# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1586 data_takahashi-kk-yk-45-i #------------------------------------------------------------------------------ _audit_creation_date 'Mon Mar 6 11:01:31 2000' _audit_creation_method 'from TEXRAY.INF file' _audit_update_record ? #------------------------------------------------------------------------------ _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan' _computing_structure_solution ? _computing_structure_refinement 'teXsan' _computing_publication_material 'teXsan' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _chemical_compound_source ? _chemical_name_common ? _chemical_formula_weight 331.43 _chemical_formula_analytical ? _chemical_formula_sum 'C20 H26 F N O2 ' _chemical_formula_moiety 'C20 H26 F N O2 ' _chemical_formula_structural ? _chemical_melting_point ? #------------------------------------------------------------------------------ _cell_length_a 8.739(9) _cell_length_b 9.404(9) _cell_length_c 6.411(8) _cell_angle_alpha 103.23(8) _cell_angle_beta 97.33(9) _cell_angle_gamma 111.00(8) _cell_volume 465(1) _cell_formula_units_Z 1 _cell_measurement_temperature 150.2 _cell_measurement_reflns_used 10 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 12.5 #------------------------------------------------------------------------------ _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1 ' _symmetry_Int_Tables_number 1 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z #------------------------------------------------------------------------------ _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'colorless' _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 178.00 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_process_details '(North, Phillips & Mathews, 1968)' _exptl_absorpt_correction_T_min 0.524 _exptl_absorpt_correction_T_max 0.993 _exptl_special_details ; ? ; #------------------------------------------------------------------------------ _diffrn_special_details ; ? ; _diffrn_ambient_temperature 150.2 _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'scintillation counter' _diffrn_measurement_device_type 'Rigaku AFC5R' _diffrn_measurement_method \w-2\q _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_decay_% -0.75 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 -1 0 -2 1 -1 2 -1 1 _diffrn_reflns_number 2278 _reflns_number_total 2143 _reflns_number_gt 1400 _reflns_observed_expression >2.0sigma(I) _diffrn_reflns_av_R_equivalents 0.015 _diffrn_reflns_av_sigmaI/netI 0.057 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 27.50 _diffrn_reflns_reduction_process 'Lp corrections applied' _diffrn_orient_matrix_UB_11 -0.11583 _diffrn_orient_matrix_UB_12 -0.00110 _diffrn_orient_matrix_UB_13 -0.02160 _diffrn_orient_matrix_UB_21 0.03716 _diffrn_orient_matrix_UB_22 0.08824 _diffrn_orient_matrix_UB_23 -0.06884 _diffrn_orient_matrix_UB_31 -0.03269 _diffrn_orient_matrix_UB_32 -0.08022 _diffrn_orient_matrix_UB_33 -0.14802 #------------------------------------------------------------------------------ loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'F' 'F' 0.017 0.010 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ 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_calc_flags _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group F(1) F 0.998(1) 0.609(1) 0.998(2) 0.0562(8) Uani 1.00 d . . . O(1) O 0.670(1) 0.491(1) 0.998(2) 0.056(1) Uani 1.00 d . . . O(2) O 0.612(1) 0.537(1) 0.670(2) 0.0365(7) Uani 1.00 d . . . N(1) N 0.983(1) 0.807(1) 0.640(2) 0.063(1) Uani 1.00 d . . . C(1) C 0.710(1) 0.528(1) 0.845(2) 0.0386(10) Uani 1.00 d . . . C(1') C 0.432(1) 0.498(1) 0.673(2) 0.0319(9) Uani 1.00 d . . . C(2) C 0.887(1) 0.560(1) 0.794(2) 0.0404(9) Uani 1.00 d . . . C(2') C 0.336(1) 0.429(1) 0.431(2) 0.0344(9) Uani 1.00 d . . . C(3) C 0.940(1) 0.700(1) 0.704(2) 0.046(1) Uani 1.00 d . . . C(3') C 0.379(1) 0.562(1) 0.316(2) 0.040(1) Uani 1.00 d . . . C(4) C 0.886(1) 0.413(1) 0.645(2) 0.0377(9) Uani 1.00 d . . . C(4') C 0.362(1) 0.710(1) 0.441(2) 0.047(1) Uani 1.00 d . . . C(5) C 0.837(1) 0.370(1) 0.418(2) 0.041(1) Uani 1.00 d . . . C(5') C 0.466(1) 0.779(1) 0.677(2) 0.043(1) Uani 1.00 d . . . C(6) C 0.820(1) 0.227(1) 0.287(2) 0.043(1) Uani 1.00 d . . . C(6') C 0.416(1) 0.649(1) 0.792(2) 0.039(1) Uani 1.00 d . . . C(7) C 0.849(1) 0.111(1) 0.378(2) 0.042(1) Uani 1.00 d . . . C(7') C 0.360(1) 0.282(1) 0.302(2) 0.041(1) Uani 1.00 d . . . C(8) C 0.904(1) 0.158(1) 0.602(2) 0.045(1) Uani 1.00 d . . . C(8') C 0.234(1) 0.201(1) 0.079(2) 0.051(1) Uani 1.00 d . . . C(9) C 0.920(1) 0.301(1) 0.737(2) 0.043(1) Uani 1.00 d . . . C(9') C 0.343(1) 0.158(1) 0.428(2) 0.056(2) Uani 1.00 d . . . C(10) C 0.827(1) -0.048(1) 0.236(2) 0.053(1) Uani 1.00 d . . . C(10') C 0.447(1) 0.929(1) 0.805(2) 0.063(2) Uani 1.00 d . . . H(1) H 0.8105 0.4388 0.3492 0.0500 Uiso 1.00 calc . . . H(2) H 0.7861 0.2026 0.1325 0.0503 Uiso 1.00 calc . . . H(3) H 0.9307 0.0849 0.6678 0.0528 Uiso 1.00 calc . . . H(4) H 0.9522 0.3228 0.8929 0.0512 Uiso 1.00 calc . . . H(5) H 0.8104 -0.0663 0.0934 0.0369 Uiso 1.00 calc . . . H(6) H 0.7336 -0.1212 0.2708 0.1574 Uiso 1.00 calc . . . H(7) H 0.9266 -0.0591 0.2910 0.2170 Uiso 1.00 calc . . . H(8) H 0.3959 0.3944 0.7574 0.0328 Uiso 1.00 calc . . . H(9) H 0.2191 0.3968 0.4345 0.0243 Uiso 1.00 calc . . . H(10) H 0.4918 0.5895 0.3008 0.0178 Uiso 1.00 calc . . . H(11) H 0.3048 0.5203 0.1748 0.0292 Uiso 1.00 calc . . . H(12) H 0.2454 0.6865 