# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Simon J Lancaster' _publ_contact_author_email S.LANCASTER@UEA.AC.UK _publ_section_title ; The Synthesis, Structure and Reactivity of 4 Nonafluorobiphenyl Complexes ; loop_ _publ_author_name 'Simon J Lancaster' 'David L Hughes' 'Mike Hursthouse' 'Louise Male' 'Edy Martin' # Attachment 'B817252H.cif' # # This files contains the seven .CIF files that accompany the MS: # # 'The synthesis, Structure and Reactivity of 4-nonafluorobiphenyl # complexes' # # by E. Martin, D.L. Hughes, M.B. Hursthouse, L. Male and S.J. Lancaster # data_em36 _database_code_depnum_ccdc_archive 'CCDC 704294' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; 4-nonafluorophenyltrimethyltin ; _chemical_name_common 4-nonafluorophenyltrimethyltin _chemical_formula_structural '[C6F5C6F4 Sn (CH3)3]' _chemical_melting_point ? _chemical_formula_moiety 'C15 H9 F9 Sn' _chemical_formula_sum 'C15 H9 F9 Sn' _chemical_formula_weight 478.91 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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 6.7641(4) _cell_length_b 11.2250(8) _cell_length_c 11.2842(8) _cell_angle_alpha 66.841(7) _cell_angle_beta 83.121(6) _cell_angle_gamma 81.090(6) _cell_volume 776.59(9) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.048 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 460 _exptl_absorpt_coefficient_mu 1.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.24 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10427 _diffrn_reflns_av_R_equivalents 0.0216 _diffrn_reflns_av_sigmaI/netI 0.0225 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3543 _reflns_number_gt 3192 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+1.8752P] 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 3543 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0991 _refine_ls_wR_factor_gt 0.0973 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.144 _refine_ls_shift/su_mean 0.002 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 Sn1 Sn 0.40606(4) 0.72496(3) 0.60605(2) 0.02292(10) Uani 1 1 d . . . C11 C 0.2681(6) 0.7285(4) 0.4380(4) 0.0237(8) Uani 1 1 d . . . C12 C 0.2061(6) 0.8460(4) 0.3425(4) 0.0232(7) Uani 1 1 d . . . C13 C 0.0986(6) 0.8567(4) 0.2422(4) 0.0224(7) Uani 1 1 d . . . C14 C 0.0480(6) 0.7461(4) 0.2310(4) 0.0213(7) Uani 1 1 d . . . C15 C 0.1138(6) 0.6269(4) 0.3245(4) 0.0222(7) Uani 1 1 d . . . C16 C 0.2197(6) 0.6186(4) 0.4248(4) 0.0215(7) Uani 1 1 d . . . F12 F 0.2546(4) 0.9579(2) 0.3461(2) 0.0308(5) Uani 1 1 d . . . F13 F 0.0437(4) 0.9751(2) 0.1522(2) 0.0297(5) Uani 1 1 d . . . F15 F 0.0722(4) 0.5164(2) 0.3167(2) 0.0273(5) Uani 1 1 d . . . F16 F 0.2769(4) 0.4981(2) 0.5118(2) 0.0275(5) Uani 1 1 d . . . C141 C -0.0743(6) 0.7541(4) 0.1277(4) 0.0219(7) Uani 1 1 d . . . C142 C -0.0038(6) 0.6937(4) 0.0405(4) 0.0241(8) Uani 1 1 d . . . C143 C -0.1217(7) 0.6926(4) -0.0492(4) 0.0274(8) Uani 1 1 d . . . C144 C -0.3163(7) 0.7549(4) -0.0569(4) 0.0286(8) Uani 1 1 d . . . C145 C -0.3909(6) 0.8161(4) 0.0262(4) 0.0280(8) Uani 1 1 d . . . C146 C -0.2695(6) 0.8147(4) 0.1165(4) 0.0234(7) Uani 1 1 d . . . F142 F 0.1852(4) 0.6352(3) 0.0449(2) 0.0317(5) Uani 1 1 d . . . F143 F -0.0524(4) 0.6318(3) -0.1293(3) 0.0374(6) Uani 1 1 d . . . F144 F -0.4328(4) 0.7544(3) -0.1439(3) 0.0410(6) Uani 1 1 d . . . F145 F -0.5801(4) 0.8743(3) 0.0198(3) 0.0357(6) Uani 1 1 d . . . F146 F -0.3476(4) 0.8716(3) 0.2001(2) 0.0311(5) Uani 1 1 d . . . C21 C 0.6978(7) 0.7835(4) 0.5406(5) 0.0334(9) Uani 1 1 d . . . H21A H 0.7517 0.8016 0.6058 0.050 Uiso 1 1 calc R . . H21B H 0.6893 0.8606 0.4628 0.050 Uiso 1 1 calc R . . H21C H 0.7837 0.7147 0.5236 0.050 Uiso 1 1 calc R . . C22 C 0.4070(6) 0.5350(4) 0.7551(4) 0.0285(8) Uani 1 1 d . . . H22A H 0.4861 0.4724 0.7252 0.043 Uiso 1 1 calc R . . H22B H 0.2720 0.5133 0.7774 0.043 Uiso 1 1 calc R . . H22C H 0.4631 0.5339 0.8297 0.043 Uiso 1 1 calc R . . C23 C 0.2086(8) 0.8639(5) 0.6630(5) 0.0388(11) Uani 1 1 d . . . H23A H 0.0734 0.8435 0.6729 0.058 Uiso 1 1 calc R . . H23B H 0.2175 0.9498 0.5981 0.058 Uiso 1 1 calc R . . H23C H 0.2461 0.8609 0.7436 0.058 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 Sn1 0.02634(16) 0.02279(15) 0.02224(15) -0.01128(11) -0.00180(10) -0.00296(10) C11 0.0225(18) 0.0255(19) 0.0262(19) -0.0135(16) -0.0010(15) -0.0025(15) C12 0.0251(18) 0.0207(18) 0.0286(19) -0.0146(16) 0.0009(15) -0.0045(14) C13 0.0259(18) 0.0176(17) 0.0226(18) -0.0079(14) 0.0023(14) -0.0017(14) C14 0.0206(17) 0.0223(18) 0.0233(18) -0.0120(15) 0.0009(14) -0.0018(14) C15 0.0232(18) 0.0212(17) 0.0266(18) -0.0139(15) 0.0020(14) -0.0047(14) C16 0.0218(17) 0.0194(17) 0.0223(17) -0.0082(14) 0.0011(14) -0.0008(14) F12 0.0413(14) 0.0201(11) 0.0355(13) -0.0133(10) -0.0076(11) -0.0055(10) F13 0.0401(14) 0.0201(11) 0.0267(12) -0.0066(9) -0.0056(10) -0.0007(10) F15 0.0348(13) 0.0200(11) 0.0313(12) -0.0130(10) -0.0049(10) -0.0045(9) F16 0.0340(13) 0.0209(11) 0.0272(12) -0.0081(9) -0.0073(10) -0.0010(9) C141 0.0264(19) 0.0218(17) 0.0196(17) -0.0098(15) 0.0011(14) -0.0055(14) C142 0.0259(19) 0.0238(18) 0.0229(18) -0.0107(15) 0.0039(15) -0.0029(15) C143 0.035(2) 0.028(2) 0.0223(18) -0.0129(16) 0.0051(16) -0.0089(16) C144 0.034(2) 0.031(2) 0.0224(18) -0.0090(16) -0.0055(16) -0.0101(17) C145 0.026(2) 0.028(2) 0.027(2) -0.0080(16) -0.0004(16) -0.0024(16) C146 0.0288(19) 0.0254(19) 0.0186(17) -0.0121(15) 0.0010(14) -0.0030(15) F142 0.0271(12) 0.0364(13) 0.0366(13) -0.0223(11) 0.0010(10) 0.0021(10) F143 0.0473(16) 0.0432(15) 0.0330(13) -0.0270(12) 0.0015(11) -0.0075(12) F144 0.0456(16) 0.0542(17) 0.0319(14) -0.0214(13) -0.0114(12) -0.0114(13) F145 0.0247(12) 0.0434(15) 0.0384(14) -0.0152(12) -0.0086(10) 0.0018(11) F146 0.0296(12) 0.0387(14) 0.0287(12) -0.0210(11) -0.0011(10) 0.0064(10) C21 0.033(2) 0.031(2) 0.038(2) -0.0133(19) 0.0010(18) -0.0114(18) C22 0.032(2) 0.0249(19) 0.0260(19) -0.0077(16) -0.0021(16) -0.0022(16) C23 0.048(3) 0.031(2) 0.036(2) -0.0163(19) 0.003(2) 0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C21 2.131(4) . ? Sn1 C22 2.133(4) . ? Sn1 C23 2.137(4) . ? Sn1 C11 2.196(4) . ? C11 C12 1.377(6) . ? C11 C16 1.390(5) . ? C12 F12 1.363(4) . ? C12 C13 1.374(5) . ? C13 F13 1.346(4) . ? C13 C14 1.392(5) . ? C14 C15 1.385(5) . ? C14 C141 1.476(5) . ? C15 F15 1.352(4) . ? C15 C16 1.376(5) . ? C16 F16 1.352(4) . ? C141 C146 1.385(6) . ? C141 C142 1.402(5) . ? C142 F142 1.340(5) . ? C142 C143 1.366(6) . ? C143 F143 1.337(4) . ? C143 C144 1.387(6) . ? C144 F144 1.332(5) . ? C144 C145 1.375(6) . ? C145 F145 1.340(5) . ? C145 C146 1.378(6) . ? C146 F146 1.351(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Sn1 C22 113.76(18) . . ? C21 Sn1 C23 112.76(19) . . ? C22 Sn1 C23 110.36(18) . . ? C21 Sn1 C11 106.95(17) . . ? C22 Sn1 C11 109.25(16) . . ? C23 Sn1 C11 103.11(18) . . ? C12 C11 C16 115.4(3) . . ? C12 C11 Sn1 120.0(3) . . ? C16 C11 Sn1 124.4(3) . . ? F12 C12 C13 117.9(3) . . ? F12 C12 C11 118.8(3) . . ? C13 C12 C11 123.3(3) . . ? F13 C13 C12 119.9(3) . . ? F13 C13 C14 119.3(3) . . ? C12 C13 C14 120.8(3) . . ? C15 C14 C13 116.5(3) . . ? C15 C14 C141 121.1(3) . . ? C13 C14 C141 122.3(3) . . ? F15 C15 C16 119.5(3) . . ? F15 C15 C14 118.9(3) . . ? C16 C15 C14 121.6(3) . . ? F16 C16 C15 117.4(3) . . ? F16 C16 C11 120.3(3) . . ? C15 C16 C11 122.3(4) . . ? C146 C141 C142 116.3(4) . . ? C146 C141 C14 121.7(3) . . ? C142 C141 C14 121.9(4) . . ? F142 C142 C143 118.8(3) . . ? F142 C142 C141 119.2(4) . . ? C143 C142 C141 122.1(4) . . ? F143 C143 C142 120.9(4) . . ? F143 C143 C144 119.5(4) . . ? C142 C143 C144 119.6(4) . . ? F144 C144 C145 119.6(4) . . ? F144 C144 C143 120.2(4) . . ? C145 C144 C143 120.2(4) . . ? F145 C145 C144 120.0(4) . . ? F145 C145 C146 120.9(4) . . ? C144 C145 C146 119.0(4) . . ? F146 C146 C145 118.2(4) . . ? F146 C146 C141 119.0(3) . . ? C145 C146 C141 122.8(4) . . ? Sn1 C21 H21A 109.5 . . ? Sn1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Sn1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Sn1 C22 H22A 109.5 . . ? Sn1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Sn1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Sn1 C23 H23A 109.5 . . ? Sn1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Sn1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C21 Sn1 C11 C12 -72.2(3) . . . . ? C22 Sn1 C11 C12 164.3(3) . . . . ? C23 Sn1 C11 C12 46.9(3) . . . . ? C21 Sn1 C11 C16 114.1(3) . . . . ? C22 Sn1 C11 C16 -9.4(4) . . . . ? C23 Sn1 C11 C16 -126.8(3) . . . . ? C16 C11 C12 F12 -177.5(3) . . . . ? Sn1 C11 C12 F12 8.2(5) . . . . ? C16 C11 C12 C13 1.8(6) . . . . ? Sn1 C11 C12 C13 -172.4(3) . . . . ? F12 C12 C13 F13 -0.5(5) . . . . ? C11 C12 C13 F13 -179.9(3) . . . . ? F12 C12 C13 C14 178.5(3) . . . . ? C11 C12 C13 C14 -0.8(6) . . . . ? F13 C13 C14 C15 178.2(3) . . . . ? C12 C13 C14 C15 -0.9(5) . . . . ? F13 C13 C14 C141 -3.5(5) . . . . ? C12 C13 C14 C141 177.4(4) . . . . ? C13 C14 C15 F15 -178.7(3) . . . . ? C141 C14 C15 F15 2.9(5) . . . . ? C13 C14 C15 C16 1.5(5) . . . . ? C141 C14 C15 C16 -176.8(3) . . . . ? F15 C15 C16 F16 -0.1(5) . . . . ? C14 C15 C16 F16 179.7(3) . . . . ? F15 C15 C16 C11 179.7(3) . . . . ? C14 C15 C16 C11 -0.5(6) . . . . ? C12 C11 C16 F16 178.6(3) . . . . ? Sn1 C11 C16 F16 -7.4(5) . . . . ? C12 C11 C16 C15 -1.1(6) . . . . ? Sn1 C11 C16 C15 172.8(3) . . . . ? C15 C14 C141 C146 116.1(4) . . . . ? C13 C14 C141 C146 -62.1(5) . . . . ? C15 C14 C141 C142 -59.8(5) . . . . ? C13 C14 C141 C142 122.0(4) . . . . ? C146 C141 C142 F142 178.9(3) . . . . ? C14 C141 C142 F142 -5.0(6) . . . . ? C146 C141 C142 C143 -1.0(6) . . . . ? C14 C141 C142 C143 175.1(4) . . . . ? F142 C142 C143 F143 1.6(6) . . . . ? C141 C142 C143 F143 -178.5(4) . . . . ? F142 C142 C143 C144 -178.7(4) . . . . ? C141 C142 C143 C144 1.2(6) . . . . ? F143 C143 C144 F144 -0.2(6) . . . . ? C142 C143 C144 F144 -179.9(4) . . . . ? F143 C143 C144 C145 179.0(4) . . . . ? C142 C143 C144 C145 -0.7(6) . . . . ? F144 C144 C145 F145 0.3(6) . . . . ? C143 C144 C145 F145 -178.9(4) . . . . ? F144 C144 C145 C146 179.3(4) . . . . ? C143 C144 C145 C146 0.1(6) . . . . ? F145 C145 C146 F146 1.2(6) . . . . ? C144 C145 C146 F146 -177.8(4) . . . . ? F145 C145 C146 C141 179.0(4) . . . . ? C144 C145 C146 C141 0.1(6) . . . . ? C142 C141 C146 F146 178.3(3) . . . . ? C14 C141 C146 F146 2.2(6) . . . . ? C142 C141 C146 C145 0.4(6) . . . . ? C14 C141 C146 C145 -175.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 4.586 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.132 #===END data_em49 _database_code_depnum_ccdc_archive 'CCDC 704295' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; Nonafluorobiphenyl dimethyl tin bromide acetonitrile solvate ; _chemical_name_common 'Nonafluorobiphenyl dimethyl tin bromide acetonitrile solvate' _chemical_formula_structural '[(C6F5C6F4)Sn(CH3)2Br].CH3CN' _chemical_melting_point ? _chemical_formula_moiety 'C14 H6 Br F9 Sn, C2 H3 N' _chemical_formula_sum 'C16 H9 Br F9 N Sn' _chemical_formula_weight 584.84 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' Br Br -0.2901 2.4595 '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' Sn Sn -0.6537 1.4246 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.8151(2) _cell_length_b 10.5666(3) _cell_length_c 18.0686(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.468(2) _cell_angle_gamma 90.00 _cell_volume 1862.01(8) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.086 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 3.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.86 _exptl_absorpt_correction_T_max 1.17 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28886 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 30.00 _reflns_number_total 5427 _reflns_number_gt 3624 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^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 5427 _refine_ls_number_parameters 254 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0606 _refine_ls_R_factor_gt 0.0283 _refine_ls_wR_factor_ref 0.0554 _refine_ls_wR_factor_gt 0.0487 _refine_ls_goodness_of_fit_ref 0.902 _refine_ls_restrained_S_all 0.902 _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 Sn1 Sn 0.237629(19) 0.102606(18) 0.189291(11) 0.02034(5) Uani 1 1 d . . . Br2 Br 0.06505(3) 0.21468(3) 0.262881(18) 0.03314(8) Uani 1 1 d . . . F142 F 0.24519(16) 0.42636(15) -0.14799(9) 0.0304(4) Uani 1 1 d . . . F13 F 0.03751(15) 0.38069(15) -0.05274(9) 0.0297(4) Uani 1 1 d . . . F143 F 0.25433(18) 0.61998(17) -0.24484(9) 0.0379(5) Uani 1 1 d . . . F15 F 0.45352(15) 0.52879(15) 0.07422(9) 0.0253(4) Uani 1 1 d . . . F146 F 0.25065(16) 0.71792(15) 0.04986(9) 0.0272(4) Uani 1 1 d . . . F12 F 0.03949(15) 0.18661(15) 0.04143(10) 0.0303(4) Uani 1 1 d . . . F145 F 0.25466(18) 0.91084(16) -0.04763(10) 0.0369(4) Uani 1 1 d . . . C144 C 0.2559(3) 0.7663(3) -0.14704(17) 0.0273(7) Uani 1 1 d . . . F144 F 0.26362(18) 0.86273(17) -0.19390(10) 0.0413(5) Uani 1 1 d . . . C14 C 0.2457(3) 0.4609(3) 0.00753(15) 0.0184(6) Uani 1 1 d . . . C13 C 0.1428(3) 0.3701(2) 0.00173(15) 0.0200(6) Uani 1 1 d . . . C11 C 0.2450(3) 0.2563(3) 0.11054(15) 0.0195(6) Uani 1 1 d . . . C15 C 0.3483(3) 0.4459(3) 0.06661(15) 0.0188(6) Uani 1 1 d . . . C12 C 0.1435(3) 0.2719(3) 0.05123(16) 0.0222(6) Uani 1 1 d . . . C142 C 0.2457(3) 0.5457(3) -0.12220(16) 0.0226(6) Uani 1 1 d . . . C143 C 0.2507(3) 0.6435(3) -0.17203(15) 0.0247(7) Uani 1 1 d . . . C146 C 0.2514(3) 0.6920(3) -0.02303(15) 0.0211(6) Uani 1 1 d . . . C141 C 0.2467(3) 0.5669(2) -0.04632(15) 0.0188(6) Uani 1 1 d . . . C145 C 0.2545(3) 0.7908(3) -0.07188(17) 0.0247(6) Uani 1 1 d . . . F16 F 0.44929(15) 0.34095(16) 0.17275(9) 0.0285(4) Uani 1 1 d . . . N1 N 0.0701(3) 0.5097(3) 0.39456(15) 0.0341(6) Uani 1 1 d . . . C2 C -0.0032(3) 0.4323(3) 0.40732(16) 0.0255(6) Uani 1 1 d . . . C16 C 0.3460(3) 0.3474(3) 0.11625(14) 0.0199(6) Uani 1 1 d . . . C21 C 0.4048(3) 