# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 182/1312 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Mark Thornton-Pett School of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_phone '+44 (0)113 2336423' _publ_contact_author_fax '+44 (0)113 2336565' _publ_contact_author_email marktp@chem.leeds.ac.uk _publ_requested_journal 'J. Chem. Soc., Chem. Commun.' _publ_contact_letter ; The following two CIFs form the supplementary data for manuscript 9/03788H. ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; New weakly coordinating counteranions for high activity polymerisation catalysts: [(C~6~F~5~)~3~B-CN-B(C~6~F~5~)~3]^-^ and [Ni{CNB(C~6~F~5~)~3~}~4~] ; loop_ _publ_author_name _publ_author_address 'Simon J. Lancaster' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Dennis A. Walker' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Mark Thornton-Pett' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Manfred Bochmann' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; #================================================================= data_daw2_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C116 H34 B4 Cl4 F60 N4 Ni' _chemical_formula_weight 2867.22 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' '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' 'Ni' 'Ni' 0.3393 1.1124 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/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 12.03400(10) _cell_length_b 14.62970(10) _cell_length_c 31.8468(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.6920(6) _cell_angle_gamma 90.00 _cell_volume 5509.41(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 129356 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.728 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2828 _exptl_absorpt_coefficient_mu 0.430 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.8607 _exptl_absorpt_correction_T_max 0.9503 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean '9.091 pixels/mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 114737 _diffrn_reflns_av_R_equivalents 0.0540 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.00 _reflns_number_total 10807 _reflns_number_gt 9064 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0376P)^2^+3.1149P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00045(14) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 10807 _refine_ls_number_parameters 854 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0453 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0857 _refine_ls_wR_factor_gt 0.0806 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.007 _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 Ni1 Ni 0.0000 1.0000 0.0000 0.02110(8) Uani 1 2 d S . . B1 B 0.00835(17) 0.75230(14) 0.08783(7) 0.0266(4) Uani 1 1 d . . . C1 C -0.00300(14) 0.90084(12) 0.03606(5) 0.0253(4) Uani 1 1 d . . . N1 N -0.00259(12) 0.83693(10) 0.05684(5) 0.0269(3) Uani 1 1 d . . . C111 C -0.05243(15) 0.78692(12) 0.12688(6) 0.0267(4) Uani 1 1 d . . . C112 C -0.16607(16) 0.81147(13) 0.11861(6) 0.0317(4) Uani 1 1 d . . . C113 C -0.22560(16) 0.83992(14) 0.14906(7) 0.0371(5) Uani 1 1 d . . . C114 C -0.17073(18) 0.84772(14) 0.19088(6) 0.0376(5) Uani 1 1 d . . . C115 C -0.05791(17) 0.82547(14) 0.20099(6) 0.0363(4) Uani 1 1 d . . . C116 C -0.00165(15) 0.79590(13) 0.16942(6) 0.0307(4) Uani 1 1 d . . . F112 F -0.22471(9) 0.80587(9) 0.07796(4) 0.0432(3) Uani 1 1 d . . . F113 F -0.33623(10) 0.85954(10) 0.13852(4) 0.0579(4) Uani 1 1 d . . . F114 F -0.22623(11) 0.87622(9) 0.22124(4) 0.0517(3) Uani 1 1 d . . . F115 F -0.00341(11) 0.83356(10) 0.24171(4) 0.0541(3) Uani 1 1 d . . . F116 F 0.10892(9) 0.77551(9) 0.18232(4) 0.0435(3) Uani 1 1 d . . . C121 C -0.05880(14) 0.66791(12) 0.06004(6) 0.0266(4) Uani 1 1 d . . . C122 C -0.13120(16) 0.60637(13) 0.07450(6) 0.0328(4) Uani 1 1 d . . . C123 C -0.18530(17) 0.53595(13) 0.05003(7) 0.0375(5) Uani 1 1 d . . . C124 C -0.16777(17) 0.52310(13) 0.00899(7) 0.0368(5) Uani 1 1 d . . . C125 C -0.09581(16) 0.58087(13) -0.00678(6) 0.0334(4) Uani 1 1 d . . . C126 C -0.04310(15) 0.65016(12) 0.01867(6) 0.0299(4) Uani 1 1 d . . . F122 F -0.15102(11) 0.61258(8) 0.11481(4) 0.0467(3) Uani 1 1 d . . . F123 F -0.25423(11) 0.47911(8) 0.06637(5) 0.0543(3) Uani 1 1 d . . . F124 F -0.21905(11) 0.45413(8) -0.01486(4) 0.0533(3) Uani 1 1 d . . . F125 F -0.07573(11) 0.56834(8) -0.04655(4) 0.0460(3) Uani 1 1 d . . . F126 F 0.03047(10) 0.70199(8) 0.00165(4) 0.0390(3) Uani 1 1 d . . . C131 C 0.14379(15) 0.72905(12) 0.10101(6) 0.0274(4) Uani 1 1 d . . . C132 C 0.18260(16) 0.64097(13) 0.11190(6) 0.0339(4) Uani 1 1 d . . . C133 C 0.29554(17) 0.61704(14) 0.12039(7) 0.0379(5) Uani 1 1 d . . . C134 C 0.37656(16) 0.68214(14) 0.11953(6) 0.0353(4) Uani 1 1 d . . . C135 C 0.34387(15) 0.77105(13) 0.11017(6) 0.0318(4) Uani 1 1 d . . . C136 C 0.22996(15) 0.79187(12) 0.10132(6) 0.0281(4) Uani 1 1 d . . . F132 F 0.10823(10) 0.57364(8) 0.11540(4) 0.0517(3) Uani 1 1 d . . . F133 F 0.32656(11) 0.53000(9) 0.13013(5) 0.0588(4) Uani 1 1 d . . . F134 F 0.48687(10) 0.66034(9) 0.12803(4) 0.0478(3) Uani 1 1 d . . . F135 F 0.42184(9) 0.83626(8) 0.10988(4) 0.0459(3) Uani 1 1 d . . . F136 F 0.20605(9) 0.88143(7) 0.09356(4) 0.0405(3) Uani 1 1 d . . . B2 B 0.26865(16) 1.16172(13) 0.09063(6) 0.0236(4) Uani 1 1 d . . . C2 C 0.10627(14) 1.06210(11) 0.03983(5) 0.0232(4) Uani 1 1 d . . . N2 N 0.17186(11) 1.10486(9) 0.06219(4) 0.0231(3) Uani 1 1 d . . . C211 C 0.33709(14) 1.08964(12) 0.12545(6) 0.0260(4) Uani 1 1 d . . . C212 C 0.27662(15) 1.03715(13) 0.14973(6) 0.0300(4) Uani 1 1 d . . . C213 C 0.32572(18) 0.97954(13) 0.18217(6) 0.0383(5) Uani 1 1 d . . . C214 C 0.4416(2) 