# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Douglas W Stephan' 'Preston A. Chase' 'Thomas M. Gilbert' 'Austin L. Gille' _publ_contact_author_name 'Douglas W Stephan' _publ_contact_author_email DSTEPHAN@CHEM.UTORONTO.CA _publ_section_title ; Frustrated Lewis Pairs Derived from N-Heterocyclic Carbenes and Lewis Acids ; # Attachment 'CIFs-revised.txt' data_C3H2(NiPr2C6H3)2.B(C6F5)3 _database_code_depnum_ccdc_archive 'CCDC 689780' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C45 H36 B F15 N2' _chemical_formula_weight 900.57 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' _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 9.1610(11) _cell_length_b 11.9932(14) _cell_length_c 19.725(2) _cell_angle_alpha 78.645(2) _cell_angle_beta 85.995(2) _cell_angle_gamma 75.689(2) _cell_volume 2058.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 0.132 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.786132 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 19967 _diffrn_reflns_av_R_equivalents 0.0616 _diffrn_reflns_av_sigmaI/netI 0.0864 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7218 _reflns_number_gt 3372 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0756P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7218 _refine_ls_number_parameters 568 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1382 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1160 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.890 _refine_ls_shift/su_max 0.000 _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 B1 B 0.0776(4) 0.2391(3) 0.2497(2) 0.0460(10) Uani 1 1 d . . . N1 N 0.3681(3) 0.1957(2) 0.20357(15) 0.0506(7) Uani 1 1 d . . . N2 N 0.3236(3) 0.3283(2) 0.26700(13) 0.0443(7) Uani 1 1 d . . . F1 F 0.3097(2) 0.09087(17) 0.35831(11) 0.0756(6) Uani 1 1 d . . . F2 F 0.2649(3) -0.0793(2) 0.45675(14) 0.1216(10) Uani 1 1 d . . . F3 F -0.0028(3) -0.1405(2) 0.47318(14) 0.1249(10) Uani 1 1 d . . . F4 F -0.2312(3) -0.0181(2) 0.38669(14) 0.1133(9) Uani 1 1 d . . . F5 F -0.1882(2) 0.15209(19) 0.28526(11) 0.0754(7) Uani 1 1 d . . . F6 F 0.0424(2) 0.00852(19) 0.21319(13) 0.0797(7) Uani 1 1 d . . . F7 F -0.0613(3) -0.0147(2) 0.09818(14) 0.1073(9) Uani 1 1 d . . . F8 F -0.1279(3) 0.1689(2) -0.00945(13) 0.1055(9) Uani 1 1 d . . . F9 F -0.0893(3) 0.3799(2) 0.00408(12) 0.0896(8) Uani 1 1 d . . . F10 F 0.0240(2) 0.40526(17) 0.11847(10) 0.0622(6) Uani 1 1 d . . . F11 F -0.2232(2) 0.40994(18) 0.18596(11) 0.0671(6) Uani 1 1 d . . . F12 F -0.3950(2) 0.57596(19) 0.24137(12) 0.0880(8) Uani 1 1 d . . . F13 F -0.3412(3) 0.6084(2) 0.36887(13) 0.1028(8) Uani 1 1 d . . . F14 F -0.1012(3) 0.4617(2) 0.43972(12) 0.0922(8) Uani 1 1 d . . . F15 F 0.0794(2) 0.29605(17) 0.38420(9) 0.0611(6) Uani 1 1 d . . . C1 C 0.0666(4) 0.1278(3) 0.31349(18) 0.0485(9) Uani 1 1 d . . . C2 C 0.1729(4) 0.0650(3) 0.3605(2) 0.0592(10) Uani 1 1 d . . . C3 C 0.1516(6) -0.0234(4) 0.4133(2) 0.0794(13) Uani 1 1 d . . . C4 C 0.0176(6) -0.0537(4) 0.4222(2) 0.0851(14) Uani 1 1 d . . . C5 C -0.0951(5) 0.0086(4) 0.3786(3) 0.0785(13) Uani 1 1 d . . . C6 C -0.0699(4) 0.0959(3) 0.3264(2) 0.0595(10) Uani 1 1 d . . . C7 C 0.0298(3) 0.2118(3) 0.17584(18) 0.0477(9) Uani 1 1 d . . . C8 C 0.0093(4) 0.1071(3) 0.1637(2) 0.0607(10) Uani 1 1 d . . . C9 C -0.0444(5) 0.0910(4) 0.1037(3) 0.0727(12) Uani 1 1 d . . . C10 C -0.0771(4) 0.1826(5) 0.0500(2) 0.0729(12) Uani 1 1 d . . . C11 C -0.0568(4) 0.2884(4) 0.0571(2) 0.0642(11) Uani 1 1 d . . . C12 C -0.0001(4) 0.2990(3) 0.1176(2) 0.0527(9) Uani 1 1 d . . . C13 C -0.0458(3) 0.3494(3) 0.27743(17) 0.0429(8) Uani 1 1 d . . . C14 C -0.1765(4) 0.4221(3) 0.24710(18) 0.0490(9) Uani 1 1 d . . . C15 C -0.2726(4) 0.5091(3) 0.2759(2) 0.0599(10) Uani 1 1 d . . . C16 C -0.2467(5) 0.5254(3) 0.3400(2) 0.0660(11) Uani 1 1 d . . . C17 C -0.1264(4) 0.4525(4) 0.3747(2) 0.0602(10) Uani 1 1 d . . . C18 C -0.0332(4) 0.3683(3) 0.34403(19) 0.0501(9) Uani 1 1 d . . . C19 C 0.2539(4) 0.2594(3) 0.23925(17) 0.0428(8) Uani 1 1 d . . . C20 C 0.5034(4) 0.2200(3) 0.2131(2) 0.0604(10) Uani 1 1 d . . . H20A H 0.5970 0.1851 0.1959 0.073 Uiso 1 1 calc R . . C21 C 0.4759(4) 0.3020(3) 0.25137(19) 0.0580(10) Uani 1 1 d . . . H21A H 0.5468 0.3360 0.2653 0.070 Uiso 1 1 calc R . . C22 C 0.3631(4) 0.1211(3) 0.1532(2) 0.0582(10) Uani 1 1 d . . . C23 C 0.3923(4) -0.0003(4) 0.1765(3) 0.0766(13) Uani 1 1 d . . . C24 C 0.3772(5) -0.0661(4) 0.1263(4) 0.1032(19) Uani 1 1 d . . . H24A H 0.3901 -0.1468 0.1390 0.124 Uiso 1 1 calc R . . C25 C 0.3440(6) -0.0129(6) 0.0598(4) 0.113(2) Uani 1 1 d . . . H25A H 0.3291 -0.0574 0.0285 0.136 Uiso 1 1 calc R . . C26 C 0.3321(5) 0.1045(5) 0.0379(3) 0.0930(15) Uani 1 1 d . . . H26A H 0.3140 0.1373 -0.0084 0.112 Uiso 1 1 calc R . . C27 C 0.3465(4) 0.1747(4) 0.0831(2) 0.0648(11) Uani 1 1 d . . . C28 C 0.4535(5) -0.0602(4) 0.2468(3) 0.0960(15) Uani 1 1 d . . . H28A H 0.4369 -0.0009 0.2762 0.115 Uiso 1 1 calc R . . C29 C 0.3769(6) -0.1575(4) 0.2827(3) 0.126(2) Uani 1 1 d . . . H29A H 0.4189 -0.1905 0.3276 0.189 Uiso 1 1 calc R . . H29B H 0.3932 -0.2175 0.2554 0.189 Uiso 1 1 calc R . . H29C H 0.2706 -0.1252 0.2877 0.189 Uiso 1 1 calc R . . C30 C 0.6251(5) -0.1118(4) 0.2412(3) 0.140(2) Uani 1 1 d . . . H30A H 0.6740 -0.0503 0.2215 0.210 Uiso 1 1 calc R . . H30B H 0.6443 -0.1697 0.2122 0.210 Uiso 1 1 calc R . . H30C H 0.6635 -0.1475 0.2864 0.210 Uiso 1 1 calc R . . C31 C 0.3585(5) 0.2994(4) 0.0561(2) 0.0738(12) Uani 1 1 d . . . H31A H 0.3150 0.3468 0.0910 0.089 Uiso 1 1 calc R . . C32 C 0.2818(6) 0.3573(5) -0.0121(2) 0.1222(19) Uani 1 1 d . . . H32A H 0.1764 0.3585 -0.0073 0.183 Uiso 1 1 calc R . . H32B H 0.3266 0.3138 -0.0474 0.183 Uiso 1 1 calc R . . H32C H 0.2939 0.4360 -0.0248 0.183 Uiso 1 1 calc R . . C33 C 0.5250(5) 0.3032(4) 0.0439(2) 0.1000(15) Uani 1 1 d . . . H33A H 0.5788 0.2692 0.0860 0.150 Uiso 1 1 calc R . . H33B H 0.5321 0.3831 0.0298 0.150 Uiso 1 1 calc R . . H33C H 0.5682 0.2598 0.0084 0.150 Uiso 1 1 calc R . . C34 C 0.2701(4) 0.4223(3) 0.30654(17) 0.0476(9) Uani 1 1 d . . . C35 C 0.1917(4) 0.5322(3) 0.27133(18) 0.0522(9) Uani 1 1 d . . . C36 C 0.1515(5) 0.6218(3) 0.3091(2) 0.0755(12) Uani 1 1 d . . . H36A H 0.0968 0.6952 0.2881 0.091 Uiso 1 1 calc R . . C37 C 0.1911(6) 0.6038(4) 0.3770(2) 0.0927(15) Uani 1 1 d . . . H37A H 0.1613 0.6646 0.4016 0.111 Uiso 1 1 calc R . . C38 C 0.2735(6) 0.4977(4) 0.4084(2) 0.0821(13) Uani 1 1 d . . . H38A H 0.3015 0.4883 0.4540 0.098 Uiso 1 1 calc R . . C39 C 0.3168(4) 0.4039(3) 0.37483(19) 0.0589(10) Uani 1 1 d . . . C40 C 0.1610(4) 0.5570(3) 0.19446(18) 0.0565(10) Uani 1 1 d . . . H40A H 0.1468 0.4846 0.1829 0.068 Uiso 1 1 calc R . . C41 C 0.0192(5) 0.6522(3) 0.1734(2) 0.0837(13) Uani 1 1 d . . . H41A H -0.0658 0.6318 0.1996 0.126 Uiso 1 1 calc R . . H41B H 0.0031 0.6595 0.1250 0.126 Uiso 1 1 calc R . . H41C H 0.0308 0.7254 0.1823 0.126 Uiso 1 1 calc R . . C42 C 0.2974(5) 0.5863(4) 0.15231(19) 0.0840(13) Uani 1 1 d . . . H42A H 0.3854 0.5249 0.1656 0.126 Uiso 1 1 calc R . . H42B H 0.3119 0.6588 0.1609 0.126 Uiso 1 1 calc R . . H42C H 0.2805 0.5935 0.1040 0.126 Uiso 1 1 calc R . . C43 C 0.4149(4) 0.2893(4) 0.41206(19) 0.0698(12) Uani 1 1 d . . . H43A H 0.4239 0.2303 0.3830 0.084 Uiso 1 1 calc R . . C44 C 0.3488(5) 0.2437(4) 0.4825(2) 0.0987(16) Uani 1 1 d . . . H44A H 0.2511 0.2317 0.4765 0.148 Uiso 1 1 calc R . . H44B H 0.3398 0.3000 0.5120 0.148 Uiso 1 1 calc R . . H44C H 0.4141 0.1709 0.5032 0.148 Uiso 1 1 calc R . . C45 C 0.5741(5) 0.3036(4) 0.4218(2) 0.0981(15) Uani 1 1 d . . . H45A H 0.6176 0.3290 0.3775 0.147 Uiso 1 1 calc R . . H45B H 0.6358 0.2299 0.4435 0.147 Uiso 1 1 calc R . . H45C H 0.5681 0.3608 0.4504 0.147 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.035(2) 0.045(2) 0.059(3) -0.015(2) -0.0029(19) -0.0068(19) N1 0.0387(17) 0.0450(17) 0.071(2) -0.0185(16) 0.0017(15) -0.0100(14) N2 0.0387(17) 0.0436(17) 0.0530(18) -0.0065(14) -0.0033(14) -0.0157(14) F1 