Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_s92 _database_code_CSD 186190 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Gale, Philip' 'Camiolo, Salvatore' 'Hursthouse, M.' 'Light, Mark E.' 'Navakhun, Korakot' _publ_contact_author_name 'Dr Philip Gale' _publ_contact_author_address ; Department of Chemistry University of Southampton Southampton SO17 1BJ UNITED KINGDOM ; _publ_contact_author_email 'PHILIP.GALE@SOTON.AC.UK' _publ_section_title ; Pendant arm pyrrolic amide cleft anion receptors ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H30 F6 N5 O4 P' _chemical_formula_weight 573.48 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' '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 16.1973(5) _cell_length_b 9.3378(2) _cell_length_c 34.0104(12) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5144.0(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.481 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2384 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type Multi-scans _exptl_absorpt_correction_T_min 0.9813 _exptl_absorpt_correction_T_max 0.9962 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 'Bruker Nonius Kappa CCD Area detector' _diffrn_measurement_method '\f and \w scans to fill the asymmetric unit' _diffrn_detector_area_resol_mean '9.091 pixels mm^1^' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18704 _diffrn_reflns_av_R_equivalents 0.1556 _diffrn_reflns_av_sigmaI/netI 0.1655 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.03 _reflns_number_total 4519 _reflns_number_gt 2080 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Hooft, 1998)' _computing_cell_refinement 'DENZO (Otwinowski and MInor, 1997)' _computing_data_reduction 'DENZO, COLLECT, MAXUS (Mackay et al., 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin, et al., 1993)' _computing_publication_material 'WINGX (Farrugia, 1998)' _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^)+(0.0803P)^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 none _refine_ls_number_reflns 4519 _refine_ls_number_parameters 382 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1738 _refine_ls_R_factor_gt 0.0653 _refine_ls_wR_factor_ref 0.1769 _refine_ls_wR_factor_gt 0.1377 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.052 _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 N1 N 0.3930(3) 0.1084(6) 1.15122(13) 0.0248(10) Uani 1 1 d . . . N2 N 0.3210(2) -0.0731(4) 1.05961(11) 0.0226(10) Uani 1 1 d . . . H2 H 0.2681 -0.0888 1.0558 0.027 Uiso 1 1 calc R . . N3 N 0.3836(2) -0.0431(4) 0.95694(10) 0.0180(9) Uani 1 1 d . . . H3 H 0.4379 -0.0414 0.9577 0.022 Uiso 1 1 calc R . . N4 N 0.3321(2) -0.0305(4) 0.85287(11) 0.0292(11) Uani 1 1 d . . . H4 H 0.2786 -0.0427 0.8559 0.035 Uiso 1 1 calc R . . N5 N 0.3316(3) 0.1231(7) 0.75166(13) 0.0348(12) Uani 1 1 d . . . O1 O 0.44618(19) -0.0482(4) 1.03207(9) 0.0312(9) Uani 1 1 d . . . O2 O 0.45620(18) -0.0346(3) 0.88352(8) 0.0278(8) Uani 1 1 d . . . C1 C 0.3479(3) 