0.0854(3) 0.27449(16) 0.0315(7) Uani 1 1 d . . . H21A H 0.3714 0.0902 0.3223 0.047 Uiso 1 1 calc R . . H21B H 0.4690 0.1528 0.2699 0.047 Uiso 1 1 calc R . . H21C H 0.4496 0.0055 0.2697 0.047 Uiso 1 1 calc R . . C22 C 0.1193(3) -0.0540(3) 0.14625(17) 0.0302(7) Uani 1 1 d . . . H22A H 0.1658 -0.1312 0.1617 0.045 Uiso 1 1 calc R . . H22B H 0.1071 -0.0498 0.0928 0.045 Uiso 1 1 calc R . . H22C H 0.0313 -0.0521 0.1647 0.045 Uiso 1 1 calc R . . C3 C -0.0966(3) 0.3318(3) 0.42380(18) 0.0308(7) Uani 1 1 d . . . H3A H -0.0594 0.2514 0.4116 0.046 Uiso 1 1 calc R . . H3B H -0.1838 0.3440 0.3948 0.046 Uiso 1 1 calc R . . H3C H -0.1084 0.3336 0.4758 0.046 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 Sn1 0.02346(10) 0.01988(10) 0.01738(9) 0.00105(9) 0.00103(7) 0.00234(8) Br2 0.03546(18) 0.03831(19) 0.02721(17) -0.00462(14) 0.01033(13) 0.00718(14) F142 0.0392(10) 0.0283(10) 0.0228(9) -0.0043(7) -0.0003(7) 0.0054(7) F13 0.0224(8) 0.0357(11) 0.0279(9) 0.0076(8) -0.0100(7) -0.0022(7) F143 0.0504(11) 0.0484(13) 0.0150(8) 0.0048(9) 0.0037(8) 0.0046(9) F15 0.0225(8) 0.0280(9) 0.0242(9) 0.0010(7) -0.0025(7) -0.0063(7) F146 0.0369(9) 0.0250(9) 0.0199(9) -0.0042(7) 0.0036(7) -0.0010(7) F12 0.0243(9) 0.0275(10) 0.0370(10) 0.0067(8) -0.0063(7) -0.0084(7) F145 0.0504(11) 0.0189(9) 0.0403(11) 0.0005(8) 0.0009(9) -0.0081(8) C144 0.0251(16) 0.0288(17) 0.0274(17) 0.0134(13) 0.0003(13) -0.0024(12) F144 0.0484(11) 0.0368(11) 0.0372(11) 0.0195(9) -0.0010(9) -0.0107(9) C14 0.0173(13) 0.0208(15) 0.0170(13) 0.0007(11) 0.0021(11) 0.0020(11) C13 0.0183(14) 0.0232(16) 0.0176(13) -0.0009(11) -0.0021(11) 0.0027(11) C11 0.0191(14) 0.0213(15) 0.0185(14) 0.0003(11) 0.0035(11) 0.0019(11) C15 0.0158(13) 0.0217(14) 0.0190(14) -0.0047(11) 0.0029(11) -0.0011(11) C12 0.0171(14) 0.0244(15) 0.0251(15) 0.0008(12) 0.0019(12) -0.0020(11) C142 0.0232(15) 0.0219(15) 0.0220(15) -0.0010(12) -0.0002(12) 0.0023(12) C143 0.0253(16) 0.0349(18) 0.0130(14) 0.0014(11) -0.0020(12) 0.0004(12) C146 0.0192(14) 0.0258(16) 0.0186(14) -0.0019(12) 0.0032(11) 0.0007(11) C141 0.0163(13) 0.0215(15) 0.0183(14) 0.0028(11) 0.0005(11) 0.0013(10) C145 0.0237(15) 0.0187(15) 0.0310(16) 0.0011(13) -0.0002(12) -0.0028(12) F16 0.0258(9) 0.0357(10) 0.0212(9) 0.0060(7) -0.0098(7) -0.0030(7) N1 0.0347(15) 0.0348(16) 0.0330(15) 0.0010(13) 0.0043(12) -0.0075(12) C2 0.0302(16) 0.0254(17) 0.0213(15) -0.0022(12) 0.0053(12) -0.0014(13) C16 0.0175(14) 0.0272(15) 0.0140(13) -0.0017(11) -0.0020(11) 0.0024(11) C21 0.0351(17) 0.0340(19) 0.0231(15) 0.0011(14) -0.0062(13) 0.0062(14) C22 0.0367(17) 0.0234(16) 0.0296(17) -0.0014(13) 0.0000(14) -0.0006(13) C3 0.0379(18) 0.0210(16) 0.0360(18) -0.0010(14) 0.0146(15) -0.0046(13) _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 Sn1 C22 2.119(3) . ? Sn1 C21 2.128(3) . ? Sn1 C11 2.166(3) . ? Sn1 Br2 2.5587(3) . ? F142 C142 1.345(3) . ? F13 C13 1.349(3) . ? F143 C143 1.343(3) . ? F15 C15 1.349(3) . ? F146 C146 1.346(3) . ? F12 C12 1.358(3) . ? F145 C145 1.342(3) . ? C144 F144 1.333(3) . ? C144 C143 1.373(4) . ? C144 C145 1.384(4) . ? C14 C13 1.389(4) . ? C14 C15 1.392(4) . ? C14 C141 1.484(4) . ? C13 C12 1.369(4) . ? C11 C16 1.378(4) . ? C11 C12 1.388(4) . ? C15 C16 1.376(4) . ? C142 C143 1.374(4) . ? C142 C141 1.388(4) . ? C146 C145 1.370(4) . ? C146 C141 1.386(4) . ? F16 C16 1.357(3) . ? N1 C2 1.130(3) . ? C2 C3 1.457(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 Sn1 C21 123.04(12) . . ? C22 Sn1 C11 113.71(11) . . ? C21 Sn1 C11 117.33(11) . . ? C22 Sn1 Br2 100.64(8) . . ? C21 Sn1 Br2 99.52(8) . . ? C11 Sn1 Br2 93.87(7) . . ? F144 C144 C143 121.1(3) . . ? F144 C144 C145 119.2(3) . . ? C143 C144 C145 119.7(3) . . ? C13 C14 C15 115.9(2) . . ? C13 C14 C141 122.0(2) . . ? C15 C14 C141 122.1(2) . . ? F13 C13 C12 119.2(2) . . ? F13 C13 C14 119.2(2) . . ? C12 C13 C14 121.6(2) . . ? C16 C11 C12 115.0(2) . . ? C16 C11 Sn1 123.50(19) . . ? C12 C11 Sn1 121.46(19) . . ? F15 C15 C16 119.5(2) . . ? F15 C15 C14 118.9(2) . . ? C16 C15 C14 121.5(2) . . ? F12 C12 C13 117.9(2) . . ? F12 C12 C11 119.0(2) . . ? C13 C12 C11 123.0(2) . . ? F142 C142 C143 118.5(3) . . ? F142 C142 C141 119.5(3) . . ? C143 C142 C141 122.0(3) . . ? F143 C143 C144 119.5(3) . . ? F143 C143 C142 120.6(3) . . ? C144 C143 C142 119.8(3) . . ? F146 C146 C145 118.5(2) . . ? F146 C146 C141 119.2(2) . . ? C145 C146 C141 122.3(3) . . ? C146 C141 C142 116.7(3) . . ? C146 C141 C14 121.5(2) . . ? C142 C141 C14 121.7(2) . . ? F145 C145 C146 120.6(3) . . ? F145 C145 C144 119.9(3) . . ? C146 C145 C144 119.5(3) . . ? N1 C2 C3 179.5(3) . . ? F16 C16 C15 117.6(2) . . ? F16 C16 C11 119.4(2) . . ? C15 C16 C11 123.0(2) . . ? Sn1 C21 H21A 109.5 . . ? Sn1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Sn1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Sn1 C22 H22A 109.5 . . ? Sn1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Sn1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 C14 C13 F13 177.9(2) . . . . ? C141 C14 C13 F13 -2.5(4) . . . . ? C15 C14 C13 C12 -0.3(4) . . . . ? C141 C14 C13 C12 179.3(3) . . . . ? C22 Sn1 C11 C16 -158.8(2) . . . . ? C21 Sn1 C11 C16 -5.0(3) . . . . ? Br2 Sn1 C11 C16 97.8(2) . . . . ? C22 Sn1 C11 C12 23.4(3) . . . . ? C21 Sn1 C11 C12 177.2(2) . . . . ? Br2 Sn1 C11 C12 -80.0(2) . . . . ? C13 C14 C15 F15 178.1(2) . . . . ? C141 C14 C15 F15 -1.5(4) . . . . ? C13 C14 C15 C16 -0.6(4) . . . . ? C141 C14 C15 C16 179.9(2) . . . . ? F13 C13 C12 F12 2.2(4) . . . . ? C14 C13 C12 F12 -179.6(2) . . . . ? F13 C13 C12 C11 -177.6(2) . . . . ? C14 C13 C12 C11 0.6(4) . . . . ? C16 C11 C12 F12 -179.8(2) . . . . ? Sn1 C11 C12 F12 -1.8(4) . . . . ? C16 C11 C12 C13 0.0(4) . . . . ? Sn1 C11 C12 C13 178.0(2) . . . . ? F144 C144 C143 F143 0.5(4) . . . . ? C145 C144 C143 F143 -178.9(2) . . . . ? F144 C144 C143 C142 178.6(2) . . . . ? C145 C144 C143 C142 -0.8(4) . . . . ? F142 C142 C143 F143 0.3(4) . . . . ? C141 C142 C143 F143 177.7(2) . . . . ? F142 C142 C143 C144 -177.8(2) . . . . ? C141 C142 C143 C144 -0.4(4) . . . . ? F146 C146 C141 C142 179.1(2) . . . . ? C145 C146 C141 C142 0.2(4) . . . . ? F146 C146 C141 C14 -2.2(4) . . . . ? C145 C146 C141 C14 179.0(2) . . . . ? F142 C142 C141 C146 178.1(2) . . . . ? C143 C142 C141 C146 0.7(4) . . . . ? F142 C142 C141 C14 -0.7(4) . . . . ? C143 C142 C141 C14 -178.0(2) . . . . ? C13 C14 C141 C146 124.0(3) . . . . ? C15 C14 C141 C146 -56.5(4) . . . . ? C13 C14 C141 C142 -57.4(4) . . . . ? C15 C14 C141 C142 122.2(3) . . . . ? F146 C146 C145 F145 -1.0(4) . . . . ? C141 C146 C145 F145 177.8(2) . . . . ? F146 C146 C145 C144 179.7(2) . . . . ? C141 C146 C145 C144 -1.4(4) . . . . ? F144 C144 C145 F145 3.0(4) . . . . ? C143 C144 C145 F145 -177.6(2) . . . . ? F144 C144 C145 C146 -177.8(2) . . . . ? C143 C144 C145 C146 1.7(4) . . . . ? F15 C15 C16 F16 2.2(4) . . . . ? C14 C15 C16 F16 -179.2(2) . . . . ? F15 C15 C16 C11 -177.5(2) . . . . ? C14 C15 C16 C11 1.2(4) . . . . ? C12 C11 C16 F16 179.5(2) . . . . ? Sn1 C11 C16 F16 1.6(4) . . . . ? C12 C11 C16 C15 -0.9(4) . . . . ? Sn1 C11 C16 C15 -178.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.705 _refine_diff_density_min -0.855 _refine_diff_density_rms 0.111 #===END data_em141 _database_code_depnum_ccdc_archive 'CCDC 704296' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; Bis(4-nonafluorobiphenyl)boronic acid hydrate ; _chemical_name_common 'Bis(4-nonafluorobiphenyl)boronic acid hydrate' _chemical_melting_point ? _chemical_formula_structural '[(C6F5C6F4)2B(OH)(OH2)].(C6D6)3' _chemical_formula_moiety 'C24 H3 B F18 O2, 3(C6D6)' _chemical_formula_sum 'C42 H3 D18 B1 F18 O2' _chemical_formula_weight 928.51 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' O O 0.0106 0.0060 '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 7.0808(2) _cell_length_b 14.5619(7) _cell_length_c 18.4705(8) _cell_angle_alpha 92.210(2) _cell_angle_beta 95.502(3) _cell_angle_gamma 99.797(2) _cell_volume 1865.15(13) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.005 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.160 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.819 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'SADABS 2007/2 (Sheldrick, G.M., 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24007 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_sigmaI/netI 0.0491 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4873 _reflns_number_gt 3638 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' #Although determined using DirAx, the cell is refined in the HKL #package during data reduction _computing_data_reduction 'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0122P)^2^+3.3215P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4873 _refine_ls_number_parameters 580 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1043 _refine_ls_wR_factor_gt 0.0935 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _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 0.8498(6) 0.4277(3) 0.5716(2) 0.0240(10) Uani 1 1 d . . . O1 O 1.0696(4) 0.4607(2) 0.58488(16) 0.0271(6) Uani 1 1 d D . . O2 O 0.7854(4) 0.50106(19) 0.52870(14) 0.0264(6) Uani 1 1 d D . . C11 C 0.7984(5) 0.3280(3) 0.52385(19) 0.0230(9) Uani 1 1 d . . . C12 C 0.9191(5) 0.2634(3) 0.51669(19) 0.0246(9) Uani 1 1 d . . . C13 C 0.8662(5) 0.1795(3) 0.4768(2) 0.0269(9) Uani 1 1 d . . . C14 C 0.6827(5) 0.1533(3) 0.44022(19) 0.0236(9) Uani 1 1 d . . . C15 C 0.5580(5) 0.2154(3) 0.44836(19) 0.0240(9) Uani 1 1 d . . . C16 C 0.6146(5) 0.2981(3) 0.48854(19) 0.0225(9) Uani 1 1 d . . . F12 F 1.1040(3) 0.28268(15) 0.54853(11) 0.0342(5) Uani 1 1 d . . . F13 F 0.9961(3) 0.12245(15) 0.47217(11) 0.0344(6) Uani 1 1 d . . . F15 F 0.3750(3) 0.19297(14) 0.41737(11) 0.0301(5) Uani 1 1 d . . . F16 F 0.4783(3) 0.35311(14) 0.49538(11) 0.0291(5) Uani 1 1 d . . . C141 C 0.6276(5) 0.0670(3) 0.39204(19) 0.0240(9) Uani 1 1 d . . . C142 C 0.6327(5) -0.0213(3) 0.4168(2) 0.0277(9) Uani 1 1 d . . . C143 C 0.5849(5) -0.1000(3) 0.3709(2) 0.0298(10) Uani 1 1 d . . . C144 C 0.5298(5) -0.0927(3) 0.2986(2) 0.0299(10) Uani 1 1 d . . . C145 C 0.5227(5) -0.0060(3) 0.2725(2) 0.0281(9) Uani 1 1 d . . . C146 C 0.5698(5) 0.0715(3) 0.3187(2) 0.0267(9) Uani 1 1 d . . . F142 F 0.6853(3) -0.03013(15) 0.48758(11) 0.0351(6) Uani 1 1 d . . . F143 F 0.5929(3) -0.18485(15) 0.39691(13) 0.0436(6) Uani 1 1 d . . . F144 F 0.4827(3) -0.16951(16) 0.25356(13) 0.0448(6) Uani 1 1 d . . . F145 F 0.4680(3) 0.00095(15) 0.20126(11) 0.0399(6) Uani 1 1 d . . . F146 F 0.5645(3) 0.15542(14) 0.29022(11) 0.0333(5) Uani 1 1 d . . . C21 C 0.7667(5) 0.4176(2) 0.65072(19) 0.0225(9) Uani 1 1 d . . . C22 C 0.6028(5) 0.4480(3) 0.67027(19) 0.0241(9) Uani 1 1 d . . . C23 C 0.5379(5) 0.4365(3) 0.7375(2) 0.0257(9) Uani 1 1 d . . . C24 C 0.6325(5) 0.3931(2) 0.79175(19) 0.0228(9) Uani 1 1 d . . . C25 C 0.7940(5) 0.3598(2) 0.77268(19) 0.0227(9) Uani 1 1 d . . . C26 C 0.8570(5) 0.3721(3) 0.7052(2) 0.0244(9) Uani 1 1 d . . . F22 F 0.4981(3) 0.49217(15) 0.62143(11) 0.0321(5) Uani 1 1 d . . . F23 F 0.3799(3) 0.47235(15) 0.75178(11) 0.0339(5) Uani 1 1 d . . . F25 F 0.8888(3) 0.31335(15) 0.82148(11) 0.0351(6) Uani 1 1 d . . . F26 F 1.0165(3) 0.33673(15) 0.69095(11) 0.0318(5) Uani 1 1 d . . . F242 F 0.2658(3) 0.29901(16) 0.81427(11) 0.0364(6) Uani 1 1 d . . . C241 C 0.5651(5) 0.3816(3) 0.86484(19) 0.0251(9) Uani 1 1 d . . . C242 C 0.3812(5) 0.3373(3) 0.8732(2) 0.0284(9) Uani 1 1 d . . . C243 C 0.3134(6) 0.3291(3) 0.9405(2) 0.0332(10) Uani 1 1 d . . . C244 C 0.4320(6) 0.3645(3) 1.0013(2) 0.0356(10) Uani 1 1 d . . . C245 C 0.6183(6) 0.4079(3) 0.9958(2) 0.0347(10) Uani 1 1 d . . . C246 C 0.6827(5) 0.4162(3) 0.9281(2) 0.0296(10) Uani 1 1 d . . . F243 F 0.1338(3) 0.28477(18) 0.94704(12) 0.0474(7) Uani 1 1 d . . . F244 F 0.3659(4) 0.35966(18) 1.06720(12) 0.0521(7) Uani 1 1 d . . . F245 F 0.7338(4) 0.44305(17) 1.05570(12) 0.0506(7) Uani 1 1 d . . . F246 F 0.8641(3) 0.46015(16) 0.92367(12) 0.0416(6) Uani 1 1 d . . . C31 C 0.0993(7) 0.3213(3) 0.3377(2) 0.0440(11) Uani 1 1 d . . . H31 H 0.1163 0.3061 0.3860 0.053 Uiso 1 1 calc R . . C32 C 0.2460(6) 0.3201(3) 0.2941(2) 0.0399(11) Uani 1 1 d . . . H32 H 0.3614 0.3040 0.3132 0.048 Uiso 1 1 calc R . . C33 C 0.2238(7) 0.3425(3) 0.2228(2) 0.0429(11) Uani 1 1 d . . . H33 H 0.3238 0.3415 0.1938 0.051 Uiso 1 1 calc R . . C34 C 0.0541(8) 0.3665(3) 0.1941(3) 0.0518(13) Uani 1 1 d . . . H34 H 0.0386 0.3815 0.1457 0.062 Uiso 1 1 calc R . . C35 C -0.0947(8) 0.3681(3) 0.2379(3) 0.0618(15) Uani 1 1 d . . . H35 H -0.2099 0.3847 0.2190 0.074 Uiso 1 1 calc R . . C36 C -0.0700(7) 0.3446(3) 0.3105(3) 0.0550(14) Uani 1 1 d . . . H36 H -0.1693 0.3449 0.3400 0.066 Uiso 1 1 calc R . . C41 C 0.0077(6) 1.0806(3) 0.2260(3) 0.0464(12) Uani 1 1 d . . . H41 H 0.0056 1.1414 0.2128 0.056 Uiso 1 1 calc R . . C42 C 0.0504(6) 1.0627(3) 0.2975(2) 0.0408(11) Uani 1 1 d . . . H42 H 0.0781 1.1118 0.3327 0.049 Uiso 1 1 calc R . . C43 C 0.0529(6) 0.9729(3) 0.3176(3) 0.0447(12) Uani 1 1 d . . . H43 H 0.0810 0.9609 0.3662 0.054 Uiso 1 1 calc R . . C44 C 0.0123(6) 0.9000(3) 0.2638(3) 0.0524(13) Uani 1 1 d . . . H44 H 0.0142 0.8389 0.2765 0.063 Uiso 1 1 calc R . . C45 C -0.0303(7) 0.9186(4) 0.1924(3) 0.0560(14) Uani 1 1 d . . . H45 H -0.0578 0.8701 0.1567 0.067 Uiso 1 1 calc R . . C46 C -0.0322(7) 1.0080(4) 0.1738(3) 0.0557(14) Uani 1 1 d . . . H46 H -0.0607 1.0201 0.1253 0.067 Uiso 1 1 calc R . . C51 C 0.4372(7) 0.1435(3) 0.0782(3) 0.0498(12) Uani 1 1 d . . . H51 H 0.3573 0.1384 0.1155 0.060 Uiso 1 1 calc R . . C52 C 0.6282(7) 0.1821(3) 0.0928(3) 0.0518(13) Uani 1 1 d . . . H52 H 0.6778 0.2034 0.1400 0.062 Uiso 1 1 calc R . . C53 C 0.7473(7) 0.1895(3) 0.0375(3) 0.0563(13) Uani 1 1 d . . . H53 H 0.8770 0.2155 0.0477 0.068 Uiso 1 1 calc R . . C54 C 0.6750(8) 0.1583(3) -0.0325(3) 0.0554(13) Uani 1 1 d . . . H54 H 0.7553 0.1629 -0.0697 0.066 Uiso 1 1 calc R . . C55 C 0.4826(8) 0.1203(3) -0.0471(3) 0.0579(14) Uani 1 1 d . . . H55 