0.97373(14) 0.19213(7) 0.0443(5) Uani 1 1 d . . . C215 C 0.50572(17) 1.02478(14) 0.16957(7) 0.0389(5) Uani 1 1 d . . . C216 C 0.45346(15) 1.08050(12) 0.13694(6) 0.0321(4) Uani 1 1 d . . . F212 F 0.16225(9) 1.04225(8) 0.14231(3) 0.0355(3) Uani 1 1 d . . . F213 F 0.26096(12) 0.93124(9) 0.20434(4) 0.0556(3) Uani 1 1 d . . . F214 F 0.49121(13) 0.91940(9) 0.22427(5) 0.0663(4) Uani 1 1 d . . . F215 F 0.61927(10) 1.02215(9) 0.17992(5) 0.0568(4) Uani 1 1 d . . . F216 F 0.52290(9) 1.12936(8) 0.11679(4) 0.0407(3) Uani 1 1 d . . . C221 C 0.21497(14) 1.24068(11) 0.11709(5) 0.0237(4) Uani 1 1 d . . . C222 C 0.28672(15) 1.28941(12) 0.14860(6) 0.0271(4) Uani 1 1 d . . . C223 C 0.25244(17) 1.35841(12) 0.17249(6) 0.0310(4) Uani 1 1 d . . . C224 C 0.14041(17) 1.38257(13) 0.16546(6) 0.0335(4) Uani 1 1 d . . . C225 C 0.06538(15) 1.33714(13) 0.13481(6) 0.0320(4) Uani 1 1 d . . . C226 C 0.10326(14) 1.26734(12) 0.11187(6) 0.0268(4) Uani 1 1 d . . . F222 F 0.39907(8) 1.27072(7) 0.15595(4) 0.0365(3) Uani 1 1 d . . . F223 F 0.32761(10) 1.40292(8) 0.20198(4) 0.0439(3) Uani 1 1 d . . . F224 F 0.10443(11) 1.45063(8) 0.18776(4) 0.0475(3) Uani 1 1 d . . . F225 F -0.04437(10) 1.36124(9) 0.12713(4) 0.0482(3) Uani 1 1 d . . . F226 F 0.02299(8) 1.22576(8) 0.08268(4) 0.0363(3) Uani 1 1 d . . . C231 C 0.34060(14) 1.20294(12) 0.05569(5) 0.0253(4) Uani 1 1 d . . . C232 C 0.38845(15) 1.14283(13) 0.03021(6) 0.0310(4) Uani 1 1 d . . . C233 C 0.44481(16) 1.16905(15) -0.00173(6) 0.0370(5) Uani 1 1 d . . . C234 C 0.45789(17) 1.26071(16) -0.00906(6) 0.0388(5) Uani 1 1 d . . . C235 C 0.41331(16) 1.32360(14) 0.01515(6) 0.0344(4) Uani 1 1 d . . . C236 C 0.35534(14) 1.29402(12) 0.04642(6) 0.0272(4) Uani 1 1 d . . . F232 F 0.37973(10) 1.05188(7) 0.03666(4) 0.0400(3) Uani 1 1 d . . . F233 F 0.48640(11) 1.10661(9) -0.02551(4) 0.0523(3) Uani 1 1 d . . . F234 F 0.51341(11) 1.28840(10) -0.03957(4) 0.0561(4) Uani 1 1 d . . . F235 F 0.42622(10) 1.41343(8) 0.00862(4) 0.0475(3) Uani 1 1 d . . . F236 F 0.31349(9) 1.36142(7) 0.06805(3) 0.0334(2) Uani 1 1 d . . . C3 C 0.77284(15) 0.21767(12) 0.13985(6) 0.0286(4) Uani 1 1 d . . . C311 C 0.76443(14) 0.18268(12) 0.09684(6) 0.0285(4) Uani 1 1 d . . . C312 C 0.76004(14) 0.24250(13) 0.06195(6) 0.0308(4) Uani 1 1 d . . . H312 H 0.7621 0.3067 0.0665 0.037 Uiso 1 1 calc R . . C313 C 0.75278(16) 0.20805(14) 0.02107(6) 0.0362(4) Uani 1 1 d . . . H313 H 0.7514 0.2486 -0.0023 0.043 Uiso 1 1 calc R . . C314 C 0.74742(17) 0.11429(15) 0.01422(7) 0.0394(5) Uani 1 1 d . . . H314 H 0.7412 0.0910 -0.0140 0.047 Uiso 1 1 calc R . . C315 C 0.75111(17) 0.05449(14) 0.04818(7) 0.0407(5) Uani 1 1 d . . . H315 H 0.7472 -0.0095 0.0432 0.049 Uiso 1 1 calc R . . C316 C 0.76048(16) 0.08748(13) 0.08918(7) 0.0350(4) Uani 1 1 d . . . H316 H 0.7643 0.0461 0.1124 0.042 Uiso 1 1 calc R . . C321 C 0.83618(16) 0.16684(12) 0.17555(6) 0.0304(4) Uani 1 1 d . . . C322 C 0.80072(17) 0.16571(13) 0.21529(6) 0.0351(4) Uani 1 1 d . . . H322 H 0.7347 0.1983 0.2187 0.042 Uiso 1 1 calc R . . C323 C 0.86107(19) 0.11782(14) 0.24917(7) 0.0409(5) Uani 1 1 d . . . H323 H 0.8353 0.1157 0.2756 0.049 Uiso 1 1 calc R . . C324 C 0.95929(19) 0.07267(15) 0.24475(7) 0.0446(5) Uani 1 1 d . . . H324 H 1.0020 0.0412 0.2685 0.054 Uiso 1 1 calc R . . C325 C 0.99576(18) 0.07300(15) 0.20595(7) 0.0428(5) Uani 1 1 d . . . H325 H 1.0634 0.0419 0.2032 0.051 Uiso 1 1 calc R . . C326 C 0.93420(16) 0.11824(13) 0.17133(7) 0.0345(4) Uani 1 1 d . . . H326 H 0.9581 0.1166 0.1445 0.041 Uiso 1 1 calc R . . C331 C 0.72020(15) 0.30295(12) 0.14739(6) 0.0295(4) Uani 1 1 d . . . C332 C 0.62099(15) 0.33306(13) 0.12028(6) 0.0329(4) Uani 1 1 d . . . H332 H 0.5878 0.2969 0.0964 0.039 Uiso 1 1 calc R . . C333 C 0.57188(17) 0.41475(14) 0.12822(7) 0.0406(5) Uani 1 1 d . . . H333 H 0.5044 0.4345 0.1101 0.049 Uiso 1 1 calc R . . C334 C 0.6206(2) 0.46818(15) 0.16260(7) 0.0470(5) Uani 1 1 d . . . H334 H 0.5863 0.5245 0.1679 0.056 Uiso 1 1 calc R . . C335 C 0.7189(2) 0.44022(15) 0.18934(7) 0.0455(5) Uani 1 1 d . . . H335 H 0.7522 0.4778 0.2126 0.055 Uiso 1 1 calc R . . C336 C 0.76839(18) 0.35833(13) 0.18232(6) 0.0365(4) Uani 1 1 d . . . H336 H 0.8352 0.3390 0.2010 0.044 Uiso 1 1 calc R . . Cl1S Cl 0.29070(7) 0.16482(5) 0.25178(3) 0.0726(2) Uani 1 1 d . . . Cl2S Cl 0.53628(7) 0.14532(6) 0.26859(2) 0.0808(2) Uani 1 1 d . . . C1S C 0.4212(3) 0.22047(19) 0.26656(10) 0.0742(9) Uani 1 1 d . . . H1SA H 0.4249 0.2491 0.2950 0.089 Uiso 1 1 calc R . . H1SB H 0.4269 0.2697 0.2458 0.089 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 Ni1 0.02311(16) 0.01799(15) 0.02025(16) 0.00143(12) -0.00106(11) -0.00297(12) B1 0.0282(10) 0.0239(10) 0.0262(10) 0.0055(8) 0.0016(8) -0.0028(8) C1 0.0223(9) 0.0280(9) 0.0234(9) -0.0016(7) -0.0016(7) -0.0031(7) N1 0.0264(8) 0.0265(8) 0.0263(8) 0.0041(6) 0.0010(6) -0.0018(6) C111 0.0297(9) 0.0216(9) 0.0276(9) 0.0040(7) 0.0021(7) -0.0011(7) C112 0.0335(10) 0.0306(10) 0.0286(10) -0.0003(8) -0.0006(8) 0.0014(8) C113 0.0288(10) 0.0388(11) 0.0423(12) -0.0039(9) 0.0029(8) 0.0057(8) C114 0.0439(12) 0.0360(11) 0.0345(11) -0.0026(9) 0.0116(9) 0.0053(9) C115 0.0418(11) 0.0379(11) 0.0273(10) 0.0003(8) 0.0015(8) 0.0019(9) C116 0.0265(9) 0.0314(10) 0.0323(10) 0.0048(8) 0.0003(8) 0.0012(7) F112 0.0345(6) 0.0565(7) 0.0338(6) -0.0071(5) -0.0065(5) 0.0100(5) F113 0.0339(7) 0.0801(10) 0.0570(8) -0.0186(7) 0.0016(6) 0.0183(6) F114 0.0542(8) 0.0613(8) 0.0422(7) -0.0086(6) 0.0155(6) 0.0150(6) F115 0.0552(8) 0.0764(9) 0.0272(6) -0.0079(6) -0.0019(5) 0.0143(7) F116 0.0311(6) 0.0652(8) 0.0309(6) 0.0023(6) -0.0022(5) 0.0064(5) C121 0.0260(9) 0.0236(9) 0.0290(9) 0.0043(7) 0.0021(7) 0.0003(7) C122 0.0379(11) 0.0272(10) 0.0349(11) 0.0021(8) 0.0113(8) -0.0020(8) C123 