0.0896(5) 1.11355(13) 0.0275(12) Uani 1 1 d . . . H1D H 0.3721 0.1536 1.0934 0.033 Uiso 1 1 calc R . . H1E H 0.2894 0.1171 1.1172 0.033 Uiso 1 1 calc R . . C2 C 0.3525(3) -0.0651(5) 1.09927(13) 0.0260(12) Uani 1 1 d . . . H2A H 0.4105 -0.0987 1.0999 0.031 Uiso 1 1 calc R . . H2B H 0.3194 -0.1274 1.1168 0.031 Uiso 1 1 calc R . . C3 C 0.3714(3) -0.0570(5) 1.02846(13) 0.0220(11) Uani 1 1 d . . . C4 C 0.3330(3) -0.0506(5) 0.98903(13) 0.0189(11) Uani 1 1 d . . . C5 C 0.2511(3) -0.0520(4) 0.97582(13) 0.0194(11) Uani 1 1 d . . . C6 C 0.2547(3) -0.0442(4) 0.93415(13) 0.0203(11) Uani 1 1 d . . . C7 C 0.3373(2) -0.0386(5) 0.92356(12) 0.0164(11) Uani 1 1 d . . . C8 C 0.3801(3) -0.0342(5) 0.88501(13) 0.0217(11) Uani 1 1 d . . . C9 C 0.3639(3) -0.0074(6) 0.81314(13) 0.0348(14) Uani 1 1 d . . . H9A H 0.3658 -0.0993 0.7986 0.042 Uiso 1 1 calc R . . H9B H 0.4205 0.0323 0.8143 0.042 Uiso 1 1 calc R . . C10 C 0.3074(4) 0.0956(6) 0.79274(14) 0.0460(15) Uani 1 1 d . . . H10A H 0.2505 0.0567 0.7932 0.055 Uiso 1 1 calc R . . H10B H 0.3071 0.1873 0.8073 0.055 Uiso 1 1 calc R . . C11 C 0.1754(3) -0.0550(5) 1.00045(13) 0.0207(11) Uani 1 1 d . . . C12 C 0.1530(3) 0.0656(5) 1.02251(14) 0.0280(12) Uani 1 1 d . . . H12 H 0.1858 0.1498 1.0211 0.034 Uiso 1 1 calc R . . C13 C 0.0840(3) 0.0641(6) 1.04626(14) 0.0331(13) Uani 1 1 d . . . H13 H 0.0698 0.1464 1.0612 0.040 Uiso 1 1 calc R . . C14 C 0.0359(3) -0.0574(6) 1.04823(15) 0.0308(13) Uani 1 1 d . . . H14 H -0.0111 -0.0598 1.0649 0.037 Uiso 1 1 calc R . . C15 C 0.0561(3) -0.1750(6) 1.02591(14) 0.0313(13) Uani 1 1 d . . . H15 H 0.0217 -0.2573 1.0266 0.038 Uiso 1 1 calc R . . C16 C 0.1256(3) -0.1755(5) 1.00246(13) 0.0272(12) Uani 1 1 d . . . H16 H 0.1393 -0.2584 0.9877 0.033 Uiso 1 1 calc R . . C17 C 0.1822(3) -0.0374(5) 0.90692(12) 0.0189(11) Uani 1 1 d . . . C18 C 0.1340(3) -0.1566(5) 0.89921(14) 0.0252(12) Uani 1 1 d . . . H18 H 0.1447 -0.2436 0.9128 0.030 Uiso 1 1 calc R . . C19 C 0.0707(3) -0.1507(6) 0.87215(14) 0.0294(13) Uani 1 1 d . . . H19 H 0.0382 -0.2336 0.8674 0.035 Uiso 1 1 calc R . . C20 C 0.0543(3) -0.0267(6) 0.85204(15) 0.0331(13) Uani 1 1 d . . . H20 H 0.0114 -0.0241 0.8330 0.040 Uiso 1 1 calc R . . C21 C 0.1008(3) 0.0949(5) 0.85963(14) 0.0272(12) Uani 1 1 d . . . H21 H 0.0900 0.1816 0.8459 0.033 Uiso 1 1 calc R . . C22 C 0.1628(3) 0.0883(5) 0.88731(13) 0.0258(12) Uani 1 1 d . . . H22 H 0.1933 0.1726 0.8931 0.031 Uiso 1 1 calc R . . H51 H 0.447(3) 0.086(6) 1.1468(15) 0.048(17) Uiso 1 1 d . . . H52 H 0.373(3) 0.053(6) 1.1720(16) 0.049(18) Uiso 1 1 d . . . H53 H 0.384(2) 0.202(6) 1.1612(12) 0.024(14) Uiso 1 1 d . . . H55 H 0.380(4) 0.188(7) 0.7534(17) 0.016(18) Uiso 0.67 1 d P . . H56 H 0.284(4) 0.166(7) 0.7369(18) 0.025(19) Uiso 0.67 1 d P . . H57 H 0.353(5) 0.052(9) 0.741(2) 0.03(3) Uiso 0.67 1 d P . . P1 P 0.13090(8) 0.24613(15) 0.70915(4) 0.0332(4) Uani 1 1 d . . . F1 F 0.07518(15) 0.3904(3) 0.72328(8) 0.0368(8) Uani 1 1 d . . . F2 F 0.1177(2) 0.1698(3) 0.75300(8) 0.0575(9) Uani 1 1 d . . . F3 F 