72 -14.8(13) . . . . ? C81 B52 C71 C72 -128.6(9) . . . . ? N51 B52 C71 C76 -69.5(9) . . . . ? C61 B52 C71 C76 165.6(7) . . . . ? C81 B52 C71 C76 51.8(10) . . . . ? C76 C71 C72 F72 -179.4(7) . . . . ? B52 C71 C72 F72 1.0(13) . . . . ? C76 C71 C72 C73 2.1(13) . . . . ? B52 C71 C72 C73 -177.5(8) . . . . ? C71 C72 C73 F73 178.8(8) . . . . ? F72 C72 C73 F73 0.2(11) . . . . ? C71 C72 C73 C74 -2.7(13) . . . . ? F72 C72 C73 C74 178.7(7) . . . . ? F73 C73 C74 C75 178.6(8) . . . . ? C72 C73 C74 C75 0.2(13) . . . . ? F73 C73 C74 F74 0.1(12) . . . . ? C72 C73 C74 F74 -178.3(7) . . . . ? F74 C74 C75 F75 1.2(14) . . . . ? C73 C74 C75 F75 -177.2(8) . . . . ? F74 C74 C75 C76 -179.0(8) . . . . ? C73 C74 C75 C76 2.5(14) . . . . ? C72 C71 C76 F76 178.1(7) . . . . ? B52 C71 C76 F76 -2.3(12) . . . . ? C72 C71 C76 C75 0.9(13) . . . . ? B52 C71 C76 C75 -179.5(8) . . . . ? F75 C75 C76 F76 -0.7(12) . . . . ? C74 C75 C76 F76 179.5(8) . . . . ? F75 C75 C76 C71 176.6(8) . . . . ? C74 C75 C76 C71 -3.2(14) . . . . ? N51 B52 C81 C86 140.4(8) . . . . ? C61 B52 C81 C86 -99.4(9) . . . . ? C71 B52 C81 C86 23.5(13) . . . . ? N51 B52 C81 C82 -48.3(11) . . . . ? C61 B52 C81 C82 71.9(10) . . . . ? C71 B52 C81 C82 -165.3(8) . . . . ? C86 C81 C82 F82 176.2(8) . . . . ? B52 C81 C82 F82 3.7(12) . . . . ? C86 C81 C82 C83 -1.0(13) . . . . ? B52 C81 C82 C83 -173.4(9) . . . . ? F82 C82 C83 F83 3.3(13) . . . . ? C81 C82 C83 F83 -179.5(8) . . . . ? F82 C82 C83 C84 -176.6(8) . . . . ? C81 C82 C83 C84 0.6(15) . . . . ? F83 C83 C84 F84 -0.4(15) . . . . ? C82 C83 C84 F84 179.5(8) . . . . ? F83 C83 C84 C85 -179.4(9) . . . . ? C82 C83 C84 C85 0.5(15) . . . . ? C83 C84 C85 F85 178.9(9) . . . . ? F84 C84 C85 F85 -0.2(14) . . . . ? C83 C84 C85 C86 -1.0(15) . . . . ? F84 C84 C85 C86 180.0(8) . . . . ? F85 C85 C86 F86 -0.5(13) . . . . ? C84 C85 C86 F86 179.4(8) . . . . ? F85 C85 C86 C81 -179.3(8) . . . . ? C84 C85 C86 C81 0.5(15) . . . . ? C82 C81 C86 F86 -178.3(7) . . . . ? B52 C81 C86 F86 -6.4(13) . . . . ? C82 C81 C86 C85 0.4(13) . . . . ? B52 C81 C86 C85 172.4(9) . . . . ? C92B C91 C92A C93 -57.3(14) . . . . ? C92A C91 C92B C93 54.8(14) . . . . ? C91 C92A C93 C94B 133(3) . . . . ? C91 C92A C93 C94A -177.9(15) . . . . ? C91 C92A C93 C92B 55.5(14) . . . . ? C91 C92B C93 C94B 169(4) . . . . ? C91 C92B C93 C94A -131(2) . . . . ? C91 C92B C93 C92A -55.7(15) . . . . ? C94B C93 C94A C95 -48(3) . . . . ? C92A C93 C94A C95 171.2(15) . . . . ? C92B C93 C94A C95 -147.8(18) . . . . ? C94A C93 C94B C95 48(3) . . . . ? C92A C93 C94B C95 119(4) . . . . ? C92B C93 C94B C95 165(3) . . . . ? C93 C94A C95 C94B 47(3) . . . . ? C93 C94B C95 C94A -48(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N51 H51A F62 0.90 2.12 2.773(8) 129.0 . N51 H51A F82 0.90 2.24 2.883(8) 127.9 . _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.628 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.097 #===END