H 0.4326 0.0999 -0.0945 0.069 Uiso 1 1 calc R . . C56 C 0.3636(7) 0.1121(3) 0.0079(3) 0.0510(13) Uani 1 1 d . . . H56 H 0.2342 0.0856 -0.0022 0.061 Uiso 1 1 calc R . . H1A H 1.119(6) 0.428(3) 0.612(2) 0.049(15) Uiso 1 1 d D . . H1B H 1.124(8) 0.471(4) 0.548(2) 0.10(2) Uiso 1 1 d D . . H2 H 0.718(7) 0.534(3) 0.541(3) 0.09(2) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 B1 0.015(2) 0.031(3) 0.027(3) 0.005(2) 0.0063(18) 0.0036(19) O1 0.0203(14) 0.0332(18) 0.0276(17) 0.0070(14) 0.0044(13) 0.0015(12) O2 0.0267(15) 0.0263(16) 0.0280(15) 0.0055(12) 0.0056(12) 0.0072(13) C11 0.019(2) 0.028(2) 0.023(2) 0.0070(17) 0.0032(16) 0.0047(17) C12 0.018(2) 0.035(3) 0.021(2) 0.0038(19) -0.0008(16) 0.0036(18) C13 0.026(2) 0.028(2) 0.031(2) 0.0074(19) 0.0079(17) 0.0122(19) C14 0.025(2) 0.025(2) 0.021(2) 0.0055(17) 0.0030(16) 0.0046(17) C15 0.016(2) 0.027(2) 0.025(2) 0.0055(18) -0.0033(16) -0.0018(17) C16 0.023(2) 0.028(2) 0.020(2) 0.0044(18) 0.0051(16) 0.0110(18) F12 0.0212(12) 0.0410(14) 0.0397(13) -0.0087(11) -0.0022(10) 0.0090(10) F13 0.0263(12) 0.0385(14) 0.0407(14) -0.0032(11) 0.0019(10) 0.0146(10) F15 0.0224(12) 0.0302(13) 0.0360(13) 0.0006(10) -0.0040(9) 0.0036(9) F16 0.0224(11) 0.0258(12) 0.0393(13) -0.0002(10) 0.0010(9) 0.0068(10) C141 0.023(2) 0.025(2) 0.025(2) 0.0015(18) 0.0058(16) 0.0039(17) C142 0.022(2) 0.035(3) 0.029(2) 0.009(2) 0.0060(17) 0.0074(18) C143 0.028(2) 0.021(2) 0.043(3) 0.008(2) 0.0118(18) 0.0051(17) C144 0.027(2) 0.027(3) 0.034(3) -0.006(2) 0.0078(18) -0.0011(18) C145 0.026(2) 0.031(3) 0.025(2) 0.001(2) 0.0001(17) 0.0018(18) C146 0.027(2) 0.020(2) 0.034(2) 0.004(2) 0.0076(17) 0.0016(17) F142 0.0396(13) 0.0390(14) 0.0303(14) 0.0088(11) 0.0061(10) 0.0144(11) F143 0.0548(16) 0.0279(14) 0.0531(16) 0.0110(12) 0.0155(12) 0.0135(11) F144 0.0486(15) 0.0313(14) 0.0514(16) -0.0102(12) 0.0069(12) 0.0000(11) F145 0.0496(15) 0.0391(15) 0.0289(14) -0.0038(11) -0.0011(11) 0.0060(11) F146 0.0451(14) 0.0262(13) 0.0276(12) 0.0020(10) -0.0006(10) 0.0055(10) C21 0.016(2) 0.022(2) 0.028(2) -0.0014(17) 0.0015(16) -0.0012(16) C22 0.025(2) 0.023(2) 0.025(2) 0.0049(17) -0.0016(17) 0.0041(17) C23 0.022(2) 0.026(2) 0.031(2) 0.0026(18) 0.0078(17) 0.0066(17) C24 0.025(2) 0.020(2) 0.021(2) 0.0016(17) 0.0016(16) -0.0004(17) C25 0.024(2) 0.024(2) 0.022(2) 0.0104(17) 0.0029(16) 0.0042(17) C26 0.018(2) 0.024(2) 0.032(2) 0.0018(18) 0.0042(17) 0.0054(17) F22 0.0268(12) 0.0431(14) 0.0300(13) 0.0119(11) 0.0051(9) 0.0132(10) F23 0.0312(13) 0.0416(14) 0.0347(13) 0.0104(11) 0.0116(10) 0.0168(11) F25 0.0331(13) 0.0470(15) 0.0305(13) 0.0168(11) 0.0071(10) 0.0163(11) F26 0.0296(12) 0.0418(14) 0.0299(12) 0.0109(10) 0.0116(9) 0.0165(10) F242 0.0270(12) 0.0484(15) 0.0318(13) 0.0054(11) 0.0029(10) 0.0004(11) C241 0.028(2) 0.026(2) 0.023(2) 0.0034(17) 0.0027(17) 0.0089(18) C242 0.026(2) 0.032(2) 0.028(2) 0.0030(19) 0.0040(18) 0.0053(18) C243 0.030(2) 0.039(3) 0.035(3) 0.009(2) 0.0117(19) 0.012(2) C244 0.048(3) 0.039(3) 0.025(3) 0.010(2) 0.015(2) 0.016(2) C245 0.049(3) 0.035(3) 0.020(2) -0.0008(19) -0.001(2) 0.010(2) C246 0.029(2) 0.026(2) 0.033(3) 0.0041(19) 0.0039(18) 0.0014(18) F243 0.0337(14) 0.0690(18) 0.0442(15) 0.0209(13) 0.0176(11) 0.0113(12) F244 0.0739(18) 0.0655(18) 0.0263(14) 0.0129(12) 0.0231(12) 0.0266(14) F245 0.0672(17) 0.0571(17) 0.0227(13) -0.0036(12) -0.0046(12) 0.0040(13) F246 0.0382(14) 0.0457(15) 0.0347(14) 0.0036(11) -0.0018(10) -0.0077(11) C31 0.058(3) 0.032(3) 0.041(3) -0.001(2) 0.015(2) 0.000(2) C32 0.051(3) 0.033(3) 0.034(3) 0.002(2) 0.003(2) 0.005(2) C33 0.055(3) 0.040(3) 0.032(3) 0.002(2) 0.005(2) 0.004(2) C34 0.074(4) 0.036(3) 0.041(3) 0.010(2) -0.004(3) 0.002(3) C35 0.059(4) 0.030(3) 0.093(5) -0.011(3) -0.017(3) 0.015(2) C36 0.054(3) 0.038(3) 0.071(4) -0.019(3) 0.024(3) -0.003(2) C41 0.044(3) 0.035(3) 0.057(3) -0.003(3) 0.006(2) -0.003(2) C42 0.032(2) 0.038(3) 0.049(3) -0.010(2) 0.007(2) -0.001(2) C43 0.027(2) 0.055(3) 0.052(3) 0.006(3) 0.006(2) 0.004(2) C44 0.040(3) 0.030(3) 0.089(4) 0.008(3) 0.017(3) 0.005(2) C45 0.052(3) 0.043(3) 0.068(4) -0.018(3) 0.018(3) -0.008(2) C46 0.056(3) 0.058(4) 0.046(3) 0.001(3) 0.011(2) -0.010(3) C51 0.055(3) 0.048(3) 0.049(3) 0.014(2) 0.012(2) 0.009(2) C52 0.066(4) 0.042(3) 0.045(3) 0.003(2) -0.001(3) 0.005(3) C53 0.048(3) 0.048(3) 0.071(4) 0.012(3) 0.006(3) 0.002(2) C54 0.066(4) 0.055(3) 0.054(3) 0.014(3) 0.023(3) 0.025(3) C55 0.084(4) 0.052(3) 0.040(3) -0.006(2) 0.001(3) 0.024(3) C56 0.050(3) 0.041(3) 0.059(3) 0.003(3) 0.000(3) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 O2 1.462(5) . ? B1 O1 1.542(5) . ? B1 C21 1.630(5) . ? B1 C11 1.637(6) . ? O1 H1A 0.806(19) . ? O1 H1B 0.83(2) . ? O2 H2 0.78(2) . ? C11 C12 1.385(5) . ? C11 C16 1.389(5) . ? C12 F12 1.361(4) . ? C12 C13 1.378(5) . ? C13 F13 1.347(4) . ? C13 C14 1.390(5) . ? C14 C15 1.381(5) . ? C14 C141 1.485(5) . ? C15 F15 1.346(4) . ? C15 C16 1.368(5) . ? C16 F16 1.367(4) . ? C141 C146 1.385(5) . ? C141 C142 1.385(5) . ? C142 F142 1.342(4) . ? C142 C143 1.373(5) . ? C143 F143 1.351(4) . ? C143 C144 1.368(5) . ? C144 F144 1.342(4) . ? C144 C145 1.376(5) . ? C145 F145 1.348(4) . ? C145 C146 1.362(5) . ? C146 F146 1.354(4) . ? C21 C22 1.384(5) . ? C21 C26 1.390(5) . ? C22 F22 1.363(4) . ? C22 C23 1.372(5) . ? C23 F23 1.356(4) . ? C23 C24 1.384(5) . ? C24 C25 1.385(5) . ? C24 C241 1.480(5) . ? C25 F25 1.345(4) . ? C25 C26 1.372(5) . ? C26 F26 1.361(4) . ? F242 C242 1.338(4) . ? C241 C242 1.377(5) . ? C241 C246 1.392(5) . ? C242 C243 1.377(5) . ? C243 F243 1.344(4) . ? C243 C244 1.363(6) . ? C244 F244 1.346(4) . ? C244 C245 1.377(6) . ? C245 F245 1.340(4) . ? C245 C246 1.375(5) . ? C246 F246 1.345(4) . ? C31 C36 1.357(6) . ? C31 C32 1.376(6) . ? C31 H31 0.9300 . ? C32 C33 1.370(6) . ? C32 H32 0.9300 . ? C33 C34 1.372(6) . ? C33 H33 0.9300 . ? C34 C35 1.391(7) . ? C34 H34 0.9300 . ? C35 C36 1.399(7) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C42 1.371(6) . ? C41 C46 1.376(6) . ? C41 H41 0.9300 . ? C42 C43 1.375(6) . ? C42 H42 0.9300 . ? C43 C44 1.399(6) . ? C43 H43 0.9300 . ? C44 C45 1.373(7) . ? C44 H44 0.9300 . ? C45 C46 1.360(7) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C52 1.370(6) . ? C51 C56 1.380(6) . ? C51 H51 0.9300 . ? C52 C53 1.381(7) . ? C52 H52 0.9300 . ? C53 C54 1.375(7) . ? C53 H53 0.9300 . ? C54 C55 1.377(7) . ? C54 H54 0.9300 . ? C55 C56 1.377(7) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? 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 O2 B1 O1 102.9(3) . . ? O2 B1 C21 114.7(3) . . ? O1 B1 C21 107.9(3) . . ? O2 B1 C11 109.7(3) . . ? O1 B1 C11 110.8(3) . . ? C21 B1 C11 110.6(3) . . ? B1 O1 H1A 111(3) . . ? B1 O1 H1B 115(4) . . ? H1A O1 H1B 114(5) . . ? B1 O2 H2 125(4) . . ? C12 C11 C16 113.0(3) . . ? C12 C11 B1 126.6(3) . . ? C16 C11 B1 120.3(3) . . ? F12 C12 C13 116.2(3) . . ? F12 C12 C11 119.8(3) . . ? C13 C12 C11 124.0(3) . . ? F13 C13 C12 119.2(3) . . ? F13 C13 C14 119.3(3) . . ? C12 C13 C14 121.4(3) . . ? C15 C14 C13 115.6(3) . . ? C15 C14 C141 122.0(3) . . ? C13 C14 C141 122.3(3) . . ? F15 C15 C16 119.2(3) . . ? F15 C15 C14 119.1(3) . . ? C16 C15 C14 121.6(3) . . ? F16 C16 C15 117.0(3) . . ? F16 C16 C11 118.6(3) . . ? C15 C16 C11 124.4(3) . . ? C146 C141 C142 116.4(3) . . ? C146 C141 C14 120.7(3) . . ? C142 C141 C14 122.8(3) . . ? F142 C142 C143 119.1(3) . . ? F142 C142 C141 119.2(3) . . ? C143 C142 C141 121.8(3) . . ? F143 C143 C144 119.8(4) . . ? F143 C143 C142 120.1(4) . . ? C144 C143 C142 120.1(4) . . ? F144 C144 C143 120.3(4) . . ? F144 C144 C145 120.3(3) . . ? C143 C144 C145 119.4(4) . . ? F145 C145 C146 120.8(3) . . ? F145 C145 C144 119.3(3) . . ? C146 C145 C144 119.9(4) . . ? F146 C146 C145 117.7(3) . . ? F146 C146 C141 119.8(3) . . ? C145 C146 C141 122.4(3) . . ? C22 C21 C26 113.6(3) . . ? C22 C21 B1 125.9(3) . . ? C26 C21 B1 120.5(3) . . ? F22 C22 C23 116.9(3) . . ? F22 C22 C21 119.7(3) . . ? C23 C22 C21 123.4(3) . . ? F23 C23 C22 118.3(3) . . ? F23 C23 C24 119.3(3) . . ? C22 C23 C24 122.3(3) . . ? C23 C24 C25 115.3(3) . . ? C23 C24 C241 122.6(3) . . ? C25 C24 C241 122.0(3) . . ? F25 C25 C26 119.6(3) . . ? F25 C25 C24 118.8(3) . . ? C26 C25 C24 121.6(3) . . ? F26 C26 C25 117.7(3) . . ? F26 C26 C21 118.5(3) . . ? C25 C26 C21 123.8(3) . . ? C242 C241 C246 116.9(3) . . ? C242 C241 C24 121.3(3) . . ? C246 C241 C24 121.8(3) . . ? F242 C242 C243 118.8(3) . . ? F242 C242 C241 119.0(3) . . ? C243 C242 C241 122.1(4) . . ? F243 C243 C244 119.8(3) . . ? F243 C243 C242 120.8(4) . . ? C244 C243 C242 119.4(4) . . ? F244 C244 C243 120.1(4) . . ? F244 C244 C245 119.4(4) . . ? C243 C244 C245 120.5(4) . . ? F245 C245 C246 120.5(4) . . ? F245 C245 C244 120.3(4) . . ? C246 C245 C244 119.2(4) . . ? F246 C246 C245 118.3(3) . . ? F246 C246 C241 119.9(3) . . ? C245 C246 C241 121.8(4) . . ? C36 C31 C32 120.4(4) . . ? C36 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C33 C32 C31 120.7(4) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 120.1(4) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C35 119.6(4) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 119.6(4) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C31 C36 C35 119.7(5) . . ? C31 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C42 C41 C46 119.6(5) . . ? C42 C41 H41 120.2 . . ? C46 C41 H41 120.2 . . ? C41 C42 C43 120.7(4) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C42 C43 C44 119.0(4) . . ? C42 C43 H43 120.5 . . ? C44 C43 H43 120.5 . . ? C45 C44 C43 119.9(4) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C46 C45 C44 120.1(5) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C41 120.8(5) . . ? C45 C46 H46 119.6 . . ? C41 C46 H46 119.6 . . ? C52 C51 C56 119.8(5) . . ? C52 C51 H51 120.1 . . ? C56 C51 H51 120.1 . . ? C51 C52 C53 120.2(5) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C54 C53 C52 120.2(5) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 119.4(5) . . ? C53 C54 H54 120.3 . . ? C55 C54 H54 120.3 . . ? C56 C55 C54 120.6(5) . . ? C56 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? C55 C56 C51 119.8(5) . . ? C55 C56 H56 120.1 . . ? C51 C56 H56 120.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 B1 C11 C12 134.6(4) . . . . ? O1 B1 C11 C12 21.7(5) . . . . ? C21 B1 C11 C12 -97.9(4) . . . . ? O2 B1 C11 C16 -49.1(4) . . . . ? O1 B1 C11 C16 -162.1(3) . . . . ? C21 B1 C11 C16 78.4(4) . . . . ? C16 C11 C12 F12 -179.8(3) . . . . ? B1 C11 C12 F12 -3.3(5) . . . . ? C16 C11 C12 C13 2.1(5) . . . . ? B1 C11 C12 C13 178.5(4) . . . . ? F12 C12 C13 F13 0.5(5) . . . . ? C11 C12 C13 F13 178.6(3) . . . . ? F12 C12 C13 C14 -178.3(3) . . . . ? C11 C12 C13 C14 -0.1(6) . . . . ? F13 C13 C14 C15 179.5(3) . . . . ? C12 C13 C14 C15 -1.8(5) . . . . ? F13 C13 C14 C141 -3.9(5) . . . . ? C12 C13 C14 C141 174.8(3) . . . . ? C13 C14 C15 F15 -176.9(3) . . . . ? C141 C14 C15 F15 6.5(5) . . . . ? C13 C14 C15 C16 1.5(5) . . . . ? C141 C14 C15 C16 -175.1(3) . . . . ? F15 C15 C16 F16 0.7(5) . . . . ? C14 C15 C16 F16 -177.7(3) . . . . ? F15 C15 C16 C11 179.0(3) . . . . ? C14 C15 C16 C11 0.6(6) . . . . ? C12 C11 C16 F16 175.9(3) . . . . ? B1 C11 C16 F16 -0.8(5) . . . . ? C12 C11 C16 C15 -2.3(5) . . . . ? B1 C11 C16 C15 -179.1(3) . . . . ? C15 C14 C141 C146 57.7(5) . . . . ? C13 C14 C141 C146 -118.7(4) . . . . ? C15 C14 C141 C142 -123.1(4) . . . . ? C13 C14 C141 C142 60.5(5) . . . . ? C146 C141 C142 F142 -179.2(3) . . . . ? C14 C141 C142 F142 1.6(5) . . . . ? C146 C141 C142 C143 0.6(5) . . . . ? C14 C141 C142 C143 -178.6(3) . . . . ? F142 C142 C143 F143 -0.6(5) . . . . ? C141 C142 C143 F143 179.6(3) . . . . ? F142 C142 C143 C144 179.6(3) . . . . ? C141 C142 C143 C144 -0.2(6) . . . . ? F143 C143 C144 F144 0.3(5) . . . . ? C142 C143 C144 F144 -179.9(3) . . . . ? F143 C143 C144 C145 -179.8(3) . . . . ? C142 C143 C144 C145 0.0(6) . . . . ? F144 C144 C145 F145 0.0(5) . . . . ? C143 C144 C145 F145 -179.9(3) . . . . ? F144 C144 C145 C146 179.7(3) . . . . ? C143 C144 C145 C146 -0.2(6) . . . . ? F145 C145 C146 F146 -1.6(5) . . . . ? C144 C145 C146 F146 178.7(3) . . . . ? F145 C145 C146 C141 -179.6(3) . . . . ? C144 C145 C146 C141 0.7(6) . . . . ? C142 C141 C146 F146 -178.8(3) . . . . ? C14 C141 C146 F146 0.4(5) . . . . ? C142 C141 C146 C145 -0.9(5) . . . . ? C14 C141 C146 C145 178.4(3) . . . . ? O2 B1 C21 C22 21.9(5) . . . . ? O1 B1 C21 C22 135.9(4) . . . . ? C11 B1 C21 C22 -102.8(4) . . . . ? O2 B1 C21 C26 -160.8(3) . . . . ? O1 B1 C21 C26 -46.7(5) . . . . ? C11 B1 C21 C26 74.6(4) . . . . ? C26 C21 C22 F22 -178.7(3) . . . . ? B1 C21 C22 F22 -1.2(5) . . . . ? C26 C21 C22 C23 1.5(5) . . . . ? B1 C21 C22 C23 179.1(4) . . . . ? F22 C22 C23 F23 -2.4(5) . . . . ? C21 C22 C23 F23 177.4(3) . . . . ? F22 C22 C23 C24 -179.7(3) . . . . ? C21 C22 C23 C24 0.0(6) . . . . ? F23 C23 C24 C25 -179.0(3) . . . . ? C22 C23 C24 C25 -1.7(5) . . . . ? F23 C23 C24 C241 1.7(5) . . . . ? C22 C23 C24 C241 179.1(4) . . . . ? C23 C24 C25 F25 -177.2(3) . . . . ? C241 C24 C25 F25 2.0(5) . . . . ? C23 C24 C25 C26 1.8(5) . . . . ? C241 C24 C25 C26 -179.0(3) . . . . ? F25 C25 C26 F26 -0.6(5) . . . . ? C24 C25 C26 F26 -179.7(3) . . . . ? F25 C25 C26 C21 178.8(3) . . . . ? C24 C25 C26 C21 -0.2(6) . . . . ? C22 C21 C26 F26 178.0(3) . . . . ? B1 C21 C26 F26 0.3(5) . . . . ? C22 C21 C26 C25 -1.4(5) . . . . ? B1 C21 C26 C25 -179.1(3) . . . . ? C23 C24 C241 C242 56.1(5) . . . . ? C25 C24 C241 C242 -123.1(4) . . . . ? C23 C24 C241 C246 -122.8(4) . . . . ? C25 C24 C241 C246 58.0(5) . . . . ? C246 C241 C242 F242 -176.9(3) . . . . ? C24 C241 C242 F242 4.2(5) . . . . ? C246 C241 C242 C243 1.5(6) . . . . ? C24 C241 C242 C243 -177.4(3) . . . . ? F242 C242 C243 F243 -1.0(6) . . . . ? C241 C242 C243 F243 -179.4(3) . . . . ? F242 C242 C243 C244 177.4(3) . . . . ? C241 C242 C243 C244 -1.1(6) . . . . ? F243 C243 C244 F244 -3.8(6) . . . . ? C242 C243 C244 F244 177.9(3) . . . . ? F243 C243 C244 C245 178.2(4) . . . . ? C242 C243 C244 C245 -0.2(6) . . . . ? F244 C244 C245 F245 1.5(6) . . . . ? C243 C244 C245 F245 179.6(4) . . . . ? F244 C244 C245 C246 -177.2(3) . . . . ? C243 C244 C245 C246 0.8(6) . . . . ? F245 C245 C246 F246 0.2(6) . . . . ? C244 C245 C246 F246 179.0(3) . . . . ? F245 C245 C246 C241 -179.1(3) . . . . ? C244 C245 C246 C241 -0.4(6) . . . . ? C242 C241 C246 F246 179.9(3) . . . . ? C24 C241 C246 F246 -1.2(5) . . . . ? C242 C241 C246 C245 -0.8(6) . . . . ? C24 C241 C246 C245 178.1(4) . . . . ? C36 C31 C32 C33 0.1(7) . . . . ? C31 C32 C33 C34 0.0(7) . . . . ? C32 C33 C34 C35 0.2(7) . . . . ? C33 C34 C35 C36 -0.5(7) . . . . ? C32 C31 C36 C35 -0.5(7) . . . . ? C34 C35 C36 C31 0.7(7) . . . . ? C46 C41 C42 C43 -0.3(7) . . . . ? C41 C42 C43 C44 0.4(6) . . . . ? C42 C43 C44 C45 -0.4(6) . . . . ? C43 C44 C45 C46 0.3(7) . . . . ? C44 C45 C46 C41 -0.2(7) . . . . ? C42 C41 C46 C45 0.2(7) . . . . ? C56 C51 C52 C53 -0.2(7) . . . . ? C51 C52 C53 C54 0.2(7) . . . . ? C52 C53 C54 C55 0.3(7) . . . . ? C53 C54 C55 C56 -0.9(7) . . . . ? C54 C55 C56 C51 0.9(7) . . . . ? C52 C51 C56 C55 -0.3(7) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1B O2 0.83(2) 1.64(2) 2.464(4) 173(6) 2_766 O1 H1A F12 0.806(19) 2.36(4) 2.710(4) 108(4) . O1 H1A F26 0.806(19) 2.10(3) 2.724(4) 134(4) . O2 H2 F22 0.78(2) 2.27(5) 2.772(3) 122(5) . O2 H2 F16 0.78(2) 2.40(4) 3.075(3) 146(5) 2_666 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.242 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.059 #===END data_em37 _database_code_depnum_ccdc_archive 'CCDC 704297' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; Bis(pentafluorophenyl)(nonfluorobiphenyl)boron acetonitrile, acetonitrile solvate ; _chemical_formula_structural '[(C6F5)2(p-C6F5-C6F4)B.CH3CN].MeCN' _chemical_name_common ; Bis(pentafluorophenyl)(nonfluorobiphenyl)boron acetonitrile, acetonitrile solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C26 H3 B F19 N, C2 H3 N' _chemical_formula_sum 'C28 H6 B F19 N2' _chemical_formula_weight 742.16 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 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 10.1502(4) _cell_length_b 9.9420(3) _cell_length_c 27.4704(11) _cell_angle_alpha 90.00 _cell_angle_beta 99.069(4) _cell_angle_gamma 90.00 _cell_volume 2737.47(17) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.801 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_absorpt_coefficient_mu 0.197 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 1.16 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28704 _diffrn_reflns_av_R_equivalents 0.0867 _diffrn_reflns_av_sigmaI/netI 0.0709 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.46 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4798 _reflns_number_gt 3031 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0255P)^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_extinction_coef ? _refine_ls_number_reflns 4798 _refine_ls_number_parameters 476 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0661 _refine_ls_wR_factor_gt 0.0575 _refine_ls_goodness_of_fit_ref 0.908 _refine_ls_restrained_S_all 0.908 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.2166(3) 0.9030(3) 0.37082(9) 0.0196(6) Uani 1 1 d . . . C11 C 0.1742(2) 0.7990(2) 0.32548(8) 0.0184(5) Uani 1 1 d . . . C12 C 0.1913(2) 0.8177(2) 0.27660(8) 0.0194(5) Uani 1 1 d . . . C13 C 0.1475(2) 0.7274(2) 0.23989(8) 0.0216(6) Uani 1 1 d . . . C14 C 0.0833(2) 0.6131(2) 0.25022(9) 0.0253(6) Uani 1 1 d . . . C15 C 0.0610(2) 0.5898(2) 0.29768(9) 0.0264(6) Uani 1 1 d . . . C16 C 0.1076(2) 0.6822(2) 0.33363(8) 0.0220(6) Uani 1 1 d . . . F12 F 0.25212(13) 0.92872(13) 0.26290(4) 0.0278(3) Uani 1 1 d . . . F13 F 0.16614(13) 0.75144(13) 0.19316(5) 0.0308(3) Uani 1 1 d . . . F14 F 0.04194(14) 0.52293(13) 0.21475(5) 0.0404(4) Uani 1 1 d . . . F15 F -0.00242(15) 0.47853(13) 0.30874(5) 0.0413(4) Uani 1 1 d . . . F16 F 0.08566(13) 0.65406(13) 0.37982(4) 0.0321(3) Uani 1 1 d . . . C21 C 0.3082(2) 0.8395(2) 0.41995(8) 0.0180(5) Uani 1 1 d . . . C22 C 0.3887(2) 0.7276(2) 0.42056(8) 0.0195(5) Uani 1 1 d . . . C23 C 0.4737(2) 0.6840(2) 0.46191(8) 0.0246(6) Uani 1 1 d . . . C24 C 0.4798(2) 0.7528(2) 0.50529(8) 0.0261(6) Uani 1 1 d . . . C25 C 0.4021(2) 0.8643(2) 0.50708(8) 0.0235(6) Uani 1 1 d . . . C26 C 0.3204(2) 0.9059(2) 0.46498(8) 0.0204(5) Uani 1 1 d . . . F22 F 0.38987(13) 0.65468(12) 0.37938(4) 0.0277(3) Uani 1 1 d . . . F23 F 0.55143(14) 0.57547(14) 0.45926(5) 0.0395(4) Uani 1 1 d . . . F24 F 0.56266(14) 0.71188(14) 0.54542(5) 0.0408(4) Uani 1 1 d . . . F25 F 0.40828(13) 0.93474(13) 0.54920(4) 0.0335(4) Uani 1 1 d . . . F26 F 0.25150(13) 1.02122(13) 0.46879(4) 0.0292(3) Uani 1 1 d . . . C31 C 0.2893(2) 1.0406(2) 0.35738(7) 0.0173(5) Uani 1 1 d . . . C32 C 0.2412(2) 1.1709(2) 0.35673(8) 0.0208(5) Uani 1 1 d . . . C33 C 0.3159(2) 1.2823(2) 0.34911(8) 0.0205(5) Uani 1 1 d . . . C34 C 0.4472(2) 1.2716(2) 0.34151(8) 0.0198(5) Uani 1 1 d . . . C35 C 0.4957(2) 1.1420(2) 0.34084(8) 0.0198(5) Uani 1 1 d . . . C36 C 0.4198(2) 1.0324(2) 0.34850(8) 0.0185(5) Uani 1 1 d . . . F32 F 0.11527(13) 1.19565(12) 0.36496(5) 0.0315(3) Uani 1 1 d . . . F33 F 0.26243(13) 1.40463(12) 0.35212(5) 0.0321(4) Uani 1 1 d . . . F35 F 0.62187(12) 1.12156(12) 0.33288(5) 0.0298(3) Uani 1 1 d . . . F36 F 0.47713(12) 0.90994(12) 0.34711(5) 0.0275(3) Uani 1 1 d . . . C341 C 0.5298(2) 1.3915(2) 0.33665(8) 0.0223(6) Uani 1 1 d . . . C342 C 0.4926(2) 1.4903(2) 0.30172(8) 0.0267(6) Uani 1 1 d . . . C343 C 0.5655(3) 1.6059(2) 0.29939(9) 0.0337(7) Uani 1 1 d . . . C344 C 0.6803(3) 1.6251(3) 0.33218(10) 0.0393(7) Uani 1 1 d . . . C345 C 0.7205(3) 1.5297(3) 0.36737(10) 0.0367(7) Uani 1 1 d . . . C346 C 0.6464(2) 1.4156(2) 0.36926(9) 0.0287(6) Uani 1 1 d . . . F342 F 0.38050(14) 1.47464(13) 0.26911(5) 0.0367(4) Uani 1 1 d . . . F343 F 0.52372(17) 1.70054(14) 0.26596(5) 0.0529(5) Uani 1 1 d . . . F344 F 0.75244(17) 1.73730(15) 0.33029(6) 0.0619(5) Uani 1 1 d . . . F345 F 0.83103(16) 1.54911(17) 0.40063(6) 0.0601(5) Uani 1 1 d . . . F346 F 0.68743(14) 1.32551(14) 0.40515(5) 0.0390(4) Uani 1 1 d . . . N4 N 0.07904(19) 0.93854(18) 0.38803(6) 0.0202(5) Uani 1 1 d . . . C41 C -0.0202(3) 0.9583(2) 0.40026(8) 0.0241(6) Uani 1 1 d . . . C42 C -0.1479(3) 0.9876(4) 0.41535(14) 0.0397(8) Uani 1 1 d . . . N5 N 1.0065(3) 0.7761(3) 0.50202(11) 0.0775(10) Uani 1 1 d . . . C51 C 0.9498(3) 0.6937(3) 0.51848(11) 0.0533(9) Uani 1 1 d . . . C52 C 0.8776(3) 0.5869(3) 0.53952(12) 0.0678(10) Uani 1 1 d . . . H52A H 0.8809 0.5060 0.5207 0.102 Uiso 1 1 calc R . . H52B H 0.7864 0.6134 0.5387 0.102 Uiso 1 1 calc R . . H52C H 0.9181 0.5710 0.5730 0.102 Uiso 1 1 calc R . . H42A H -0.137(4) 0.992(6) 0.4515(16) 0.012(12) Uiso 0.50 1 d P . . H42C H -0.181(5) 1.088(6) 0.400(2) 0.041(16) Uiso 0.50 1 d P . . H42B H -0.203(6) 0.907(7) 0.400(3) 0.06(2) Uiso 0.50 1 d P . . H42E H -0.219(5) 0.986(6) 0.3879(17) 0.020(13) Uiso 0.50 1 d P . . H42F H -0.180(6) 0.912(7) 0.434(3) 0.06(2) Uiso 0.50 1 d P . . H42D H -0.143(6) 1.072(7) 0.433(3) 0.06(2) Uiso 0.50 1 d P . . 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 0.0169(15) 0.0207(15) 0.0223(15) -0.0006(12) 0.0060(12) -0.0015(12) C11 0.0137(12) 0.0210(14) 0.0200(13) 0.0023(11) 0.0008(10) 0.0012(10) C12 0.0163(13) 0.0176(13) 0.0245(14) 0.0030(11) 0.0042(10) -0.0019(11) C13 0.0214(13) 0.0267(14) 0.0168(14) -0.0013(11) 0.0036(10) 0.0066(12) C14 0.0269(14) 0.0222(14) 0.0240(14) -0.0093(12) -0.0046(11) -0.0014(12) C15 0.0265(14) 0.0205(14) 0.0296(15) 0.0041(12) -0.0036(11) -0.0072(12) C16 0.0223(14) 0.0263(15) 0.0164(13) 0.0044(11) 0.0004(10) -0.0031(11) F12 0.0348(8) 0.0280(8) 0.0221(7) 0.0013(6) 0.0088(6) -0.0083(7) F13 0.0329(8) 0.0405(8) 0.0199(7) -0.0057(6) 0.0069(6) 0.0027(7) F14 0.0508(10) 0.0331(8) 0.0333(8) -0.0105(7) -0.0052(7) -0.0087(8) F15 0.0505(10) 0.0293(8) 0.0399(9) 0.0045(7) -0.0059(7) -0.0216(8) F16 0.0392(9) 0.0346(8) 0.0224(8) 0.0058(6) 0.0040(6) -0.0150(7) C21 0.0178(12) 0.0191(13) 0.0179(13) 0.0001(10) 0.0057(10) -0.0042(11) C22 0.0229(14) 0.0211(13) 0.0160(13) -0.0041(11) 0.0078(11) -0.0014(11) C23 0.0237(14) 0.0234(14) 0.0267(14) 0.0027(12) 0.0040(11) 0.0080(11) C24 0.0221(14) 0.0377(16) 0.0172(14) 0.0063(12) -0.0004(11) -0.0003(12) C25 0.0240(14) 0.0320(15) 0.0152(13) -0.0047(11) 0.0055(11) -0.0017(12) C26 0.0176(13) 0.0203(14) 0.0246(14) -0.0017(11) 0.0076(11) -0.0004(11) F22 0.0353(8) 0.0258(7) 0.0216(7) -0.0045(6) 0.0030(6) 0.0059(7) F23 0.0454(10) 0.0408(9) 0.0314(8) 0.0028(7) 0.0037(7) 0.0215(8) F24 0.0386(9) 0.0603(10) 0.0208(8) 0.0038(7) -0.0043(7) 0.0146(8) F25 0.0355(9) 0.0459(9) 0.0187(7) -0.0092(7) 0.0032(6) 0.0007(7) F26 0.0329(8) 0.0286(8) 0.0259(7) -0.0060(6) 0.0037(6) 0.0060(7) C31 0.0193(13) 0.0209(13) 0.0114(12) -0.0005(10) 0.0010(10) 0.0002(11) C32 0.0152(13) 0.0246(14) 0.0228(13) -0.0007(11) 0.0037(10) 0.0020(11) C33 0.0228(14) 0.0159(13) 0.0222(13) -0.0020(11) 0.0016(10) 0.0023(11) C34 0.0256(14) 0.0196(13) 0.0142(12) -0.0018(10) 0.0027(10) -0.0022(11) C35 0.0145(13) 0.0271(14) 0.0187(13) 0.0011(11) 0.0048(10) -0.0001(12) C36 0.0217(13) 0.0157(13) 0.0177(12) 0.0006(10) 0.0019(10) 0.0046(11) F32 0.0209(8) 0.0243(8) 0.0507(9) 0.0007(7) 0.0104(7) 0.0019(6) F33 0.0322(8) 0.0180(8) 0.0479(9) -0.0018(7) 0.0123(7) 0.0017(7) F35 0.0222(8) 0.0289(8) 0.0407(9) 0.0025(7) 0.0124(6) 0.0003(6) F36 0.0267(8) 0.0201(7) 0.0382(8) 0.0018(6) 0.0130(6) 0.0032(6) C341 0.0257(14) 0.0220(14) 0.0216(13) -0.0037(11) 0.0110(11) -0.0033(11) C342 0.0354(16) 0.0252(15) 0.0210(14) -0.0058(12) 0.0095(12) -0.0023(13) C343 0.060(2) 0.0188(15) 0.0281(15) 0.0015(12) 0.0238(14) -0.0074(14) C344 0.0515(19) 0.0290(16) 0.0442(18) -0.0095(14) 0.0287(15) -0.0231(15) C345 0.0294(16) 0.0435(18) 0.0390(17) -0.0132(14) 0.0112(13) -0.0167(14) C346 0.0286(15) 0.0302(15) 0.0292(15) 0.0004(12) 0.0103(12) 0.0003(13) F342 0.0493(10) 0.0318(8) 0.0273(8) 0.0025(7) 0.0005(7) -0.0019(7) F343 0.0977(14) 0.0286(9) 0.0366(9) 0.0059(8) 0.0237(9) -0.0131(9) F344 0.0759(13) 0.0431(10) 0.0733(12) -0.0126(9) 0.0319(10) -0.0363(10) F345 0.0383(10) 0.0721(12) 0.0680(11) -0.0137(9) 0.0028(9) -0.0295(9) F346 0.0304(9) 0.0435(9) 0.0404(9) 0.0037(8) -0.0032(7) -0.0051(7) N4 0.0204(12) 0.0202(11) 0.0200(11) 0.0022(9) 0.0030(9) 0.0005(9) C41 0.0256(15) 0.0245(15) 0.0212(13) 0.0037(11) 0.0012(12) -0.0005(12) C42 0.0237(17) 0.058(3) 0.040(2) -0.003(2) 0.0115(16) 0.0059(17) N5 0.110(3) 0.061(2) 0.064(2) 0.0077(17) 0.0211(18) 0.0046(19) C51 0.068(2) 0.054(2) 0.040(2) 0.0012(17) 0.0136(17) 0.0224(19) C52 0.069(2) 0.071(2) 0.069(2) 0.012(2) 0.0281(19) 0.022(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag B1 N4 1.583(3) . ? B1 C11 1.624(3) . ? B1 C31 1.624(3) . ? B1 C21 1.640(3) . ? C11 C16 1.380(3) . ? C11 C12 1.393(3) . ? C12 F12 1.347(2) . ? C12 C13 1.371(3) . ? C13 F13 1.348(2) . ? C13 C14 1.362(3) . ? C14 F14 1.342(2) . ? C14 C15 1.378(3) . ? C15 F15 1.339(2) . ? C15 C16 1.376(3) . ? C16 F16 1.352(2) . ? C21 C22 1.380(3) . ? C21 C26 1.390(3) . ? C22 F22 1.345(2) . ? C22 C23 1.383(3) . ? C23 F23 1.345(2) . ? C23 C24 1.367(3) . ? C24 F24 1.340(3) . ? C24 C25 1.366(3) . ? C25 F25 1.345(2) . ? C25 C26 1.376(3) . ? C26 F26 1.356(2) . ? C31 C32 1.384(3) . ? C31 C36 1.386(3) . ? C32 F32 1.355(2) . ? C32 C33 1.376(3) . ? C33 F33 1.340(2) . ? C33 C34 1.385(3) . ? C34 C35 1.381(3) . ? C34 C341 1.475(3) . ? C35 F35 1.348(2) . ? C35 C36 1.370(3) . ? C36 F36 1.352(2) . ? C341 C342 1.383(3) . ? C341 C346 1.389(3) . ? C342 F342 1.341(3) . ? C342 C343 1.374(3) . ? C343 F343 1.337(3) . ? C343 C344 1.369(4) . ? C344 F344 1.340(3) . ? C344 C345 1.369(4) . ? C345 F345 1.345(3) . ? C345 C346 1.366(3) . ? C346 F346 1.349(3) . ? N4 C41 1.129(3) . ? C41 C42 1.451(4) . ? C42 H42A 0.98(4) . ? C42 H42C 1.11(5) . ? C42 H42B 1.03(6) . ? C42 H42E 0.96(5) . ? C42 H42F 0.99(6) . ? C42 H42D 0.97(6) . ? N5 C51 1.136(4) . ? C51 C52 1.460(4) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 B1 C11 103.38(18) . . ? N4 B1 C31 109.50(19) . . ? C11 B1 C31 115.91(18) . . ? N4 B1 C21 104.63(17) . . ? C11 B1 C21 115.70(19) . . ? C31 B1 C21 106.99(18) . . ? C16 C11 C12 114.0(2) . . ? C16 C11 B1 119.29(19) . . ? C12 C11 B1 126.6(2) . . ? F12 C12 C13 116.17(19) . . ? F12 C12 C11 120.71(19) . . ? C13 C12 C11 123.1(2) . . ? F13 C13 C14 119.3(2) . . ? F13 C13 C12 120.4(2) . . ? C14 C13 C12 120.2(2) . . ? F14 C14 C13 120.8(2) . . ? F14 C14 C15 119.7(2) . . ? C13 C14 C15 119.5(2) . . ? F15 C15 C16 120.8(2) . . ? F15 C15 C14 120.7(2) . . ? C16 C15 C14 118.5(2) . . ? F16 C16 C15 116.5(2) . . ? F16 C16 C11 118.92(19) . . ? C15 C16 C11 124.5(2) . . ? C22 C21 C26 113.7(2) . . ? C22 C21 B1 125.4(2) . . ? C26 C21 B1 120.6(2) . . ? F22 C22 C21 120.5(2) . . ? F22 C22 C23 115.8(2) . . ? C21 C22 C23 123.7(2) . . ? F23 C23 C24 120.2(2) . . ? F23 C23 C22 120.1(2) . . ? C24 C23 C22 119.7(2) . . ? F24 C24 C25 120.5(2) . . ? F24 C24 C23 120.1(2) . . ? C25 C24 C23 119.4(2) . . ? F25 C25 C24 120.3(2) . . ? F25 C25 C26 120.5(2) . . ? C24 C25 C26 119.2(2) . . ? F26 C26 C25 116.0(2) . . ? F26 C26 C21 119.7(2) . . ? C25 C26 C21 124.3(2) . . ? C32 C31 C36 113.4(2) . . ? C32 C31 B1 128.3(2) . . ? C36 C31 B1 118.12(19) . . ? F32 C32 C33 115.87(19) . . ? F32 C32 C31 120.5(2) . . ? C33 C32 C31 123.6(2) . . ? F33 C33 C32 118.8(2) . . ? F33 C33 C34 119.2(2) . . ? C32 C33 C34 121.9(2) . . ? C35 C34 C33 115.2(2) . . ? C35 C34 C341 123.0(2) . . ? C33 C34 C341 121.7(2) . . ? F35 C35 C36 118.5(2) . . ? F35 C35 C34 119.5(2) . . ? C36 C35 C34 122.0(2) . . ? F36 C36 C35 117.2(2) . . ? F36 C36 C31 119.0(2) . . ? C35 C36 C31 123.8(2) . . ? C342 C341 C346 115.9(2) . . ? C342 C341 C34 122.7(2) . . ? C346 C341 C34 121.3(2) . . ? F342 C342 C343 118.2(2) . . ? F342 C342 C341 119.4(2) . . ? C343 C342 C341 122.4(2) . . ? F343 C343 C344 119.9(2) . . ? F343 C343 C342 120.4(3) . . ? C344 C343 C342 119.7(2) . . ? F344 C344 C343 120.3(3) . . ? F344 C344 C345 120.0(3) . . ? C343 C344 C345 