data_global _journal_name_full Org.Biomol.Chem. _journal_coden_Cambridge 0177 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Andreas Kirschning' _publ_contact_author_email ANDREAS.KIRSCHNING@OCI.UNI-HANNOVER.DE _publ_section_title ; Synthetic and structural studies on macrocyclic amino cyclitols - conformational chameleons ; loop_ _publ_author_name 'Andreas Kirschning' 'Dieter Albert' 'Benjamin Oelze' # Attachment 'andreas.cif' data_wart_oelze1i _database_code_depnum_ccdc_archive 'CCDC 673913' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Acetic acid 1R,8S,9R,11R,13R,20R-9-acetoxy-11,22-bis-(2,2,2-trifluoro-acetylamino)- 2,7,14,19-tetraoxa-tricyclo[18.3.1.08,13]tetracos-24-yl ester ; _chemical_name_common ; Acetic acid 1R,8S,9R,11R,13R,20R-9-acetoxy-11,22-bis-(2,2,2- trifluoro-acetylamino)-2,7,14,19-tetraoxa- tricyclo(18.3.1.08,13)tetracos-24-yl ester ; _chemical_melting_point ' 478 - 481 K ' _chemical_formula_moiety ? _chemical_formula_sum 'C28 H40 F6 N2 O10' _chemical_formula_weight 678.62 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' N N 0.0061 0.0033 '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 monoclinic _symmetry_space_group_name_H-M 'P 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.949(2) _cell_length_b 9.313(1) _cell_length_c 15.289(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.84(2) _cell_angle_gamma 90.00 _cell_volume 1665.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 300(2) _cell_measurement_reflns_used 4197 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 20.8 _exptl_crystal_description 'elongated || [010]' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.123 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; IPDS measurement on 6.7.2004. Short descriptions of the IPDS are given in (e.g.) : Schuett W et al., J. Organomet. Chem. 443 (1993) C33-C36 and Sheldrick G M et al., Acta Crystallogr. B51 (1995) 89-98. Completeness of unique data set in Laue class 2/m 100 %, but Friedel pairs kept separate in the refinement, because the substance is a pure enantiomer for chemical reasons. 24171 measured reflections including unobserved and forbidden ones. Only 19 % of the measured reflections are observed(I>2\s(I)). R~int~ of the observed reflections is 0.033 using program LAUE of L. J. Farrugia. Possible hydrogen bonds : N29-H1...O28#, O28# is derived from O28 by the symmetry operation 1-X,1/2+Y,-Z , N36-H2...O2 . ; _diffrn_ambient_temperature 300(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS area detector diffractometer' _diffrn_measurement_method '240 exposures, \D \f 1.5 \%' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 24154 _diffrn_reflns_av_R_equivalents 0.1031 _diffrn_reflns_av_sigmaI/netI 0.2538 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.42 _diffrn_reflns_theta_max 26.22 _reflns_number_total 6594 _reflns_number_gt 1826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Stoe IPDS software' _computing_cell_refinement 'Stoe IPDS software' _computing_data_reduction 'Stoe IPDS software SHELXL-97' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 1990)' _computing_publication_material ? _refine_special_details ; Last refinement cycle on 27.02.2008 at 17:39. Because of the low amount of observed reflections (19 %), only the atoms F, N, O were refined anisotropically. The hydrogen atoms were handled as riding atoms. The methyl groups were allowed to rotate. The hydrogen atoms at N29 and N36 were kept in reasonable distances to neighbouring atoms by distance restraints : EQIV $1 1-X,1/2+Y,-Z DFIX 1.0 0.01 N29 H1 N36 H2 DFIX 2.1 0.05 H1 O28_$1 DFIX 2.0 0.02 H2 C22 H2 C37 . 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. The weighting scheme is that recommended by SHELXL. The goodness of fit S = 0.588 is to low due to the small amount of observed reflections in the data set. Its value is 0.967 for the observed reflections using program SHELXL-93. The Flack x parameter -0.1(10) is unreliable for this light atom structure using Mo Kalpha radiation. Therefore the assumed absolute configuration could not be proven by this X-ray investigation. ; _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^)+(0.0080P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(10) _refine_ls_number_reflns 6594 _refine_ls_number_parameters 285 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1769 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0730 _refine_ls_wR_factor_gt 0.0593 _refine_ls_goodness_of_fit_ref 0.588 _refine_ls_restrained_S_all 0.588 _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 F32 F -0.0451(4) 0.7116(8) -0.1498(3) 0.257(4) Uani 1 1 d . . . F33 F -0.0037(6) 0.5939(6) -0.2435(4) 0.258(4) Uani 1 1 d . . . F34 F 0.0695(3) 0.7718(6) -0.2145(3) 0.180(2) Uani 1 1 d . . . F39 F 0.9784(3) 0.7230(5) 0.2587(2) 0.1424(18) Uani 1 1 d . . . F40 F 1.0796(4) 0.5827(5) 0.2073(2) 0.1443(17) Uani 1 1 d . . . F41 F 1.1541(4) 0.7175(5) 0.3076(3) 0.180(2) Uani 1 1 d . . . O2 O 0.7972(2) 0.7145(4) 0.42247(19) 0.0532(9) Uani 1 1 d . . . O7 O 0.5184(3) 0.7968(4) 0.13579(19) 0.0571(10) Uani 1 1 d . . . O14 O 0.4020(2) 0.4429(4) 0.15333(19) 0.0532(9) Uani 1 1 d . . . O19 O 0.6511(2) 0.2945(4) 0.37745(19) 0.0588(10) Uani 1 1 d . . . O25 O 0.6290(2) 0.6425(4) 0.01969(19) 0.0560(10) Uani 1 1 d . . . O28 O 0.7210(2) 0.4621(4) 0.1010(2) 0.0707(11) Uani 1 1 d . . . O35 O 0.0973(3) 0.4745(4) -0.0838(3) 0.0933(14) Uani 1 1 d . . . O42 O 1.1233(3) 0.4272(4) 0.3640(2) 0.0742(12) Uani 1 1 d . . . O43 O 0.5917(2) 0.5692(4) 0.43690(19) 0.0576(10) Uani 1 1 d . . . O46 O 0.5202(3) 0.4551(4) 0.5425(2) 0.0804(12) Uani 1 1 d . . . N29 N 0.2221(3) 0.6572(5) -0.0858(3) 0.0506(12) Uani 1 1 d D . . H1 H 0.209(3) 0.7632(13) -0.089(3) 0.077(18) Uiso 1 1 d D . . N36 N 0.9651(3) 0.5440(5) 0.3892(2) 0.0563(13) Uani 1 1 d D . . H2 H 0.920(3) 0.633(3) 0.380(2) 0.10(2) Uiso 1 1 d D . . C1 C 0.7880(4) 0.6249(6) 0.4988(3) 0.0533(14) Uiso 1 1 d . . . H3 H 0.7658 0.6820 0.5463 0.064 Uiso 1 1 calc R . . C3 C 0.7327(4) 0.8453(5) 0.4150(3) 0.0599(15) Uiso 1 1 d . . . H4 H 0.7600 0.9056 0.4667 0.072 Uiso 1 1 calc R . . H5 H 0.6526 0.8243 0.4123 0.072 Uiso 1 1 calc R . . C4 C 0.7467(4) 0.9203(5) 0.3329(3) 0.0530(13) Uiso 1 1 d . . . H6 H 0.8279 0.9334 0.3358 0.064 Uiso 1 1 calc R . . H7 H 0.7131 1.0150 0.3332 0.064 Uiso 1 1 calc R . . C5 C 0.6953(4) 0.8490(6) 0.2425(3) 0.0634(16) Uiso 1 1 d . . . H8 H 0.7221 0.8990 0.1951 0.076 Uiso 1 1 calc R . . H9 H 0.7212 0.7503 0.2431 0.076 Uiso 1 1 calc R . . C6 C 0.5670(4) 0.8520(6) 0.2240(3) 0.0635(16) Uiso 1 1 d . . . H10 H 0.5401 0.7947 0.2685 0.076 Uiso 1 1 calc R . . H11 H 0.5413 0.9499 0.2288 0.076 Uiso 1 1 calc R . . C8 C 0.5105(4) 0.6462(6) 0.1329(3) 0.0465(13) Uiso 1 1 d . . . H12 H 0.5718 0.6051 0.1786 0.056 Uiso 1 1 calc R . . C9 C 0.5208(3) 0.5914(5) 0.0423(2) 0.0415(12) Uiso 1 1 d . . . H13 H 0.5196 0.4862 0.0423 0.050 Uiso 1 1 calc R . . C10 C 0.4258(3) 0.6474(5) -0.0311(3) 0.0471(13) Uiso 1 1 d . . . H14 H 0.4285 0.7514 -0.0324 0.056 Uiso 1 1 calc R . . H15 H 0.4364 0.6119 -0.0885 0.056 Uiso 1 1 calc R . . C11 C 0.3129(3) 0.6003(5) -0.0157(3) 0.0437(12) Uiso 1 1 d . . . H16 H 0.3097 0.4952 -0.0179 0.052 Uiso 1 1 calc R . . C12 C 0.2968(3) 0.6501(5) 0.0770(3) 0.0486(13) Uiso 1 1 d . . . H17 H 0.2935 0.7542 0.0784 0.058 Uiso 1 1 calc R . . H18 H 0.2252 0.6129 0.0881 0.058 Uiso 1 1 calc R . . C13 C 0.3955(3) 0.5973(5) 0.1496(3) 0.0442(13) Uiso 1 1 d . . . H19 H 0.3856 0.6341 0.2076 0.053 Uiso 1 1 calc R . . C15 C 0.3186(4) 0.3738(6) 0.1933(3) 0.0593(15) Uiso 1 1 d . . . H20 H 0.2472 0.3636 0.1501 0.071 Uiso 1 1 calc R . . H21 H 0.3043 0.4298 0.2434 0.071 Uiso 1 1 calc R . . C16 C 0.3661(4) 0.2272(6) 0.2249(3) 0.0583(14) Uiso 1 1 d . . . H22 H 0.3958 0.1820 0.1772 0.070 Uiso 1 1 calc R . . H23 H 0.3042 0.1679 0.2367 0.070 Uiso 1 1 calc R . . C17 C 0.4606(3) 0.2324(6) 0.3087(3) 0.0519(13) Uiso 1 1 d . . . H24 H 0.4308 0.2776 0.3563 0.062 Uiso 1 1 calc R . . H25 H 0.4821 0.1348 0.3272 0.062 Uiso 1 1 calc R . . C18 C 0.5664(4) 0.3127(6) 0.2966(3) 0.0607(15) Uiso 1 1 d . . . H26 H 0.5942 0.2744 0.2460 0.073 Uiso 1 1 calc R . . H27 H 0.5492 0.4138 0.2859 0.073 Uiso 1 1 calc R . . C20 C 0.7314(3) 0.4099(5) 0.3967(3) 0.0394(12) Uiso 1 1 d . . . H28 H 0.7305 0.4670 0.3427 0.047 Uiso 1 1 calc R . . C21 C 0.8483(4) 0.3455(5) 0.4292(3) 0.0492(14) Uiso 1 1 d . . . H29 