0.4532 0.0521 Uiso 1.00 calc . . . H(13) H 0.3946 0.7927 0.3756 0.0477 Uiso 1.00 calc . . . H(14) H 0.3012 0.6250 0.8115 0.0409 Uiso 1.00 calc . . . H(15) H 0.4857 0.6909 0.9453 0.0403 Uiso 1.00 calc . . . H(16) H 0.5814 0.8096 0.6794 0.0383 Uiso 1.00 calc . . . H(17) H 0.5326 0.9836 0.9435 0.0816 Uiso 1.00 calc . . . H(18) H 0.4497 1.0137 0.7119 0.1792 Uiso 1.00 calc . . . H(19) H 0.3391 0.8973 0.8533 0.0560 Uiso 1.00 calc . . . H(20) H 0.2292 0.2825 0.0202 0.1320 Uiso 1.00 calc . . . H(21) H 0.1245 0.1470 0.1082 0.0995 Uiso 1.00 calc . . . H(22) H 0.2566 0.1136 -0.0406 0.0346 Uiso 1.00 calc . . . H(23) H 0.4681 0.3147 0.2747 0.0491 Uiso 1.00 calc . . . H(24) H 0.2287 0.1081 0.4474 0.0576 Uiso 1.00 calc . . . H(25) H 0.3777 0.0802 0.3642 0.0611 Uiso 1.00 calc . . . H(26) H 0.4299 0.2352 0.6046 0.1199 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 F(1) 0.056(2) 0.066(2) 0.046(1) 0.041(1) -0.020(1) 0.006(1) O(1) 0.063(2) 0.094(3) 0.042(2) 0.054(2) 0.008(1) 0.040(2) O(2) 0.032(1) 0.051(2) 0.042(2) 0.025(1) 0.006(1) 0.031(1) N(1) 0.043(2) 0.048(2) 0.111(4) 0.019(2) 0.011(2) 0.049(2) C(1) 0.040(2) 0.050(2) 0.037(2) 0.033(2) -0.003(1) 0.016(2) C(1') 0.029(1) 0.045(2) 0.033(2) 0.021(2) 0.007(1) 0.024(1) C(2) 0.034(2) 0.046(2) 0.040(2) 0.020(2) -0.005(1) 0.013(1) C(2') 0.030(2) 0.046(2) 0.036(2) 0.022(2) 0.006(1) 0.017(1) C(3) 0.027(2) 0.046(3) 0.074(3) 0.019(2) 0.007(2) 0.028(2) C(3') 0.038(2) 0.051(2) 0.039(2) 0.023(2) 0.004(2) 0.026(2) C(4) 0.032(2) 0.041(2) 0.050(2) 0.021(2) 0.001(2) 0.024(1) C(4') 0.053(3) 0.046(3) 0.056(2) 0.028(2) 0.008(2) 0.029(2) C(5) 0.034(2) 0.051(2) 0.050(2) 0.023(2) 0.004(2) 0.027(2) C(5') 0.038(2) 0.046(2) 0.059(2) 0.026(2) 0.007(2) 0.027(2) C(6) 0.039(2) 0.053(2) 0.046(2) 0.023(2) 0.002(2) 0.028(2) C(6') 0.032(2) 0.044(2) 0.047(2) 0.021(2) 0.001(2) 0.016(2) C(7) 0.033(2) 0.041(2) 0.055(2) 0.015(2) 0.002(2) 0.021(2) C(7') 0.040(2) 0.042(2) 0.049(2) 0.025(2) 0.006(2) 0.017(2) C(8) 0.047(2) 0.047(2) 0.055(2) 0.028(2) 0.005(2) 0.029(2) C(8') 0.056(3) 0.049(3) 0.048(2) 0.028(2) 0.000(2) 0.008(2) C(9) 0.046(2) 0.047(2) 0.051(2) 0.028(2) 0.003(2) 0.030(2) C(9') 0.070(3) 0.042(3) 0.070(3) 0.033(2) 0.006(2) 0.029(2) C(10) 0.055(3) 0.044(2) 0.056(3) 0.023(2) -0.006(2) 0.011(2) C(10') 0.060(3) 0.050(3) 0.083(4) 0.040(3) -0.004(3) 0.006(2) #------------------------------------------------------------------------------ _refine_special_details ; Refinement based on F against all reflections. The weighted R-factor (wR) and goodness of fit (S) are based on F, conventional R-factors (R) are calculated on F, with F set to zero for negative F. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. thus the refinement was done using all reflections. ; _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_weighting_scheme unit _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_number_reflns 1570 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_number_constraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_all ? _refine_ls_wR_factor_ref 0.0622 _refine_ls_wR_factor_gt 0.0623 _refine_ls_goodness_of_fit_all ? _refine_ls_goodness_of_fit_ref 2.832 _refine_ls_shift/su_max 0.1880 _refine_ls_shift/su_mean 0.0500 _refine_diff_density_min -0.21 _refine_diff_density_max 0.22 #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag F(1) C(2) 1.396(7) 1_555 1_555 yes O(1) C(1) 1.166(8) 1_555 1_555 yes O(2) C(1) 1.360(7) 1_555 1_555 yes O(2) C(1') 1.482(7) 1_555 1_555 yes N(1) C(3) 1.131(9) 1_555 1_555 yes C(1) C(2) 1.563(9) 1_555 1_555 yes C(1') C(2') 1.531(8) 1_555 1_555 yes C(1') C(6') 1.512(10) 1_555 1_555 yes C(1') H(8) 1.187 1_555 1_555 no C(2) C(3) 1.500(10) 1_555 1_555 yes C(2) C(4) 1.49(1) 1_555 1_555 yes C(2') C(3') 1.548(9) 1_555 1_555 yes C(2') C(7') 1.541(10) 1_555 1_555 yes C(2') H(9) 0.963 1_555 1_555 no C(3') C(4') 1.51(1) 1_555 1_555 yes C(3') H(10) 0.949 1_555 1_555 no C(3') H(11) 0.947 1_555 1_555 no C(4) C(5) 1.387(10) 1_555 1_555 yes C(4) C(9) 1.421(8) 1_555 1_555 yes C(4') C(5') 1.52(1) 1_555 1_555 yes C(4') H(12) 0.984 1_555 1_555 no C(4') H(13) 0.934 1_555 1_555 no C(5) C(6) 1.35(1) 1_555 1_555 yes C(5) H(1) 0.935 1_555 1_555 no C(5') C(6') 1.532(10) 1_555 1_555 yes C(5') C(10') 1.53(1) 1_555 1_555 yes C(5') H(16) 0.944 1_555 1_555 no C(6) C(7) 1.437(9) 1_555 1_555 yes C(6) H(2) 0.946 1_555 1_555 no C(6') H(14) 0.978 1_555 1_555 no C(6') H(15) 0.995 1_555 1_555 no C(7) C(8) 1.36(1) 1_555 1_555 yes C(7) C(10) 1.49(1) 1_555 1_555 yes C(7') C(8') 1.532(10) 1_555 1_555 yes C(7') C(9') 1.537(10) 1_555 1_555 yes C(7') H(23) 0.933 1_555 1_555 no C(8) C(9) 1.37(1) 1_555 1_555 yes C(8) H(3) 0.962 1_555 1_555 no C(8') H(20) 0.943 1_555 1_555 no C(8') H(21) 0.972 1_555 1_555 no C(8') H(22) 1.079 1_555 1_555 no C(9) H(4) 0.956 1_555 1_555 no C(9') H(24) 0.975 1_555 1_555 no C(9') H(25) 0.925 1_555 1_555 no C(9') H(26) 1.183 1_555 1_555 no C(10) H(5) 0.870 1_555 1_555 no C(10) H(6) 0.952 1_555 1_555 no C(10) H(7) 0.952 1_555 1_555 no C(10') H(17) 0.979 1_555 1_555 no C(10') H(18) 1.097 1_555 1_555 no C(10') H(19) 0.997 1_555 1_555 no #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C(1) O(2) C(1') 116.9(5) 1_555 1_555 1_555 yes O(1) C(1) O(2) 128.2(6) 1_555 1_555 1_555 yes O(1) C(1) C(2) 124.7(5) 1_555 1_555 1_555 yes O(2) C(1) C(2) 106.8(5) 1_555 1_555 1_555 yes O(2) C(1') C(2') 105.7(5) 1_555 1_555 1_555 yes O(2) C(1') C(6') 108.4(5) 1_555 1_555 1_555 yes O(2) C(1') H(8) 104.2(9) 1_555 1_555 1_555 no