0.0340(11) 0.0244(9) 0.0549(13) 0.0028(9) 0.0100(9) -0.0039(8) C124 0.0342(10) 0.0262(10) 0.0462(12) -0.0081(8) -0.0029(9) 0.0013(8) C125 0.0374(11) 0.0314(10) 0.0299(10) -0.0010(8) 0.0021(8) 0.0085(8) C126 0.0277(9) 0.0278(9) 0.0335(10) 0.0048(8) 0.0040(8) 0.0025(7) F122 0.0671(8) 0.0361(6) 0.0435(7) 0.0011(5) 0.0272(6) -0.0143(6) F123 0.0541(8) 0.0347(7) 0.0780(10) -0.0008(6) 0.0227(7) -0.0184(6) F124 0.0551(8) 0.0337(7) 0.0654(9) -0.0172(6) -0.0036(6) -0.0054(6) F125 0.0595(8) 0.0445(7) 0.0324(6) -0.0069(5) 0.0050(5) 0.0092(6) F126 0.0443(7) 0.0394(6) 0.0363(6) 0.0037(5) 0.0153(5) -0.0049(5) C131 0.0312(9) 0.0271(9) 0.0231(9) 0.0032(7) 0.0034(7) 0.0014(7) C132 0.0364(11) 0.0303(10) 0.0338(10) 0.0083(8) 0.0035(8) -0.0003(8) C133 0.0421(12) 0.0319(10) 0.0385(11) 0.0081(9) 0.0040(9) 0.0121(9) C134 0.0299(10) 0.0451(12) 0.0304(10) 0.0041(9) 0.0043(8) 0.0108(9) C135 0.0285(10) 0.0368(10) 0.0299(10) -0.0004(8) 0.0050(8) -0.0013(8) C136 0.0315(10) 0.0244(9) 0.0273(9) -0.0005(7) 0.0029(7) 0.0025(7) F132 0.0448(7) 0.0334(6) 0.0720(9) 0.0253(6) -0.0017(6) -0.0038(5) F133 0.0544(8) 0.0365(7) 0.0820(10) 0.0196(7) 0.0034(7) 0.0172(6) F134 0.0315(6) 0.0620(8) 0.0499(7) 0.0091(6) 0.0073(5) 0.0173(6) F135 0.0282(6) 0.0457(7) 0.0623(8) 0.0006(6) 0.0047(5) -0.0060(5) F136 0.0320(6) 0.0233(5) 0.0616(8) 0.0003(5) -0.0034(5) -0.0016(4) B2 0.0212(9) 0.0238(10) 0.0241(10) -0.0034(8) -0.0002(7) -0.0030(7) C2 0.0259(9) 0.0203(8) 0.0229(9) 0.0033(7) 0.0033(7) 0.0016(7) N2 0.0231(7) 0.0229(7) 0.0229(7) -0.0005(6) 0.0027(6) -0.0002(6) C211 0.0262(9) 0.0242(9) 0.0256(9) -0.0046(7) -0.0003(7) 0.0004(7) C212 0.0295(10) 0.0303(9) 0.0282(10) -0.0027(8) 0.0003(7) 0.0014(8) C213 0.0517(13) 0.0300(10) 0.0307(10) 0.0037(8) 0.0011(9) -0.0023(9) C214 0.0556(14) 0.0301(10) 0.0379(12) 0.0019(9) -0.0157(10) 0.0072(9) C215 0.0309(10) 0.0313(10) 0.0473(12) -0.0061(9) -0.0116(9) 0.0048(8) C216 0.0299(10) 0.0263(9) 0.0373(11) -0.0044(8) -0.0008(8) 0.0002(7) F212 0.0299(6) 0.0427(6) 0.0349(6) 0.0052(5) 0.0087(5) -0.0006(5) F213 0.0718(9) 0.0504(8) 0.0435(7) 0.0186(6) 0.0075(6) -0.0062(7) F214 0.0777(10) 0.0467(8) 0.0599(9) 0.0187(7) -0.0249(7) 0.0105(7) F215 0.0329(7) 0.0474(7) 0.0782(10) -0.0031(7) -0.0210(6) 0.0094(5) F216 0.0226(5) 0.0405(6) 0.0571(8) 0.0018(6) 0.0025(5) -0.0020(5) C221 0.0252(9) 0.0227(8) 0.0232(9) 0.0019(7) 0.0049(7) -0.0025(7) C222 0.0269(9) 0.0274(9) 0.0263(9) -0.0005(7) 0.0030(7) -0.0018(7) C223 0.0420(11) 0.0266(9) 0.0238(9) -0.0043(7) 0.0046(8) -0.0071(8) C224 0.0468(12) 0.0258(9) 0.0318(10) -0.0027(8) 0.0174(9) 0.0021(8) C225 0.0283(10) 0.0318(10) 0.0387(11) 0.0028(8) 0.0136(8) 0.0036(8) C226 0.0259(9) 0.0270(9) 0.0270(9) -0.0007(7) 0.0038(7) -0.0021(7) F222 0.0251(5) 0.0389(6) 0.0419(6) -0.0106(5) -0.0033(5) -0.0031(4) F223 0.0554(7) 0.0394(6) 0.0336(6) -0.0147(5) 0.0000(5) -0.0077(5) F224 0.0652(8) 0.0368(7) 0.0455(7) -0.0128(5) 0.0232(6) 0.0073(6) F225 0.0314(6) 0.0493(7) 0.0667(9) -0.0098(6) 0.0162(6) 0.0098(5) F226 0.0222(5) 0.0410(6) 0.0432(6) -0.0107(5) -0.0006(5) 0.0009(4) C231 0.0205(8) 0.0291(9) 0.0247(9) -0.0031(7) 0.0002(7) -0.0014(7) C232 0.0284(9) 0.0307(10) 0.0333(10) -0.0052(8) 0.0043(8) -0.0011(8) C233 0.0317(10) 0.0498(12) 0.0312(10) -0.0082(9) 0.0105(8) 0.0044(9) C234 0.0319(10) 0.0573(13) 0.0289(10) 0.0062(9) 0.0104(8) 0.0016(9) C235 0.0310(10) 0.0363(11) 0.0355(11) 0.0081(8) 0.0051(8) -0.0004(8) C236 0.0223(9) 0.0304(9) 0.0277(9) -0.0012(7) 0.0017(7) 0.0014(7) F232 0.0448(7) 0.0297(6) 0.0482(7) -0.0107(5) 0.0154(5) -0.0006(5) F233 0.0551(8) 0.0617(8) 0.0464(7) -0.0135(6) 0.0255(6) 0.0078(6) F234 0.0559(8) 0.0749(10) 0.0452(7) 0.0137(7) 0.0292(6) 0.0037(7) F235 0.0503(7) 0.0407(7) 0.0548(8) 0.0170(6) 0.0184(6) -0.0010(6) F236 0.0391(6) 0.0260(5) 0.0365(6) 0.0006(5) 0.0108(5) 0.0021(4) C3 0.0237(9) 0.0274(9) 0.0357(10) 0.0005(8) 0.0085(7) -0.0043(7) C311 0.0233(9) 0.0301(9) 0.0325(10) -0.0025(8) 0.0059(7) -0.0002(7) C312 0.0237(9) 0.0312(10) 0.0369(11) -0.0018(8) 0.0044(8) -0.0024(7) C313 0.0299(10) 0.0452(12) 0.0334(11) 0.0002(9) 0.0055(8) -0.0038(8) C314 0.0350(11) 0.0472(12) 0.0370(11) -0.0108(9) 0.0091(9) -0.0028(9) C315 0.0412(12) 0.0330(11) 0.0488(13) -0.0120(9) 0.0105(9) -0.0016(9) C316 0.0339(10) 0.0312(10) 0.0407(11) -0.0008(8) 0.0086(8) 0.0001(8) C321 0.0320(10) 0.0271(9) 0.0328(10) 0.0012(8) 0.0073(8) -0.0010(7) C322 0.0366(11) 0.0323(10) 0.0382(11) 0.0003(8) 0.0120(9) 0.0014(8) C323 0.0511(13) 0.0387(11) 0.0357(11) 0.0071(9) 0.0153(9) -0.0005(9) C324 0.0451(12) 0.0454(12) 0.0438(12) 0.0188(10) 0.0092(10) 0.0034(10) C325 0.0358(11) 0.0456(12) 0.0488(13) 0.0167(10) 0.0129(9) 0.0097(9) C326 0.0347(10) 0.0341(10) 0.0372(11) 0.0055(8) 0.0127(8) 0.0025(8) C331 0.0291(9) 0.0285(9) 0.0315(10) 0.0008(8) 0.0072(8) 0.0004(7) C332 0.0287(10) 0.0334(10) 0.0365(11) 0.0000(8) 0.0057(8) -0.0010(8) C333 0.0330(11) 0.0386(11) 0.0495(13) 0.0023(10) 0.0062(9) 0.0080(9) C334 0.0535(14) 0.0368(11) 0.0513(14) -0.0041(10) 0.0111(11) 0.0139(10) C335 0.0582(14) 0.0373(12) 0.0391(12) -0.0088(9) 0.0042(10) 0.0071(10) C336 0.0412(11) 0.0337(10) 0.0329(10) 0.0000(8) 0.0023(9) 0.0041(8) Cl1S 0.0892(5) 0.0466(4) 0.0822(5) 0.0002(3) 0.0163(4) -0.0102(3) Cl2S 0.0846(5) 0.1043(6) 0.0554(4) -0.0165(4) 0.0181(4) -0.0091(4) C1S 0.097(2) 0.0533(16) 0.0633(18) 0.0094(13) -0.0096(16) -0.0134(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 Ni1 C1 1.8547(18) . ? Ni1 C2 1.8621(17) . ? B1 N1 1.574(2) . ? B1 C111 1.635(3) . ? B1 C121 1.642(3) . ? B1 C131 1.642(3) . ? C1 N1 1.145(2) . ? C111 C116 1.385(3) . ? C111 C112 1.391(3) . ? C112 F112 1.357(2) . ? C112 C113 1.373(3) . ? C113 F113 1.342(2) . ? C113 C114 1.377(3) . ? C114 F114 1.339(2) . ? C114 C115 1.375(3) . ? C115 