119.7(2) . . ? F345 C345 C346 119.9(3) . . ? F345 C345 C344 120.3(2) . . ? C346 C345 C344 119.8(3) . . ? F346 C346 C345 118.1(2) . . ? F346 C346 C341 119.4(2) . . ? C345 C346 C341 122.5(2) . . ? C41 N4 B1 177.1(2) . . ? N4 C41 C42 178.3(3) . . ? C41 C42 H42A 110(2) . . ? C41 C42 H42C 108(3) . . ? H42A C42 H42C 109(4) . . ? C41 C42 H42B 100(3) . . ? H42A C42 H42B 115(4) . . ? H42C C42 H42B 116(5) . . ? C41 C42 H42E 111(3) . . ? H42A C42 H42E 138(4) . . ? H42C C42 H42E 65(3) . . ? H42B C42 H42E 51(4) . . ? C41 C42 H42F 112(3) . . ? H42A C42 H42F 60(4) . . ? H42C C42 H42F 140(4) . . ? H42B C42 H42F 55(4) . . ? H42E C42 H42F 98(5) . . ? C41 C42 H42D 110(4) . . ? H42A C42 H42D 58(4) . . ? H42C C42 H42D 53(4) . . ? H42B C42 H42D 150(5) . . ? H42E C42 H42D 113(5) . . ? H42F C42 H42D 113(5) . . ? N5 C51 C52 179.6(4) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 B1 C11 C16 -57.9(3) . . . . ? C31 B1 C11 C16 -177.7(2) . . . . ? C21 B1 C11 C16 55.9(3) . . . . ? N4 B1 C11 C12 118.3(2) . . . . ? C31 B1 C11 C12 -1.6(3) . . . . ? C21 B1 C11 C12 -128.0(2) . . . . ? C16 C11 C12 F12 178.65(19) . . . . ? B1 C11 C12 F12 2.4(3) . . . . ? C16 C11 C12 C13 -0.8(3) . . . . ? B1 C11 C12 C13 -177.1(2) . . . . ? F12 C12 C13 F13 0.1(3) . . . . ? C11 C12 C13 F13 179.57(19) . . . . ? F12 C12 C13 C14 -179.17(19) . . . . ? C11 C12 C13 C14 0.3(3) . . . . ? F13 C13 C14 F14 1.8(3) . . . . ? C12 C13 C14 F14 -178.9(2) . . . . ? F13 C13 C14 C15 -178.4(2) . . . . ? C12 C13 C14 C15 0.9(3) . . . . ? F14 C14 C15 F15 -0.5(3) . . . . ? C13 C14 C15 F15 179.7(2) . . . . ? F14 C14 C15 C16 178.3(2) . . . . ? C13 C14 C15 C16 -1.5(3) . . . . ? F15 C15 C16 F16 0.0(3) . . . . ? C14 C15 C16 F16 -178.8(2) . . . . ? F15 C15 C16 C11 179.8(2) . . . . ? C14 C15 C16 C11 1.0(4) . . . . ? C12 C11 C16 F16 179.99(19) . . . . ? B1 C11 C16 F16 -3.4(3) . . . . ? C12 C11 C16 C15 0.1(3) . . . . ? B1 C11 C16 C15 176.7(2) . . . . ? N4 B1 C21 C22 137.2(2) . . . . ? C11 B1 C21 C22 24.2(3) . . . . ? C31 B1 C21 C22 -106.7(2) . . . . ? N4 B1 C21 C26 -49.5(3) . . . . ? C11 B1 C21 C26 -162.5(2) . . . . ? C31 B1 C21 C26 66.7(2) . . . . ? C26 C21 C22 F22 -178.57(18) . . . . ? B1 C21 C22 F22 -4.8(3) . . . . ? C26 C21 C22 C23 0.2(3) . . . . ? B1 C21 C22 C23 173.9(2) . . . . ? F22 C22 C23 F23 0.3(3) . . . . ? C21 C22 C23 F23 -178.5(2) . . . . ? F22 C22 C23 C24 179.47(19) . . . . ? C21 C22 C23 C24 0.6(4) . . . . ? F23 C23 C24 F24 -0.4(3) . . . . ? C22 C23 C24 F24 -179.5(2) . . . . ? F23 C23 C24 C25 178.8(2) . . . . ? C22 C23 C24 C25 -0.4(4) . . . . ? F24 C24 C25 F25 0.3(3) . . . . ? C23 C24 C25 F25 -178.9(2) . . . . ? F24 C24 C25 C26 178.4(2) . . . . ? C23 C24 C25 C26 -0.8(3) . . . . ? F25 C25 C26 F26 1.5(3) . . . . ? C24 C25 C26 F26 -176.6(2) . . . . ? F25 C25 C26 C21 179.8(2) . . . . ? C24 C25 C26 C21 1.7(4) . . . . ? C22 C21 C26 F26 176.86(18) . . . . ? B1 C21 C26 F26 2.8(3) . . . . ? C22 C21 C26 C25 -1.4(3) . . . . ? B1 C21 C26 C25 -175.5(2) . . . . ? N4 B1 C31 C32 -4.3(3) . . . . ? C11 B1 C31 C32 112.1(3) . . . . ? C21 B1 C31 C32 -117.2(2) . . . . ? N4 B1 C31 C36 170.67(18) . . . . ? C11 B1 C31 C36 -72.9(3) . . . . ? C21 B1 C31 C36 57.8(2) . . . . ? C36 C31 C32 F32 -179.77(19) . . . . ? B1 C31 C32 F32 -4.6(3) . . . . ? C36 C31 C32 C33 -1.3(3) . . . . ? B1 C31 C32 C33 173.9(2) . . . . ? F32 C32 C33 F33 2.5(3) . . . . ? C31 C32 C33 F33 -176.1(2) . . . . ? F32 C32 C33 C34 178.4(2) . . . . ? C31 C32 C33 C34 -0.1(4) . . . . ? F33 C33 C34 C35 177.55(19) . . . . ? C32 C33 C34 C35 1.7(3) . . . . ? F33 C33 C34 C341 0.0(3) . . . . ? C32 C33 C34 C341 -175.9(2) . . . . ? C33 C34 C35 F35 178.95(19) . . . . ? C341 C34 C35 F35 -3.6(3) . . . . ? C33 C34 C35 C36 -1.7(3) . . . . ? C341 C34 C35 C36 175.8(2) . . . . ? F35 C35 C36 F36 -0.5(3) . . . . ? C34 C35 C36 F36 -179.94(19) . . . . ? F35 C35 C36 C31 179.57(19) . . . . ? C34 C35 C36 C31 0.2(3) . . . . ? C32 C31 C36 F36 -178.56(18) . . . . ? B1 C31 C36 F36 5.7(3) . . . . ? C32 C31 C36 C35 1.3(3) . . . . ? B1 C31 C36 C35 -174.4(2) . . . . ? C35 C34 C341 C342 126.3(2) . . . . ? C33 C34 C341 C342 -56.3(3) . . . . ? C35 C34 C341 C346 -57.7(3) . . . . ? C33 C34 C341 C346 119.6(3) . . . . ? C346 C341 C342 F342 -179.6(2) . . . . ? C34 C341 C342 F342 -3.4(3) . . . . ? C346 C341 C342 C343 -0.5(3) . . . . ? C34 C341 C342 C343 175.7(2) . . . . ? F342 C342 C343 F343 1.2(3) . . . . ? C341 C342 C343 F343 -178.0(2) . . . . ? F342 C342 C343 C344 179.9(2) . . . . ? C341 C342 C343 C344 0.8(4) . . . . ? F343 C343 C344 F344 -1.3(4) . . . . ? C342 C343 C344 F344 179.9(2) . . . . ? F343 C343 C344 C345 177.9(2) . . . . ? C342 C343 C344 C345 -0.8(4) . . . . ? F344 C344 C345 F345 1.1(4) . . . . ? C343 C344 C345 F345 -178.2(2) . . . . ? F344 C344 C345 C346 179.8(2) . . . . ? C343 C344 C345 C346 0.6(4) . . . . ? F345 C345 C346 F346 0.3(4) . . . . ? C344 C345 C346 F346 -178.5(2) . . . . ? F345 C345 C346 C341 178.5(2) . . . . ? C344 C345 C346 C341 -0.3(4) . . . . ? C342 C341 C346 F346 178.37(19) . . . . ? C34 C341 C346 F346 2.1(3) . . . . ? C342 C341 C346 C345 0.2(3) . . . . ? C34 C341 C346 C345 -176.0(2) . . . . ? C11 B1 N4 C41 47(5) . . . . ? C31 B1 N4 C41 171(91) . . . . ? C21 B1 N4 C41 -74(5) . . . . ? B1 N4 C41 C42 -153(9) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.225 _refine_diff_density_min -0.200 _refine_diff_density_rms 0.043 #===END data_em54 _database_code_depnum_ccdc_archive 'CCDC 704298' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; Tris(p-Nonafluorobiphenyl)boron acetonitrile bis(dichloromethane) solvate ; _chemical_formula_structural '[(C6F5C6F4)3B(NCCH3)].(CH2Cl2)2' _chemical_name_common ;Tris(p-Nonafluorobiphenyl)boron acetonitrile bis(dichloromethane) solvate ; _chemical_melting_point ? _chemical_formula_moiety 'C38 H3 B F27 N, 2(CH2Cl2)' _chemical_formula_sum 'C40 H7 B Cl4 F27 N' _chemical_formula_weight 1167.08 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' Cl Cl 0.1484 0.1585 '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 9.2820(4) _cell_length_b 13.8838(5) _cell_length_c 17.4899(7) _cell_angle_alpha 104.808(3) _cell_angle_beta 89.136(3) _cell_angle_gamma 105.715(3) _cell_volume 2094.05(14) _cell_formula_units_Z 2 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.851 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.09 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23775 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_sigmaI/netI 0.1282 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.11 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7309 _reflns_number_gt 3380 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0354P)^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 7309 _refine_ls_number_parameters 694 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1434 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.0908 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 0.847 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group B1 B 0.1836(5) 0.1079(4) 0.2217(2) 0.0285(11) Uani 1 1 d . . . C11 C 0.2949(4) 0.1660(3) 0.3002(2) 0.0243(9) Uani 1 1 d . . . C12 C 0.3488(4) 0.2731(3) 0.3244(2) 0.0275(10) Uani 1 1 d . . . C13 C 0.4376(4) 0.3268(3) 0.3919(2) 0.0282(10) Uani 1 1 d . . . C14 C 0.4809(4) 0.2764(3) 0.4421(2) 0.0269(10) Uani 1 1 d . . . C15 C 0.4298(4) 0.1698(3) 0.4196(2) 0.0328(10) Uani 1 1 d . . . C16 C 0.3414(4) 0.1180(3) 0.3514(2) 0.0297(10) Uani 1 1 d . . . F12 F 0.3108(2) 0.33070(16) 0.27942(12) 0.0393(6) Uani 1 1 d . . . F13 F 0.4823(2) 0.43156(17) 0.40990(12) 0.0430(6) Uani 1 1 d . . . F15 F 0.3015(2) 0.01324(17) 0.33459(13) 0.0453(6) Uani 1 1 d . . . F16 F 0.4684(2) 0.11544(17) 0.46585(13) 0.0494(7) Uani 1 1 d . . . C141 C 0.5737(4) 0.3334(3) 0.5169(2) 0.0310(10) Uani 1 1 d . . . C142 C 0.7176(5) 0.3916(3) 0.5158(2) 0.0457(12) Uani 1 1 d . . . C143 C 0.8058(4) 0.4442(4) 0.5846(2) 0.0499(13) Uani 1 1 d . . . C144 C 0.7496(5) 0.4374(3) 0.6556(2) 0.0441(12) Uani 1 1 d . . . C145 C 0.6052(5) 0.3811(3) 0.6594(2) 0.0374(11) Uani 1 1 d . . . C146 C 0.5192(4) 0.3306(3) 0.5900(2) 0.0343(10) Uani 1 1 d . . . F142 F 0.7768(2) 0.3987(2) 0.44613(14) 0.0730(9) Uani 1 1 d . . . F143 F 0.9472(3) 0.5003(2) 0.58220(15) 0.0906(11) Uani 1 1 d . . . F144 F 0.8377(3) 0.48775(19) 0.72387(13) 0.0592(7) Uani 1 1 d . . . F145 F 0.5464(3) 0.3771(2) 0.72906(13) 0.0580(8) Uani 1 1 d . . . F146 F 0.3776(2) 0.2760(2) 0.59480(13) 0.0556(7) Uani 1 1 d . . . C21 C 0.0923(4) -0.0119(3) 0.2159(2) 0.0244(9) Uani 1 1 d . . . C22 C -0.0145(4) -0.0354(3) 0.2703(2) 0.0275(9) Uani 1 1 d . . . C23 C -0.0996(4) -0.1336(3) 0.2673(2) 0.0281(10) Uani 1 1 d . . . C24 C -0.0848(4) -0.2184(3) 0.2089(2) 0.0279(10) Uani 1 1 d . . . C25 C 0.0231(4) -0.1972(3) 0.1555(2) 0.0265(9) Uani 1 1 d . . . C26 C 0.1083(4) -0.0979(3) 0.1597(2) 0.0253(9) Uani 1 1 d . . . F22 F -0.0364(2) 0.04190(16) 0.32997(12) 0.0428(6) Uani 1 1 d . . . F23 F -0.2016(2) -0.14876(16) 0.32185(12) 0.0449(6) Uani 1 1 d . . . F25 F 0.0425(2) -0.27565(16) 0.09633(12) 0.0384(6) Uani 1 1 d . . . F26 F 0.2104(2) -0.08802(16) 0.10420(12) 0.0382(6) Uani 1 1 d . . . C241 C -0.1775(4) -0.3257(3) 0.2035(2) 0.0306(10) Uani 1 1 d . . . C242 C -0.1667(4) -0.3774(3) 0.2604(2) 0.0382(11) Uani 1 1 d . . . C243 C -0.2501(5) -0.4763(4) 0.2552(3) 0.0433(11) Uani 1 1 d . . . C244 C -0.3500(5) -0.5281(3) 0.1910(3) 0.0456(12) Uani 1 1 d . . . C245 C -0.3669(4) -0.4789(3) 0.1337(3) 0.0402(11) Uani 1 1 d . . . C246 C -0.2821(4) -0.3799(3) 0.1408(2) 0.0321(10) Uani 1 1 d . . . F242 F -0.0671(3) -0.32863(18) 0.32240(13) 0.0559(7) Uani 1 1 d . . . F243 F -0.2359(3) -0.5240(2) 0.31080(15) 0.0672(8) Uani 1 1 d . . . F244 F -0.4312(3) -0.62754(19) 0.18432(15) 0.0618(7) Uani 1 1 d . . . F245 F -0.4643(3) -0.52884(19) 0.07144(15) 0.0636(8) Uani 1 1 d . . . F246 F -0.3001(2) -0.33391(17) 0.08407(13) 0.0436(6) Uani 1 1 d . . . C31 C 0.2605(4) 0.1217(3) 0.1392(2) 0.0240(9) Uani 1 1 d . . . C32 C 0.1752(4) 0.1140(3) 0.0720(2) 0.0288(10) Uani 1 1 d . . . C33 C 0.2355(4) 0.1209(3) 0.0009(2) 0.0304(10) Uani 1 1 d . . . C34 C 0.3862(4) 0.1341(3) -0.0104(2) 0.0267(9) Uani 1 1 d . . . C35 C 0.4733(4) 0.1403(3) 0.0558(2) 0.0281(10) Uani 1 1 d . . . C36 C 0.4111(4) 0.1349(3) 0.1267(2) 0.0270(10) Uani 1 1 d . . . F32 F 0.0256(2) 0.09824(17) 0.07474(11) 0.0385(6) Uani 1 1 d . . . F33 F 0.1443(2) 0.11740(17) -0.05980(11) 0.0384(6) Uani 1 1 d . . . F35 F 0.6217(2) 0.15131(18) 0.04992(12) 0.0428(6) Uani 1 1 d . . . F36 F 0.5058(2) 0.14015(17) 0.18698(11) 0.0382(6) Uani 1 1 d . . . C341 C 0.4483(4) 0.1396(3) -0.0886(2) 0.0268(9) Uani 1 1 d . . . C342 C 0.3889(4) 0.0633(3) -0.1571(2) 0.0307(10) Uani 1 1 d . . . C343 C 0.4371(5) 0.0686(3) -0.2308(2) 0.0371(11) Uani 1 1 d . . . C344 C 0.5479(5) 0.1528(3) -0.2382(2) 0.0374(11) Uani 1 1 d . . . C345 C 0.6130(4) 0.2298(3) -0.1714(2) 0.0350(10) Uani 1 1 d . . . C346 C 0.5620(4) 0.2225(3) -0.0985(2) 0.0302(10) Uani 1 1 d . . . F342 F 0.2776(2) -0.02052(17) -0.15243(12) 0.0401(6) Uani 1 1 d . . . F343 F 0.3754(2) -0.00790(18) -0.29520(12) 0.0493(7) Uani 1 1 d . . . F344 F 0.5963(2) 0.16184(17) -0.31233(13) 0.0490(7) Uani 1 1 d . . . F345 F 0.7227(2) 0.31256(18) -0.17822(13) 0.0479(6) Uani 1 1 d . . . F346 F 0.6240(2) 0.30077(16) -0.03526(12) 0.0407(6) Uani 1 1 d . . . N41 N 0.0577(3) 0.1687(2) 0.23228(16) 0.0261(8) Uani 1 1 d . . . C42 C -0.0319(5) 0.2104(3) 0.2422(2) 0.0358(11) Uani 1 1 d . . . C43 C -0.1430(5) 0.2671(4) 0.2542(3) 0.0737(17) Uani 1 1 d . . . H43A H -0.0959 0.3387 0.2795 0.111 Uiso 1 1 calc R . . H43B H -0.2178 0.2389 0.2871 0.111 Uiso 1 1 calc R . . H43C H -0.1894 0.2614 0.2039 0.111 Uiso 1 1 calc R . . C100 C 0.8688(8) 0.5560(7) 0.9285(4) 0.055(2) Uani 0.802(4) 1 d P A 1 H10A H 0.8059 0.4861 0.9066 0.066 Uiso 0.802(4) 1 calc PR A 1 H10B H 0.8590 0.5735 0.9853 0.066 Uiso 0.802(4) 1 calc PR A 1 Cl11 Cl 0.8048(2) 0.63994(17) 0.88912(12) 0.0595(6) Uani 0.802(4) 1 d P A 1 Cl12 Cl 1.05413(19) 0.55887(17) 0.91004(10) 0.0801(9) Uani 0.802(4) 1 d P A 1 C400 C 0.871(6) 0.647(4) 0.913(3) 0.13(2) Uiso 0.198(4) 1 d P A 2 H40A H 0.8505 0.6999 0.9562 0.161 Uiso 0.198(4) 1 calc PR A 2 H40B H 0.8094 0.6355 0.8651 0.161 Uiso 0.198(4) 1 calc PR A 2 Cl41 Cl 1.0816(11) 0.6614(9) 0.8962(6) 0.127(5) Uiso 0.198(4) 1 d P A 2 Cl42 Cl 0.885(4) 0.535(3) 0.937(2) 0.348(18) Uiso 0.198(4) 1 d P A 2 C200 C 0.9623(7) 0.8335(15) 0.4931(16) 0.098(3) Uani 0.865(4) 1 d PD B 1 H20A H 0.8939 0.8131 0.4468 0.117 Uiso 0.865(4) 1 calc PR B 1 H20B H 0.9322 0.8861 0.5330 0.117 Uiso 0.865(4) 1 calc PR B 1 Cl21 Cl 1.1420(3) 0.8841(2) 0.46822(18) 0.1421(13) Uani 0.865(4) 1 d PD B 1 Cl22 Cl 0.9514(2) 0.72322(15) 0.53070(9) 0.0879(8) Uani 0.865(4) 1 d PD B 1 C300 C 0.978(3) 0.821(9) 0.502(12) 0.098(3) Uani 0.135(4) 1 d PDU B 2 H30A H 0.9176 0.8302 0.5481 0.117 Uiso 0.135(4) 1 calc PR B 2 H30B H 0.9188 0.7656 0.4593 0.117 Uiso 0.135(4) 1 calc PR B 2 Cl31 Cl 1.142(2) 0.7962(15) 0.5249(10) 0.172(10) Uani 0.135(4) 1 d PDU B 2 Cl32 Cl 1.050(4) 0.939(2) 0.4733(13) 0.239(13) Uani 0.135(4) 1 d PDU . 