0.0562(14) 0.0657(14) 0.0967(17) 0.0082(12) -0.0227(12) -0.0118(11) F2 0.123(2) 0.094(2) 0.119(2) 0.0402(17) -0.0356(19) -0.0114(17) F3 0.164(3) 0.0855(19) 0.118(2) 0.0212(17) 0.0246(19) -0.0546(19) F4 0.102(2) 0.121(2) 0.133(2) -0.0162(18) 0.0323(17) -0.0706(18) F5 0.0440(13) 0.0850(16) 0.1005(17) -0.0152(14) -0.0025(12) -0.0229(12) F6 0.0837(16) 0.0573(15) 0.1051(18) -0.0290(14) 0.0066(14) -0.0209(12) F7 0.111(2) 0.1010(19) 0.142(2) -0.0794(18) 0.0133(17) -0.0459(16) F8 0.0978(19) 0.152(2) 0.0929(18) -0.0754(18) -0.0080(15) -0.0351(17) F9 0.0962(18) 0.112(2) 0.0616(15) -0.0209(15) -0.0227(13) -0.0175(15) F10 0.0690(14) 0.0604(14) 0.0602(13) -0.0131(11) -0.0099(10) -0.0171(11) F11 0.0486(12) 0.0760(14) 0.0744(15) -0.0261(12) -0.0151(11) 0.0028(10) F12 0.0575(14) 0.0720(15) 0.122(2) -0.0286(14) -0.0196(14) 0.0205(12) F13 0.0911(18) 0.0924(18) 0.123(2) -0.0610(17) 0.0106(15) 0.0110(15) F14 0.0954(18) 0.115(2) 0.0720(16) -0.0463(15) 0.0056(13) -0.0145(15) F15 0.0599(13) 0.0649(13) 0.0573(13) -0.0092(11) -0.0083(11) -0.0126(11) C1 0.040(2) 0.043(2) 0.066(2) -0.0146(19) -0.0006(19) -0.0108(17) C2 0.048(2) 0.049(2) 0.079(3) -0.002(2) -0.006(2) -0.016(2) C3 0.086(3) 0.052(3) 0.087(3) 0.013(2) -0.012(3) -0.009(3) C4 0.112(4) 0.056(3) 0.085(3) 0.006(3) 0.017(3) -0.036(3) C5 0.077(3) 0.075(3) 0.092(4) -0.013(3) 0.019(3) -0.042(3) C6 0.049(2) 0.055(2) 0.075(3) -0.011(2) 0.000(2) -0.014(2) C7 0.0319(19) 0.050(2) 0.066(3) -0.021(2) 0.0016(17) -0.0094(17) C8 0.052(2) 0.052(3) 0.082(3) -0.024(2) 0.008(2) -0.014(2) C9 0.063(3) 0.081(3) 0.097(4) -0.061(3) 0.010(3) -0.028(3) C10 0.055(3) 0.108(4) 0.070(3) -0.050(3) 0.002(2) -0.022(3) C11 0.055(3) 0.082(3) 0.062(3) -0.030(3) -0.003(2) -0.015(2) C12 0.046(2) 0.055(3) 0.063(3) -0.027(2) -0.0023(19) -0.0102(19) C13 0.038(2) 0.042(2) 0.050(2) -0.0094(17) -0.0018(17) -0.0096(17) C14 0.045(2) 0.048(2) 0.055(2) -0.0120(19) -0.0031(19) -0.0104(19) C15 0.043(2) 0.049(2) 0.083(3) -0.018(2) -0.003(2) 0.003(2) C16 0.060(3) 0.054(3) 0.085(3) -0.035(2) 0.011(2) -0.002(2) C17 0.059(3) 0.070(3) 0.058(3) -0.028(2) 0.008(2) -0.017(2) C18 0.038(2) 0.051(2) 0.059(2) -0.007(2) -0.0026(19) -0.0097(18) C19 0.039(2) 0.0376(19) 0.051(2) -0.0101(17) -0.0024(17) -0.0065(16) C20 0.033(2) 0.065(3) 0.087(3) -0.022(2) -0.0007(19) -0.0129(19) C21 0.041(2) 0.062(3) 0.077(3) -0.017(2) -0.005(2) -0.0197(19) C22 0.033(2) 0.053(3) 0.097(3) -0.038(2) 0.011(2) -0.0103(18) C23 0.055(3) 0.055(3) 0.124(4) -0.036(3) 0.025(3) -0.013(2) C24 0.084(4) 0.069(3) 0.177(6) -0.069(4) 0.058(4) -0.035(3) C25 0.087(4) 0.131(6) 0.160(6) -0.102(5) 0.045(4) -0.053(4) C26 0.072(3) 0.117(4) 0.113(4) -0.072(4) 0.024(3) -0.033(3) C27 0.041(2) 0.079(3) 0.084(3) -0.043(3) 0.010(2) -0.012(2) C28 0.083(4) 0.047(3) 0.150(5) -0.021(3) 0.023(3) -0.007(2) C29 0.103(4) 0.060(3) 0.198(6) -0.012(4) 0.035(4) -0.007(3) C30 0.076(4) 0.092(4) 0.233(7) -0.012(4) 0.001(4) 0.001(3) C31 0.069(3) 0.078(3) 0.074(3) -0.025(2) 0.004(2) -0.009(2) C32 0.095(4) 0.165(5) 0.090(4) -0.009(4) -0.001(3) -0.013(4) C33 0.091(4) 0.104(4) 0.113(4) -0.025(3) 0.019(3) -0.041(3) C34 0.059(2) 0.042(2) 0.046(2) -0.0097(18) 0.0025(18) -0.0195(18) C35 0.061(2) 0.047(2) 0.053(2) -0.0123(19) -0.0009(19) -0.0191(19) C36 0.107(4) 0.054(3) 0.069(3) -0.022(2) -0.002(3) -0.018(2) C37 0.140(5) 0.072(3) 0.075(3) -0.036(3) 0.009(3) -0.028(3) C38 0.125(4) 0.080(3) 0.054(3) -0.020(3) -0.005(3) -0.042(3) C39 0.071(3) 0.063(3) 0.050(2) -0.007(2) -0.004(2) -0.033(2) C40 0.062(3) 0.047(2) 0.062(3) -0.0046(19) -0.013(2) -0.017(2) C41 0.083(3) 0.069(3) 0.086(3) 0.007(2) -0.014(3) -0.007(2) C42 0.084(3) 0.109(4) 0.057(3) 0.001(3) -0.005(2) -0.031(3) C43 0.077(3) 0.079(3) 0.054(3) 0.009(2) -0.017(2) -0.034(2) C44 0.107(4) 0.122(4) 0.067(3) 0.024(3) -0.020(3) -0.055(3) C45 0.086(3) 0.121(4) 0.087(3) 0.014(3) -0.026(3) -0.043(3) _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 B1 C1 1.661(5) . ? B1 C7 1.664(5) . ? B1 C13 1.669(5) . ? B1 C19 1.685(5) . ? N1 C19 1.374(4) . ? N1 C20 1.375(4) . ? N1 C22 1.472(4) . ? N2 C19 1.370(4) . ? N2 C21 1.379(4) . ? N2 C34 1.463(4) . ? F1 C2 1.359(4) . ? F2 C3 1.348(5) . ? F3 C4 1.337(4) . ? F4 C5 1.354(5) . ? F5 C6 1.354(4) . ? F6 C8 1.362(4) . ? F7 C9 1.341(4) . ? F8 C10 1.345(4) . ? F9 C11 1.348(4) . ? F10 C12 1.349(4) . ? F11 C14 1.353(4) . ? F12 C15 1.346(4) . ? F13 C16 1.339(4) . ? F14 C17 1.349(4) . ? F15 C18 1.358(4) . ? C1 C2 1.365(5) . ? C1 C6 1.389(5) . ? C2 C3 1.373(5) . ? C3 C4 1.354(6) . ? C4 C5 1.362(6) . ? C5 C6 1.368(5) . ? C7 C8 1.381(5) . ? C7 C12 1.384(5) . ? C8 C9 1.378(5) . ? C9 C10 1.358(6) . ? C10 C11 1.361(5) . ? C11 C12 1.375(5) . ? C13 C14 1.389(4) . ? C13 C18 1.394(4) . ? C14 C15 1.377(5) . ? C15 C16 1.361(5) . ? C16 C17 1.357(5) . ? C17 C18 1.363(5) . ? C20 C21 1.320(4) . ? C22 C23 1.402(5) . ? C22 C27 1.406(5) . ? C23 C24 1.414(6) . ? C23 C28 1.508(6) . ? C24 C25 1.361(7) . ? C25 C26 1.368(7) . ? C26 C27 1.374(5) . ? C27 C31 1.514(5) . ? C28 C29 1.538(6) . ? C28 C30 1.546(6) . ? C31 C32 1.520(5) . ? C31 C33 1.538(5) . ? C34 C39 1.401(4) . ? C34 C35 1.406(4) . ? C35 C36 1.388(5) . ? C35 C40 1.519(4) . ? C36 C37 1.374(5) . ? C37 C38 1.361(5) . ? C38 C39 1.378(5) . ? C39 C43 1.524(5) . ? C40 C41 1.523(5) . ? C40 C42 1.527(5) . ? C43 C44 1.531(5) . ? C43 C45 1.539(5) . ? 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 C1 B1 C7 109.6(3) . . ? C1 B1 C13 101.3(3) . . ? C7 B1 C13 113.4(3) . . ? C1 B1 C19 111.5(3) . . ? C7 B1 C19 107.8(3) . . ? C13 B1 C19 113.1(3) . . ? C19 N1 C20 110.7(3) . . ? C19 N1 C22 130.6(3) . . ? C20 N1 C22 118.3(3) . . ? C19 N2 C21 110.2(3) . . ? C19 N2 C34 133.8(3) . . ? C21 N2 C34 116.0(3) . . ? C2 C1 C6 112.4(3) . . ? C2 C1 B1 128.8(3) . . ? C6 C1 B1 118.6(3) . . ? F1 C2 C1 120.0(3) . . ? F1 C2 C3 115.3(4) . . ? C1 C2 C3 124.6(4) . . ? F2 C3 C4 120.0(4) . . ? F2 C3 C2 119.4(4) . . ? C4 C3 C2 120.6(4) . . ? F3 C4 C3 120.6(5) . . ? F3 C4 C5 121.7(5) . . ? C3 C4 C5 117.7(4) . . ? F4 C5 C4 119.4(4) . . ? F4 C5 C6 120.4(4) . . ? C4 C5 C6 120.2(4) . . ? F5 C6 C5 115.9(4) . . ? F5 C6 C1 119.7(3) . . ? C5 C6 C1 124.4(4) . . ? C8 C7 C12 111.3(3) . . ? C8 C7 B1 127.3(3) . . ? C12 C7 B1 121.3(3) . . ? F6 C8 C9 114.1(4) . . ? F6 C8 C7 120.4(4) . . ? C9 C8 C7 125.5(4) . . ? F7 C9 C10 120.6(4) . . ? F7 C9 C8 120.2(5) . . ? C10 C9 C8 119.3(4) . . ? F8 C10 C9 120.5(4) . . ? F8 C10 C11 120.6(5) . . ? C9 C10 C11 119.0(4) . . ? F9 C11 C10 119.3(4) . . ? F9 C11 C12 121.3(4) . . ? C10 C11 C12 119.3(4) . . ? F10 C12 C11 115.1(4) . . ? F10 C12 C7 119.6(3) . . ? C11 C12 C7 125.3(4) . . ? C14 C13 C18 110.7(3) . . ? C14 C13 B1 129.8(3) . . ? C18 C13 B1 119.0(3) . . ? F11 C14 C15 113.6(3) . . ? F11 C14 C13 121.6(3) . . ? C15 C14 C13 124.7(3) . . ? F12 C15 C16 119.9(3) . . ? F12 C15 C14 119.7(4) . . ? C16 C15 C14 120.3(4) . . ? F13 C16 C17 121.1(4) . . ? F13 C16 C15 120.6(4) . . ? C17 C16 C15 118.3(4) . . ? F14 C17 C16 120.2(4) . . ? F14 C17 C18 120.3(4) . . ? C16 C17 C18 119.6(4) . . ? F15 C18 C17 115.1(3) . . ? F15 C18 C13 118.7(3) . . ? C17 C18 C13 126.2(3) . . ? N2 C19 N1 103.6(3) . . ? N2 C19 B1 131.6(3) . . ? N1 C19 B1 124.4(3) . . ? C21 C20 N1 107.4(3) . . ? C20 C21 N2 108.0(3) . . ? C23 C22 C27 123.6(4) . . ? C23 C22 N1 118.2(4) . . ? C27 C22 N1 117.8(3) . . ? C22 C23 C24 115.2(5) . . ? C22 C23 C28 123.5(4) . . ? C24 C23 C28 120.9(5) . . ? C25 C24 C23 120.8(5) . . ? C24 C25 C26 121.7(5) . . ? C25 C26 C27 121.2(5) . . ? C26 C27 C22 116.4(4) . . ? C26 C27 C31 120.2(5) . . ? C22 C27 C31 123.1(3) . . ? C23 C28 C29 113.7(4) . . ? C23 C28 C30 110.1(4) . . ? C29 C28 C30 109.3(4) . . ? C27 C31 C32 115.3(4) . . ? C27 C31 C33 110.0(3) . . ? C32 C31 C33 105.9(4) . . ? C39 C34 C35 122.7(3) . . ? C39 C34 N2 118.6(3) . . ? C35 C34 N2 118.1(3) . . ? C36 C35 C34 116.8(3) . . ? C36 C35 C40 120.2(3) . . ? C34 C35 C40 122.8(3) . . ? C37 C36 C35 121.1(4) . . ? C38 C37 C36 120.5(4) . . ? C37 C38 C39 122.1(4) . . ? C38 C39 C34 116.7(4) . . ? C38 C39 C43 119.3(4) . . ? C34 C39 C43 123.9(4) . . ? C35 C40 C41 114.0(3) . . ? C35 C40 C42 110.5(3) . . ? C41 C40 C42 110.5(3) . . ? C39 C43 C44 113.0(4) . . ? C39 C43 C45 110.4(3) . . ? C44 C43 C45 109.2(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.177 _refine_diff_density_min -0.162 _refine_diff_density_rms 0.038 #===end data_Et2NHB(C6F5)3.0.5(C6H14) _database_code_depnum_ccdc_archive 'CCDC 689781' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C23.50 H13.50 B F15 N' _chemical_formula_weight 605.66 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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7771(12) _cell_length_b 12.3780(14) _cell_length_c 19.156(2) _cell_angle_alpha 72.8740(10) _cell_angle_beta 74.3570(10) _cell_angle_gamma 85.354(2) _cell_volume 2351.