H 0.8698 0.2919 0.3808 0.059 Uiso 1 1 calc R . . H30 H 0.8448 0.2785 0.4772 0.059 Uiso 1 1 calc R . . C22 C 0.9406(4) 0.4584(5) 0.4631(3) 0.0523(13) Uiso 1 1 d D . . H31 H 1.0108 0.4081 0.4912 0.063 Uiso 1 1 calc R . . C23 C 0.9073(4) 0.5560(5) 0.5313(3) 0.0580(14) Uiso 1 1 d . . . H32 H 0.9640 0.6316 0.5457 0.070 Uiso 1 1 calc R . . H33 H 0.9072 0.5019 0.5855 0.070 Uiso 1 1 calc R . . C24 C 0.7036(3) 0.5035(5) 0.4695(3) 0.0458(13) Uiso 1 1 d . . . H34 H 0.6997 0.4435 0.5214 0.055 Uiso 1 1 calc R . . C26 C 0.7225(4) 0.5641(6) 0.0542(3) 0.0571(16) Uiso 1 1 d . . . C27 C 0.8239(4) 0.6204(6) 0.0197(3) 0.0790(18) Uiso 1 1 d . . . H35 H 0.8421 0.7156 0.0423 0.118 Uiso 1 1 calc R . . H36 H 0.8055 0.6230 -0.0444 0.118 Uiso 1 1 calc R . . H37 H 0.8885 0.5586 0.0392 0.118 Uiso 1 1 calc R . . C30 C 0.1248(5) 0.5875(7) -0.1099(3) 0.0588(15) Uiso 1 1 d . . . C31 C 0.0330(6) 0.6683(8) -0.1763(4) 0.078(2) Uiso 1 1 d . . . C37 C 1.0533(4) 0.5234(6) 0.3491(3) 0.0524(14) Uiso 1 1 d D . . C38 C 1.0654(5) 0.6375(8) 0.2828(4) 0.0742(17) Uiso 1 1 d . . . C44 C 0.5048(4) 0.5335(6) 0.4785(3) 0.0561(15) Uiso 1 1 d . . . C45 C 0.3990(4) 0.6070(6) 0.4366(3) 0.0644(15) Uiso 1 1 d . . . H38 H 0.4039 0.6366 0.3773 0.097 Uiso 1 1 calc R . . H39 H 0.3883 0.6897 0.4714 0.097 Uiso 1 1 calc R . . H40 H 0.3355 0.5427 0.4335 0.097 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 F32 0.146(4) 0.480(11) 0.170(4) 0.185(6) 0.091(4) 0.199(6) F33 0.339(8) 0.156(6) 0.176(5) -0.048(4) -0.186(6) 0.053(5) F34 0.094(3) 0.224(6) 0.182(4) 0.126(4) -0.069(3) -0.028(3) F39 0.127(3) 0.168(4) 0.157(3) 0.106(3) 0.085(3) 0.085(3) F40 0.216(5) 0.146(4) 0.089(3) 0.020(3) 0.074(3) 0.043(3) F41 0.149(4) 0.164(5) 0.200(5) 0.075(4) -0.031(3) -0.085(4) O2 0.0434(19) 0.045(2) 0.072(2) -0.001(2) 0.0153(17) 0.0097(17) O7 0.077(2) 0.038(2) 0.0445(19) -0.0028(17) -0.0147(17) -0.0002(19) O14 0.047(2) 0.054(3) 0.055(2) 0.0156(19) 0.0016(15) -0.0009(19) O19 0.0486(19) 0.058(3) 0.057(2) 0.0154(19) -0.0196(16) -0.0150(19) O25 0.0387(18) 0.057(3) 0.069(2) 0.0202(19) 0.0047(16) 0.0067(17) O28 0.042(2) 0.050(3) 0.113(3) 0.014(3) 0.0004(19) 0.009(2) O35 0.062(2) 0.076(3) 0.126(3) 0.028(3) -0.019(2) -0.019(2) O42 0.054(2) 0.085(3) 0.081(3) 0.009(2) 0.0073(18) 0.028(2) O43 0.0287(17) 0.076(3) 0.072(2) 0.013(2) 0.0190(15) 0.0040(18) O46 0.078(2) 0.088(3) 0.083(3) 0.005(3) 0.036(2) -0.003(2) N29 0.030(2) 0.050(3) 0.061(3) 0.000(3) -0.0145(19) -0.001(2) N36 0.037(2) 0.073(4) 0.060(3) 0.013(3) 0.013(2) 0.011(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag F32 C31 1.162(7) . ? F33 C31 1.243(7) . ? F34 C31 1.252(7) . ? F39 C38 1.301(6) . ? F40 C38 1.305(6) . ? F41 C38 1.287(6) . ? O2 C3 1.433(5) . ? O2 C1 1.458(5) . ? O7 C8 1.406(5) . ? O7 C6 1.449(5) . ? O14 C15 1.426(5) . ? O14 C13 