F115 1.345(2) . ? C115 C116 1.382(3) . ? C116 F116 1.351(2) . ? C121 C126 1.390(3) . ? C121 C122 1.389(3) . ? C122 F122 1.351(2) . ? C122 C123 1.380(3) . ? C123 F123 1.346(2) . ? C123 C124 1.375(3) . ? C124 F124 1.342(2) . ? C124 C125 1.370(3) . ? C125 F125 1.345(2) . ? C125 C126 1.377(3) . ? C126 F126 1.353(2) . ? C131 C136 1.384(3) . ? C131 C132 1.392(3) . ? C132 F132 1.349(2) . ? C132 C133 1.381(3) . ? C133 F133 1.347(2) . ? C133 C134 1.367(3) . ? C134 F134 1.343(2) . ? C134 C135 1.375(3) . ? C135 F135 1.339(2) . ? C135 C136 1.381(3) . ? C136 F136 1.354(2) . ? B2 N2 1.574(2) . ? B2 C221 1.632(3) . ? B2 C211 1.637(3) . ? B2 C231 1.646(3) . ? C2 N2 1.146(2) . ? C211 C212 1.388(3) . ? C211 C216 1.387(3) . ? C212 F212 1.355(2) . ? C212 C213 1.379(3) . ? C213 F213 1.345(2) . ? C213 C214 1.374(3) . ? C214 F214 1.345(2) . ? C214 C215 1.370(3) . ? C215 F215 1.345(2) . ? C215 C216 1.377(3) . ? C216 F216 1.349(2) . ? C221 C226 1.380(2) . ? C221 C222 1.393(2) . ? C222 F222 1.356(2) . ? C222 C223 1.373(3) . ? C223 F223 1.345(2) . ? C223 C224 1.371(3) . ? C224 F224 1.341(2) . ? C224 C225 1.372(3) . ? C225 F225 1.345(2) . ? C225 C226 1.381(3) . ? C226 F226 1.354(2) . ? C231 C236 1.383(2) . ? C231 C232 1.392(3) . ? C232 F232 1.353(2) . ? C232 C233 1.377(3) . ? C233 F233 1.341(2) . ? C233 C234 1.375(3) . ? C234 F234 1.340(2) . ? C234 C235 1.372(3) . ? C235 F235 1.344(2) . ? C235 C236 1.387(3) . ? C236 F236 1.353(2) . ? C3 C331 1.439(3) . ? C3 C311 1.448(3) . ? C3 C321 1.451(3) . ? C311 C312 1.408(3) . ? C311 C316 1.413(3) . ? C312 C313 1.384(3) . ? C313 C314 1.389(3) . ? C314 C315 1.386(3) . ? C315 C316 1.377(3) . ? C321 C326 1.405(3) . ? C321 C322 1.409(3) . ? C322 C323 1.375(3) . ? C323 C324 1.384(3) . ? C324 C325 1.386(3) . ? C325 C326 1.378(3) . ? C331 C332 1.408(3) . ? C331 C336 1.411(3) . ? C332 C333 1.377(3) . ? C333 C334 1.384(3) . ? C334 C335 1.385(3) . ? C335 C336 1.375(3) . ? Cl1S C1S 1.754(3) . ? Cl2S C1S 1.760(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 C1 Ni1 C2 87.15(7) . 3_575 ? C1 Ni1 C2 92.85(7) . . ? N1 B1 C111 103.65(14) . . ? N1 B1 C121 106.14(14) . . ? C111 B1 C121 113.45(15) . . ? N1 B1 C131 106.67(14) . . ? C111 B1 C131 115.64(15) . . ? C121 B1 C131 110.37(15) . . ? N1 C1 Ni1 176.47(16) . . ? C1 N1 B1 174.82(17) . . ? C116 C111 C112 113.60(17) . . ? C116 C111 B1 126.48(16) . . ? C112 C111 B1 119.92(16) . . ? F112 C112 C113 116.43(16) . . ? F112 C112 C111 118.93(16) . . ? C113 C112 C111 124.63(17) . . ? F113 C113 C112 120.77(18) . . ? F113 C113 C114 119.96(18) . . ? C112 C113 C114 119.27(18) . . ? F114 C114 C115 120.51(18) . . ? F114 C114 C113 120.66(18) . . ? C115 C114 C113 118.82(18) . . ? F115 C115 C114 119.23(18) . . ? F115 C115 C116 120.79(17) . . ? C114 C115 C116 119.98(18) . . ? F116 C116 C111 120.50(17) . . ? F116 C116 C115 115.82(16) . . ? C111 C116 C115 123.68(17) . . ? C126 C121 C122 113.39(16) . . ? C126 C121 B1 120.78(16) . . ? C122 C121 B1 125.78(16) . . ? F122 C122 C123 116.01(17) . . ? F122 C122 C121 120.22(17) . . ? C123 C122 C121 123.75(18) . . ? F123 C123 C124 119.84(18) . . ? F123 C123 C122 120.20(19) . . ? C124 C123 C122 119.96(18) . . ? F124 C124 C125 120.77(19) . . ? F124 C124 C123 120.34(19) . . ? C125 C124 C123 118.88(18) . . ? F125 C125 C124 119.80(18) . . ? F125 C125 C126 120.73(18) . . ? C124 C125 C126 119.46(18) . . ? F126 C126 C125 116.17(17) . . ? F126 C126 C121 119.28(16) . . ? C125 C126 C121 124.53(17) . . ? C136 C131 C132 113.35(17) . . ? C136 C131 B1 124.84(15) . . ? C132 C131 B1 121.78(16) . . ? F132 C132 C133 116.27(17) . . ? F132 C132 C131 119.95(17) . . ? C133 C132 C131 123.77(18) . . ? F133 C133 C134 119.68(18) . . ? F133 C133 C132 120.37(19) . . ? C134 C133 C132 119.95(18) . . ? F134 C134 C133 120.83(18) . . ? F134 C134 C135 120.04(18) . . ? C133 C134 C135 119.13(17) . . ? F135 C135 C134 120.17(17) . . ? F135 C135 C136 120.77(17) . . ? C134 C135 C136 119.07(17) . . ? F136 C136 C131 120.49(16) . . ? F136 C136 C135 114.82(16) . . ? C131 C136 C135 124.67(17) . . ? N2 B2 C221 110.46(14) . . ? N2 B2 C211 105.95(14) . . ? C221 B2 C211 107.68(14) . . ? N2 B2 C231 103.33(13) . . ? C221 B2 C231 113.45(14) . . ? C211 B2 C231 115.61(14) . . ? N2 C2 Ni1 175.22(15) . . ? C2 N2 B2 175.58(17) . . ? C212 C211 C216 114.07(16) . . ? C212 C211 B2 118.93(15) . . ? C216 C211 B2 126.68(16) . . ? F212 C212 C213 116.40(17) . . ? F212 C212 C211 119.56(16) . . ? C213 C212 C211 124.04(18) . . ? F213 C213 C214 120.55(18) . . ? F213 C213 C212 120.34(19) . . ? C214 C213 C212 119.10(19) . . ? F214 C214 C215 120.5(2) . . ? F214 C214 C213 120.0(2) . . ? C215 C214 C213 119.46(18) . . ? F215 C215 C214 120.10(18) . . ? F215 C215 C216 120.2(2) . . ? C214 C215 C216 119.70(18) . . ? F216 C216 C215 115.85(17) . . ? F216 C216 C211 120.51(16) . . ? C215 C216 C211 123.61(19) . . ? C226 C221 C222 113.72(16) . . ? C226 C221 B2 127.43(15) . . ? C222 C221 B2 118.85(15) . . ? F222 C222 C223 116.42(15) . . ? F222 C222 C221 119.09(15) . . ? C223 C222 C221 124.46(17) . . ? F223 C223 C224 120.18(16) . . ? F223 C223 C222 120.71(17) . . ? C224 C223 C222 119.10(17) . . ? F224 C224 C223 120.61(18) . . ? F224 C224 C225 120.13(18) . . ? C223 C224 C225 119.25(17) . . ? F225 C225 C224 119.80(17) . . ? F225 C225 C226 120.45(17) . . ? C224 C225 C226 119.75(17) . . ? F226 C226 C221 120.72(15) . . ? F226 C226 C225 115.58(15) . . ? C221 C226 C225 123.70(17) . . ? C236 C231 C232 113.63(16) . . ? C236 C231 B2 126.99(15) . . ? C232 C231 B2 119.29(16) . . ? F232 C232 C233 116.64(17) . . ? F232 C232 C231 118.72(16) . . ? C233 C232 C231 124.63(18) . . ? F233 C233 C234 120.12(18) . . ? F233 C233 C232 120.91(19) . . ? C234 C233 C232 118.97(18) . . ? F234 C234 