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.711 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1206 _exptl_absorpt_coefficient_mu 0.183 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.841584 _exptl_absorpt_correction_T_max 1.000000 _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 22668 _diffrn_reflns_av_R_equivalents 0.0662 _diffrn_reflns_av_sigmaI/netI 0.0979 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8258 _reflns_number_gt 4504 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 8258 _refine_ls_number_parameters 730 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1179 _refine_ls_R_factor_gt 0.0533 _refine_ls_wR_factor_ref 0.1597 _refine_ls_wR_factor_gt 0.1231 _refine_ls_goodness_of_fit_ref 0.820 _refine_ls_restrained_S_all 0.820 _refine_ls_shift/su_max 0.000 _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 B1 B 0.8566(4) 0.2536(4) 0.2932(2) 0.0235(10) Uani 1 1 d . . . B2 B 0.4280(4) 0.8227(4) 0.2381(2) 0.0223(10) Uani 1 1 d . . . N1 N 0.7764(3) 0.3179(3) 0.35609(17) 0.0240(7) Uani 1 1 d . . . N2 N 0.3962(3) 0.8648(3) 0.15529(17) 0.0240(7) Uani 1 1 d . . . F1 F 0.8411(3) 0.10009(19) 0.19901(13) 0.0451(7) Uani 1 1 d . . . F2 F 0.7517(3) 0.1551(2) 0.07825(15) 0.0621(8) Uani 1 1 d . . . F3 F 0.6484(3) 0.3621(2) 0.03047(15) 0.0641(9) Uani 1 1 d . . . F4 F 0.6408(2) 0.5166(2) 0.10711(14) 0.0493(7) Uani 1 1 d . . . F5 F 0.7339(2) 0.46625(19) 0.22769(13) 0.0371(6) Uani 1 1 d . . . F6 F 1.0792(2) 0.1547(2) 0.20947(14) 0.0470(7) Uani 1 1 d . . . F7 F 1.2970(2) 0.2545(3) 0.12287(15) 0.0622(8) Uani 1 1 d . . . F8 F 1.3452(2) 0.4712(3) 0.11216(15) 0.0648(9) Uani 1 1 d . . . F9 F 1.1605(2) 0.5892(2) 0.18767(14) 0.0504(7) Uani 1 1 d . . . F10 F 0.9450(2) 0.49246(19) 0.27694(13) 0.0397(6) Uani 1 1 d . . . F11 F 0.6585(2) 0.07766(18) 0.33062(13) 0.0378(6) Uani 1 1 d . . . F12 F 0.6608(2) -0.13304(19) 0.41401(14) 0.0461(7) Uani 1 1 d . . . F13 F 0.8626(3) -0.2146(2) 0.47462(14) 0.0515(7) Uani 1 1 d . . . F14 F 1.0628(2) -0.0761(2) 0.44866(13) 0.0428(6) Uani 1 1 d . . . F15 F 1.0649(2) 0.13513(19) 0.36505(13) 0.0371(6) Uani 1 1 d . . . F16 F 0.5529(2) 0.6807(2) 0.35213(13) 0.0412(6) Uani 1 1 d . . . F17 F 0.7985(2) 0.6755(2) 0.34951(16) 0.0610(8) Uani 1 1 d . . . F18 F 0.9739(2) 0.7993(3) 0.22737(19) 0.0758(10) Uani 1 1 d . . . F19 F 0.8933(2) 0.9278(2) 0.10553(16) 0.0583(8) Uani 1 1 d . . . F20 F 0.6486(2) 0.9312(2) 0.10435(13) 0.0385(6) Uani 1 1 d . . . F21 F 0.15431(19) 0.80004(17) 0.33368(12) 0.0298(5) Uani 1 1 d . . . F22 F 0.0231(2) 0.61132(19) 0.40300(13) 0.0377(6) Uani 1 1 d . . . F23 F 0.1305(2) 0.40824(19) 0.39123(15) 0.0492(7) Uani 1 1 d . . . F24 F 0.3758(2) 0.40233(18) 0.30574(15) 0.0490(7) Uani 1 1 d . . . F25 F 0.5128(2) 0.58789(18) 0.23958(13) 0.0375(6) Uani 1 1 d . . . F26 F 0.4605(2) 1.06873(17) 0.16573(12) 0.0379(6) Uani 1 1 d . . . F27 F 0.4385(2) 1.22922(17) 0.23420(13) 0.0436(7) Uani 1 1 d . . . F28 F 0.3654(2) 1.17625(18) 0.38845(13) 0.0418(6) Uani 1 1 d . . . F29 F 0.3216(2) 0.95818(18) 0.47017(12) 0.0398(6) Uani 1 1 d . . . F30 F 0.3412(2) 0.79649(17) 0.40448(12) 0.0324(6) Uani 1 1 d . . . C1 C 0.7864(4) 0.2784(3) 0.2234(2) 0.0260(9) Uani 1 1 d . . . C2 C 0.7895(4) 0.2049(3) 0.1806(2) 0.0320(10) Uani 1 1 d . . . C3 C 0.7434(4) 0.2316(4) 0.1168(2) 0.0408(12) Uani 1 1 d . . . C4 C 0.6912(4) 0.3365(4) 0.0923(2) 0.0398(11) Uani 1 1 d . . . C5 C 0.6874(4) 0.4129(4) 0.1312(2) 0.0332(10) Uani 1 1 d . . . C6 C 0.7354(4) 0.3836(3) 0.1943(2) 0.0283(10) Uani 1 1 d . . . C7 C 0.9986(4) 0.3162(3) 0.2500(2) 0.0261(9) Uani 1 1 d . . . C8 C 1.0951(4) 0.2625(4) 0.2077(2) 0.0330(10) Uani 1 1 d . . . C9 C 1.2092(4) 0.3122(4) 0.1620(2) 0.0409(12) Uani 1 1 d . . . C10 C 1.2341(4) 0.4221(4) 0.1558(2) 0.0415(12) Uani 1 1 d . . . C11 C 1.1408(4) 0.4804(4) 0.1945(2) 0.0349(11) Uani 1 1 d . . . C12 C 1.0285(4) 0.4272(4) 0.2405(2) 0.0307(10) Uani 1 1 d . . . C13 C 0.8630(4) 0.1201(3) 0.3407(2) 0.0257(9) Uani 1 1 d . . . C14 C 0.7638(4) 0.0434(3) 0.3574(2) 0.0271(9) Uani 1 1 d . . . C15 C 0.7618(4) -0.0667(3) 0.4001(2) 0.0304(10) Uani 1 1 d . . . C16 C 0.8632(4) -0.1081(3) 0.4310(2) 0.0335(10) Uani 1 1 d . . . C17 C 0.9640(4) -0.0374(4) 0.4177(2) 0.0308(10) Uani 1 1 d . . . C18 C 0.9619(4) 0.0724(3) 0.3740(2) 0.0270(9) Uani 1 1 d . . . C19 C 0.6353(4) 0.2834(3) 0.3863(2) 0.0324(10) Uani 1 1 d . . . H19A H 0.6021 0.2804 0.3434 0.039 Uiso 1 1 calc R . . H19B H 0.6294 0.2062 0.4215 0.039 Uiso 1 1 calc R . . C20 C 0.5499(4) 0.3606(4) 0.4266(3) 0.0442(12) Uani 1 1 d . . . H20A H 0.4613 0.3321 0.4445 0.066 Uiso 1 1 calc R . . H20B H 0.5522 0.4368 0.3917 0.066 Uiso 1 1 calc R . . H20C H 0.5805 0.3630 0.4698 0.066 Uiso 1 1 calc R . . C21 C 0.8430(4) 0.3013(3) 0.4188(2) 0.0274(9) Uani 1 1 d . . . H21A H 0.8124 0.2295 0.4578 0.033 Uiso 1 1 calc R . . H21B H 0.9367 0.2934 0.3977 0.033 Uiso 1 1 calc R . . C22 C 0.8222(4) 0.3944(4) 0.4564(2) 0.0392(11) Uani 1 1 d . . . H22A H 0.8684 0.3765 0.4960 0.059 Uiso 1 1 calc R . . H22B H 0.7299 0.4018 0.4789 0.059 Uiso 1 1 calc R . . H22C H 0.8547 0.4657 0.4188 0.059 Uiso 1 1 calc R . . C23 C 0.5851(3) 0.8057(3) 0.2288(2) 0.0241(9) Uani 1 1 d . . . C24 C 0.6332(4) 0.7428(3) 0.2882(2) 0.0308(10) Uani 1 1 d . . . C25 C 0.7601(4) 0.7388(4) 0.2891(3) 0.0393(11) Uani 1 1 d . . . C26 C 0.8492(4) 0.8009(4) 0.2272(3) 0.0472(13) Uani 1 1 d . . . C27 C 0.8089(4) 0.8652(4) 0.1665(3) 0.0420(12) Uani 1 1 d . . . C28 C 0.6798(4) 0.8656(3) 0.1679(2) 0.0283(9) Uani 1 1 d . . . C29 C 0.3432(3) 0.7059(3) 0.2836(2) 0.0193(8) Uani 1 1 d . . . C30 C 0.2165(3) 0.7031(3) 0.3257(2) 0.0230(9) Uani 1 1 d . . . C31 C 0.1450(4) 0.6060(3) 0.3620(2) 0.0277(9) Uani 1 1 d . . . C32 C 0.1987(4) 0.5039(3) 0.3566(2) 0.0309(10) Uani 1 1 d . . . C33 C 0.3220(4) 0.5008(3) 0.3144(2) 0.0308(10) Uani 1 1 d . . . C34 C 0.3910(4) 0.6002(3) 0.2793(2) 0.0256(9) Uani 1 1 d . . . C35 C 0.3955(3) 0.9233(3) 0.2806(2) 0.0210(9) Uani 1 1 d . . . C36 C 0.4197(4) 1.0370(3) 0.2423(2) 0.0252(9) Uani 1 1 d . . . C37 C 0.4097(4) 1.1222(3) 0.2762(2) 0.0265(9) Uani 1 1 d . . . C38 C 0.3747(4) 1.0957(3) 0.3533(2) 0.0267(9) Uani 1 1 d . . . C39 C 0.3519(4) 0.9855(3) 0.3946(2) 0.0263(9) Uani 1 1 d . . . C40 C 0.3630(3) 0.9028(3) 0.3582(2) 0.0223(9) Uani 1 1 d . . . C41 C 0.4387(4) 0.7782(3) 0.1115(2) 0.0345(10) Uani 1 1 d . . . H41A H 0.5146 0.7371 0.1262 0.041 Uiso 1 1 calc R . . H41B H 0.3686 0.7224 0.1265 0.041 Uiso 1 1 calc R . . C42 C 0.4724(5) 0.8265(4) 0.0273(2) 0.0516(13) Uani 1 1 d . . . H42A H 0.4986 0.7654 0.0035 0.077 Uiso 1 1 calc R . . H42B H 0.5435 0.8803 0.0115 0.077 Uiso 1 1 calc R . . H42C H 0.3972 0.8656 0.0118 0.077 Uiso 1 1 calc R . . C43 C 0.2561(3) 0.8954(3) 0.1630(2) 0.0305(10) Uani 1 1 d . . . H43A H 0.2065 0.8248 0.1772 0.037 Uiso 1 1 calc R . . H43B H 0.2265 0.9300 0.2051 0.037 Uiso 1 1 calc R . . C44 C 0.2244(5) 0.9742(5) 0.0945(3) 0.0623(16) Uani 1 1 d . . . H44A H 0.1314 0.9888 0.1053 0.094 Uiso 1 1 calc R . . H44B H 0.2502 0.9400 0.0526 0.094 Uiso 1 1 calc R . . H44C H 0.2707 1.0455 0.0805 0.094 Uiso 1 1 calc R . . C45 C 0.1049(8) 0.2514(5) 0.0012(4) 0.104(3) Uani 1 1 d . . . H45A H 0.1061 0.2001 -0.0293 0.157 Uiso 1 1 calc R . . H45B H 0.0576 0.2162 0.0536 0.157 Uiso 1 1 calc R . . H45C H 0.1935 0.2671 -0.0004 0.157 Uiso 1 1 calc R . . C46 C 0.0392(6) 0.3610(5) -0.0301(3) 0.0664(16) Uani 1 1 d . . . H46A H 0.0867 0.3954 -0.0833 0.080 Uiso 1 1 calc R . . H46B H -0.0493 0.3443 -0.0296 0.080 Uiso 1 1 calc R . . C47 C 0.0327(5) 0.4450(4) 0.0143(3) 0.0509(13) Uani 1 1 d . . . H47A H -0.0137 0.4095 0.0675 0.061 Uiso 1 1 calc R . . H47B H 0.1215 0.4613 0.0136 0.061 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.021(2) 0.026(3) 0.026(3) -0.008(2) -0.010(2) -0.0011(19) B2 0.020(2) 0.021(2) 0.027(3) -0.009(2) -0.004(2) -0.0011(19) N1 0.0244(17) 0.0269(18) 0.0224(18) -0.0078(15) -0.0075(14) -0.0014(14) N2 0.0195(16) 0.0307(19) 0.0259(18) -0.0123(15) -0.0080(14) 0.0006(14) F1 0.0744(19) 0.0293(14) 0.0420(15) -0.0148(12) -0.0277(14) 0.0030(13) F2 0.106(2) 0.0486(17) 0.0512(18) -0.0201(14) -0.0441(17) -0.0085(16) F3 0.088(2) 0.0679(19) 0.0497(18) -0.0046(15) -0.0508(17) -0.0075(17) F4 0.0539(16) 0.0479(17) 0.0447(16) -0.0037(13) -0.0248(13) 0.0136(13) F5 0.0455(15) 0.0340(14) 0.0363(14) -0.0138(11) -0.0171(12) 0.0124(11) F6 0.0482(16) 0.0460(17) 0.0441(16) -0.0207(13) 0.0010(12) 0.0006(13) F7 0.0404(16) 0.085(2) 0.0521(18) -0.0226(16) 0.0031(14) 0.0088(15) F8 0.0306(15) 0.093(2) 0.0508(18) 0.0047(16) 0.0009(13) -0.0196(15) F9 0.0515(16) 0.0487(17) 0.0457(16) 0.0038(13) -0.0154(13) -0.0257(13) F10 0.0412(15) 0.0310(14) 0.0439(15) -0.0086(12) -0.0061(12) -0.0069(11) F11 0.0300(13) 0.0350(14) 0.0509(16) -0.0052(12) -0.0210(12) -0.0035(11) F12 0.0465(15) 0.0315(14) 0.0577(17) -0.0071(12) -0.0118(13) -0.0124(12) F13 0.0696(19) 0.0284(14) 0.0494(17) -0.0012(13) -0.0169(14) 0.0081(13) F14 0.0399(14) 0.0486(16) 0.0419(15) -0.0110(12) -0.0211(12) 0.0183(12) F15 0.0269(13) 0.0443(15) 0.0425(15) -0.0094(12) -0.0167(11) 0.0017(11) F16 0.0331(14) 0.0489(15) 0.0390(15) -0.0031(13) -0.0162(12) 0.0021(12) F17 0.0452(17) 0.075(2) 0.074(2) -0.0193(17) -0.0406(16) 0.0190(15) F18 0.0184(14) 0.109(3) 0.108(3) -0.035(2) -0.0242(15) 0.0013(15) F19 0.0272(14) 0.074(2) 0.070(2) -0.0257(16) 0.0042(14) -0.0189(14) F20 0.0269(13) 0.0453(15) 0.0371(14) -0.0055(12) -0.0019(11) -0.0112(11) F21 0.0204(11) 0.0261(13) 0.0408(14) -0.0113(11) -0.0029(10) 0.0011(10) F22 0.0233(13) 0.0457(15) 0.0394(14) -0.0058(12) -0.0036(11) -0.0136(11) F23 0.0539(16) 0.0267(14) 0.0652(18) 0.0040(13) -0.0251(14) -0.0201(12) F24 0.0615(17) 0.0205(13) 0.0739(19) -0.0176(13) -0.0294(15) 0.0059(12) F25 0.0309(13) 0.0320(13) 0.0530(16) -0.0217(12) -0.0088(12) 0.0095(11) F26 0.0589(16) 0.0234(13) 0.0262(14) -0.0050(10) -0.0020(12) -0.0088(11) F27 0.0663(17) 0.0156(12) 0.0422(15) -0.0024(11) -0.0071(13) -0.0077(12) F28 0.0567(16) 0.0261(13) 0.0458(16) -0.0194(12) -0.0066(13) -0.0059(12) F29 0.0599(17) 0.0345(14) 0.0247(14) -0.0110(11) -0.0053(12) -0.0074(12) F30 0.0494(15) 0.0204(12) 0.0258(13) -0.0031(10) -0.0088(11) -0.0075(11) C1 0.025(2) 0.025(2) 0.027(2) -0.0037(18) -0.0070(18) -0.0042(17) C2 0.040(3) 0.026(2) 0.030(2) -0.0029(19) -0.014(2) -0.0038(19) C3 0.055(3) 0.042(3) 0.031(3) -0.012(2) -0.016(2) -0.013(2) C4 0.047(3) 0.044(3) 0.033(3) -0.002(2) -0.027(2) -0.006(2) C5 0.028(2) 0.032(3) 0.036(3) 0.000(2) -0.013(2) 0.0026(19) C6 0.023(2) 0.035(2) 0.028(2) -0.007(2) -0.0085(18) -0.0005(18) C7 0.024(2) 0.031(2) 0.025(2) -0.0060(18) -0.0122(18) -0.0009(18) C8 0.032(2) 0.038(3) 0.029(2) -0.009(2) -0.008(2) -0.002(2) C9 0.027(2) 0.064(3) 0.026(2) -0.010(2) -0.003(2) 0.006(2) C10 0.026(2) 0.061(3) 0.029(3) 0.004(2) -0.008(2) -0.015(2) C11 0.035(3) 0.037(3) 0.030(3) 0.004(2) -0.016(2) -0.012(2) C12 0.030(2) 0.038(3) 0.024(2) -0.006(2) -0.0086(19) -0.002(2) C13 0.025(2) 0.029(2) 0.025(2) -0.0098(18) -0.0093(18) 0.0038(18) C14 0.030(2) 0.025(2) 0.030(2) -0.0099(19) -0.0136(19) 0.0018(18) C15 0.038(2) 0.027(2) 0.028(2) -0.0100(19) -0.008(2) 0.000(2) C16 0.048(3) 0.021(2) 0.029(2) -0.0069(19) -0.008(2) 0.008(2) C17 0.033(2) 0.037(3) 0.026(2) -0.013(2) -0.0124(19) 0.013(2) C18 0.023(2) 0.031(2) 0.028(2) -0.0115(19) -0.0058(18) 0.0018(18) C19 0.030(2) 0.033(2) 0.033(2) -0.005(2) -0.010(2) -0.0027(19) C20 0.029(2) 0.059(3) 0.054(3) -0.028(3) -0.016(2) 0.011(2) C21 0.032(2) 0.032(2) 0.018(2) -0.0036(18) -0.0093(18) -0.0038(18) C22 0.043(3) 0.045(3) 0.034(3) -0.013(2) -0.010(2) -0.015(2) C23 0.020(2) 0.026(2) 0.032(2) -0.0154(19) -0.0075(18) 0.0008(17) C24 0.027(2) 0.033(2) 0.034(3) -0.012(2) -0.010(2) 0.0033(19) C25 0.030(2) 0.048(3) 0.051(3) -0.022(2) -0.023(2) 0.008(2) C26 0.018(2) 0.067(3) 0.068(4) -0.032(3) -0.016(2) 0.004(2) C27 0.021(2) 0.050(3) 0.059(3) -0.024(3) -0.003(2) -0.008(2) C28 0.026(2) 0.029(2) 0.031(2) -0.012(2) -0.0044(19) -0.0026(18) C29 0.023(2) 0.017(2) 0.020(2) -0.0063(16) -0.0079(17) -0.0016(16) C30 0.024(2) 0.021(2) 0.028(2) -0.0099(18) -0.0115(18) 0.0012(17) C31 0.024(2) 0.033(2) 0.026(2) -0.0034(19) -0.0094(18) -0.0084(19) C32 0.039(3) 0.017(2) 0.040(3) 0.0029(19) -0.022(2) -0.0132(19) C33 0.038(3) 0.018(2) 0.042(3) -0.009(2) -0.021(2) 0.0030(19) C34 0.024(2) 0.029(2) 0.028(2) -0.0138(19) -0.0104(18) 0.0030(18) C35 0.0158(19) 0.020(2) 0.027(2) -0.0063(17) -0.0058(17) -0.0018(16) C36 0.025(2) 0.028(2) 0.022(2) -0.0040(18) -0.0064(18) -0.0042(18) C37 0.026(2) 0.016(2) 0.037(3) -0.0061(19) -0.0074(19) -0.0037(17) C38 0.026(2) 0.021(2) 0.037(3) -0.0165(19) -0.0052(19) -0.0007(17) C39 0.027(2) 0.027(2) 0.024(2) -0.0084(19) -0.0037(18) -0.0027(18) C40 0.022(2) 0.015(2) 0.026(2) 0.0001(17) -0.0065(17) -0.0043(16) C41 0.038(2) 0.036(3) 0.034(3) -0.018(2) -0.008(2) -0.006(2) C42 0.065(3) 0.062(3) 0.033(3) -0.019(3) -0.011(2) -0.013(3) C43 0.019(2) 0.042(3) 0.029(2) -0.005(2) -0.0085(18) -0.0035(18) C44 0.041(3) 0.076(4) 0.052(3) 0.013(3) -0.017(3) 0.004(3) C45 0.166(8) 0.069(5) 0.076(5) -0.020(4) -0.041(5) 0.035(5) C46 0.084(4) 0.067(4) 0.043(3) -0.011(3) -0.013(3) 0.004(3) C47 0.043(3) 0.065(3) 0.038(3) -0.007(3) -0.010(2) 0.001(3) _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 B1 C13 1.641(6) . ? B1 C1 1.650(6) . ? B1 N1 1.650(5) . ? B1 C7 1.660(5) . ? B2 N2 1.638(5) . ? B2 C35 1.645(5) . ? B2 C29 1.651(5) . ? B2 C23 1.657(5) . ? N1 C21 1.516(5) . ? N1 C19 1.521(5) . ? N2 C43 1.505(5) . ? N2 C41 1.519(5) . ? F1 C2 1.355(4) . ? F2 C3 1.345(5) . ? F3 C4 1.329(5) . ? F4 C5 1.335(4) . ? F5 C6 1.354(4) . ? F6 C8 1.348(5) . ? F7 C9 1.339(5) . ? F8 C10 1.334(5) . ? F9 C11 1.342(5) . ? F10 C12 1.351(4) . ? F11 C14 1.356(4) . ? F12 C15 1.338(4) . ? F13 C16 1.336(4) . ? F14 C17 1.344(4) . ? F15 C18 1.351(4) . ? F16 C24 1.350(4) . ? F17 C25 1.341(5) . ? F18 C26 1.344(5) . ? F19 C27 1.342(5) . ? F20 C28 1.360(4) . ? F21 C30 1.355(4) . ? F22 C31 1.343(4) . ? F23 C32 1.341(4) . ? F24 C33 1.342(4) . ? F25 C34 1.350(4) . ? F26 C36 1.356(4) . ? F27 C37 1.343(4) . ? F28 C38 1.341(4) . ? F29 C39 1.338(4) . ? F30 C40 1.350(4) . ? C1 C2 1.386(5) . ? C1 C6 1.389(5) . ? C2 C3 1.384(6) . ? C3 C4 1.375(6) . ? C4 C5 1.358(6) . ? C5 C6 1.382(5) . ? C7 C12 1.384(5) . ? C7 C8 1.390(5) . ? C8 C9 1.372(6) . ? C9 C10 1.373(6) . ? C10 C11 1.370(6) . ? C11 C12 1.374(5) . ? C13 C18 1.390(5) . ? C13 C14 1.396(5) . ? C14 C15 1.366(5) . ? C15 C16 1.374(6) . ? C16 C17 1.372(6) . ? C17 C18 1.373(5) . ? C19 C20 1.505(6) . ? C21 C22 1.503(5) . ? C23 C24 1.378(5) . ? C23 C28 1.386(5) . ? C24 C25 1.369(6) . ? C25 C26 1.373(6) . ? C26 C27 1.358(6) . ? C27 C28 1.384(6) . ? C29 C30 1.383(5) . ? C29 C34 1.384(5) . ? C30 C31 1.376(5) . ? C31 C32 1.367(5) . ? C32 C33 1.361(6) . ? C33 C34 1.383(5) . ? C35 C40 1.382(5) . ? C35 C36 1.392(5) . ? C36 C37 1.375(5) . ? C37 C38 1.367(5) . ? C38 C39 1.364(5) . ? C39 C40 1.380(5) . ? C41 C42 1.497(6) . ? C43 C44 1.491(6) . ? C45 C46 1.515(8) . ? C46 C47 1.510(7) . ? C47 C47 1.505(9) 2_565 ? 