2 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 0.028(3) 0.031(3) 0.024(3) 0.004(2) -0.006(2) 0.007(2) C11 0.021(2) 0.023(3) 0.026(2) 0.0040(19) 0.0030(17) 0.0039(18) C12 0.026(2) 0.035(3) 0.024(2) 0.011(2) -0.0061(18) 0.010(2) C13 0.030(2) 0.016(3) 0.031(2) 0.0039(19) -0.0008(18) -0.0041(19) C14 0.025(2) 0.033(3) 0.019(2) 0.0067(19) -0.0018(17) 0.0025(19) C15 0.034(3) 0.037(3) 0.032(2) 0.017(2) -0.0072(19) 0.008(2) C16 0.030(2) 0.021(3) 0.035(2) 0.005(2) -0.0053(19) 0.0026(19) F12 0.0452(14) 0.0307(15) 0.0370(14) 0.0108(11) -0.0149(11) -0.0003(11) F13 0.0530(15) 0.0305(16) 0.0354(14) 0.0048(11) -0.0133(11) -0.0022(12) F15 0.0530(15) 0.0271(16) 0.0491(15) 0.0051(12) -0.0230(11) 0.0031(12) F16 0.0584(16) 0.0403(16) 0.0459(15) 0.0152(13) -0.0235(12) 0.0028(12) C141 0.033(3) 0.031(3) 0.025(2) 0.0080(19) 0.0000(18) 0.001(2) C142 0.042(3) 0.061(3) 0.023(2) 0.016(2) 0.000(2) -0.009(2) C143 0.028(3) 0.064(4) 0.040(3) 0.017(2) -0.012(2) -0.020(2) C144 0.048(3) 0.049(3) 0.025(3) 0.005(2) -0.013(2) 0.000(2) C145 0.046(3) 0.054(3) 0.016(2) 0.012(2) 0.002(2) 0.018(2) C146 0.023(3) 0.045(3) 0.033(3) 0.012(2) 0.0025(19) 0.003(2) F142 0.0410(16) 0.120(3) 0.0362(15) 0.0286(16) -0.0025(12) -0.0218(15) F143 0.0527(18) 0.128(3) 0.0538(18) 0.0328(18) -0.0214(14) -0.0463(17) F144 0.0628(17) 0.0638(19) 0.0360(15) 0.0054(13) -0.0194(13) -0.0010(14) F145 0.0584(17) 0.092(2) 0.0282(14) 0.0127(14) 0.0044(12) 0.0317(15) F146 0.0320(15) 0.088(2) 0.0391(15) 0.0230(14) 0.0027(11) -0.0026(14) C21 0.020(2) 0.029(3) 0.022(2) 0.0043(19) -0.0057(17) 0.0061(18) C22 0.037(3) 0.019(3) 0.022(2) -0.0012(19) -0.0012(18) 0.007(2) C23 0.025(2) 0.032(3) 0.026(2) 0.012(2) 0.0049(18) 0.003(2) C24 0.028(2) 0.023(3) 0.030(2) 0.006(2) -0.0043(18) 0.0037(19) C25 0.029(2) 0.024(3) 0.024(2) -0.0003(19) -0.0020(18) 0.009(2) C26 0.019(2) 0.032(3) 0.022(2) 0.0063(19) 0.0018(17) 0.0038(19) F22 0.0539(16) 0.0299(15) 0.0335(13) -0.0020(11) 0.0128(11) 0.0036(12) F23 0.0534(16) 0.0346(16) 0.0384(14) 0.0079(12) 0.0183(12) 0.0010(12) F25 0.0447(15) 0.0296(15) 0.0341(13) -0.0016(11) 0.0055(10) 0.0087(11) F26 0.0389(14) 0.0347(15) 0.0382(14) 0.0067(11) 0.0116(11) 0.0086(11) C241 0.034(3) 0.028(3) 0.029(2) 0.006(2) 0.0058(19) 0.009(2) C242 0.042(3) 0.033(3) 0.032(3) 0.004(2) -0.004(2) 0.002(2) C243 0.066(3) 0.030(3) 0.041(3) 0.018(2) 0.012(2) 0.017(3) C244 0.041(3) 0.027(3) 0.063(3) 0.010(3) 0.020(2) 0.003(2) C245 0.031(3) 0.031(3) 0.047(3) -0.003(2) -0.001(2) 0.000(2) C246 0.030(2) 0.033(3) 0.034(3) 0.010(2) 0.0056(19) 0.007(2) F242 0.0804(19) 0.0495(18) 0.0368(15) 0.0108(13) -0.0138(13) 0.0159(14) F243 0.103(2) 0.0517(19) 0.0620(18) 0.0371(15) 0.0154(15) 0.0248(16) F244 0.0675(18) 0.0280(17) 0.081(2) 0.0157(14) 0.0200(14) -0.0020(14) F245 0.0502(17) 0.0488(18) 0.0690(19) -0.0020(15) -0.0136(14) -0.0086(13) F246 0.0464(15) 0.0414(16) 0.0407(14) 0.0127(12) -0.0096(11) 0.0058(12) C31 0.025(2) 0.016(2) 0.028(2) 0.0050(18) -0.0053(18) 0.0020(17) C32 0.020(2) 0.029(3) 0.032(2) 0.0048(19) -0.0037(19) 0.0018(18) C33 0.026(3) 0.033(3) 0.028(2) 0.0045(19) -0.0103(19) 0.0046(19) C34 0.029(3) 0.025(3) 0.023(2) 0.0050(18) -0.0005(18) 0.0040(19) C35 0.017(2) 0.036(3) 0.031(2) 0.010(2) -0.0025(18) 0.0055(19) C36 0.031(3) 0.029(3) 0.020(2) 0.0065(18) -0.0070(18) 0.0071(19) F32 0.0201(14) 0.0598(17) 0.0301(13) 0.0089(12) -0.0052(10) 0.0044(11) F33 0.0324(13) 0.0527(17) 0.0303(13) 0.0140(12) -0.0100(10) 0.0085(11) F35 0.0234(14) 0.0699(18) 0.0367(14) 0.0169(12) -0.0002(10) 0.0125(12) F36 0.0277(13) 0.0597(17) 0.0278(13) 0.0140(12) -0.0056(10) 0.0103(11) C341 0.028(2) 0.026(3) 0.028(2) 0.011(2) -0.0022(18) 0.007(2) C342 0.031(3) 0.027(3) 0.034(3) 0.009(2) -0.0012(19) 0.006(2) C343 0.047(3) 0.033(3) 0.026(2) 0.001(2) -0.004(2) 0.009(2) C344 0.045(3) 0.042(3) 0.030(3) 0.014(2) 0.007(2) 0.016(2) C345 0.033(3) 0.031(3) 0.040(3) 0.014(2) 0.004(2) 0.003(2) C346 0.036(3) 0.024(3) 0.025(2) 0.0006(19) -0.0026(19) 0.006(2) F342 0.0425(14) 0.0328(15) 0.0349(13) 0.0019(11) -0.0022(10) 0.0000(12) F343 0.0631(17) 0.0480(17) 0.0281(13) -0.0011(12) -0.0032(11) 0.0112(13) F344 0.0642(17) 0.0419(17) 0.0475(15) 0.0175(13) 0.0140(13) 0.0206(13) F345 0.0466(16) 0.0461(17) 0.0518(16) 0.0261(13) 0.0054(12) 0.0017(13) F346 0.0385(14) 0.0374(16) 0.0368(14) 0.0063(12) -0.0034(11) -0.0019(11) N41 0.027(2) 0.021(2) 0.0234(18) 0.0004(15) -0.0064(15) 0.0000(16) C42 0.030(3) 0.029(3) 0.040(3) -0.007(2) -0.011(2) 0.009(2) C43 0.047(3) 0.056(4) 0.102(4) -0.024(3) -0.020(3) 0.028(3) C100 0.044(4) 0.063(6) 0.041(4) -0.008(3) -0.004(3) 0.009(3) Cl11 0.0611(13) 0.0705(13) 0.0662(12) 0.0327(9) 0.0129(10) 0.0365(10) Cl12 0.0679(13) 0.131(2) 0.0717(12) 0.0425(12) 0.0266(9) 0.0631(12) C200 0.080(5) 0.143(8) 0.049(8) 0.009(4) -0.004(5) 0.012(5) Cl21 0.0903(18) 0.145(3) 0.143(2) 0.017(2) 0.0413(16) -0.0259(16) Cl22 0.0928(16) 0.1110(18) 0.0585(11) 0.0167(10) 0.0128(9) 0.0313(12) C300 0.080(5) 0.143(8) 0.049(8) 0.009(4) -0.004(5) 0.012(5) Cl31 0.157(16) 0.182(18) 0.164(16) -0.059(12) -0.015(11) 0.126(15) Cl32 0.41(4) 0.216(19) 0.109(15) 0.096(16) 0.030(19) 0.066(18) _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 N41 1.600(5) . ? B1 C11 1.621(5) . ? B1 C21 1.627(6) . ? B1 C31 1.632(5) . ? C11 C16 1.380(5) . ? C11 C12 1.387(5) . ? C12 F12 1.366(4) . ? C12 C13 1.369(5) . ? C13 F13 1.353(4) . ? C13 C14 1.378(5) . ? C14 C15 1.378(5) . ? C14 C141 1.489(5) . ? C15 F16 1.348(4) . ? C15 C16 1.373(5) . ? C16 F15 1.354(4) . ? C141 C142 1.364(5) . ? C141 C146 1.374(5) . ? C142 F142 1.345(4) . ? C142 C143 1.381(5) . ? C143 F143 1.339(4) . ? C143 C144 1.355(5) . ? C144 C145 1.367(5) . ? C144 F144 1.370(4) . ? C145 F145 1.336(4) . ? C145 C146 1.376(5) . ? C146 F146 1.341(4) . ? C21 C26 1.381(5) . ? C21 C22 1.396(5) . ? C22 F22 1.349(4) . ? C22 C23 1.366(5) . ? C23 F23 1.349(4) . ? C23 C24 1.384(5) . ? C24 C25 1.384(5) . ? C24 C241 1.485(5) . ? C25 F25 1.347(4) . ? C25 C26 1.376(5) . ? C26 F26 1.352(4) . ? C241 C242 1.387(5) . ? C241 C246 1.387(5) . ? C242 F242 1.343(4) . ? C242 C243 1.362(5) . ? C243 F243 1.335(4) . ? C243 C244 1.376(6) . ? C244 F244 1.358(4) . ? C244 C245 1.383(6) . ? C245 F245 1.336(4) . ? C245 C246 1.362(5) . ? C246 F246 1.344(4) . ? C31 C36 1.382(5) . ? C31 C32 1.392(5) . ? C32 F32 1.348(4) . ? C32 C33 1.372(5) . ? C33 F33 1.350(4) . ? C33 C34 1.378(5) . ? C34 C35 1.392(5) . ? C34 C341 1.488(5) . ? C35 F35 1.350(4) . ? C35 C36 1.372(5) . ? C36 F36 1.358(4) . ? C341 C346 1.381(5) . ? C341 C342 1.385(5) . ? C342 F342 1.350(4) . ? C342 C343 1.372(5) . ? C343 F343 1.342(4) . ? C343 C344 1.365(5) . ? C344 C345 1.381(5) . ? C344 F344 1.390(4) . ? C345 F345 1.342(4) . ? C345 C346 1.371(5) . ? C346 F346 1.342(4) . ? N41 C42 1.124(4) . ? C42 C43 1.441(5) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C100 Cl11 1.727(10) . ? C100 Cl12 1.737(8) . ? C100 H10A 0.9700 . ? C100 H10B 0.9700 . ? C400 Cl42 1.75(6) . ? C400 Cl41 1.93(5) . ? C400 H40A 0.9700 . ? C400 H40B 0.9700 . ? Cl41 Cl42 2.41(4) . ? C200 Cl21 1.722(9) . ? C200 Cl22 1.793(9) . ? C200 H20A 0.9700 . ? C200 H20B 0.9700 . ? C300 Cl31 1.72(2) . ? C300 Cl32 1.80(3) . ? C300 H30A 0.9700 . ? C300 H30B 0.9700 . ? Cl32 Cl32 2.16(6) 2_776 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N41 B1 C11 103.6(3) . . ? N41 B1 C21 104.8(3) . . ? C11 B1 C21 115.1(3) . . ? N41 B1 C31 105.8(3) . . ? C11 B1 C31 114.0(3) . . ? C21 B1 C31 112.2(3) . . ? C16 C11 C12 112.7(3) . . ? C16 C11 B1 125.7(4) . . ? C12 C11 B1 121.6(3) . . ? F12 C12 C13 116.6(4) . . ? F12 C12 C11 119.0(3) . . ? C13 C12 C11 124.4(4) . . ? F13 C13 C12 119.2(3) . . ? F13 C13 C14 119.4(3) . . ? C12 C13 C14 121.4(4) . . ? C13 C14 C15 115.8(3) . . ? C13 C14 C141 122.2(4) . . ? C15 C14 C141 122.0(4) . . ? F16 C15 C16 119.5(4) . . ? F16 C15 C14 118.9(3) . . ? C16 C15 C14 121.6(4) . . ? F15 C16 C15 116.1(4) . . ? F15 C16 C11 119.7(3) . . ? C15 C16 C11 124.2(4) . . ? C142 C141 C146 116.8(4) . . ? C142 C141 C14 121.1(3) . . ? C146 C141 C14 122.0(3) . . ? F142 C142 C141 119.7(3) . . ? F142 C142 C143 118.4(4) . . ? C141 C142 C143 121.9(4) . . ? F143 C143 C144 119.4(4) . . ? F143 C143 C142 121.0(4) . . ? C144 C143 C142 119.6(4) . . ? C143 C144 C145 120.3(4) . . ? C143 C144 F144 119.8(4) . . ? C145 C144 F144 119.9(4) . . ? F145 C145 C144 120.9(4) . . ? F145 C145 C146 120.2(4) . . ? C144 C145 C146 118.9(4) . . ? F146 C146 C141 119.5(3) . . ? F146 C146 C145 118.1(4) . . ? C141 C146 C145 122.4(4) . . ? C26 C21 C22 113.7(3) . . ? C26 C21 B1 125.8(3) . . ? C22 C21 B1 120.5(3) . . ? F22 C22 C23 117.0(3) . . ? F22 C22 C21 119.3(3) . . ? C23 C22 C21 123.7(4) . . ? F23 C23 C22 119.5(3) . . ? F23 C23 C24 118.9(3) . . ? C22 C23 C24 121.6(3) . . ? C25 C24 C23 115.7(4) . . ? C25 C24 C241 121.6(4) . . ? C23 C24 C241 122.7(3) . . ? F25 C25 C26 118.9(3) . . ? F25 C25 C24 119.2(4) . . ? C26 C25 C24 121.9(4) . . ? F26 C26 C25 115.9(3) . . ? F26 C26 C21 120.7(3) . . ? C25 C26 C21 123.3(4) . . ? C242 C241 C246 116.0(4) . . ? C242 C241 C24 122.6(4) . . ? C246 C241 C24 121.4(4) . . ? F242 C242 C243 118.7(4) . . ? F242 C242 C241 118.5(4) . . ? C243 C242 C241 122.8(4) . . ? F243 C243 C242 121.2(4) . . ? F243 C243 C244 119.5(4) . . ? C242 C243 C244 119.3(4) . . ? F244 C244 C243 119.8(4) . . ? F244 C244 C245 120.4(4) . . ? C243 C244 C245 119.9(4) . . ? F245 C245 C246 120.6(4) . . ? F245 C245 C244 120.1(4) . . ? C246 C245 C244 119.3(4) . . ? F246 C246 C245 118.1(4) . . ? F246 C246 C241 119.2(4) . . ? C245 C246 C241 122.7(4) . . ? C36 C31 C32 113.4(3) . . ? C36 C31 B1 124.8(3) . . ? C32 C31 B1 121.7(3) . . ? F32 C32 C33 116.8(3) . . ? F32 C32 C31 120.0(3) . . ? C33 C32 C31 123.2(3) . . ? F33 C33 C32 118.6(3) . . ? F33 C33 C34 118.8(3) . . ? C32 C33 C34 122.5(3) . . ? C33 C34 C35 115.2(3) . . ? C33 C34 C341 121.4(3) . . ? C35 C34 C341 123.3(3) . . ? F35 C35 C36 119.3(3) . . ? F35 C35 C34 119.4(3) . . ? C36 C35 C34 121.3(3) . . ? F36 C36 C35 116.4(3) . . ? F36 C36 C31 119.2(3) . . ? C35 C36 C31 124.3(3) . . ? C346 C341 C342 115.8(3) . . ? C346 C341 C34 122.9(3) . . ? C342 C341 C34 121.3(4) . . ? F342 C342 C343 117.5(3) . . ? F342 C342 C341 119.5(3) . . ? C343 C342 C341 123.0(4) . . ? F343 C343 C344 120.2(4) . . ? F343 C343 C342 120.4(4) . . ? C344 C343 C342 119.4(4) . . ? C343 C344 C345 119.7(4) . . ? C343 C344 F344 120.7(4) . . ? C345 C344 F344 119.5(4) . . ? F345 C345 C346 120.4(4) . . ? F345 C345 C344 120.0(4) . . ? C346 C345 C344 119.5(4) . . ? F346 C346 C345 117.9(4) . . ? F346 C346 C341 119.5(3) . . ? C345 C346 C341 122.6(4) . . ? C42 N41 B1 177.5(4) . . ? N41 C42 C43 177.9(5) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Cl11 C100 Cl12 113.6(5) . . ? Cl11 C100 H10A 108.8 . . ? Cl12 C100 H10A 108.8 . . ? Cl11 C100 H10B 108.8 . . ? Cl12 C100 H10B 108.8 . . ? H10A C100 H10B 107.7 . . ? Cl42 C400 Cl41 81(3) . . ? Cl42 C400 H40A 115.1 . . ? Cl41 C400 H40A 115.1 . . ? Cl42 C400 H40B 115.1 . . ? Cl41 C400 H40B 115.1 . . ? H40A C400 H40B 112.1 . . ? C400 Cl41 Cl42 46.1(18) . . ? C400 Cl42 Cl41 53(2) . . ? Cl21 C200 Cl22 110.7(5) . . ? Cl21 C200 H20A 109.5 . . ? Cl22 C200 H20A 109.5 . . ? Cl21 C200 H20B 109.5 . . ? Cl22 C200 H20B 109.5 . . ? H20A C200 H20B 108.1 . . ? Cl31 C300 Cl32 100.5(17) . . ? Cl31 C300 H30A 111.7 . . ? Cl32 C300 H30A 111.7 . . ? Cl31 C300 H30B 111.7 . . ? Cl32 C300 H30B 111.7 . . ? H30A C300 H30B 109.4 . . ? C300 Cl32 Cl32 115(5) . 2_776 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N41 B1 C11 C16 128.4(4) . . . . ? C21 B1 C11 C16 14.6(5) . . . . ? C31 B1 C11 C16 -117.1(4) . . . . ? N41 B1 C11 C12 -48.7(4) . . . . ? C21 B1 C11 C12 -162.5(3) . . . . ? C31 B1 C11 C12 65.8(5) . . . . ? C16 C11 C12 F12 -179.6(3) . . . . ? B1 C11 C12 F12 -2.1(5) . . . . ? C16 C11 C12 C13 -0.5(5) . . . . ? B1 C11 C12 C13 177.0(4) . . . . ? F12 C12 C13 F13 -0.2(5) . . . . ? C11 C12 C13 F13 -179.3(3) . . . . ? F12 C12 C13 C14 179.1(3) . . . . ? C11 C12 C13 C14 0.0(6) . . . . ? F13 C13 C14 C15 179.6(3) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? F13 C13 C14 C141 1.1(5) . . . . ? C12 C13 C14 C141 -178.2(3) . . . . ? C13 C14 C15 F16 179.7(3) . . . . ? C141 C14 C15 F16 -1.8(5) . . . . ? C13 C14 C15 C16 0.0(5) . . . . ? C141 C14 C15 C16 178.5(4) . . . . ? F16 C15 C16 F15 -1.5(5) . . . . ? C14 C15 C16 F15 178.3(3) . . . . ? F16 C15 C16 C11 179.7(3) . . . . ? C14 C15 C16 C11 -0.6(6) . . . . ? C12 C11 C16 F15 -178.0(3) . . . . ? B1 C11 C16 F15 4.6(6) . . . . ? C12 C11 C16 C15 0.8(5) . . . . ? B1 C11 C16 C15 -176.6(4) . . . . ? C13 C14 C141 C142 -65.4(5) . . . . ? C15 C14 C141 C142 116.1(5) . . . . ? C13 C14 C141 C146 114.3(4) . . . . ? C15 C14 C141 C146 -64.1(6) . . . . ? C146 C141 C142 F142 -179.0(4) . . . . ? C14 C141 C142 F142 0.7(7) . . . . ? C146 C141 C142 C143 0.9(7) . . . . ? C14 C141 C142 C143 -179.3(4) . . . . ? F142 C142 C143 F143 -0.5(7) . . . . ? C141 C142 C143 F143 179.5(4) . . . . ? F142 C142 C143 C144 -179.2(4) . . . . ? C141 C142 C143 C144 0.8(8) . . . . ? F143 C143 C144 C145 179.6(4) . . . . ? C142 C143 C144 C145 -1.7(7) . . . . ? F143 C143 C144 F144 0.0(7) . . . . ? C142 C143 C144 F144 178.7(4) . . . . ? C143 C144 C145 F145 -177.3(4) . . . . ? F144 C144 C145 F145 2.3(6) . . . . ? C143 C144 C145 C146 0.9(7) . . . . ? F144 C144 C145 C146 -179.6(4) . . . . ? C142 C141 C146 F146 179.0(4) . . . . ? C14 C141 C146 F146 -0.8(6) . . . . ? C142 C141 C146 C145 -1.8(6) . . . . ? C14 C141 C146 C145 178.4(4) . . . . ? F145 C145 C146 F146 -1.6(6) . . . . ? C144 C145 C146 F146 -179.8(4) . . . . ? F145 C145 C146 C141 179.1(4) . . . . ? C144 C145 C146 C141 1.0(7) . . . . ? N41 B1 C21 C26 132.0(3) . . . . ? C11 B1 C21 C26 -114.9(4) . . . . ? C31 B1 C21 C26 17.6(5) . . . . ? N41 B1 C21 C22 -47.3(4) . . . . ? C11 B1 C21 C22 65.8(4) . . . . ? C31 B1 C21 C22 -161.7(3) . . . . ? C26 C21 C22 F22 177.5(3) . . . . ? B1 C21 C22 F22 -3.1(5) . . . . ? C26 C21 C22 C23 -2.1(5) . . . . ? B1 C21 C22 C23 177.3(3) . . . . ? F22 C22 C23 F23 1.2(5) . . . . ? C21 C22 C23 F23 -179.1(3) . . . . ? F22 C22 C23 C24 -179.3(3) . . . . ? C21 C22 C23 C24 0.3(6) . . . . ? F23 C23 C24 C25 -179.3(3) . . . . ? C22 C23 C24 C25 1.2(5) . . . . ? F23 C23 C24 C241 0.5(5) . . . . ? C22 C23 C24 C241 -179.0(4) . . . . ? C23 C24 C25 F25 -179.0(3) . . . . ? C241 C24 C25 F25 1.2(5) . . . . ? C23 C24 C25 C26 -0.9(5) . . . . ? C241 C24 C25 C26 179.3(3) . . . . ? F25 C25 C26 F26 -2.4(5) . . . . ? C24 C25 C26 F26 179.6(3) . . . . ? F25 C25 C26 C21 177.1(3) . . . . ? C24 C25 C26 C21 -1.0(6) . . . . ? C22 C21 C26 F26 -178.2(3) . . . . ? B1 C21 C26 F26 2.5(5) . . . . ? C22 C21 C26 C25 2.4(5) . . . . ? B1 C21 C26 C25 -176.9(3) . . . . ? C25 C24 C241 C242 113.3(4) . . . . ? C23 C24 C241 C242 -66.4(5) . . . . ? C25 C24 C241 C246 -67.4(5) . . . . ? C23 C24 C241 C246 112.8(4) . . . . ? C246 C241 C242 F242 179.9(3) . . . . ? C24 C241 C242 F242 -0.8(6) . . . . ? C246 C241 