1.441(5) . ? O19 C20 1.430(5) . ? O19 C18 1.438(5) . ? O25 C26 1.348(6) . ? O25 C9 1.483(4) . ? O28 C26 1.191(5) . ? O35 C30 1.195(6) . ? O42 C37 1.215(5) . ? O43 C44 1.366(6) . ? O43 C24 1.461(4) . ? O46 C44 1.204(5) . ? N29 C30 1.316(6) . ? N29 C11 1.458(5) . ? N36 C37 1.338(5) . ? N36 C22 1.460(5) . ? C1 C24 1.520(6) . ? C1 C23 1.550(6) . ? C3 C4 1.476(5) . ? C4 C5 1.542(5) . ? C5 C6 1.500(5) . ? C8 C9 1.506(5) . ? C8 C13 1.519(5) . ? C9 C10 1.516(5) . ? C10 C11 1.482(5) . ? C11 C12 1.541(5) . ? C12 C13 1.525(5) . ? C15 C16 1.519(6) . ? C16 C17 1.525(5) . ? C17 C18 1.513(5) . ? C20 C24 1.503(5) . ? C20 C21 1.508(5) . ? C21 C22 1.536(6) . ? C22 C23 1.497(5) . ? C26 C27 1.512(6) . ? C30 C31 1.530(7) . ? C37 C38 1.496(7) . ? C44 C45 1.464(6) . ? 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 C3 O2 C1 115.0(3) . . ? C8 O7 C6 113.2(3) . . ? C15 O14 C13 115.5(4) . . ? C20 O19 C18 114.3(3) . . ? C26 O25 C9 115.3(4) . . ? C44 O43 C24 118.0(4) . . ? C30 N29 C11 120.5(5) . . ? C37 N36 C22 125.3(4) . . ? O2 C1 C24 110.1(4) . . ? O2 C1 C23 106.1(4) . . ? C24 C1 C23 107.4(4) . . ? O2 C3 C4 108.5(4) . . ? C3 C4 C5 117.7(4) . . ? C6 C5 C4 111.4(4) . . ? O7 C6 C5 111.6(4) . . ? O7 C8 C9 110.5(4) . . ? O7 C8 C13 110.6(4) . . ? C9 C8 C13 107.5(4) . . ? O25 C9 C8 110.2(3) . . ? O25 C9 C10 105.9(3) . . ? C8 C9 C10 112.0(4) . . ? C11 C10 C9 110.4(4) . . ? N29 C11 C10 109.9(4) . . ? N29 C11 C12 110.6(4) . . ? C10 C11 C12 110.2(3) . . ? C13 C12 C11 110.4(4) . . ? O14 C13 C8 105.2(4) . . ? O14 C13 C12 112.2(3) . . ? C8 C13 C12 111.9(4) . . ? O14 C15 C16 107.1(4) . . ? C15 C16 C17 113.8(4) . . ? C18 C17 C16 114.0(4) . . ? O19 C18 C17 107.2(4) . . ? O19 C20 C24 110.3(4) . . ? O19 C20 C21 107.8(4) . . ? C24 C20 C21 108.5(3) . . ? C20 C21 C22 113.0(4) . . ? N36 C22 C23 109.4(4) . . ? N36 C22 C21 110.9(4) . . ? C23 C22 C21 112.0(4) . . ? C22 C23 C1 112.7(4) . . ? O43 C24 C20 108.4(3) . . ? O43 C24 C1 107.1(4) . . ? C20 C24 C1 114.6(4) . . ? O28 C26 O25 123.6(5) . . ? O28 C26 C27 126.8(5) . . ? O25 C26 C27 109.5(5) . . ? O35 C30 N29 128.9(6) . . ? O35 C30 C31 116.5(6) . . ? N29 C30 C31 114.5(6) . . ? F32 C31 F33 108.0(7) . . ? F32 C31 F34 106.1(7) . . ? F33 C31 F34 98.1(6) . . ? F32 C31 C30 117.2(6) . . ? F33 C31 C30 110.9(6) . . ? F34 C31 C30 114.6(6) . . ? O42 C37 N36 126.6(5) . . ? O42 C37 C38 119.6(5) . . ? N36 C37 C38 113.8(5) . . ? F41 C38 F39 106.9(7) . . ? F41 C38 F40 103.8(6) . . ? F39 C38 F40 103.4(5) . . ? F41 C38 C37 113.5(5) . . ? F39 C38 C37 116.4(5) . . ? F40 C38 C37 111.7(6) . . ? O46 C44 O43 121.4(5) . . ? O46 C44 C45 127.9(5) . . ? O43 C44 C45 110.7(5) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.22 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.272 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.039 # _eof