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 C13 B1 C1 115.2(3) . . ? C13 B1 N1 105.4(3) . . ? C1 B1 N1 109.8(3) . . ? C13 B1 C7 115.2(3) . . ? C1 B1 C7 102.3(3) . . ? N1 B1 C7 108.9(3) . . ? N2 B2 C35 110.7(3) . . ? N2 B2 C29 105.0(3) . . ? C35 B2 C29 114.6(3) . . ? N2 B2 C23 110.9(3) . . ? C35 B2 C23 101.7(3) . . ? C29 B2 C23 114.1(3) . . ? C21 N1 C19 112.3(3) . . ? C21 N1 B1 110.7(3) . . ? C19 N1 B1 112.4(3) . . ? C43 N2 C41 112.0(3) . . ? C43 N2 B2 111.0(3) . . ? C41 N2 B2 111.7(3) . . ? C2 C1 C6 113.0(4) . . ? C2 C1 B1 124.3(4) . . ? C6 C1 B1 122.0(3) . . ? F1 C2 C3 115.1(4) . . ? F1 C2 C1 120.9(4) . . ? C3 C2 C1 123.9(4) . . ? F2 C3 C4 120.3(4) . . ? F2 C3 C2 119.8(4) . . ? C4 C3 C2 119.9(4) . . ? F3 C4 C5 121.4(4) . . ? F3 C4 C3 119.6(4) . . ? C5 C4 C3 118.9(4) . . ? F4 C5 C4 119.9(4) . . ? F4 C5 C6 120.6(4) . . ? C4 C5 C6 119.5(4) . . ? F5 C6 C5 115.8(4) . . ? F5 C6 C1 119.4(3) . . ? C5 C6 C1 124.7(4) . . ? C12 C7 C8 112.8(4) . . ? C12 C7 B1 126.8(4) . . ? C8 C7 B1 119.6(3) . . ? F6 C8 C9 115.7(4) . . ? F6 C8 C7 120.0(4) . . ? C9 C8 C7 124.3(4) . . ? F7 C9 C8 120.5(4) . . ? F7 C9 C10 119.3(4) . . ? C8 C9 C10 120.2(4) . . ? F8 C10 C11 121.1(4) . . ? F8 C10 C9 120.8(4) . . ? C11 C10 C9 118.1(4) . . ? F9 C11 C10 119.5(4) . . ? F9 C11 C12 120.5(4) . . ? C10 C11 C12 120.0(4) . . ? F10 C12 C11 114.6(4) . . ? F10 C12 C7 120.8(3) . . ? C11 C12 C7 124.6(4) . . ? C18 C13 C14 112.1(3) . . ? C18 C13 B1 124.4(3) . . ? C14 C13 B1 123.3(3) . . ? F11 C14 C15 115.1(3) . . ? F11 C14 C13 119.5(3) . . ? C15 C14 C13 125.4(4) . . ? F12 C15 C14 120.8(4) . . ? F12 C15 C16 119.9(4) . . ? C14 C15 C16 119.2(4) . . ? F13 C16 C17 120.5(4) . . ? F13 C16 C15 120.7(4) . . ? C17 C16 C15 118.8(4) . . ? F14 C17 C16 119.5(4) . . ? F14 C17 C18 120.7(4) . . ? C16 C17 C18 119.8(4) . . ? F15 C18 C17 115.0(3) . . ? F15 C18 C13 120.3(3) . . ? C17 C18 C13 124.7(4) . . ? C20 C19 N1 114.7(3) . . ? C22 C21 N1 115.1(3) . . ? C24 C23 C28 112.8(3) . . ? C24 C23 B2 121.3(3) . . ? C28 C23 B2 125.0(3) . . ? F16 C24 C25 115.0(4) . . ? F16 C24 C23 120.1(3) . . ? C25 C24 C23 124.9(4) . . ? F17 C25 C24 121.0(4) . . ? F17 C25 C26 119.6(4) . . ? C24 C25 C26 119.5(4) . . ? F18 C26 C27 120.6(4) . . ? F18 C26 C25 120.4(5) . . ? C27 C26 C25 119.0(4) . . ? F19 C27 C26 120.4(4) . . ? F19 C27 C28 120.1(4) . . ? C26 C27 C28 119.5(4) . . ? F20 C28 C27 115.3(4) . . ? F20 C28 C23 120.3(3) . . ? C27 C28 C23 124.4(4) . . ? C30 C29 C34 113.0(3) . . ? C30 C29 B2 124.4(3) . . ? C34 C29 B2 122.5(3) . . ? F21 C30 C31 115.2(3) . . ? F21 C30 C29 120.4(3) . . ? C31 C30 C29 124.4(4) . . ? F22 C31 C32 120.2(3) . . ? F22 C31 C30 120.2(4) . . ? C32 C31 C30 119.6(4) . . ? F23 C32 C33 120.3(4) . . ? F23 C32 C31 120.7(4) . . ? C33 C32 C31 119.0(3) . . ? F24 C33 C32 120.4(3) . . ? F24 C33 C34 120.1(4) . . ? C32 C33 C34 119.5(4) . . ? F25 C34 C33 114.9(3) . . ? F25 C34 C29 120.7(3) . . ? C33 C34 C29 124.4(4) . . ? C40 C35 C36 112.6(3) . . ? C40 C35 B2 123.5(3) . . ? C36 C35 B2 123.0(3) . . ? F26 C36 C37 115.8(3) . . ? F26 C36 C35 119.1(3) . . ? C37 C36 C35 125.1(4) . . ? F27 C37 C38 120.4(3) . . ? F27 C37 C36 120.5(4) . . ? C38 C37 C36 119.0(3) . . ? F28 C38 C39 120.1(4) . . ? F28 C38 C37 120.8(3) . . ? C39 C38 C37 119.2(3) . . ? F29 C39 C38 119.6(3) . . ? F29 C39 C40 120.5(3) . . ? C38 C39 C40 119.8(4) . . ? F30 C40 C39 114.8(3) . . ? F30 C40 C35 120.8(3) . . ? C39 C40 C35 124.3(3) . . ? C42 C41 N2 114.7(3) . . ? C44 C43 N2 115.9(3) . . ? C47 C46 C45 112.9(5) . . ? C47 C47 C46 114.9(5) 2_565 . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.565 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.057 #===end data_[tBu2N2C3H3][PhNHB(C6F5)3] _database_code_depnum_ccdc_archive 'CCDC 689782' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C35 H27 B F15 N3' _chemical_formula_weight 785.41 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 18.552(2) _cell_length_b 18.677(2) _cell_length_c 22.029(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.055(2) _cell_angle_gamma 90.00 _cell_volume 7215.1(13) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 0.139 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.691455 _exptl_absorpt_correction_T_max 1.0000 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 34157 _diffrn_reflns_av_R_equivalents 0.1676 _diffrn_reflns_av_sigmaI/netI 0.1320 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6363 _reflns_number_gt 2222 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1570P)^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 constr _refine_ls_extinction_method none _refine_ls_number_reflns 6356 _refine_ls_number_parameters 497 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.2216 _refine_ls_R_factor_gt 0.0769 _refine_ls_wR_factor_ref 0.2980 _refine_ls_wR_factor_gt 0.1999 _refine_ls_goodness_of_fit_ref 0.919 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.000 _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 N1 N 0.2791(3) -0.0069(3) 0.3627(2) 0.0606(14) Uani 1 1 d . . . H1A H 0.3269 -0.0003 0.3691 0.073 Uiso 1 1 calc R . . N2 N 0.8351(4) 0.1985(3) 0.3315(3) 0.0802(19) Uani 1 1 d D . . N3 N 0.7210(5) 0.2073(3) 0.2699(3) 0.097(2) Uani 1 1 d D . . B1 B 0.2540(4) 0.0030(4) 0.4221(3) 0.056(2) Uani 1 1 d . . . F1 F 0.0853(2) -0.0090(2) 0.4161(2) 0.0903(13) Uani 1 1 d . . . F2 F 0.0115(3) -0.1295(3) 0.4159(2) 0.1152(17) Uani 1 1 d . . . F3 F 0.0819(3) -0.2577(3) 0.4205(2) 0.1173(17) Uani 1 1 d . . . F4 F 0.2305(3) -0.2618(2) 0.4284(2) 0.1017(15) Uani 1 1 d . . . F5 F 0.3078(3) -0.1417(2) 0.43363(19) 0.0861(12) Uani 1 1 d . . . F6 F 0.2079(2) 0.12439(19) 0.32214(17) 0.0798(12) Uani 1 1 d . . . F7 F 0.1605(3) 0.2521(2) 0.3414(2) 0.1026(15) Uani 1 1 d . . . F8 F 0.1345(3) 0.2846(2) 0.4526(2) 0.1131(17) Uani 1 1 d . . . F9 F 0.1568(3) 0.1824(3) 0.5440(2) 0.1217(17) Uani 1 1 d . . . F10 F 0.2053(2) 0.0527(2) 0.52681(18) 0.0929(14) Uani 1 1 d . . . F11 F 0.2972(2) -0.0748(2) 0.55250(17) 0.0868(13) Uani 1 1 d . . . F12 F 0.4240(3) -0.0588(3) 0.64868(19) 0.1213(18) Uani 1 1 d . . . F13 F 0.5348(2) 0.0320(3) 0.6394(2) 0.1158(17) Uani 1 1 d . . . F14 F 0.5122(2) 0.1084(2) 0.5300(2) 0.0943(14) Uani 1 1 d . . . F15 F 0.3840(2) 0.0952(2) 0.43308(18) 0.0777(12) Uani 1 1 d . . . C1 C 0.2010(4) -0.0677(4) 0.4257(3) 0.0583(17) Uani 1 1 d . . . C2 C 0.1263(4) -0.0703(4) 0.4211(3) 0.0659(19) Uani 1 1 d . . . C3 C 0.0856(5) -0.1328(5) 0.4196(3) 0.076(2) Uani 1 1 d . . . C4 C 0.1217(6) -0.1963(5) 0.4225(3) 0.080(2) Uani 1 1 d . . . C5 C 0.1956(5) -0.1982(4) 0.4263(3) 0.071(2) Uani 1 1 d . . . C6 C 0.2334(4) -0.1347(4) 0.4282(3) 0.0615(18) Uani 1 1 d . . . C7 C 0.2117(3) 0.0805(3) 0.4242(3) 0.0489(15) Uani 1 1 d . . . C8 C 0.1973(4) 0.1355(3) 0.3796(3) 0.0542(16) Uani 1 1 d . . . C9 C 0.1727(4) 0.2027(4) 0.3880(4) 0.0685(19) Uani 1 1 d . . . C10 C 0.1591(4) 0.2195(4) 0.4433(4) 0.077(2) Uani 1 1 d . . . C11 C 0.1704(4) 0.1673(5) 0.4891(4) 0.076(2) Uani 1 1 d . . . C12 C 0.1950(4) 0.1013(4) 0.4791(3) 0.0652(18) Uani 1 1 d . . . C13 C 0.3332(3) 0.0082(3) 0.4849(3) 0.0506(16) Uani 1 1 d . . . C14 C 0.3483(4) -0.0282(4) 0.5430(3) 0.0648(18) Uani 1 1 d . . . C15 C 0.4147(5) -0.0206(4) 0.5945(3) 0.077(2) Uani 1 1 d . . . C16 C 0.4699(4) 0.0248(4) 0.5895(4) 0.077(2) Uani 1 1 d . . . C17 C 0.4578(4) 0.0626(4) 0.5343(3) 0.0655(19) Uani 1 1 d . . . C18 C 0.3913(4) 0.0539(3) 0.4849(3) 0.0570(17) Uani 1 1 d . . . C19 C 0.2364(4) -0.0247(3) 0.3009(3) 0.0588(17) Uani 1 1 d . . . C20 C 0.2729(4) -0.0434(3) 0.2571(3) 0.075(2) Uani 1 1 d . . . H20A H 0.3259 -0.0450 0.2713 0.090 Uiso 1 1 calc R . . C21 C 0.2344(6) -0.0596(4) 0.1939(4) 0.090(2) Uani 1 1 d . . . H21A H 0.2610 -0.0701 0.1658 0.108 Uiso 1 1 calc R . . C22 C 0.1569(6) -0.0601(4) 0.1730(4) 0.095(3) Uani 1 1 d . . . H22A H 0.1300 -0.0726 0.1308 0.115 Uiso 1 1 calc R . . C23 C 0.1186(5) -0.0420(4) 0.2150(4) 0.089(2) Uani 1 1 d . . . H23A H 0.0656 -0.0417 0.2005 0.107 Uiso 1 1 calc R . . C24 C 0.1575(4) -0.0243(4) 0.2781(3) 0.0698(19) Uani 1 1 d . . . H24A H 0.1305 -0.0120 0.3055 0.084 Uiso 