C235 120.3(2) . . ? F234 C234 C233 120.41(19) . . ? C235 C234 C233 119.31(18) . . ? F235 C235 C234 120.01(18) . . ? F235 C235 C236 120.29(18) . . ? C234 C235 C236 119.70(18) . . ? F236 C236 C231 121.26(16) . . ? F236 C236 C235 115.00(16) . . ? C231 C236 C235 123.74(17) . . ? C331 C3 C311 120.57(17) . . ? C331 C3 C321 119.80(17) . . ? C311 C3 C321 119.62(16) . . ? C312 C311 C316 118.77(17) . . ? C312 C311 C3 120.84(16) . . ? C316 C311 C3 120.39(17) . . ? C313 C312 C311 120.19(18) . . ? C312 C313 C314 120.05(19) . . ? C315 C314 C313 120.48(19) . . ? C316 C315 C314 120.27(19) . . ? C315 C316 C311 120.23(19) . . ? C326 C321 C322 118.66(17) . . ? C326 C321 C3 120.86(17) . . ? C322 C321 C3 120.49(17) . . ? C323 C322 C321 120.45(19) . . ? C322 C323 C324 120.01(19) . . ? C323 C324 C325 120.45(19) . . ? C326 C325 C324 120.19(19) . . ? C325 C326 C321 120.19(19) . . ? C332 C331 C336 118.79(17) . . ? C332 C331 C3 121.21(17) . . ? C336 C331 C3 120.00(17) . . ? C333 C332 C331 120.18(19) . . ? C332 C333 C334 120.15(19) . . ? C333 C334 C335 120.5(2) . . ? C336 C335 C334 120.3(2) . . ? C335 C336 C331 120.10(19) . . ? Cl1S C1S Cl2S 112.28(16) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.527 _refine_diff_density_min -0.422 _refine_diff_density_rms 0.044 #===END data_mb56 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H15 B2 F30 N' _chemical_formula_weight 1293.31 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' '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' _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 13.3342(2) _cell_length_b 14.8405(2) _cell_length_c 15.8631(2) _cell_angle_alpha 116.4370(6) _cell_angle_beta 90.9440(7) _cell_angle_gamma 113.6410(5) _cell_volume 2501.10(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 56512 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 0.178 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9005 _exptl_absorpt_correction_T_max 0.9686 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58348 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.00 _reflns_number_total 9800 _reflns_number_gt 8664 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (McArdle, 1995)' _computing_publication_material 'local program' _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^)+(0.0394P)^2^+1.0052P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0048(11) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 9800 _refine_ls_number_parameters 803 _refine_ls_number_restraints 333 _refine_ls_R_factor_all 0.0405 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.022 _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 -0.13238(11) 0.10290(11) 0.29168(9) 0.0312(3) Uani 1 1 d . . . B1 B -0.03782(13) 0.19807(14) 0.27616(11) 0.0257(3) Uani 1 1 d D . . C111 C -0.09998(12) 0.23499(11) 0.21671(10) 0.0262(3) Uani 1 1 d D . . C112 C -0.21159(12) 0.21430(12) 0.20633(10) 0.0288(3) Uani 1 1 d D . . C113 C -0.26140(14) 0.24460(14) 0.15302(11) 0.0349(3) Uani 1 1 d D . . C114 C -0.19789(16) 0.29968(14) 0.10774(11) 0.0402(4) Uani 1 1 d D . . C115 C -0.08622(16) 0.32339(14) 0.11616(11) 0.0391(4) Uani 1 1 d D . . C116 C -0.04026(13) 0.29217(13) 0.17017(11) 0.0313(3) Uani 1 1 d D . . F112 F -0.27976(7) 0.16342(8) 0.25065(7) 0.0363(2) Uani 1 1 d . . . F113 F -0.36956(8) 0.22412(9) 0.14830(8) 0.0475(3) Uani 1 1 d . . . F114 F -0.24433(11) 0.33220(10) 0.05770(8) 0.0591(3) Uani 1 1 d . . . F115 F -0.02305(10) 0.37787(10) 0.07250(8) 0.0553(3) Uani 1 1 d . . . F116 F 0.07147(8) 0.32337(8) 0.18072(7) 0.0386(2) Uani 1 1 d . . . C121 C 0.03194(12) 0.13430(12) 0.21031(10) 0.0261(3) Uani 1 1 d D . . C122 C -0.02461(12) 0.02577(13) 0.13147(10) 0.0287(3) Uani 1 1 d D . . C123 C 0.02708(14) -0.03710(13) 0.07732(10) 0.0327(3) Uani 1 1 d D . . C124 C 0.14309(14) 0.01033(14) 0.09886(11) 0.0351(3) Uani 1 1 d D . . C125 C 0.20411(13) 0.11875(14) 0.17439(11) 0.0338(3) Uani 1 1 d D . . C126 C 0.14877(12) 0.17816(13) 0.22783(10) 0.0293(3) Uani 1 1 d D . . F122 F -0.13852(7) -0.02537(8) 0.10405(6) 0.0359(2) Uani 1 1 d . . . F123 F -0.03460(9) -0.14301(8) 0.00393(7) 0.0439(2) Uani 1 1 d . . . F124 F 0.19515(10) -0.04871(10) 0.04698(7) 0.0499(3) Uani 1 1 d . . . F125 F 0.31714(8) 0.16573(10) 0.19780(7) 0.0470(3) Uani 1 1 d . . . F126 F 0.21540(7) 0.28395(8) 0.30053(7) 0.0398(2) Uani 1 1 d . . . C131 C 0.03810(11) 0.29884(12) 0.38597(10) 0.0273(3) Uani 1 1 d D . . C132 C 0.07807(12) 0.27288(13) 0.44921(11) 0.0317(3) Uani 1 1 d D . . C133 C 0.13949(14) 0.35149(15) 0.54369(11) 0.0382(4) Uani 1 1 d D . . C134 C 0.16695(13) 0.46337(15) 0.57798(11) 0.0392(4) Uani 1 1 d D . . C135 C 0.13270(13) 0.49483(13) 0.51794(11) 0.0356(4) Uani 1 1 d D . . C136 C 0.06865(12) 0.41303(13) 0.42486(11) 0.0303(3) Uani 1 1 d D . . F132 F 0.05843(8) 0.16548(8) 0.41853(6) 0.0377(2) Uani 1 1 d . . . F133 F 0.17342(10) 0.31996(10) 0.60171(7) 0.0544(3) Uani 1 1 d . . . F134 F 0.22759(9) 0.54144(9) 0.66920(7) 0.0538(3) Uani 1 1 d . . . F135 F 0.16137(8) 0.60446(8) 0.54986(7) 0.0455(2) Uani 1 1 d . . . F136 F 0.03658(8) 0.45168(7) 0.37203(6) 0.0375(2) Uani 1 1 d . . . C2 C -0.19380(10) 0.02977(11) 0.30119(9) 0.0188(2) Uani 1 1 d . . . B2 B -0.27961(13) -0.07925(13) 0.30385(11) 0.0252(3) Uani 1 1 d D . . C211 C -0.40294(12) -0.08989(12) 0.27203(10) 0.0274(3) Uani 1 1 d D . . C212 C -0.48169(13) -0.08568(13) 0.32782(11) 0.0316(3) Uani 1 1 d D . . C213 C -0.58230(13) -0.08944(14) 0.29909(13) 0.0386(4) Uani 1 1 d D . . C214 C -0.60839(13) -0.09619(15) 0.21203(13) 0.0412(4) Uani 1 1 d D . . C215 C -0.53331(14) -0.09995(15) 0.15355(12) 0.0403(4) Uani 1 1 d D . . C216 C -0.43438(13) -0.09787(13) 0.18408(11) 0.0328(3) Uani 1 1 d D . . F212 F -0.46365(8) -0.07737(9) 