0.21574(16) 0.3265(3) 0.72639(10) 0.0588(10) Uani 1 1 d . . . F4 F 0.18974(16) 0.1022(3) 0.69562(8) 0.0408(8) Uani 1 1 d . . . F5 F 0.1461(2) 0.3214(3) 0.66516(8) 0.0626(10) Uani 1 1 d . . . F6 F 0.04814(17) 0.1652(3) 0.69228(9) 0.0526(9) Uani 1 1 d . . . O1W O -0.0765(3) 0.3714(5) 0.75809(14) 0.0664(13) Uani 1 1 d D . . H1W H -0.1150(14) 0.398(8) 0.7404(10) 0.10(3) Uiso 1 1 d D . . H2W H -0.0217(4) 0.371(5) 0.7539(10) 0.031 Uiso 1 1 d D . . O2W O 0.1613(2) 0.6121(4) 0.65742(12) 0.0442(10) Uani 1 1 d D . . H3W H 0.146(3) 0.554(10) 0.638(2) 0.27(7) Uiso 1 1 d D . . H4W H 0.2126(13) 0.618(6) 0.6675(15) 0.10(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 N1 0.032(3) 0.019(3) 0.023(3) -0.003(2) 0.002(2) 0.001(2) N2 0.017(2) 0.030(3) 0.021(2) -0.0021(19) 0.0014(17) -0.0036(18) N3 0.0146(19) 0.021(2) 0.018(2) -0.0008(19) 0.0015(17) 0.0007(17) N4 0.025(2) 0.043(3) 0.020(2) 0.002(2) -0.0018(19) 0.003(2) N5 0.040(3) 0.040(3) 0.025(3) 0.006(3) 0.000(2) 0.010(3) O1 0.0225(19) 0.046(2) 0.025(2) 0.0040(16) 0.0001(15) -0.0030(17) O2 0.0213(19) 0.036(2) 0.0259(19) -0.0004(16) -0.0007(15) 0.0013(16) C1 0.030(3) 0.030(3) 0.023(3) 0.000(2) -0.005(2) 0.001(2) C2 0.022(2) 0.035(3) 0.021(3) -0.003(2) 0.003(2) -0.001(2) C3 0.026(3) 0.016(3) 0.025(3) 0.003(2) -0.003(2) -0.003(2) C4 0.025(3) 0.014(3) 0.018(3) 0.001(2) 0.001(2) 0.003(2) C5 0.019(2) 0.015(3) 0.024(3) 0.000(2) 0.002(2) -0.002(2) C6 0.024(3) 0.012(3) 0.025(3) -0.003(2) 0.000(2) -0.001(2) C7 0.017(2) 0.019(3) 0.013(3) -0.002(2) -0.003(2) -0.001(2) C8 0.029(3) 0.015(3) 0.021(3) 0.004(2) -0.004(2) -0.002(2) C9 0.030(3) 0.058(4) 0.017(3) 0.003(3) 0.001(2) 0.003(3) C10 0.060(4) 0.051(4) 0.027(3) 0.006(3) 0.008(3) 0.015(3) C11 0.022(3) 0.019(3) 0.020(3) 0.005(2) -0.005(2) 0.005(2) C12 0.026(3) 0.021(3) 0.036(3) -0.001(3) 0.000(2) -0.002(2) C13 0.032(3) 0.029(3) 0.038(3) -0.010(3) 0.012(3) 0.002(3) C14 0.018(3) 0.033(4) 0.041(3) 0.009(3) 0.007(2) 0.006(3) C15 0.022(3) 0.030(3) 0.042(3) 0.007(3) 0.001(2) -0.007(2) C16 0.025(3) 0.021(3) 0.036(3) -0.002(3) -0.001(2) -0.002(2) C17 0.017(2) 0.023(3) 0.017(3) -0.003(2) -0.0010(19) -0.002(2) C18 0.027(3) 0.019(3) 0.030(3) -0.004(2) -0.001(2) 0.002(2) C19 0.025(3) 0.031(3) 0.033(3) -0.007(3) 0.001(2) -0.013(3) C20 0.031(3) 0.036(4) 0.033(3) -0.001(3) -0.007(2) 0.004(3) C21 0.027(3) 0.020(3) 0.035(3) 0.005(2) -0.008(2) 0.003(2) C22 0.027(3) 0.024(3) 0.026(3) -0.004(3) -0.001(2) 0.000(2) P1 0.0353(8) 0.0289(9) 0.0355(9) -0.0018(7) -0.0031(6) 0.0029(7) F1 0.0336(15) 0.0345(18) 0.0424(18) -0.0058(14) -0.0059(13) 0.0126(13) F2 0.099(2) 0.040(2) 0.0334(19) 0.0057(16) 0.0086(17) 0.0079(17) F3 0.0311(16) 0.040(2) 0.105(3) -0.0267(19) -0.0210(17) 0.0050(15) F4 0.0347(16) 0.0315(18) 0.056(2) -0.0103(15) 0.0040(14) 0.0043(14) F5 0.123(3) 0.0289(19) 0.036(2) -0.0009(16) 0.0239(19) -0.0020(19) F6 0.0444(18) 0.0365(19) 0.077(2) -0.0108(17) -0.0267(17) -0.0013(15) O1W 0.050(2) 0.068(3) 0.081(3) -0.013(3) 0.018(3) -0.011(3) O2W 0.037(2) 0.039(3) 0.057(3) 