1 1 calc R . . C25 C 0.7540(7) 0.2799(6) 0.2765(7) 0.081(4) Uiso 0.50 1 d PD . . C25A C 0.7253(10) 0.1361(7) 0.3006(8) 0.120(7) Uiso 0.50 1 d PD . . C26 C 0.7732(7) 0.1567(7) 0.3031(7) 0.085(5) Uiso 0.50 1 d PD . . C26A C 0.7889(8) 0.2485(10) 0.2857(12) 0.191(13) Uiso 0.50 1 d PD . . C27 C 0.8301(8) 0.2751(5) 0.3217(7) 0.084(5) Uiso 0.50 1 d PD . . C27A C 0.8039(10) 0.1295(7) 0.3404(10) 0.127(7) Uiso 0.50 1 d PD . . C28 C 0.9104(9) 0.1623(7) 0.3775(6) 0.100(8) Uani 0.50 1 d PD . . C28A C 0.9164(10) 0.2095(9) 0.3564(6) 0.124(9) Uani 0.50 1 d PD . . C29 C 0.8820(9) 0.1002(8) 0.4094(8) 0.097(5) Uani 0.50 1 d PD . . C29A C 0.9194(12) 0.2881(11) 0.3335(10) 0.130(7) Uiso 0.50 1 d PD . . C30 C 0.9569(5) 0.1496(6) 0.3315(5) 0.132(4) Uani 1 1 d D . . C31 C 0.9451(5) 0.2179(5) 0.4300(4) 0.125(3) Uani 1 1 d D . . C32 C 0.6386(4) 0.2099(4) 0.2237(3) 0.076(2) Uani 1 1 d . . . C33 C 0.5984(5) 0.2623(7) 0.2545(4) 0.145(4) Uani 1 1 d . . . H33A H 0.5977 0.2435 0.2949 0.217 Uiso 1 1 calc R . . H33B H 0.5470 0.2695 0.2267 0.217 Uiso 1 1 calc R . . H33C H 0.6250 0.3073 0.2615 0.217 Uiso 1 1 calc R . . C34 C 0.6068(8) 0.1364(7) 0.2145(5) 0.202(7) Uani 1 1 d . . . H34A H 0.6359 0.1070 0.1953 0.303 Uiso 1 1 calc R . . H34B H 0.5546 0.1379 0.1868 0.303 Uiso 1 1 calc R . . H34C H 0.6091 0.1166 0.2553 0.303 Uiso 1 1 calc R . . C35 C 0.6418(4) 0.2374(4) 0.1611(3) 0.093(2) Uani 1 1 d . . . H35A H 0.6680 0.2034 0.1431 0.140 Uiso 1 1 calc R . . H35B H 0.6686 0.2822 0.1679 0.140 Uiso 1 1 calc R . . H35C H 0.5909 0.2442 0.1321 0.140 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N1 0.057(3) 0.074(4) 0.047(3) -0.009(3) 0.010(3) -0.005(3) N2 0.113(6) 0.059(4) 0.085(4) 0.012(3) 0.055(4) 0.021(4) N3 0.156(7) 0.087(5) 0.063(4) 0.001(3) 0.057(4) 0.042(5) B1 0.057(5) 0.060(5) 0.046(4) -0.003(3) 0.010(4) -0.004(4) F1 0.057(3) 0.090(3) 0.119(3) 0.022(3) 0.021(2) 0.008(2) F2 0.066(3) 0.134(4) 0.134(4) 0.022(3) 0.018(3) -0.027(3) F3 0.135(4) 0.091(3) 0.112(4) 0.002(3) 0.020(3) -0.045(3) F4 0.137(4) 0.058(3) 0.104(3) -0.007(2) 0.031(3) -0.001(3) F5 0.076(3) 0.071(3) 0.108(3) -0.006(2) 0.025(2) 0.010(2) F6 0.114(3) 0.069(3) 0.061(2) 0.010(2) 0.034(2) 0.007(2) F7 0.120(4) 0.070(3) 0.121(4) 0.028(3) 0.045(3) 0.021(3) F8 0.111(4) 0.074(3) 0.152(4) -0.021(3) 0.040(3) 0.026(3) F9 0.158(5) 0.134(4) 0.091(3) -0.018(3) 0.064(3) 0.034(3) F10 0.117(4) 0.108(3) 0.060(2) 0.017(2) 0.037(2) 0.027(3) F11 0.084(3) 0.103(3) 0.062(2) 0.020(2) 0.008(2) -0.016(3) F12 0.114(4) 0.160(4) 0.063(3) 0.042(3) -0.008(2) -0.006(3) F13 0.071(3) 0.148(4) 0.093(3) -0.002(3) -0.022(3) -0.010(3) F14 0.075(3) 0.092(3) 0.108(3) -0.020(3) 0.019(2) -0.029(3) F15 0.083(3) 0.077(3) 0.068(3) 0.003(2) 0.018(2) -0.021(2) C1 0.055(5) 0.063(5) 0.050(4) -0.001(3) 0.009(3) -0.003(4) C2 0.058(5) 0.071(5) 0.063(4) 0.010(4) 0.011(4) 0.003(5) C3 0.049(5) 0.095(7) 0.075(5) 0.009(5) 0.006(4) -0.018(5) C4 0.096(7) 0.065(6) 0.069(5) -0.003(4) 0.014(5) -0.027(6) C5 0.082(6) 0.059(6) 0.063(4) -0.006(4) 0.012(4) -0.001(5) C6 0.059(5) 0.062(5) 0.055(4) -0.005(3) 0.008(3) -0.007(4) C7 0.040(4) 0.053(4) 0.050(4) -0.005(3) 0.009(3) 0.002(3) C8 0.058(4) 0.054(4) 0.048(4) -0.001(3) 0.014(3) -0.001(3) C9 0.064(5) 0.060(5) 0.078(5) 0.014(4) 0.018(4) 0.003(4) C10 0.074(6) 0.058(5) 0.104(6) -0.015(5) 0.036(5) 0.001(4) C11 0.075(5) 0.094(6) 0.063(5) -0.017(5) 0.028(4) 0.012(5) C12 0.067(5) 0.073(5) 0.054(4) 0.001(4) 0.016(4) 0.012(4) C13 0.054(4) 0.046(4) 0.045(4) 0.001(3) 0.007(3) 0.004(3) C14 0.062(5) 0.069(5) 0.059(4) -0.001(4) 0.014(4) -0.012(4) C15 0.072(6) 0.089(6) 0.056(5) 0.010(4) 0.002(4) 0.007(5) C16 0.047(5) 0.096(6) 0.066(5) -0.014(5) -0.011(4) -0.003(4) C17 0.055(5) 0.066(5) 0.068(5) -0.010(4) 0.009(4) -0.004(4) C18 0.066(5) 0.051(4) 0.049(4) 0.000(3) 0.013(4) 0.004(4) C19 0.077(5) 0.045(4) 0.050(4) -0.007(3) 0.015(4) 0.002(4) C20 0.087(6) 0.071(5) 0.059(4) -0.004(4) 0.015(4) 0.007(4) C21 0.122(8) 0.089(6) 0.057(5) -0.014(4) 0.026(5) -0.008(6) C22 0.138(9) 0.075(5) 0.049(5) -0.011(4) -0.003(6) -0.015(6) C23 0.090(6) 0.093(6) 0.061(5) -0.007(4) -0.010(5) -0.020(5) C24 0.067(5) 0.075(5) 0.057(4) -0.002(4) 0.005(4) -0.008(4) C28 0.070(13) 0.059(12) 0.128(16) -0.031(11) -0.029(11) 0.016(11) C28A 0.037(11) 0.15(2) 0.16(2) -0.069(18) -0.005(12) 0.032(14) C29 0.104(13) 0.067(10) 0.114(13) 0.043(9) 0.029(10) 0.025(10) C30 0.067(6) 0.173(10) 0.160(9) -0.063(8) 0.041(6) 0.028(6) C31 0.131(9) 0.121(8) 0.094(7) -0.011(6) -0.004(6) 0.005(6) C32 0.057(5) 0.105(6) 0.058(4) -0.001(4) 0.007(4) -0.006(4) C33 0.087(7) 0.245(13) 0.100(7) -0.036(8) 0.026(5) 0.058(8) C34 0.307(18) 0.186(12) 0.121(9) -0.043(8) 0.081(10) -0.176(12) C35 0.094(6) 0.101(6) 0.080(5) 0.012(5) 0.022(5) 0.021(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 N1 C19 1.375(7) . ? N1 B1 1.534(8) . ? N2 C26 1.360(9) . ? N2 C26A 1.437(10) . ? N2 C28A 1.441(19) . ? N2 C27 1.447(9) . ? N2 C27A 1.452(9) . ? N2 C28 1.584(19) . ? N3 C26 1.380(9) . ? N3 C26A 1.421(10) . ? N3 C25 1.476(9) . ? N3 C25A 1.481(9) . ? N3 C32 1.536(9) . ? B1 C7 1.655(9) . ? B1 C13 1.660(9) . ? B1 C1 1.664(10) . ? F1 C2 1.360(8) . ? F2 C3 1.350(8) . ? F3 C4 1.358(8) . ? F4 C5 1.346(8) . ? F5 C6 1.353(7) . ? F6 C8 1.358(7) . ? F7 C9 1.342(7) . ? F8 C10 1.337(8) . ? F9 C11 1.344(7) . ? F10 C12 1.354(7) . ? F11 C14 1.353(7) . ? F12 C15 1.352(8) . ? F13 C16 1.347(7) . ? F14 C17 1.349(8) . ? F15 C18 1.347(7) . ? C1 C2 1.356(9) . ? C1 C6 1.381(9) . ? C2 C3 1.387(10) . ? C3 C4 1.353(10) . ? C4 C5 1.346(10) . ? C5 C6 1.370(9) . ? C7 C8 1.387(8) . ? C7 C12 1.398(8) . ? C8 C9 1.369(9) . ? C9 C10 1.359(10) . ? C10 C11 1.369(10) . ? C11 C12 1.356(9) . ? C13 C18 1.375(8) . ? C13 C14 1.395(8) . ? C14 C15 1.383(9) . ? C15 C16 1.360(10) . ? C16 C17 1.360(10) . ? C17 C18 1.364(9) . ? C19 C24 1.384(9) . ? C19 C20 1.391(9) . ? C20 C21 1.377(9) . ? C21 C22 1.358(11) . ? C22 C23 1.380(11) . ? C23 C24 1.381(9) . ? C25 C26A 0.85(2) . ? C25 C27 1.441(10) . ? C25A C26 0.95(2) . ? C25A C27A 1.441(10) . ? C26 C27A 0.975(19) . ? C26 C26A 1.80(2) . ? C26A C27 1.03(2) . ? C27 C29A 1.61(2) . ? C27 C28A 1.962(17) . ? C27A C29 1.81(2) . ? C27A C28 1.97(2) . ? C28 C28A 1.02(2) . ? C28 C31 1.531(9) . ? C28 C29 1.535(9) . ? C28 C30 1.550(9) . ? C28A C31 1.541(9) . ? C28A C30 1.545(9) . ? C28A C29A 1.559(10) . ? C32 C34 1.482(12) . ? C32 C35 1.490(10) . ? C32 C33 1.520(11) . ? 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 C19 N1 B1 129.5(6) . . ? C26 N2 C26A 80.2(9) . . ? C26 N2 C28A 151.5(9) . . ? C26A N2 C28A 119.0(10) . . ? C26 N2 C27 119.7(9) . . ? C26A N2 C27 42.0(9) . . ? C28A N2 C27 85.6(9) . . ? C26 N2 C27A 40.4(8) . . ? C26A N2 C27A 120.0(10) . . ? C28A N2 C27A 119.3(11) . . ? C27 N2 C27A 152.8(11) . . ? C26 N2 C28 119.0(7) . . ? C26A N2 C28 157.9(9) . . ? C28A N2 C28 39.1(8) . . ? C27 N2 C28 121.2(8) . . ? C27A N2 C28 80.9(9) . . ? C26 N3 C26A 80.1(9) . . ? C26 N3 C25 112.3(9) . . ? C26A N3 C25 33.9(10) . . ? C26 N3 C25A 38.8(8) . . ? C26A N3 C25A 117.7(10) . . ? C25 N3 C25A 145.2(10) . . ? C26 N3 C32 138.4(8) . . ? C26A N3 C32 139.1(7) . . ? C25 N3 C32 109.1(7) . . ? C25A N3 C32 103.0(9) . . ? N1 B1 C7 114.1(5) . . ? N1 B1 C13 106.6(5) . . ? C7 B1 C13 102.9(5) . . ? N1 B1 C1 107.1(5) . . ? C7 B1 C1 113.6(5) . . ? C13 B1 C1 112.5(5) . . ? C2 C1 C6 113.0(7) . . ? C2 C1 B1 129.0(7) . . ? C6 C1 B1 117.7(6) . . ? C1 C2 F1 120.5(7) . . ? C1 C2 C3 124.6(7) . . ? F1 C2 C3 114.8(7) . . ? F2 C3 C4 121.5(8) . . ? F2 C3 C2 119.9(8) . . ? C4 C3 C2 118.6(8) . . ? C5 C4 C3 120.4(8) . . ? C5 C4 F3 120.8(9) . . ? C3 C4 F3 118.9(9) . . ? F4 C5 C4 119.6(8) . . ? F4 C5 C6 121.8(8) . . ? C4 C5 C6 118.6(8) . . ? F5 C6 C5 114.6(7) . . ? F5 C6 C1 120.5(6) . . ? C5 C6 C1 124.8(7) . . ? C8 C7 C12 111.2(6) . . ? C8 C7 B1 127.6(5) . . ? C12 C7 B1 120.6(6) . . ? F6 C8 C9 115.0(6) . . ? F6 C8 C7 119.7(5) . . ? C9 C8 C7 125.3(6) . . ? F7 C9 C10 119.4(7) . . ? F7 C9 C8 120.4(7) . . ? C10 C9 C8 120.1(7) . . ? F8 C10 