0.41557(7) 0.0437(2) Uani 1 1 d . . . F213 F -0.65507(9) -0.08656(11) 0.35708(9) 0.0581(3) Uani 1 1 d . . . F214 F -0.70597(9) -0.10020(11) 0.18363(9) 0.0619(3) Uani 1 1 d . . . F215 F -0.55635(10) -0.10636(11) 0.06781(8) 0.0599(3) Uani 1 1 d . . . F216 F -0.36449(8) -0.10274(9) 0.12342(6) 0.0431(2) Uani 1 1 d . . . C221 C -0.25531(12) -0.18232(12) 0.22574(10) 0.0274(3) Uani 1 1 d D . . C222 C -0.33668(13) -0.29157(13) 0.16201(11) 0.0333(3) Uani 1 1 d D . . C223 C -0.31216(15) -0.37723(14) 0.10006(11) 0.0406(4) Uani 1 1 d D . . C224 C -0.20171(16) -0.35377(15) 0.09818(11) 0.0414(4) Uani 1 1 d D . . C225 C -0.11736(13) -0.24675(15) 0.15807(11) 0.0349(3) Uani 1 1 d D . . C226 C -0.14523(12) -0.16513(13) 0.22206(10) 0.0295(3) Uani 1 1 d D . . F222 F -0.44719(8) -0.32042(8) 0.15857(7) 0.0432(2) Uani 1 1 d . . . F223 F -0.39409(10) -0.48213(9) 0.04160(8) 0.0575(3) Uani 1 1 d . . . F224 F -0.17600(11) -0.43488(10) 0.03781(8) 0.0606(3) Uani 1 1 d . . . F225 F -0.00964(8) -0.22243(9) 0.15402(7) 0.0453(2) Uani 1 1 d . . . F226 F -0.05832(7) -0.06392(8) 0.28324(7) 0.0357(2) Uani 1 1 d . . . C231 C -0.25005(12) -0.06231(12) 0.41189(10) 0.0267(3) Uani 1 1 d D . . C232 C -0.18036(12) 0.03800(12) 0.49457(10) 0.0276(3) Uani 1 1 d D . . C233 C -0.15390(13) 0.04660(13) 0.58336(10) 0.0302(3) Uani 1 1 d D . . C234 C -0.20192(13) -0.04807(14) 0.59356(11) 0.0320(3) Uani 1 1 d D . . C235 C -0.27356(13) -0.15021(14) 0.51410(11) 0.0322(3) Uani 1 1 d D . . C236 C -0.29554(12) -0.15495(13) 0.42670(11) 0.0306(3) Uani 1 1 d D . . F232 F -0.13552(8) 0.13704(7) 0.49350(6) 0.0375(2) Uani 1 1 d . . . F233 F -0.08500(9) 0.14695(8) 0.65976(6) 0.0427(2) Uani 1 1 d . . . F234 F -0.18195(8) -0.04053(9) 0.67997(7) 0.0421(2) Uani 1 1 d . . . F235 F -0.32081(8) -0.24385(9) 0.52238(7) 0.0445(2) Uani 1 1 d . . . F236 F -0.36964(8) -0.25680(8) 0.35225(7) 0.0414(2) Uani 1 1 d . . . C3 C 0.35295(12) 0.56391(12) 0.30501(11) 0.0299(3) Uani 1 1 d D . . C311 C 0.38735(12) 0.48301(13) 0.23888(11) 0.0301(3) Uani 1 1 d D . . C312 C 0.31617(13) 0.39593(13) 0.14673(11) 0.0317(3) Uani 1 1 d D . . H312 H 0.2460 0.3918 0.1272 0.038 Uiso 1 1 calc R . . C313 C 0.34777(14) 0.31678(14) 0.08492(11) 0.0366(3) Uani 1 1 d D . . H313 H 0.2982 0.2566 0.0241 0.044 Uiso 1 1 calc R . . C314 C 0.45264(15) 0.32535(15) 0.11195(12) 0.0409(4) Uani 1 1 d D . . H314 H 0.4751 0.2719 0.0687 0.049 Uiso 1 1 calc R . . C315 C 0.52443(14) 0.41139(15) 0.20150(12) 0.0390(4) Uani 1 1 d D . . H315 H 0.5961 0.4171 0.2189 0.047 Uiso 1 1 calc R . . C316 C 0.49220(13) 0.48867(14) 0.26537(11) 0.0335(3) Uani 1 1 d D . . H316 H 0.5407 0.5459 0.3274 0.040 Uiso 1 1 calc R . . C321 C 0.38738(12) 0.61113(13) 0.40900(11) 0.0320(3) Uani 1 1 d D . . C322 C 0.39772(13) 0.54494(14) 0.44714(11) 0.0339(3) Uani 1 1 d D . . H322 H 0.3852 0.4698 0.4048 0.041 Uiso 1 1 calc R . . C323 C 0.42616(14) 0.58974(16) 0.54655(12) 0.0399(4) Uani 1 1 d D . . H323 H 0.4312 0.5443 0.5721 0.048 Uiso 1 1 calc R . . C324 C 0.44728(15) 0.69982(16) 0.60905(12) 0.0449(4) Uani 1 1 d D . . H324 H 0.4677 0.7299 0.6771 0.054 Uiso 1 1 calc R . . C325 C 0.43870(16) 0.76648(15) 0.57261(13) 0.0456(4) Uani 1 1 d D . . H325 H 0.4537 0.8423 0.6157 0.055 Uiso 1 1 calc R . . C326 C 0.40829(14) 0.72286(14) 0.47364(12) 0.0386(4) Uani 1 1 d D . . H326 H 0.4015 0.7685 0.4491 0.046 Uiso 1 1 calc R . . C331 C 0.28214(13) 0.59717(12) 0.26870(11) 0.0312(3) Uani 1 1 d D . . C332 C 0.20179(14) 0.62222(13) 0.31835(12) 0.0370(4) Uani 1 1 d D . . H332 H 0.1973 0.6211 0.3776 0.044 Uiso 1 1 calc R . . C333 C 0.13000(16) 0.64824(15) 0.28134(14) 0.0451(4) Uani 1 1 d D . . H333 H 0.0740 0.6620 0.3136 0.054 Uiso 1 1 calc R . . C334 C 0.13933(17) 0.65438(16) 0.19704(14) 0.0479(4) Uani 1 1 d D . . H334 H 0.0900 0.6731 0.1722 0.058 Uiso 1 1 calc R . . C335 C 0.21985(16) 0.63349(14) 0.14848(12) 0.0415(4) Uani 1 1 d D . . H335 H 0.2268 0.6402 0.0918 0.050 Uiso 1 1 calc R . . C336 C 0.28983(14) 0.60295(13) 0.18231(11) 0.0339(3) Uani 1 1 d D . . H336 H 0.3430 0.5859 0.1476 0.041 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 0.0325(7) 0.0358(7) 0.0251(6) 0.0106(5) 0.0053(5) 0.0205(6) B1 0.0243(7) 0.0259(8) 0.0242(7) 0.0107(6) 0.0057(6) 0.0110(6) C111 0.0302(7) 0.0212(7) 0.0225(6) 0.0075(5) 0.0055(5) 0.0115(6) C112 0.0330(8) 0.0269(7) 0.0264(7) 0.0124(6) 0.0067(6) 0.0143(6) C113 0.0386(8) 0.0335(8) 0.0309(7) 0.0117(7) 0.0027(6) 0.0200(7) C114 0.0583(11) 0.0364(9) 0.0306(8) 0.0170(7) 0.0033(7) 0.0256(8) C115 0.0579(11) 0.0311(8) 0.0306(8) 0.0184(7) 0.0138(7) 0.0186(8) C116 0.0351(8) 0.0262(7) 0.0291(7) 0.0119(6) 0.0101(6) 0.0127(6) F112 0.0299(5) 0.0449(5) 0.0453(5) 0.0285(5) 0.0136(4) 0.0198(4) F113 0.0425(5) 0.0561(7) 0.0515(6) 0.0262(5) 0.0032(4) 0.0298(5) F114 0.0797(8) 0.0627(7) 0.0531(6) 0.0383(6) 0.0041(6) 0.0380(6) F115 0.0761(8) 0.0518(7) 0.0506(6) 0.0384(6) 0.0242(6) 0.0249(6) F116 0.0363(5) 0.0352(5) 0.0446(5) 0.0222(4) 0.0174(4) 0.0134(4) C121 0.0286(7) 0.0276(7) 0.0251(7) 0.0149(6) 0.0084(5) 0.0131(6) C122 0.0301(7) 0.0307(8) 0.0255(7) 0.0151(6) 0.0084(6) 0.0128(6) C123 0.0460(9) 0.0290(8) 0.0238(7) 0.0117(6) 0.0097(6) 0.0190(7) C124 0.0491(9) 0.0450(9) 0.0309(7) 0.0226(7) 0.0185(7) 0.0340(8) C125 0.0309(8) 0.0485(10) 0.0355(8) 0.0272(8) 0.0134(6) 0.0226(7) C126 0.0289(7) 0.0308(8) 0.0269(7) 0.0141(6) 0.0074(6) 0.0125(6) F122 0.0302(5) 0.0333(5) 0.0278(4) 0.0081(4) 0.0041(3) 0.0080(4) F123 0.0610(6) 0.0323(5) 0.0300(5) 0.0076(4) 0.0120(4) 0.0224(5) F124 0.0644(7) 0.0629(7) 0.0444(5) 0.0248(5) 0.0262(5) 0.0500(6) F125 0.0311(5) 0.0685(7) 0.0499(6) 0.0309(5) 0.0159(4) 0.0281(5) F126 0.0268(4) 0.0360(5) 0.0382(5) 0.0100(4) 0.0069(4) 0.0076(4) C131 0.0229(7) 0.0294(8) 0.0256(7) 0.0097(6) 0.0080(5) 