C242 C243 1.6(6) . . . . ? C24 C241 C242 C243 -179.1(4) . . . . ? F242 C242 C243 F243 1.1(6) . . . . ? C241 C242 C243 F243 179.4(4) . . . . ? F242 C242 C243 C244 -178.4(4) . . . . ? C241 C242 C243 C244 -0.1(6) . . . . ? F243 C243 C244 F244 -1.0(6) . . . . ? C242 C243 C244 F244 178.5(4) . . . . ? F243 C243 C244 C245 179.1(4) . . . . ? C242 C243 C244 C245 -1.4(6) . . . . ? F244 C244 C245 F245 0.4(6) . . . . ? C243 C244 C245 F245 -179.7(4) . . . . ? F244 C244 C245 C246 -178.7(3) . . . . ? C243 C244 C245 C246 1.2(6) . . . . ? F245 C245 C246 F246 0.6(6) . . . . ? C244 C245 C246 F246 179.7(3) . . . . ? F245 C245 C246 C241 -178.7(3) . . . . ? C244 C245 C246 C241 0.4(6) . . . . ? C242 C241 C246 F246 179.0(3) . . . . ? C24 C241 C246 F246 -0.3(5) . . . . ? C242 C241 C246 C245 -1.7(6) . . . . ? C24 C241 C246 C245 179.0(4) . . . . ? N41 B1 C31 C36 142.8(3) . . . . ? C11 B1 C31 C36 29.6(5) . . . . ? C21 B1 C31 C36 -103.5(4) . . . . ? N41 B1 C31 C32 -41.7(5) . . . . ? C11 B1 C31 C32 -154.9(3) . . . . ? C21 B1 C31 C32 72.1(5) . . . . ? C36 C31 C32 F32 178.3(3) . . . . ? B1 C31 C32 F32 2.3(5) . . . . ? C36 C31 C32 C33 -1.2(5) . . . . ? B1 C31 C32 C33 -177.2(4) . . . . ? F32 C32 C33 F33 3.6(5) . . . . ? C31 C32 C33 F33 -176.9(3) . . . . ? F32 C32 C33 C34 -178.2(3) . . . . ? C31 C32 C33 C34 1.3(6) . . . . ? F33 C33 C34 C35 178.0(3) . . . . ? C32 C33 C34 C35 -0.2(6) . . . . ? F33 C33 C34 C341 -2.9(5) . . . . ? C32 C33 C34 C341 179.0(4) . . . . ? C33 C34 C35 F35 178.8(3) . . . . ? C341 C34 C35 F35 -0.4(6) . . . . ? C33 C34 C35 C36 -0.8(5) . . . . ? C341 C34 C35 C36 180.0(4) . . . . ? F35 C35 C36 F36 -0.6(5) . . . . ? C34 C35 C36 F36 179.0(3) . . . . ? F35 C35 C36 C31 -178.7(3) . . . . ? C34 C35 C36 C31 0.9(6) . . . . ? C32 C31 C36 F36 -177.9(3) . . . . ? B1 C31 C36 F36 -2.0(5) . . . . ? C32 C31 C36 C35 0.1(5) . . . . ? B1 C31 C36 C35 176.0(4) . . . . ? C33 C34 C341 C346 123.5(4) . . . . ? C35 C34 C341 C346 -57.4(6) . . . . ? C33 C34 C341 C342 -52.9(5) . . . . ? C35 C34 C341 C342 126.2(4) . . . . ? C346 C341 C342 F342 179.9(3) . . . . ? C34 C341 C342 F342 -3.5(5) . . . . ? C346 C341 C342 C343 -0.6(6) . . . . ? C34 C341 C342 C343 176.0(4) . . . . ? F342 C342 C343 F343 -0.6(6) . . . . ? C341 C342 C343 F343 179.9(3) . . . . ? F342 C342 C343 C344 179.0(3) . . . . ? C341 C342 C343 C344 -0.5(6) . . . . ? F343 C343 C344 C345 -178.5(4) . . . . ? C342 C343 C344 C345 1.9(6) . . . . ? F343 C343 C344 F344 1.4(6) . . . . ? C342 C343 C344 F344 -178.2(3) . . . . ? C343 C344 C345 F345 179.6(4) . . . . ? F344 C344 C345 F345 -0.3(6) . . . . ? C343 C344 C345 C346 -2.2(6) . . . . ? F344 C344 C345 C346 177.9(3) . . . . ? F345 C345 C346 F346 0.7(6) . . . . ? C344 C345 C346 F346 -177.5(3) . . . . ? F345 C345 C346 C341 179.2(3) . . . . ? C344 C345 C346 C341 1.1(6) . . . . ? C342 C341 C346 F346 178.9(3) . . . . ? C34 C341 C346 F346 2.3(6) . . . . ? C342 C341 C346 C345 0.3(6) . . . . ? C34 C341 C346 C345 -176.2(4) . . . . ? C11 B1 N41 C42 -59(9) . . . . ? C21 B1 N41 C42 62(9) . . . . ? C31 B1 N41 C42 -180(100) . . . . ? B1 N41 C42 C43 135(11) . . . . ? Cl31 C300 Cl32 Cl32 -132(6) . . . 2_776 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.451 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.052 #===END data_em28 _database_code_depnum_ccdc_archive 'CCDC 704299' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic ; 4-Nonafluorobiphenylzinc chloride ether ; _chemical_formula_structural '[{(C6F4C6F5)ClZnO(CH2CH3)2}2]' _chemical_name_common '4-Nonafluorobiphenylzinc chloride ether' _chemical_melting_point ? _chemical_formula_moiety 'C32 H20 Cl2 F18 O2 Zn2' _chemical_formula_sum 'C32 H20 Cl2 F18 O2 Zn2' _chemical_formula_weight 980.12 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' F F 0.0171 0.0103 '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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 7.9926(12) _cell_length_b 10.3081(15) _cell_length_c 11.1367(13) _cell_angle_alpha 78.391(11) _cell_angle_beta 88.745(11) _cell_angle_gamma 76.934(13) _cell_volume 875.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 484 _exptl_absorpt_coefficient_mu 1.651 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.11 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11781 _diffrn_reflns_av_R_equivalents 0.0516 _diffrn_reflns_av_sigmaI/netI 0.0751 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 27.49 _reflns_number_total 3976 _reflns_number_gt 2532 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.28c4 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0869P)^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 3976 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0927 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1449 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.946 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.41763(7) 0.60126(5) 0.59096(5) 0.03135(19) Uani 1 1 d . . . Cl1 Cl 0.40943(14) 0.62329(10) 0.37715(9) 0.0247(2) Uani 1 1 d . . . C11 C 0.4887(6) 0.7373(4) 0.6697(4) 0.0282(10) Uani 1 1 d . A . C12 C 0.4255(6) 0.8756(5) 0.6353(4) 0.0297(10) Uani 1 1 d . . . C13 C 0.4847(6) 0.9698(4) 0.6831(4) 0.0279(10) Uani 1 1 d . A . C14 C 0.6182(5) 0.9305(4) 0.7686(4) 0.0279(10) Uani 1 1 d . . . C15 C 0.6821(6) 0.7933(5) 0.8069(4) 0.0300(10) Uani 1 1 d . A . C16 C 0.6177(6) 0.7002(4) 0.7586(4) 0.0298(10) Uani 1 1 d . . . F12 F 0.2984(3) 0.9235(3) 0.5476(3) 0.0392(7) Uani 1 1 d . A . F13 F 0.4173(3) 1.1029(3) 0.6421(3) 0.0376(7) Uani 1 1 d . . . F16 F 0.6881(4) 0.5665(3) 0.8024(3) 0.0428(7) Uani 1 1 d . A . F15 F 0.8100(4) 0.7473(3) 0.8916(3) 0.0399(7) Uani 1 1 d . . . C141 C 0.6927(5) 1.0301(4) 0.8181(4) 0.0270(10) Uani 1 1 d . A . C142 C 0.6009(5) 1.1203(5) 0.8828(4) 0.0281(10) Uani 1 1 d . . . C143 C 0.6714(6) 1.2108(5) 0.9287(4) 0.0300(10) Uani 1 1 d . A . C144 C 0.8420(6) 1.2107(5) 0.9096(5) 0.0343(11) Uani 1 1 d . . . C145 C 0.9389(6) 1.1214(5) 0.8449(5) 0.0385(12) Uani 1 1 d . A . C146 C 0.8653(6) 1.0326(5) 0.8002(5) 0.0338(11) Uani 1 1 d . . . F142 F 0.4337(3) 1.1227(3) 0.9038(3) 0.0379(7) Uani 1 1 d . A . F143 F 0.5779(4) 1.2980(3) 0.9921(3) 0.0462(7) Uani 1 1 d . . . F144 F 0.9124(4) 1.2997(3) 0.9509(3) 0.0503(8) Uani 1 1 d . A . F145 F 1.1053(4) 1.1220(4) 0.8251(4) 0.0613(10) Uani 1 1 d . . . F146 F 0.9627(4) 0.9478(3) 0.7369(3) 0.0518(8) Uani 1 1 d . A . O2a O 0.1787(4) 0.5649(4) 0.6309(3) 0.0403(8) Uani 0.347(12) 1 d P A 1 C21A C 0.2221(9) 0.4901(7) 0.8514(6) 0.0643(18) Uani 0.347(12) 1 d P A 1 H21A H 0.1699 0.4212 0.8976 0.096 Uiso 0.347(12) 1 calc PR A 1 H21B H 0.2490 0.5456 0.9046 0.096 Uiso 0.347(12) 1 calc PR A 1 H21C H 0.3257 0.4479 0.8160 0.096 Uiso 0.347(12) 1 calc PR A 1 C22A C 0.115(3) 0.566(4) 0.764(2) 0.100(10) Uani 0.347(12) 1 d P A 1 H22A H 0.0912 0.6591 0.7758 0.120 Uiso 0.347(12) 1 calc PR A 1 H22B H 0.0082 0.5364 0.7719 0.120 Uiso 0.347(12) 1 calc PR A 1 C23A C 0.032(2) 0.6052(18) 0.5469(19) 0.058(6) Uani 0.347(12) 1 d P A 1 H23A H 0.0577 0.5582 0.4792 0.070 Uiso 0.347(12) 1 calc PR A 1 H23B H -0.0654 0.5773 0.5889 0.070 Uiso 0.347(12) 1 calc PR A 1 C24A C -0.0132(12) 0.7488(9) 0.4992(8) 0.105(3) Uani 0.347(12) 1 d P A 1 H24A H -0.1150 0.7706 0.4483 0.157 Uiso 0.347(12) 1 calc PR A 1 H24B H 0.0793 0.7759 0.4516 0.157 Uiso 0.347(12) 1 calc PR A 1 H24C H -0.0341 0.7962 0.5659 0.157 Uiso 0.347(12) 1 calc PR A 1 O2b O 0.1787(4) 0.5649(4) 0.6309(3) 0.0403(8) Uani 0.653(12) 1 d P A 2 C21B C 0.2221(9) 0.4901(7) 0.8514(6) 0.0643(18) Uani 0.653(12) 1 d P A 2 H21D H 0.1497 0.4607 0.9162 0.096 Uiso 0.653(12) 1 calc PR A 2 H21E H 0.2097 0.5867 0.8399 0.096 Uiso 0.653(12) 1 calc PR A 2 H21F H 0.3397 0.4451 0.8725 0.096 Uiso 0.653(12) 1 calc PR A 2 C22B C 0.1715(11) 0.4557(8) 0.7360(8) 0.040(2) Uani 0.653(12) 1 d P A 2 H22C H 0.2481 0.3722 0.7236 0.048 Uiso 0.653(12) 1 calc PR A 2 H22D H 0.0558 0.4410 0.7427 0.048 Uiso 0.653(12) 1 calc PR A 2 C23B C 0.0396(12) 0.6729(10) 0.6146(9) 0.054(3) Uani 0.653(12) 1 d P A 2 H23C H 0.0618 0.7354 0.6635 0.065 Uiso 0.653(12) 1 calc PR A 2 H23D H -0.0577 0.6387 0.6503 0.065 Uiso 0.653(12) 1 calc PR A 2 C24B C -0.0132(12) 0.7488(9) 0.4992(8) 0.105(3) Uani 0.653(12) 1 d P A 2 H24D H -0.1101 0.8211 0.5063 0.157 Uiso 0.653(12) 1 calc PR A 2 H24E H -0.0451 0.6916 0.4498 0.157 Uiso 0.653(12) 1 calc PR A 2 H24F H 0.0791 0.7865 0.4616 0.157 Uiso 0.653(12) 1 calc PR A 2 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 Zn1 0.0336(3) 0.0290(3) 0.0345(3) -0.0083(2) -0.0002(2) -0.0114(2) Cl1 0.0369(6) 0.0159(5) 0.0193(5) -0.0025(4) -0.0018(4) -0.0025(4) C11 0.027(2) 0.029(2) 0.032(3) -0.0081(19) 0.0039(19) -0.0103(19) C12 0.025(2) 0.031(3) 0.033(3) -0.005(2) -0.0049(19) -0.007(2) C13 0.026(2) 0.021(2) 0.036(3) -0.0034(18) -0.0027(19) -0.0049(18) C14 0.024(2) 0.028(2) 0.034(3) -0.0087(19) 0.0042(19) -0.0096(19) C15 0.026(2) 0.034(3) 0.029(2) -0.002(2) -0.0061(18) -0.009(2) C16 0.029(2) 0.025(2) 0.033(3) -0.0021(19) 0.0028(19) -0.0051(19) F12 0.0390(16) 0.0349(15) 0.0439(17) -0.0069(13) -0.0166(13) -0.0080(12) F13 0.0382(15) 0.0256(14) 0.0489(17) -0.0056(12) -0.0129(12) -0.0070(12) F16 0.0492(18) 0.0270(15) 0.0499(18) -0.0035(13) -0.0120(14) -0.0064(13) F15 0.0355(15) 0.0393(16) 0.0432(17) -0.0035(13) -0.0162(12) -0.0075(13) C141 0.021(2) 0.030(2) 0.032(2) -0.0046(19) -0.0018(18) -0.0110(18) C142 0.020(2) 0.034(2) 0.033(2) -0.002(2) -0.0028(18) -0.0145(19) C143 0.031(2) 0.031(2) 0.030(2) -0.0084(19) -0.0011(19) -0.009(2) C144 0.032(3) 0.039(3) 0.039(3) -0.010(2) -0.006(2) -0.019(2) C145 0.023(2) 0.043(3) 0.053(3) -0.008(2) -0.004(2) -0.017(2) C146 0.026(2) 0.035(3) 0.045(3) -0.015(2) 0.004(2) -0.010(2) F142 0.0240(13) 0.0470(17) 0.0482(18) -0.0148(14) 0.0060(12) -0.0151(12) F143 0.0470(17) 0.0524(18) 0.0505(19) -0.0277(15) 0.0093(14) -0.0197(15) F144 0.0450(17) 0.0556(19) 0.063(2) -0.0232(16) -0.0085(15) -0.0272(15) F145 0.0254(15) 0.073(2) 0.099(3) -0.033(2) 0.0074(16) -0.0246(16) F146 0.0307(15) 0.058(2) 0.079(2) -0.0341(17) 0.0188(15) -0.0185(14) O2A 0.0349(19) 0.044(2) 0.043(2) -0.0073(16) 0.0013(15) -0.0116(16) C21A 0.071(4) 0.075(5) 0.045(4) -0.004(3) 0.001(3) -0.019(4) C22A 0.064(15) 0.15(3) 0.074(17) -0.020(17) 0.023(12) -0.011(17) C23A 0.050(10) 0.052(11) 0.082(14) -0.037(10) -0.012(9) -0.011(9) C24A 0.110(7) 0.097(7) 0.084(6) -0.020(5) -0.035(5) 0.030(6) O2B 0.0349(19) 0.044(2) 0.043(2) -0.0073(16) 0.0013(15) -0.0116(16) C21B 0.071(4) 0.075(5) 0.045(4) -0.004(3) 0.001(3) -0.019(4) C22B 0.041(5) 0.034(5) 0.046(5) -0.003(4) 0.012(4) -0.019(4) C23B 0.041(5) 0.048(6) 0.065(7) -0.013(5) -0.004(4) 0.007(4) C24B 0.110(7) 0.097(7) 0.084(6) -0.020(5) -0.035(5) 0.030(6) _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 Zn1 C11 1.984(4) . ? Zn1 O2A 2.050(3) . ? Zn1 Cl1 2.3470(12) . ? Zn1 Cl1 2.3746(12) 2_666 ? Cl1 Zn1 2.3746(12) 2_666 ? C11 C12 1.377(6) . ? C11 C16 1.379(6) . ? C12 F12 1.361(5) . ? C12 C13 1.370(6) . ? C13 F13 1.344(5) . ? C13 C14 1.380(6) . ? C14 C15 1.373(6) . ? C14 C141 1.494(6) . ? C15 F15 1.342(5) . ? C15 C16 1.385(6) . ? C16 F16 1.358(5) . ? C141 C142 1.364(6) . ? C141 C146 1.395(6) . ? C142 F142 1.347(5) . ? C142 C143 1.375(6) . ? C143 F143 1.339(5) . ? C143 C144 1.376(6) . ? C144 F144 1.336(5) . ? C144 C145 1.374(7) . ? C145 F145 1.345(5) . ? C145 C146 1.368(7) . ? C146 F146 1.335(5) . ? O2A C23A 1.446(17) . ? O2A C22A 1.56(2) . ? C21A C22A 1.31(3) . ? C21A H21A 0.9600 . ? C21A H21B 0.9600 . ? C21A H21C 0.9600 . ? C22A H22A 0.9700 . ? C22A H22B 0.9700 . ? C23A C24A 1.434(19) . ? C23A H23A 0.9700 . ? C23A H23B 0.9700 . ? C24A H24A 0.9600 . ? C24A H24B 0.9600 . ? C24A H24C 0.9600 . ? C22B H22C 0.9700 . ? C22B H22D 0.9700 . ? C23B H23C 0.9700 . ? C23B H23D 0.9700 . ? 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 C11 Zn1 O2A 116.97(16) . . ? C11 Zn1 Cl1 121.92(13) . . ? O2A Zn1 Cl1 99.73(10) . . ? C11 Zn1 Cl1 119.03(13) . 2_666 ? O2A Zn1 Cl1 101.46(10) . 2_666 ? Cl1 Zn1 Cl1 93.13(4) . 2_666 ? Zn1 Cl1 Zn1 86.87(4) . 2_666 ? C12 C11 C16 114.1(4) . . ? C12 C11 Zn1 124.0(3) . . ? C16 C11 Zn1 121.7(3) . . ? F12 C12 C13 117.2(4) . . ? F12 C12 C11 119.0(4) . . ? C13 C12 C11 123.9(4) . . ? F13 C13 C12 119.6(4) . . ? F13 C13 C14 119.3(4) . . ? C12 C13 C14 121.0(4) . . ? C15 C14 C13 116.7(4) . . ? C15 C14 C141 120.5(4) . . ? C13 C14 C141 122.7(4) . . ? F15 C15 C14 120.1(4) . . ? F15 C15 C16 118.9(4) . . ? C14 C15 C16 121.0(4) . . ? F16 C16 C11 119.9(4) . . ? F16 C16 C15 116.8(4) . . ? C11 C16 C15 123.3(4) . . ? C142 C141 C146 116.7(4) . . ? C142 C141 C14 123.4(4) . . ? C146 C141 C14 119.9(4) . . ? F142 C142 C141 119.6(4) . . ? F142 C142 C143 117.5(4) . . ? C141 C142 C143 122.9(4) . . ? F143 C143 C142 121.4(4) . . ? F143 C143 C144 119.5(4) . . ? C142 C143 C144 119.1(4) . . ? F144 C144 C145 119.9(4) . . ? F144 C144 C143 120.2(4) . . ? C145 C144 C143 119.9(4) . . ? F145 C145 C146 120.2(5) . . ? F145 C145 C144 120.0(4) . . ? C146 C145 C144 119.8(4) . . ? F146 C146 C145 118.3(4) . . ? F146 C146 C141 119.9(4) . . ? C145 C146 C141 121.7(4) . . ? C23A O2A C22A 109.3(12) . . ? C23A O2A Zn1 125.4(9) . . ? C22A O2A Zn1 117.7(11) . . ? C22A C21A H21A 109.5 . . ? C22A C21A H21B 109.5 . . ? H21A C21A H21B 109.5 . . ? C22A C21A H21C 109.5 . . ? H21A C21A H21C 109.5 . . ? H21B C21A H21C 109.5 . . ? C21A C22A O2A 115.6(17) . . ? C21A C22A H22A 108.4 . . ? O2A C22A H22A 108.4 . . ? C21A C22A H22B 108.4 . . ? O2A C22A H22B 108.4 . . ? H22A C22A H22B 107.5 . . ? C24A C23A O2A 112.9(12) . . ? C24A C23A H23A 109.0 . . ? O2A C23A H23A 109.0 . . ? C24A C23A H23B 109.0 . . ? O2A C23A H23B 109.0 . . ? H23A C23A H23B 107.8 . . ? C23A C24A H24A 109.5 . . ? C23A C24A H24B 109.5 . . ? H24A C24A H24B 109.5 . . ? C23A C24A H24C 109.5 . . ? H24A C24A H24C 109.5 . . ? H24B C24A H24C 109.5 . . ? H22C C22B H22D 108.0 . . ? H23C C23B H23D 106.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Zn1 Cl1 Zn1 127.35(15) . . . 2_666 ? O2A Zn1 Cl1 Zn1 -102.20(10) . . . 