0.008(2) -0.011(2) -0.0013(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N1 C1 1.485(6) . ? N2 C3 1.345(5) . ? N2 C2 1.444(5) . ? N3 C7 1.361(5) . ? N3 C4 1.367(5) . ? N4 C8 1.342(5) . ? N4 C9 1.462(5) . ? N5 C10 1.474(6) . ? O1 C3 1.221(5) . ? O2 C8 1.234(5) . ? C1 C2 1.526(7) . ? C3 C4 1.479(6) . ? C4 C5 1.400(6) . ? C5 C6 1.420(6) . ? C5 C11 1.485(6) . ? C6 C7 1.387(6) . ? C6 C17 1.497(6) . ? C7 C8 1.484(6) . ? C9 C10 1.498(7) . ? C11 C16 1.386(6) . ? C11 C12 1.401(6) . ? C12 C13 1.379(6) . ? C13 C14 1.378(7) . ? C14 C15 1.375(7) . ? C15 C16 1.380(6) . ? C17 C18 1.384(6) . ? C17 C22 1.386(6) . ? C18 C19 1.378(6) . ? C19 C20 1.372(7) . ? C20 C21 1.386(7) . ? C21 C22 1.378(6) . ? P1 F6 1.642(3) . ? P1 F2 1.667(3) . ? P1 F5 1.671(3) . ? P1 F3 1.672(3) . ? P1 F1 1.691(3) . ? P1 F4 1.710(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 N2 C2 121.1(4) . . ? C7 N3 C4 109.7(3) . . ? C8 N4 C9 123.6(4) . . ? N1 C1 C2 111.2(4) . . ? N2 C2 C1 109.2(4) . . ? O1 C3 N2 122.0(4) . . ? O1 C3 C4 120.4(4) . . ? N2 C3 C4 117.6(4) . . ? N3 C4 C5 108.2(4) . . ? N3 C4 C3 118.3(4) . . ? C5 C4 C3 133.5(4) . . ? C4 C5 C6 106.3(4) . . ? C4 C5 C11 126.9(4) . . ? C6 C5 C11 126.7(4) . . ? C7 C6 C5 107.5(4) . . ? C7 C6 C17 126.5(4) . . ? C5 C6 C17 126.0(4) . . ? N3 C7 C6 108.3(4) . . ? N3 C7 C8 118.7(4) . . ? C6 C7 C8 132.9(4) . . ? O2 C8 N4 123.0(4) . . ? O2 C8 C7 120.2(4) . . ? N4 C8 C7 116.8(4) . . ? N4 C9 C10 107.9(4) . . ? N5 C10 C9 112.8(4) . . ? C16 C11 C12 118.4(4) . . ? C16 C11 C5 121.6(4) . . ? C12 C11 C5 120.1(4) . . ? C13 C12 C11 121.0(4) . . ? C14 C13 C12 119.7(5) . . ? C15 C14 C13 119.7(4) . . ? C14 C15 C16 121.0(5) . . ? C15 C16 C11 120.1(5) . . ? C18 C17 C22 117.5(4) . . ? C18 C17 C6 121.7(4) . . ? C22 C17 C6 120.7(4) . . ? C19 C18 C17 120.9(5) . . ? C20 C19 C18 120.7(5) . . ? C19 C20 C21 119.6(5) . . ? C22 C21 C20 119.1(5) . . ? C21 C22 C17 122.1(4) . . ? F6 P1 F2 90.62(18) . . ? F6 P1 F5 90.04(18) . . ? F2 P1 F5 178.9(2) . . ? F6 P1 F3 179.28(18) . . ? F2 P1 F3 89.07(18) . . ? F5 P1 F3 90.25(19) . . ? F6 P1 F1 91.73(15) . . ? F2 P1 F1 91.01(16) . . ? F5 P1 F1 89.88(16) . . ? F3 P1 F1 88.92(14) . . ? F6 P1 F4 89.96(15) . . ? F2 P1 F4 88.64(16) . . ? F5 P1 F4 90.44(16) . . ? F3 P1 F4 89.38(15) . . ? F1 P1 F4 178.28(16) . . ? 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 N5 H56 F3 1.00(7) 1.90(7) 2.806(6) 149(5) . N5 H56 F4 1.00(7) 2.16(7) 2.992(6) 139(5) . O2W H3W F5 0.9000(13) 2.37(12) 2.739(5) 105(8) . O2W H4W F4 0.9000(12) 1.855(14) 2.742(5) 168(6) 8_665 N3 H3 O1 0.88 2.09 2.911(5) 155.8 5_657 N1 H51 O2 0.91(5) 1.94(6) 2.800(6) 157(5) 5_657 N1 H52 F4 0.93(6) 1.95(6) 2.818(6) 155(5) 2 N1 H52 F6 0.93(6) 2.50(5) 3.064(6) 119(4) 2 N1 H53 O2W 0.94(5) 1.89(5) 2.762(6) 152(4) 2_565 N5 H55 O1W 0.99(7) 1.89(7) 2.775(7) 147(5) 6_657 N5 H57 F1 0.83(8) 2.00(8) 2.816(7) 168(7) 8_655 N5 H57 F3 0.83(8) 2.43(8) 2.999(7) 126(6) 8_655 _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.681 _refine_diff_density_min -0.501 _refine_diff_density_rms 0.079