0.0127(6) C132 0.0290(7) 0.0321(8) 0.0304(7) 0.0101(6) 0.0063(6) 0.0170(6) C133 0.0370(8) 0.0480(10) 0.0282(7) 0.0120(7) 0.0040(6) 0.0261(8) C134 0.0293(8) 0.0408(9) 0.0263(7) 0.0008(7) 0.0004(6) 0.0153(7) C135 0.0284(7) 0.0271(8) 0.0362(8) 0.0058(7) 0.0086(6) 0.0104(6) C136 0.0263(7) 0.0292(8) 0.0302(7) 0.0115(6) 0.0095(6) 0.0116(6) F132 0.0437(5) 0.0360(5) 0.0332(5) 0.0116(4) 0.0014(4) 0.0245(4) F133 0.0666(7) 0.0653(7) 0.0322(5) 0.0140(5) -0.0028(5) 0.0430(6) F134 0.0491(6) 0.0511(6) 0.0301(5) -0.0040(5) -0.0064(4) 0.0233(5) F135 0.0409(5) 0.0269(5) 0.0439(5) 0.0037(4) 0.0069(4) 0.0095(4) F136 0.0449(5) 0.0267(5) 0.0354(5) 0.0140(4) 0.0085(4) 0.0130(4) C2 0.0181(6) 0.0193(6) 0.0194(6) 0.0099(5) 0.0049(5) 0.0085(5) B2 0.0242(8) 0.0243(8) 0.0273(7) 0.0136(6) 0.0067(6) 0.0101(6) C211 0.0244(7) 0.0235(7) 0.0319(7) 0.0129(6) 0.0061(6) 0.0097(6) C212 0.0308(7) 0.0299(8) 0.0363(8) 0.0171(7) 0.0100(6) 0.0149(6) C213 0.0305(8) 0.0360(9) 0.0513(10) 0.0190(8) 0.0153(7) 0.0195(7) C214 0.0274(8) 0.0378(9) 0.0560(10) 0.0196(8) 0.0014(7) 0.0170(7) C215 0.0360(9) 0.0405(9) 0.0391(9) 0.0186(8) -0.0029(7) 0.0144(7) C216 0.0285(7) 0.0329(8) 0.0320(7) 0.0142(7) 0.0048(6) 0.0116(6) F212 0.0422(5) 0.0649(7) 0.0435(5) 0.0340(5) 0.0231(4) 0.0329(5) F213 0.0415(6) 0.0782(8) 0.0697(7) 0.0363(7) 0.0294(5) 0.0402(6) F214 0.0382(6) 0.0742(8) 0.0809(8) 0.0370(7) 0.0032(5) 0.0341(6) F215 0.0517(6) 0.0815(9) 0.0481(6) 0.0347(6) -0.0042(5) 0.0292(6) F216 0.0369(5) 0.0634(7) 0.0317(5) 0.0254(5) 0.0092(4) 0.0229(5) C221 0.0306(7) 0.0285(7) 0.0266(7) 0.0149(6) 0.0077(6) 0.0150(6) C222 0.0317(8) 0.0333(8) 0.0325(7) 0.0150(7) 0.0052(6) 0.0142(7) C223 0.0489(10) 0.0301(8) 0.0302(8) 0.0066(7) -0.0014(7) 0.0166(8) C224 0.0558(11) 0.0431(10) 0.0276(7) 0.0096(7) 0.0061(7) 0.0337(9) C225 0.0380(8) 0.0465(10) 0.0302(7) 0.0189(7) 0.0093(6) 0.0281(8) C226 0.0330(8) 0.0310(8) 0.0272(7) 0.0147(6) 0.0058(6) 0.0167(6) F222 0.0302(5) 0.0326(5) 0.0476(5) 0.0111(4) 0.0026(4) 0.0076(4) F223 0.0585(7) 0.0314(6) 0.0498(6) -0.0007(5) -0.0072(5) 0.0158(5) F224 0.0758(8) 0.0552(7) 0.0411(6) 0.0005(5) 0.0050(5) 0.0480(6) F225 0.0442(6) 0.0625(7) 0.0404(5) 0.0210(5) 0.0134(4) 0.0390(5) F226 0.0269(4) 0.0328(5) 0.0433(5) 0.0144(4) 0.0049(4) 0.0149(4) C231 0.0268(7) 0.0311(8) 0.0291(7) 0.0174(6) 0.0107(6) 0.0162(6) C232 0.0309(7) 0.0282(7) 0.0299(7) 0.0159(6) 0.0115(6) 0.0170(6) C233 0.0332(8) 0.0344(8) 0.0253(7) 0.0118(6) 0.0074(6) 0.0208(7) C234 0.0350(8) 0.0475(9) 0.0310(7) 0.0248(7) 0.0139(6) 0.0279(7) C235 0.0306(8) 0.0383(9) 0.0425(8) 0.0284(7) 0.0160(6) 0.0189(7) C236 0.0270(7) 0.0320(8) 0.0337(7) 0.0169(7) 0.0082(6) 0.0134(6) F232 0.0542(6) 0.0260(5) 0.0286(4) 0.0128(4) 0.0083(4) 0.0158(4) F233 0.0567(6) 0.0395(5) 0.0261(4) 0.0100(4) 0.0017(4) 0.0240(5) F234 0.0501(6) 0.0621(7) 0.0348(5) 0.0323(5) 0.0152(4) 0.0342(5) F235 0.0462(6) 0.0482(6) 0.0550(6) 0.0393(5) 0.0177(5) 0.0197(5) F236 0.0403(5) 0.0324(5) 0.0406(5) 0.0201(4) 0.0050(4) 0.0047(4) C3 0.0280(7) 0.0261(7) 0.0332(7) 0.0169(6) 0.0074(6) 0.0074(6) C311 0.0317(8) 0.0284(8) 0.0328(7) 0.0183(6) 0.0080(6) 0.0124(6) C312 0.0300(7) 0.0338(8) 0.0336(8) 0.0196(7) 0.0080(6) 0.0130(6) C313 0.0420(9) 0.0342(8) 0.0314(8) 0.0151(7) 0.0064(7) 0.0167(7) C314 0.0490(10) 0.0434(10) 0.0398(9) 0.0209(8) 0.0150(7) 0.0288(8) C315 0.0369(9) 0.0444(10) 0.0439(9) 0.0243(8) 0.0099(7) 0.0230(8) C316 0.0331(8) 0.0330(8) 0.0351(8) 0.0192(7) 0.0051(6) 0.0131(7) C321 0.0300(7) 0.0307(8) 0.0318(7) 0.0155(6) 0.0066(6) 0.0106(6) C322 0.0304(8) 0.0353(8) 0.0355(8) 0.0189(7) 0.0067(6) 0.0129(7) C323 0.0354(8) 0.0515(10) 0.0381(8) 0.0271(8) 0.0085(7) 0.0188(8) C324 0.0402(9) 0.0536(11) 0.0300(8) 0.0171(8) 0.0060(7) 0.0158(8) C325 0.0482(10) 0.0344(9) 0.0365(9) 0.0102(7) 0.0078(7) 0.0117(8) C326 0.0419(9) 0.0316(8) 0.0371(8) 0.0160(7) 0.0091(7) 0.0132(7) C331 0.0332(8) 0.0256(7) 0.0327(7) 0.0142(6) 0.0064(6) 0.0120(6) C332 0.0408(9) 0.0310(8) 0.0408(8) 0.0177(7) 0.0128(7) 0.0178(7) C333 0.0472(10) 0.0410(10) 0.0533(10) 0.0214(8) 0.0149(8) 0.0274(8) C334 0.0557(11) 0.0393(10) 0.0499(10) 0.0170(8) 0.0012(8) 0.0287(9) C335 0.0579(11) 0.0323(9) 0.0329(8) 0.0142(7) 0.0025(7) 0.0217(8) C336 0.0392(8) 0.0278(8) 0.0311(7) 0.0129(6) 0.0054(6) 0.0141(7) _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 C2 1.1439(18) . ? N1 B1 1.593(2) . ? B1 C111 1.636(2) . ? B1 C131 1.644(2) . ? B1 C121 1.646(2) . ? C111 C112 1.384(2) . ? C111 C116 1.391(2) . ? C112 F112 1.3542(17) . ? C112 C113 1.385(2) . ? C113 F113 1.3426(19) . ? C113 C114 1.374(2) . ? C114 F114 1.3458(18) . ? C114 C115 1.375(3) . ? C115 F115 1.3470(19) . ? C115 C116 1.374(2) . ? C116 F116 1.3534(18) . ? C121 C122 1.389(2) . ? C121 C126 1.393(2) . ? C122 F122 1.3535(17) . ? C122 C123 1.380(2) . ? C123 F123 1.3434(18) . ? C123 C124 1.379(2) . ? C124 F124 1.3385(17) . ? C124 C125 1.374(2) . ? C125 F125 1.3430(18) . ? C125 C126 1.385(2) . ? C126 F126 1.3490(17) . ? C131 C136 1.388(2) . ? C131 C132 1.389(2) . ? C132 F132 1.3476(18) . ? C132 C133 1.384(2) . ? C133 F133 1.3454(19) . ? C133 C134 1.374(2) . ? C134 F134 1.3443(17) . ? C134 C135 1.373(2) . ? C135 F135 1.3457(19) . ? C135 C136 1.384(2) . ? C136 F136 1.3516(18) . ? C2 B2 1.5831(19) . ? B2 C231 1.634(2) . ? B2 C211 1.636(2) . ? B2 C221 1.644(2) . ? C211 C212 1.387(2) . ? C211 C216 1.389(2) . ? C212 F212 1.3502(18) . ? C212 C213 1.381(2) . ? C213 F213 1.3480(19) . ? C213 C214 1.368(2) . ? C214 F214 1.3395(18) . ? C214 C215 1.377(3) . ? C215 F215 1.3421(19) . ? C215 C216 1.382(2) . ? C216 F216 1.3496(18) . ? C221 C222 1.386(2) . ? C221 C226 1.392(2) . ? C222 F222 1.3521(18) . ? C222 C223 1.386(2) . ? C223 F223 1.3395(19) . ? C223 C224 1.375(2) . ? C224 F224 1.3412(18) . ? C224 C225 