C9 121.3(8) . . ? F8 C10 C11 120.9(8) . . ? C9 C10 C11 117.8(7) . . ? F9 C11 C12 120.6(8) . . ? F9 C11 C10 118.9(7) . . ? C12 C11 C10 120.5(7) . . ? F10 C12 C11 116.9(6) . . ? F10 C12 C7 118.0(6) . . ? C11 C12 C7 125.0(7) . . ? C18 C13 C14 112.3(6) . . ? C18 C13 B1 121.1(5) . . ? C14 C13 B1 126.5(6) . . ? F11 C14 C15 114.9(6) . . ? F11 C14 C13 120.9(6) . . ? C15 C14 C13 124.1(7) . . ? F12 C15 C16 121.1(7) . . ? F12 C15 C14 119.5(7) . . ? C16 C15 C14 119.4(7) . . ? F13 C16 C15 119.5(7) . . ? F13 C16 C17 121.3(8) . . ? C15 C16 C17 119.1(6) . . ? F14 C17 C16 118.9(7) . . ? F14 C17 C18 121.4(7) . . ? C16 C17 C18 119.6(7) . . ? F15 C18 C17 115.0(6) . . ? F15 C18 C13 119.6(6) . . ? C17 C18 C13 125.4(6) . . ? N1 C19 C24 123.9(6) . . ? N1 C19 C20 119.6(7) . . ? C24 C19 C20 116.5(6) . . ? C21 C20 C19 123.2(8) . . ? C22 C21 C20 119.1(8) . . ? C21 C22 C23 119.4(7) . . ? C22 C23 C24 121.2(8) . . ? C23 C24 C19 120.5(7) . . ? C26A C25 C27 45.0(17) . . ? C26A C25 N3 69.5(10) . . ? C27 C25 N3 107.1(10) . . ? C26 C25A C27A 42.2(11) . . ? C26 C25A N3 64.9(8) . . ? C27A C25A N3 104.3(12) . . ? C25A C26 C27A 96.6(15) . . ? C25A C26 N2 153(2) . . ? C27A C26 N2 74.9(9) . . ? C25A C26 N3 76.4(9) . . ? C27A C26 N3 157(2) . . ? N2 C26 N3 101.1(9) . . ? C25A C26 C26A 125.7(12) . . ? C27A C26 C26A 125.8(12) . . ? N2 C26 C26A 51.8(6) . . ? N3 C26 C26A 51.0(6) . . ? C25 C26A C27 100(3) . . ? C25 C26A N3 76.6(11) . . ? C27 C26A N3 146(3) . . ? C25 C26A N2 148(3) . . ? C27 C26A N2 69.6(9) . . ? N3 C26A N2 95.5(9) . . ? C25 C26A C26 123.0(15) . . ? C27 C26A C26 115.1(12) . . ? N3 C26A C26 48.9(6) . . ? N2 C26A C26 48.0(5) . . ? C26A C27 C25 35.4(14) . . ? C26A C27 N2 68.5(9) . . ? C25 C27 N2 99.5(9) . . ? C26A C27 C29A 131(2) . . ? C25 C27 C29A 145.9(14) . . ? N2 C27 C29A 96.5(10) . . ? C26A C27 C28A 107.7(15) . . ? C25 C27 C28A 143.0(10) . . ? N2 C27 C28A 47.1(7) . . ? C29A C27 C28A 50.6(6) . . ? C26 C27A C25A 41.1(11) . . ? C26 C27A N2 64.7(8) . . ? C25A C27A N2 102.2(12) . . ? C26 C27A C29 162.2(13) . . ? C25A C27A C29 155.7(13) . . ? N2 C27A C29 97.8(10) . . ? C26 C27A C28 114.7(12) . . ? C25A C27A C28 154.6(11) . . ? N2 C27A C28 52.4(7) . . ? C29 C27A C28 47.7(6) . . ? C28A C28 C31 71.2(8) . . ? C28A C28 C29 165.2(19) . . ? C31 C28 C29 106.8(11) . . ? C28A C28 C30 70.5(8) . . ? C31 C28 C30 114.3(9) . . ? C29 C28 C30 122.1(12) . . ? C28A C28 N2 62.9(15) . . ? C31 C28 N2 105.1(9) . . ? C29 C28 N2 104.7(10) . . ? C30 C28 N2 102.1(9) . . ? C28A C28 C27A 108.9(19) . . ? C31 C28 C27A 129.9(11) . . ? C29 C28 C27A 60.6(8) . . ? C30 C28 C27A 112.2(10) . . ? N2 C28 C27A 46.6(6) . . ? C28 C28A N2 78.0(19) . . ? C28 C28A C31 70.0(9) . . ? N2 C28A C31 111.9(12) . . ? C28 C28A C30 71.0(8) . . ? N2 C28A C30 109.3(11) . . ? C31 C28A C30 114.0(9) . . ? C28 C28A C29A 169.1(14) . . ? N2 C28A C29A 98.9(11) . . ? C31 C28A C29A 102.0(12) . . ? C30 C28A C29A 119.7(15) . . ? C28 C28A C27 121(2) . . ? N2 C28A C27 47.3(5) . . ? C31 C28A C27 107.7(8) . . ? C30 C28A C27 138.0(9) . . ? C29A C28A C27 52.8(9) . . ? C28 C29 C27A 71.8(9) . . ? C28A C29A C27 76.5(10) . . ? C28A C30 C28 38.5(8) . . ? C28 C31 C28A 38.8(8) . . ? C34 C32 C35 109.1(7) . . ? C34 C32 C33 115.3(9) . . ? C35 C32 C33 111.4(7) . . ? C34 C32 N3 109.1(8) . . ? C35 C32 N3 107.0(6) . . ? C33 C32 N3 104.6(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.632 _refine_diff_density_min -0.376 _refine_diff_density_rms 0.055 _vrf_PLAT601_[tBu2N2C3H3][PhNHB(C6F5)3] ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.53 Ratio RESPONSE: The cation is disordered and the best (chemically meaningful) model found involved a constrained twofold disorder The two models also give rise to the erroneous C-C bond distances. ; #===end data_[tBu2N2C3H3][HB(C6F5)3] _database_code_depnum_ccdc_archive 'CCDC 689783' _audit_creation_method SHELXL-97 _chemical_formula_sum 'C29 H22 B F15 N2' _chemical_formula_weight 694.30 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4897(14) _cell_length_b 9.7960(9) _cell_length_c 20.1789(19) _cell_angle_alpha 90.00 _cell_angle_beta 107.0520(10) _cell_angle_gamma 90.00 _cell_volume 2927.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 25.0 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.17 _exptl_crystal_density_diffrn 1.575 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1400 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.841921 _exptl_absorpt_correction_T_max 1.00000 _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_reflns_number 27461 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5167 _reflns_number_gt 3138 _reflns_threshold_expression >2sigma(I) _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5167 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0861 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1582 _refine_ls_wR_factor_gt 0.1249 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.000 _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 B1 B 0.2590(2) 0.4329(3) 0.27021(17) 0.0464(8) Uani 1 1 d . . . H1 H 0.3178(15) 0.393(2) 0.3121(12) 0.037(6) Uiso 1 1 d . . . F1 F 0.21429(13) 0.61415(17) 0.14292(8) 0.0686(5) Uani 1 1 d . . . F2 F 0.24564(13) 0.87965(18) 0.14146(9) 0.0735(5) Uani 1 1 d . . . F3 F 0.32622(15) 1.0143(2) 0.26047(12) 0.0994(7) Uani 1 1 d . . . F4 F 0.37620(16) 0.8747(2) 0.38295(10) 0.0981(7) Uani 1 1 d . . . F5 F 0.34238(13) 0.6100(2) 0.38621(8) 0.0751(6) Uani 1 1 d . . . F6 F 0.24070(12) 0.23470(19) 0.37528(10) 0.0790(6) Uani 1 1 d . . . F7 F 0.09923(15) 0.1986(2) 0.42116(12) 0.0961(7) Uani 1 1 d . . . F8 F -0.05463(13) 0.3437(2) 0.36693(11) 0.0925(7) Uani 1 1 d . . . F9 F -0.06247(12) 0.5292(2) 0.26524(11) 0.0842(6) Uani 1 1 d . . . F10 F 0.07959(11) 0.5692(2) 0.21908(10) 0.0745(6) Uani 1 1 d . . . F11 F 0.10553(11) 0.2783(2) 0.16627(10) 0.0756(6) Uani 1 1 d . . . F12 F 0.12142(14) 0.1343(2) 0.06002(11) 0.0893(6) Uani 1 1 d . . . F13 F 0.28083(15) 0.1215(2) 0.02999(10) 0.0906(7) Uani 1 1 d . . . F14 F 0.42690(14) 0.2577(2) 0.11222(11) 0.0873(7) Uani 1 1 d . . . F15 F 0.41231(11) 0.40606(19) 0.21902(10) 0.0716(5) Uani 1 1 d . . . N1 N 0.23193(14) 0.6743(2) -0.01230(11) 0.0445(5) Uani 1 1 d . . . N2 N 0.37288(14) 0.6961(2) 0.04720(11) 0.0443(5) Uani 1 1 d . . . C1 C 0.27716(17) 0.5961(3) 0.26436(13) 0.0443(6) Uani 1 1 d . . . C2 C 0.25484(18) 0.6732(3) 0.20444(14) 0.0473(7) Uani 1 1 d . . . C3 C 0.27003(19) 0.8110(3) 0.20203(15) 0.0517(7) Uani 1 1 d . . . C4 C 0.3112(2) 0.8796(3) 0.26177(18) 0.0613(8) Uani 1 1 d . . . C5 C 0.3363(2) 0.8090(4) 0.32324(16) 0.0616(8) Uani 1 1 d . . . C6 C 0.31853(19) 0.6715(3) 0.32313(14) 0.0530(7) Uani 1 1 d . . . C7 C 0.16915(17) 0.4071(3) 0.29542(13) 0.0460(7) Uani 1 1 d . . . C8 C 0.1676(2) 0.3133(3) 0.34608(15) 0.0536(7) Uani 1 1 d . . . C9 C 0.0946(2) 0.2910(3) 0.37062(17) 0.0616(8) Uani 1 1 d . . . C10 C 0.0172(2) 0.3631(3) 0.34393(17) 0.0611(8) Uani 1 1 d . . . C11 C 0.01394(19) 0.4576(3) 0.29309(16) 0.0565(8) Uani 1 1 d . . . C12 C 0.08866(19) 0.4770(3) 0.27045(14) 0.0503(7) Uani 1 1 d . . . C13 C 0.25867(18) 0.3489(3) 0.20014(14) 0.0466(7) Uani 1 1 d . . . C14 C 0.18800(19) 0.2773(3) 0.15606(16) 0.0546(8) Uani 1 1 d . . . C15 C 0.1938(2) 0.2014(3) 0.09990(17) 0.0613(8) Uani 1 1 d . . . C16 C 0.2741(2) 0.1946(3) 0.08512(17) 0.0631(8) Uani 1 1 d . . . C17 C 0.3469(2) 0.2624(3) 0.12626(18) 0.0601(8) Uani 1 1 d . . . C18 C 0.33778(19) 0.3378(3) 0.18103(16) 0.0533(7) Uani 1 1 d . . . C19 C 0.5275(2) 0.7267(5) 0.0438(2) 0.0988(14) Uani 1 1 d . . . H19A H 0.5063 0.7717 -0.0003 0.148 Uiso 1 1 calc R . . H19B H 0.5301 0.6301 0.0367 0.148 Uiso 1 1 calc R . . H19C H 0.5866 0.7599 0.0681 0.148 Uiso 1 1 calc R . . C20 C 0.4945(2) 0.6864(4) 0.15598(18) 0.0832(11) Uani 1 1 d . . . H20A H 0.4528 0.7064 0.1817 0.125 Uiso 1 1 calc R . . H20B H 0.5534 0.7193 0.1810 0.125 Uiso 1 1 calc R . . H20C H 0.4970 0.5895 0.1496 0.125 Uiso 1 1 calc R . . C21 C 0.4530(2) 0.9072(3) 