2_666 ? Cl1 Zn1 Cl1 Zn1 0.0 2_666 . . 2_666 ? O2A Zn1 C11 C12 -74.1(4) . . . . ? Cl1 Zn1 C11 C12 48.6(4) . . . . ? Cl1 Zn1 C11 C12 163.4(3) 2_666 . . . ? O2A Zn1 C11 C16 111.1(4) . . . . ? Cl1 Zn1 C11 C16 -126.1(3) . . . . ? Cl1 Zn1 C11 C16 -11.4(4) 2_666 . . . ? C16 C11 C12 F12 179.6(4) . . . . ? Zn1 C11 C12 F12 4.5(6) . . . . ? C16 C11 C12 C13 0.6(7) . . . . ? Zn1 C11 C12 C13 -174.5(4) . . . . ? F12 C12 C13 F13 -0.3(6) . . . . ? C11 C12 C13 F13 178.8(4) . . . . ? F12 C12 C13 C14 -177.3(4) . . . . ? C11 C12 C13 C14 1.8(7) . . . . ? F13 C13 C14 C15 -179.9(4) . . . . ? C12 C13 C14 C15 -2.9(7) . . . . ? F13 C13 C14 C141 -0.3(7) . . . . ? C12 C13 C14 C141 176.7(4) . . . . ? C13 C14 C15 F15 -178.9(4) . . . . ? C141 C14 C15 F15 1.5(7) . . . . ? C13 C14 C15 C16 1.7(7) . . . . ? C141 C14 C15 C16 -177.9(4) . . . . ? C12 C11 C16 F16 178.5(4) . . . . ? Zn1 C11 C16 F16 -6.3(6) . . . . ? C12 C11 C16 C15 -1.7(7) . . . . ? Zn1 C11 C16 C15 173.5(4) . . . . ? F15 C15 C16 F16 1.0(6) . . . . ? C14 C15 C16 F16 -179.6(4) . . . . ? F15 C15 C16 C11 -178.8(4) . . . . ? C14 C15 C16 C11 0.6(7) . . . . ? C15 C14 C141 C142 -118.5(5) . . . . ? C13 C14 C141 C142 61.9(6) . . . . ? C15 C14 C141 C146 60.7(6) . . . . ? C13 C14 C141 C146 -118.9(5) . . . . ? C146 C141 C142 F142 -179.7(4) . . . . ? C14 C141 C142 F142 -0.5(7) . . . . ? C146 C141 C142 C143 0.3(7) . . . . ? C14 C141 C142 C143 179.5(4) . . . . ? F142 C142 C143 F143 0.1(7) . . . . ? C141 C142 C143 F143 -179.9(4) . . . . ? F142 C142 C143 C144 179.6(4) . . . . ? C141 C142 C143 C144 -0.4(7) . . . . ? F143 C143 C144 F144 -2.0(7) . . . . ? C142 C143 C144 F144 178.5(4) . . . . ? F143 C143 C144 C145 179.9(5) . . . . ? C142 C143 C144 C145 0.4(7) . . . . ? F144 C144 C145 F145 1.2(8) . . . . ? C143 C144 C145 F145 179.4(5) . . . . ? F144 C144 C145 C146 -178.5(5) . . . . ? C143 C144 C145 C146 -0.3(8) . . . . ? F145 C145 C146 F146 -0.2(8) . . . . ? C144 C145 C146 F146 179.5(5) . . . . ? F145 C145 C146 C141 -179.4(5) . . . . ? C144 C145 C146 C141 0.2(8) . . . . ? C142 C141 C146 F146 -179.5(4) . . . . ? C14 C141 C146 F146 1.3(7) . . . . ? C142 C141 C146 C145 -0.2(7) . . . . ? C14 C141 C146 C145 -179.5(5) . . . . ? C11 Zn1 O2A C23A 109.4(9) . . . . ? Cl1 Zn1 O2A C23A -24.2(9) . . . . ? Cl1 Zn1 O2A C23A -119.4(9) 2_666 . . . ? C11 Zn1 O2A C22A -36.9(14) . . . . ? Cl1 Zn1 O2A C22A -170.4(14) . . . . ? Cl1 Zn1 O2A C22A 94.3(14) 2_666 . . . ? C23A O2A C22A C21A 158(2) . . . . ? Zn1 O2A C22A C21A -51(3) . . . . ? C22A O2A C23A C24A 91(2) . . . . ? Zn1 O2A C23A C24A -57.6(17) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.267 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.123 #===END data_em27 _database_code_depnum_ccdc_archive 'CCDC 704300' _audit_creation_method 'SHELXL-97 and CrysAlis RED' _chemical_name_systematic 'Bis(4-nonafluorobiphenyl)bis(diethylether) zinc' _chemical_formula_structural '[(C6F5C6F4)2 Zn {(CH3CH2)2O]2}]' _chemical_name_common 'Bis(4-nonafluorobiphenyl)bis(diethylether) zinc' _chemical_melting_point ? _chemical_formula_moiety 'C32 H20 F18 O2 Zn' _chemical_formula_sum 'C32 H20 F18 O2 Zn' _chemical_formula_weight 843.85 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' O O 0.0106 0.0060 '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' Zn Zn 0.2839 1.4301 '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 19.078(4) _cell_length_b 8.1176(8) _cell_length_c 20.494(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.363(14) _cell_angle_gamma 90.00 _cell_volume 3172.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 140(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.59 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 0.912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.13 _exptl_absorpt_process_details 'SADABS V2.10 (Sheldrick, G.M., 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur 3/CCD' _diffrn_measurement_method 'Thin slice \f and \w scans' _diffrn_detector_area_resol_mean 16.0050 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8721 _diffrn_reflns_av_R_equivalents 0.1035 _diffrn_reflns_av_sigmaI/netI 0.0799 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 4.02 _diffrn_reflns_theta_max 20.00 _reflns_number_total 1460 _reflns_number_gt 997 _reflns_threshold_expression I>2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.27p20 beta ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997a)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997b)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997b)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0177P)^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 1460 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0889 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.0584 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Zn1 Zn 0.5000 0.42812(12) 0.2500 0.0285(3) Uani 1 2 d S . . C11 C 0.4514(3) 0.3120(7) 0.3230(3) 0.0222(15) Uani 1 1 d . . . C12 C 0.3949(3) 0.2218(7) 0.3133(3) 0.0231(15) Uani 1 1 d . . . C13 C 0.3625(3) 0.1286(6) 0.3612(3) 0.0294(16) Uani 1 1 d . . . C14 C 0.3896(3) 0.1223(6) 0.4232(3) 0.0249(15) Uani 1 1 d . . . C15 C 0.4485(3) 0.2126(7) 0.4342(3) 0.0301(16) Uani 1 1 d . . . C16 C 0.4790(3) 0.3018(7) 0.3849(3) 0.0320(16) Uani 1 1 d . . . F12 F 0.36328(17) 0.2149(3) 0.25318(16) 0.0448(9) Uani 1 1 d . . . F13 F 0.30371(17) 0.0417(4) 0.34659(14) 0.0431(9) Uani 1 1 d . . . F15 F 0.47903(17) 0.2096(4) 0.49438(15) 0.0469(10) Uani 1 1 d . . . F16 F 0.53979(18) 0.3800(4) 0.40145(14) 0.0489(10) Uani 1 1 d . . . C141 C 0.3578(3) 0.0225(7) 0.4750(3) 0.0253(16) Uani 1 1 d . . . C142 C 0.3255(3) 0.0909(7) 0.5269(3) 0.0290(15) Uani 1 1 d . . . C143 C 0.2972(3) 0.0003(8) 0.5761(3) 0.0314(17) Uani 1 1 d . . . C144 C 0.3018(3) -0.1681(9) 0.5734(3) 0.0316(16) Uani 1 1 d . . . C145 C 0.3328(3) -0.2434(7) 0.5225(3) 0.0281(16) Uani 1 1 d . . . C146 C 0.3603(3) -0.1478(8) 0.4735(3) 0.0295(16) Uani 1 1 d . . . F142 F 0.32093(16) 0.2562(4) 0.53156(14) 0.0421(9) Uani 1 1 d . . . F143 F 0.26474(16) 0.0724(4) 0.62568(15) 0.0511(9) Uani 1 1 d . . . F144 F 0.27439(17) -0.2598(4) 0.62081(15) 0.0494(10) Uani 1 1 d . . . F145 F 0.33648(15) -0.4079(4) 0.51925(14) 0.0456(9) Uani 1 1 d . . . F146 F 0.39029(17) -0.2239(3) 0.42370(15) 0.0424(9) Uani 1 1 d . . . O2 O 0.5621(2) 0.6159(4) 0.28974(16) 0.0303(10) Uani 1 1 d . . . C21 C 0.6722(3) 0.6545(7) 0.2375(3) 0.059(2) Uani 1 1 d . . . H21A H 0.7219 0.6389 0.2425 0.089 Uiso 1 1 calc R . . H21B H 0.6623 0.7695 0.2313 0.089 Uiso 1 1 calc R . . H21C H 0.6551 0.5938 0.2002 0.089 Uiso 1 1 calc R . . C22 C 0.6372(3) 0.5950(7) 0.2966(3) 0.0392(16) Uani 1 1 d . . . H22A H 0.6481 0.4795 0.3034 0.047 Uiso 1 1 calc R . . H22B H 0.6545 0.6561 0.3343 0.047 Uiso 1 1 calc R . . C23 C 0.5336(3) 0.7187(7) 0.3398(3) 0.0482(19) Uani 1 1 d . . . H23A H 0.5517 0.6817 0.3820 0.058 Uiso 1 1 calc R . . H23B H 0.4830 0.7053 0.3395 0.058 Uiso 1 1 calc R . . C24 C 0.5501(3) 0.8963(6) 0.3322(3) 0.067(2) Uani 1 1 d . . . H24A H 0.5296 0.9576 0.3670 0.100 Uiso 1 1 calc R . . H24B H 0.5314 0.9349 0.2911 0.100 Uiso 1 1 calc R . . H24C H 0.6000 0.9113 0.3336 0.100 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 Zn1 0.0325(8) 0.0282(6) 0.0250(6) 0.000 0.0042(5) 0.000 C11 0.017(4) 0.025(4) 0.025(5) -0.004(3) -0.002(3) -0.002(3) C12 0.036(5) 0.024(4) 0.009(4) 0.003(3) -0.010(4) 0.002(3) C13 0.032(5) 0.025(4) 0.031(5) -0.005(3) -0.006(4) -0.007(3) C14 0.031(5) 0.023(4) 0.021(4) 0.001(3) 0.000(4) -0.005(3) C15 0.031(5) 0.036(4) 0.023(5) 0.000(3) -0.008(4) -0.008(4) C16 0.021(5) 0.033(4) 0.042(5) 0.001(4) 0.003(4) -0.016(3) F12 0.055(3) 0.045(2) 0.034(2) 0.0060(17) -0.002(2) -0.0182(18) F13 0.046(3) 0.048(2) 0.035(2) 0.0103(17) -0.0075(18) -0.020(2) F15 0.048(3) 0.062(2) 0.030(2) 0.0092(17) -0.010(2) -0.022(2) F16 0.038(2) 0.070(3) 0.039(2) 0.0187(17) -0.0078(18) -0.022(2) C141 0.032(5) 0.024(5) 0.020(4) -0.007(4) 0.000(3) -0.001(3) C142 0.042(5) 0.014(4) 0.031(4) 0.003(4) -0.005(4) -0.004(4) C143 0.040(5) 0.031(5) 0.023(5) 0.000(4) 0.004(4) -0.002(3) C144 0.024(5) 0.046(5) 0.025(5) 0.013(4) -0.002(4) -0.014(4) C145 0.024(5) 0.026(5) 0.033(5) 0.007(4) -0.009(4) -0.009(4) C146 0.032(5) 0.034(5) 0.024(5) -0.008(4) 0.010(4) 0.000(4) F142 0.054(3) 0.026(2) 0.046(2) -0.0009(17) 0.0122(19) -0.0053(17) F143 0.061(3) 0.057(2) 0.036(2) -0.006(2) 0.019(2) -0.011(2) F144 0.059(3) 0.052(2) 0.037(2) 0.0153(18) 0.006(2) -0.0235(19) F145 0.054(2) 0.025(2) 0.057(2) 0.0101(19) -0.0114(18) -0.0042(19) F146 0.047(3) 0.039(2) 0.041(2) -0.0047(18) 0.005(2) 0.0045(18) O2 0.028(3) 0.033(3) 0.030(2) -0.0073(18) 0.003(2) 0.003(2) C21 0.043(5) 0.086(5) 0.048(5) 0.004(4) 0.008(4) -0.012(4) C22 0.042(5) 0.034(4) 0.041(4) -0.008(3) -0.004(4) -0.001(4) C23 0.042(5) 0.054(5) 0.050(5) -0.025(4) 0.013(4) 0.001(4) C24 0.092(6) 0.031(5) 0.075(5) -0.016(4) -0.035(4) 0.010(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 C11 2.013(6) . ? Zn1 C11 2.013(6) 2_655 ? Zn1 O2 2.084(3) . ? Zn1 O2 2.084(3) 2_655 ? C11 C12 1.315(7) . ? C11 C16 1.364(7) . ? C12 F12 1.361(5) . ? C12 C13 1.394(7) . ? C13 F13 1.352(6) . ? C13 C14 1.362(7) . ? C14 C15 1.356(7) . ? C14 C141 1.478(7) . ? C15 F15 1.352(6) . ? C15 C16 1.382(7) . ? C16 F16 1.359(6) . ? C141 C142 1.359(7) . ? C141 C146 1.384(6) . ? C142 F142 1.348(6) . ? C142 C143 1.370(7) . ? C143 F143 1.337(6) . ? C143 C144 1.371(6) . ? C144 F144 1.339(6) . ? C144 C145 1.358(7) . ? C145 F145 1.339(6) . ? C145 C146 1.382(7) . ? C146 F146 1.333(6) . ? O2 C23 1.440(6) . ? O2 C22 1.447(6) . ? C21 C22 1.478(7) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.485(7) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Zn1 C11 124.2(3) . 2_655 ? C11 Zn1 O2 108.6(2) . . ? C11 Zn1 O2 111.43(19) 2_655 . ? C11 Zn1 O2 111.43(19) . 2_655 ? C11 Zn1 O2 108.6(2) 2_655 2_655 ? O2 Zn1 O2 85.98(19) . 2_655 ? C12 C11 C16 113.7(5) . . ? C12 C11 Zn1 122.7(5) . . ? C16 C11 Zn1 123.0(5) . . ? C11 C12 F12 120.2(5) . . ? C11 C12 C13 124.9(5) . . ? F12 C12 C13 114.9(6) . . ? F13 C13 C14 118.8(6) . . ? F13 C13 C12 120.5(6) . . ? C14 C13 C12 120.8(6) . . ? C15 C14 C13 115.5(5) . . ? C15 C14 C141 122.0(6) . . ? C13 C14 C141 122.5(6) . . ? F15 C15 C14 118.6(6) . . ? F15 C15 C16 119.8(6) . . ? C14 C15 C16 121.5(6) . . ? F16 C16 C11 120.8(6) . . ? F16 C16 C15 115.7(6) . . ? C11 C16 C15 123.5(6) . . ? C142 C141 C146 116.3(6) . . ? C142 C141 C14 122.7(5) . . ? C146 C141 C14 121.1(6) . . ? F142 C142 C141 119.6(5) . . ? F142 C142 C143 117.0(6) . . ? C141 C142 C143 123.4(6) . . ? F143 C143 C142 121.5(6) . . ? F143 C143 C144 119.8(6) . . ? C142 C143 C144 118.7(6) . . ? F144 C144 C145 119.5(6) . . ? F144 C144 C143 119.9(6) . . ? C145 C144 C143 120.6(6) . . ? F145 C145 C144 120.8(6) . . ? F145 C145 C146 120.2(6) . . ? C144 C145 C146 119.1(6) . . ? F146 C146 C145 118.3(6) . . ? F146 C146 C141 119.7(6) . . ? C145 C146 C141 122.0(6) . . ? C23 O2 C22 112.9(4) . . ? C23 O2 Zn1 118.8(3) . . ? C22 O2 Zn1 120.3(3) . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O2 C22 C21 110.4(5) . . ? O2 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? O2 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? O2 C23 C24 113.7(5) . . ? O2 C23 H23A 108.8 . . ? C24 C23 H23A 108.8 . . ? O2 C23 H23B 108.8 . . ? C24 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Zn1 C11 C12 -65.9(5) 2_655 . . . ? O2 Zn1 C11 C12 160.1(4) . . . . ? O2 Zn1 C11 C12 67.1(5) 2_655 . . . ? C11 Zn1 C11 C16 105.2(5) 2_655 . . . ? O2 Zn1 C11 C16 -28.8(5) . . . . ? O2 Zn1 C11 C16 -121.8(4) 2_655 . . . ? C16 C11 C12 F12 -177.4(5) . . . . ? Zn1 C11 C12 F12 -5.6(7) . . . . ? C16 C11 C12 C13 2.8(9) . . . . ? Zn1 C11 C12 C13 174.6(4) . . . . ? C11 C12 C13 F13 179.0(5) . . . . ? F12 C12 C13 F13 -0.8(7) . . . . ? C11 C12 C13 C14 -1.5(9) . . . . ? F12 C12 C13 C14 178.7(4) . . . . ? F13 C13 C14 C15 -179.9(5) . . . . ? C12 C13 C14 C15 0.5(8) . . . . ? F13 C13 C14 C141 0.7(8) . . . . ? C12 C13 C14 C141 -178.8(5) . . . . ? C13 C14 C15 F15 -178.8(5) . . . . ? C141 C14 C15 F15 0.5(8) . . . . ? C13 C14 C15 C16 -1.2(8) . . . . ? C141 C14 C15 C16 178.2(5) . . . . ? C12 C11 C16 F16 176.0(5) . . . . ? Zn1 C11 C16 F16 4.2(7) . . . . ? C12 C11 C16 C15 -3.4(8) . . . . ? Zn1 C11 C16 C15 -175.2(4) . . . . ? F15 C15 C16 F16 0.9(8) . . . . ? C14 C15 C16 F16 -176.7(5) . . . . ? F15 C15 C16 C11 -179.6(5) . . . . ? C14 C15 C16 C11 2.8(9) . . . . ? C15 C14 C141 C142 69.7(8) . . . . ? C13 C14 C141 C142 -111.0(7) . . . . ? C15 C14 C141 C146 -109.4(7) . . . . ? C13 C14 C141 C146 69.8(8) . . . . ? C146 C141 C142 F142 -179.8(5) . . . . ? C14 C141 C142 F142 1.0(8) . . . . ? C146 C141 C142 C143 0.8(9) . . . . ? C14 C141 C142 C143 -178.4(6) . . . . ? F142 C142 C143 F143 1.8(8) . . . . ? C141 C142 C143 F143 -178.8(5) . . . . ? F142 C142 C143 C144 -179.0(5) . . . . ? C141 C142 C143 C144 0.3(9) . . . . ? F143 C143 C144 F144 -0.7(9) . . . . ? C142 C143 C144 F144 -179.8(5) . . . . ? F143 C143 C144 C145 178.2(5) . . . . ? C142 C143 C144 C145 -1.0(10) . . . . ? F144 C144 C145 F145 -0.2(8) . . . . ? C143 C144 C145 F145 -179.0(5) . . . . ? F144 C144 C145 C146 179.3(5) . . . . ? C143 C144 C145 C146 0.5(9) . . . . ? F145 C145 C146 F146 -0.2(8) . . . . ? C144 C145 C146 F146 -179.7(5) . . . . ? F145 C145 C146 C141 -179.8(5) . . . . ? C144 C145 C146 C141 0.7(9) . . . . ? C142 C141 C146 F146 179.1(5) . . . . ? C14 C141 C146 F146 -1.7(9) . . . . ? C142 C141 C146 C145 -1.3(9) . . . . ? C14 C141 C146 C145 177.9(5) . . . . ? C11 Zn1 O2 C23 -43.6(4) . . . . ? C11 Zn1 O2 C23 176.1(4) 2_655 . . . ? O2 Zn1 O2 C23 67.7(4) 2_655 . . . ? C11 Zn1 O2 C22 103.1(4) . . . . ? C11 Zn1 O2 C22 -37.2(4) 2_655 . . . ? O2 Zn1 O2 C22 -145.7(4) 2_655 . . . ? C23 O2 C22 C21 -121.0(5) . . . . ? Zn1 O2 C22 C21 90.5(5) . . . . ? C22 O2 C23 C24 73.1(6) . . . . ? Zn1 O2 C23 C24 -137.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.333 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.055 #===END