1.371(2) . ? C225 F225 1.3436(18) . ? C225 C226 1.384(2) . ? C226 F226 1.3454(17) . ? C231 C232 1.383(2) . ? C231 C236 1.392(2) . ? C232 F232 1.3550(17) . ? C232 C233 1.383(2) . ? C233 F233 1.3378(18) . ? C233 C234 1.376(2) . ? C234 F234 1.3378(16) . ? C234 C235 1.377(2) . ? C235 F235 1.3447(18) . ? C235 C236 1.377(2) . ? C236 F236 1.3528(18) . ? C3 C331 1.441(2) . ? C3 C311 1.445(2) . ? C3 C321 1.453(2) . ? C311 C316 1.412(2) . ? C311 C312 1.413(2) . ? C312 C313 1.380(2) . ? C313 C314 1.394(2) . ? C314 C315 1.387(2) . ? C315 C316 1.379(2) . ? C321 C326 1.409(2) . ? C321 C322 1.409(2) . ? C322 C323 1.385(2) . ? C323 C324 1.382(3) . ? C324 C325 1.387(3) . ? C325 C326 1.383(2) . ? C331 C332 1.412(2) . ? C331 C336 1.414(2) . ? C332 C333 1.375(2) . ? C333 C334 1.385(3) . ? C334 C335 1.387(3) . ? C335 C336 1.380(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 C2 N1 B1 173.55(14) . . ? N1 B1 C111 108.41(11) . . ? N1 B1 C131 104.75(11) . . ? C111 B1 C131 115.21(12) . . ? N1 B1 C121 103.76(11) . . ? C111 B1 C121 111.02(11) . . ? C131 B1 C121 112.75(11) . . ? C112 C111 C116 113.71(13) . . ? C112 C111 B1 126.01(12) . . ? C116 C111 B1 120.28(13) . . ? F112 C112 C111 120.87(12) . . ? F112 C112 C113 115.16(13) . . ? C111 C112 C113 123.95(14) . . ? F113 C113 C114 120.12(14) . . ? F113 C113 C112 120.49(14) . . ? C114 C113 C112 119.35(15) . . ? F114 C114 C113 120.05(16) . . ? F114 C114 C115 120.63(15) . . ? C113 C114 C115 119.31(14) . . ? F115 C115 C116 120.89(16) . . ? F115 C115 C114 119.79(15) . . ? C116 C115 C114 119.31(14) . . ? F116 C116 C115 116.85(14) . . ? F116 C116 C111 118.76(13) . . ? C115 C116 C111 124.35(15) . . ? C122 C121 C126 113.48(13) . . ? C122 C121 B1 120.91(12) . . ? C126 C121 B1 125.57(12) . . ? F122 C122 C123 115.74(13) . . ? F122 C122 C121 119.65(13) . . ? C123 C122 C121 124.61(14) . . ? F123 C123 C124 120.18(14) . . ? F123 C123 C122 120.59(14) . . ? C124 C123 C122 119.24(14) . . ? F124 C124 C125 120.70(15) . . ? F124 C124 C123 120.33(15) . . ? C125 C124 C123 118.97(14) . . ? F125 C125 C124 119.92(14) . . ? F125 C125 C126 120.17(14) . . ? C124 C125 C126 119.88(14) . . ? F126 C126 C125 115.80(13) . . ? F126 C126 C121 120.44(13) . . ? C125 C126 C121 123.76(14) . . ? C136 C131 C132 113.85(13) . . ? C136 C131 B1 126.02(13) . . ? C132 C131 B1 120.13(13) . . ? F132 C132 C133 116.37(14) . . ? F132 C132 C131 119.55(13) . . ? C133 C132 C131 124.08(15) . . ? F133 C133 C134 119.83(14) . . ? F133 C133 C132 120.93(15) . . ? C134 C133 C132 119.24(15) . . ? F134 C134 C135 120.31(16) . . ? F134 C134 C133 120.30(16) . . ? C135 C134 C133 119.39(14) . . ? F135 C135 C134 119.98(14) . . ? F135 C135 C136 120.54(15) . . ? C134 C135 C136 119.48(15) . . ? F136 C136 C135 115.22(14) . . ? F136 C136 C131 120.88(13) . . ? C135 C136 C131 123.91(15) . . ? N1 C2 B2 174.50(14) . . ? C2 B2 C231 109.12(11) . . ? C2 B2 C211 103.56(11) . . ? C231 B2 C211 115.13(11) . . ? C2 B2 C221 104.98(11) . . ? C231 B2 C221 108.82(11) . . ? C211 B2 C221 114.51(11) . . ? C212 C211 C216 113.67(13) . . ? C212 C211 B2 126.08(13) . . ? C216 C211 B2 120.14(12) . . ? F212 C212 C213 115.40(13) . . ? F212 C212 C211 121.05(13) . . ? C213 C212 C211 123.54(15) . . ? F213 C213 C214 119.92(14) . . ? F213 C213 C212 119.83(15) . . ? C214 C213 C212 120.26(15) . . ? F214 C214 C213 120.54(16) . . ? F214 C214 C215 120.47(16) . . ? C213 C214 C215 118.99(14) . . ? F215 C215 C214 120.42(15) . . ? F215 C215 C216 120.52(16) . . ? C214 C215 C216 119.06(15) . . ? F216 C216 C215 116.44(14) . . ? F216 C216 C211 119.10(13) . . ? C215 C216 C211 124.46(15) . . ? C222 C221 C226 114.03(13) . . ? C222 C221 B2 125.59(13) . . ? C226 C221 B2 120.34(13) . . ? F222 C222 C223 115.98(14) . . ? F222 C222 C221 120.32(14) . . ? C223 C222 C221 123.69(15) . . ? F223 C223 C224 119.48(15) . . ? F223 C223 C222 121.21(16) . . ? C224 C223 C222 119.31(15) . . ? F224 C224 C225 119.77(16) . . ? F224 C224 C223 120.40(16) . . ? C225 C224 C223 119.83(15) . . ? F225 C225 C224 120.03(14) . . ? F225 C225 C226 121.04(15) . . ? C224 C225 C226 118.93(15) . . ? F226 C226 C225 116.11(13) . . ? F226 C226 C221 119.81(13) . . ? C225 C226 C221 124.08(14) . . ? C232 C231 C236 113.62(13) . . ? C232 C231 B2 126.45(13) . . ? C236 C231 B2 119.93(13) . . ? F232 C232 C231 120.71(12) . . ? F232 C232 C233 115.23(13) . . ? C231 C232 C233 124.03(14) . . ? F233 C233 C234 120.10(13) . . ? F233 C233 C232 120.26(14) . . ? C234 C233 C232 119.60(14) . . ? F234 C234 C233 120.55(14) . . ? F234 C234 C235 120.39(14) . . ? C233 C234 C235 119.03(13) . . ? F235 C235 C234 119.97(13) . . ? F235 C235 C236 120.80(14) . . ? C234 C235 C236 119.23(14) . . ? F236 C236 C235 116.44(13) . . ? F236 C236 C231 119.07(13) . . ? C235 C236 C231 124.45(14) . . ? C331 C3 C311 120.48(13) . . ? C331 C3 C321 119.04(13) . . ? C311 C3 C321 120.47(13) . . ? C316 C311 C312 118.66(14) . . ? C316 C311 C3 120.71(14) . . ? C312 C311 C3 120.62(14) . . ? C313 C312 C311 120.48(14) . . ? C312 C313 C314 119.79(15) . . ? C315 C314 C313 120.49(15) . . ? C316 C315 C314 120.29(15) . . ? C315 C316 C311 120.22(15) . . ? C326 C321 C322 118.76(14) . . ? C326 C321 C3 120.70(14) . . ? C322 C321 C3 120.52(14) . . ? C323 C322 C321 119.79(16) . . ? C324 C323 C322 120.76(16) . . ? C323 C324 C325 120.13(16) . . ? C326 C325 C324 120.13(17) . . ? C325 C326 C321 120.40(16) . . ? C332 C331 C336 118.90(14) . . ? C332 C331 C3 120.05(14) . . ? C336 C331 C3 121.03(14) . . ? C333 C332 C331 120.30(16) . . ? C332 C333 C334 119.97(17) . . ? C333 C334 C335 120.81(16) . . ? C336 C335 C334 120.15(16) . . ? C335 C336 C331 119.80(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.507 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.042