0.0948(2) 0.0850(12) Uani 1 1 d . . . H21A H 0.4333 0.9498 0.0500 0.128 Uiso 1 1 calc R . . H21B H 0.5100 0.9452 0.1208 0.128 Uiso 1 1 calc R . . H21C H 0.4092 0.9228 0.1191 0.128 Uiso 1 1 calc R . . C22 C 0.46347(18) 0.7557(3) 0.08600(15) 0.0527(8) Uani 1 1 d . . . C23 C 0.3559(2) 0.5590(3) 0.03453(16) 0.0568(8) Uani 1 1 d . . . H23A H 0.3972 0.4883 0.0490 0.068 Uiso 1 1 calc R . . C24 C 0.2692(2) 0.5462(3) -0.00235(16) 0.0578(8) Uani 1 1 d . . . H24A H 0.2394 0.4649 -0.0184 0.069 Uiso 1 1 calc R . . C25 C 0.29683(16) 0.7628(3) 0.01784(13) 0.0435(6) Uani 1 1 d . . . H25A H 0.2898 0.8571 0.0182 0.052 Uiso 1 1 calc R . . C26 C 0.13557(17) 0.7072(3) -0.05112(14) 0.0498(7) Uani 1 1 d . . . C27 C 0.1213(2) 0.6664(4) -0.12636(16) 0.0797(11) Uani 1 1 d . . . H27A H 0.1598 0.7203 -0.1456 0.120 Uiso 1 1 calc R . . H27B H 0.0594 0.6817 -0.1523 0.120 Uiso 1 1 calc R . . H27C H 0.1356 0.5715 -0.1286 0.120 Uiso 1 1 calc R . . C28 C 0.1196(2) 0.8583(3) -0.04457(19) 0.0761(10) Uani 1 1 d . . . H28A H 0.1577 0.9093 -0.0655 0.114 Uiso 1 1 calc R . . H28B H 0.1335 0.8822 0.0035 0.114 Uiso 1 1 calc R . . H28C H 0.0575 0.8793 -0.0677 0.114 Uiso 1 1 calc R . . C29 C 0.07569(19) 0.6242(3) -0.01833(16) 0.0643(9) Uani 1 1 d . . . H29A H 0.0862 0.6521 0.0290 0.096 Uiso 1 1 calc R . . H29B H 0.0897 0.5290 -0.0198 0.096 Uiso 1 1 calc R . . H29C H 0.0135 0.6393 -0.0435 0.096 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.0353(16) 0.056(2) 0.0454(18) 0.0063(15) 0.0080(14) 0.0049(14) F1 0.0948(13) 0.0602(11) 0.0410(9) -0.0004(8) 0.0043(9) -0.0005(9) F2 0.0919(13) 0.0644(12) 0.0674(12) 0.0182(10) 0.0285(10) 0.0007(10) F3 0.1174(18) 0.0598(13) 0.1136(18) -0.0092(12) 0.0226(14) -0.0263(12) F4 0.1185(17) 0.0930(16) 0.0707(13) -0.0338(12) 0.0088(12) -0.0209(13) F5 0.0888(14) 0.0896(14) 0.0403(10) -0.0003(9) 0.0085(9) 0.0028(10) F6 0.0705(12) 0.0757(13) 0.0918(14) 0.0382(11) 0.0254(11) 0.0174(10) F7 0.1095(16) 0.0881(15) 0.1064(16) 0.0351(13) 0.0563(14) -0.0053(12) F8 0.0750(13) 0.1088(17) 0.1129(17) -0.0114(13) 0.0573(13) -0.0157(11) F9 0.0552(11) 0.0963(15) 0.1005(15) -0.0067(12) 0.0217(10) 0.0187(10) F10 0.0587(11) 0.0849(14) 0.0771(12) 0.0287(11) 0.0158(9) 0.0165(9) F11 0.0491(10) 0.0977(14) 0.0788(13) -0.0237(11) 0.0168(9) -0.0033(9) F12 0.0844(14) 0.0881(15) 0.0851(14) -0.0326(12) 0.0087(11) 0.0013(11) F13 0.1187(17) 0.0813(14) 0.0798(14) -0.0162(11) 0.0415(12) 0.0247(12) F14 0.0849(14) 0.0915(15) 0.1078(16) 0.0027(12) 0.0628(13) 0.0137(11) F15 0.0560(11) 0.0767(12) 0.0873(13) -0.0001(10) 0.0291(10) -0.0085(9) N1 0.0413(12) 0.0441(14) 0.0442(13) 0.0004(10) 0.0065(10) -0.0038(10) N2 0.0395(12) 0.0453(13) 0.0468(13) 0.0004(11) 0.0106(10) 0.0014(10) C1 0.0372(14) 0.0552(17) 0.0407(15) -0.0012(13) 0.0117(12) 0.0012(12) C2 0.0501(16) 0.0518(18) 0.0395(16) -0.0056(13) 0.0123(12) -0.0006(13) C3 0.0573(17) 0.0520(19) 0.0499(18) 0.0049(15) 0.0221(14) -0.0005(14) C4 0.066(2) 0.0473(19) 0.075(2) -0.0069(17) 0.0273(17) -0.0093(15) C5 0.0584(19) 0.071(2) 0.0531(19) -0.0208(17) 0.0123(15) -0.0109(16) C6 0.0487(16) 0.069(2) 0.0408(16) -0.0016(15) 0.0128(13) -0.0006(15) C7 0.0448(16) 0.0488(17) 0.0434(16) -0.0001(13) 0.0114(12) 0.0009(13) C8 0.0542(17) 0.0538(18) 0.0534(18) 0.0074(15) 0.0165(14) 0.0036(14) C9 0.075(2) 0.0521(18) 0.064(2) 0.0021(16) 0.0297(17) -0.0081(17) C10 0.0583(19) 0.063(2) 0.072(2) -0.0143(18) 0.0354(17) -0.0147(16) C11 0.0421(16) 0.0606(19) 0.066(2) -0.0136(17) 0.0142(15) 0.0042(14) C12 0.0522(17) 0.0528(17) 0.0452(16) 0.0020(14) 0.0129(14) 0.0011(14) C13 0.0471(16) 0.0420(16) 0.0494(16) 0.0086(13) 0.0122(13) 0.0045(12) C14 0.0505(18) 0.0555(19) 0.0580(19) 0.0003(15) 0.0164(15) 0.0074(14) C15 0.062(2) 0.0522(19) 0.064(2) -0.0054(16) 0.0083(16) 0.0073(16) C16 0.084(2) 0.0498(19) 0.058(2) 0.0005(16) 0.0239(18) 0.0158(17) C17 0.071(2) 0.0528(19) 0.069(2) 0.0116(16) 0.0389(18) 0.0166(16) C18 0.0515(17) 0.0485(17) 0.0623(19) 0.0105(15) 0.0203(15) -0.0005(14) C19 0.052(2) 0.152(4) 0.098(3) -0.027(3) 0.031(2) -0.017(2) C20 0.071(2) 0.094(3) 0.068(2) 0.007(2) -0.0057(18) -0.006(2) C21 0.052(2) 0.063(2) 0.124(3) -0.007(2) 0.001(2) -0.0124(17) C22 0.0370(15) 0.064(2) 0.0535(18) 0.0001(15) 0.0070(13) -0.0029(13) C23 0.0542(18) 0.0441(17) 0.068(2) 0.0020(15) 0.0124(15) 0.0056(14) C24 0.0587(19) 0.0427(17) 0.068(2) -0.0048(15) 0.0121(15) -0.0035(14) C25 0.0393(15) 0.0447(16) 0.0445(15) 0.0002(13) 0.0091(12) 0.0025(12) C26 0.0385(15) 0.0615(19) 0.0447(16) 0.0036(14) 0.0047(12) -0.0028(13) C27 0.0519(19) 0.131(3) 0.051(2) -0.003(2) 0.0071(15) -0.010(2) C28 0.0500(19) 0.063(2) 0.099(3) 0.0110(19) -0.0036(18) 0.0071(15) C29 0.0480(18) 0.076(2) 0.068(2) 0.0039(17) 0.0150(15) -0.0061(15) _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 B1 C1 1.633(4) . ? B1 C13 1.635(4) . ? B1 C7 1.636(4) . ? F1 C2 1.346(3) . ? F2 C3 1.348(3) . ? F3 C4 1.341(3) . ? F4 C5 1.346(3) . ? F5 C6 1.358(3) . ? F6 C8 1.353(3) . ? F7 C9 1.350(3) . ? F8 C10 1.338(3) . ? F9 C11 1.349(3) . ? F10 C12 1.351(3) . ? F11 C14 1.352(3) . ? F12 C15 1.344(4) . ? F13 C16 1.353(3) . ? F14 C17 1.350(3) . ? F15 C18 1.360(3) . ? N1 C25 1.331(3) . ? N1 C24 1.371(4) . ? N1 C26 1.503(3) . ? N2 C25 1.325(3) . ? N2 C23 1.378(4) . ? N2 C22 1.509(3) . ? C1 C2 1.381(4) . ? C1 C6 1.385(4) . ? C2 C3 1.374(4) . ? C3 C4 1.364(4) . ? C4 C5 1.373(4) . ? C5 C6 1.375(4) . ? C7 C8 1.380(4) . ? C7 C12 1.382(4) . ? C8 C9 1.378(4) . ? C9 C10 1.359(4) . ? C10 C11 1.372(4) . ? C11 C12 1.376(4) . ? C13 C14 1.382(4) . ? C13 C18 1.392(4) . ? C14 C15 1.381(4) . ? C15 C16 1.362(4) . ? C16 C17 1.362(5) . ? C17 C18 1.371(4) . ? C19 C22 1.511(4) . ? C20 C22 1.513(4) . ? C21 C22 1.509(4) . ? C23 C24 1.337(4) . ? C26 C28 1.513(4) . ? C26 C27 1.522(4) . ? C26 C29 1.523(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 C1 B1 C13 112.8(2) . . ? C1 B1 C7 110.7(2) . . ? C13 B1 C7 113.8(2) . . ? C25 N1 C24 107.5(2) . . ? C25 N1 C26 126.9(2) . . ? C24 N1 C26 125.6(2) . . ? C25 N2 C23 107.5(2) . . ? C25 N2 C22 127.6(2) . . ? C23 N2 C22 124.8(2) . . ? C2 C1 C6 113.1(3) . . ? C2 C1 B1 126.5(2) . . ? C6 C1 B1 120.4(2) . . ? F1 C2 C3 115.3(2) . . ? F1 C2 C1 120.1(2) . . ? C3 C2 C1 124.5(3) . . ? F2 C3 C4 119.3(3) . . ? F2 C3 C2 121.1(3) . . ? C4 C3 C2 119.6(3) . . ? F3 C4 C3 120.4(3) . . ? F3 C4 C5 120.5(3) . . ? C3 C4 C5 119.0(3) . . ? F4 C5 C4 120.1(3) . . ? F4 C5 C6 120.6(3) . . ? C4 C5 C6 119.2(3) . . ? F5 C6 C5 115.7(3) . . ? F5 C6 C1 119.8(3) . . ? C5 C6 C1 124.5(3) . . ? C8 C7 C12 113.0(3) . . ? C8 C7 B1 122.3(2) . . ? C12 C7 B1 124.7(3) . . ? F6 C8 C9 115.0(3) . . ? F6 C8 C7 120.5(3) . . ? C9 C8 C7 124.5(3) . . ? F7 C9 C10 119.5(3) . . ? F7 C9 C8 120.7(3) . . ? C10 C9 C8 119.8(3) . . ? F8 C10 C9 121.0(3) . . ? F8 C10 C11 120.2(3) . . ? C9 C10 C11 118.8(3) . . ? F9 C11 C10 119.8(3) . . ? F9 C11 C12 120.7(3) . . ? C10 C11 C12 119.5(3) . . ? F10 C12 C11 116.0(2) . . ? F10 C12 C7 119.4(2) . . ? C11 C12 C7 124.5(3) . . ? C14 C13 C18 112.2(3) . . ? C14 C13 B1 127.8(3) . . ? C18 C13 B1 119.9(2) . . ? F11 C14 C15 114.9(3) . . ? F11 C14 C13 120.2(3) . . ? C15 C14 C13 124.9(3) . . ? F12 C15 C16 120.0(3) . . ? F12 C15 C14 120.7(3) . . ? C16 C15 C14 119.3(3) . . ? F13 C16 C17 120.6(3) . . ? F13 C16 C15 120.1(3) . . ? C17 C16 C15 119.3(3) . . ? F14 C17 C16 120.2(3) . . ? F14 C17 C18 120.4(3) . . ? C16 C17 C18 119.4(3) . . ? F15 C18 C17 116.6(3) . . ? F15 C18 C13 118.4(3) . . ? C17 C18 C13 124.9(3) . . ? C21 C22 N2 109.0(2) . . ? C21 C22 C19 111.2(3) . . ? N2 C22 C19 107.4(2) . . ? C21 C22 C20 110.3(3) . . ? N2 C22 C20 107.7(2) . . ? C19 C22 C20 111.1(3) . . ? C24 C23 N2 107.5(3) . . ? C23 C24 N1 107.8(3) . . ? N2 C25 N1 109.7(2) . . ? N1 C26 C28 109.1(2) . . ? N1 C26 C27 107.2(2) . . ? C28 C26 C27 111.4(3) . . ? N1 C26 C29 107.3(2) . . ? C28 C26 C29 110.4(3) . . ? C27 C26 C29 111.4(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.170 _refine_diff_density_min -0.191 _refine_diff_density_rms 0.038 #===end