C(2') C(1') C(6') 113.4(5) 1_555 1_555 1_555 yes C(2') C(1') H(8) 108.7(10) 1_555 1_555 1_555 no C(6') C(1') H(8) 115(1) 1_555 1_555 1_555 no F(1) C(2) C(1) 105.1(6) 1_555 1_555 1_555 yes F(1) C(2) C(3) 106.2(6) 1_555 1_555 1_555 yes F(1) C(2) C(4) 111.8(5) 1_555 1_555 1_555 yes C(1) C(2) C(3) 109.6(5) 1_555 1_555 1_555 yes C(1) C(2) C(4) 110.2(6) 1_555 1_555 1_555 yes C(3) C(2) C(4) 113.5(6) 1_555 1_555 1_555 yes C(1') C(2') C(3') 110.2(6) 1_555 1_555 1_555 yes C(1') C(2') C(7') 114.3(5) 1_555 1_555 1_555 yes C(1') C(2') H(9) 105(1) 1_555 1_555 1_555 no C(3') C(2') C(7') 111.8(6) 1_555 1_555 1_555 yes C(3') C(2') H(9) 107(1) 1_555 1_555 1_555 no C(7') C(2') H(9) 107(1) 1_555 1_555 1_555 no N(1) C(3) C(2) 178.2(7) 1_555 1_555 1_555 yes C(2') C(3') C(4') 113.5(6) 1_555 1_555 1_555 yes C(2') C(3') H(10) 108(1) 1_555 1_555 1_555 no C(2') C(3') H(11) 108(1) 1_555 1_555 1_555 no C(4') C(3') H(10) 108(1) 1_555 1_555 1_555 no C(4') C(3') H(11) 108(1) 1_555 1_555 1_555 no H(10) C(3') H(11) 109(1) 1_555 1_555 1_555 no C(2) C(4) C(5) 123.4(6) 1_555 1_555 1_555 yes C(2) C(4) C(9) 119.6(6) 1_555 1_555 1_555 yes C(5) C(4) C(9) 116.7(7) 1_555 1_555 1_555 yes C(3') C(4') C(5') 112.9(5) 1_555 1_555 1_555 yes C(3') C(4') H(12) 110(1) 1_555 1_555 1_555 no C(3') C(4') H(13) 113(1) 1_555 1_555 1_555 no C(5') C(4') H(12) 104(1) 1_555 1_555 1_555 no C(5') C(4') H(13) 106(1) 1_555 1_555 1_555 no H(12) C(4') H(13) 107(1) 1_555 1_555 1_555 no C(4) C(5) C(6) 122.3(6) 1_555 1_555 1_555 yes C(4) C(5) H(1) 120(1) 1_555 1_555 1_555 no C(6) C(5) H(1) 117(1) 1_555 1_555 1_555 no C(4') C(5') C(6') 108.8(6) 1_555 1_555 1_555 yes C(4') C(5') C(10') 113.0(6) 1_555 1_555 1_555 yes C(4') C(5') H(16) 110(1) 1_555 1_555 1_555 no C(6') C(5') C(10') 111.2(7) 1_555 1_555 1_555 yes C(6') C(5') H(16) 107(1) 1_555 1_555 1_555 no C(10') C(5') H(16) 106(1) 1_555 1_555 1_555 no C(5) C(6) C(7) 121.5(7) 1_555 1_555 1_555 yes C(5) C(6) H(2) 119(1) 1_555 1_555 1_555 no C(7) C(6) H(2) 118(1) 1_555 1_555 1_555 no C(1') C(6') C(5') 113.4(6) 1_555 1_555 1_555 yes C(1') C(6') H(14) 110(1) 1_555 1_555 1_555 no C(1') C(6') H(15) 109(1) 1_555 1_555 1_555 no C(5') C(6') H(14) 109(1) 1_555 1_555 1_555 no C(5') C(6') H(15) 109(1) 1_555 1_555 1_555 no H(14) C(6') H(15) 103(1) 1_555 1_555 1_555 no C(6) C(7) C(8) 115.5(7) 1_555 1_555 1_555 yes C(6) C(7) C(10) 121.7(6) 1_555 1_555 1_555 yes C(8) C(7) C(10) 122.8(6) 1_555 1_555 1_555 yes C(2') C(7') C(8') 110.9(5) 1_555 1_555 1_555 yes C(2') C(7') C(9') 112.9(6) 1_555 1_555 1_555 yes C(2') C(7') H(23) 108(1) 1_555 1_555 1_555 no C(8') C(7') C(9') 108.5(6) 1_555 1_555 1_555 yes C(8') C(7') H(23) 107(1) 1_555 1_555 1_555 no C(9') C(7') H(23) 107(1) 1_555 1_555 1_555 no C(7) C(8) C(9) 123.9(6) 1_555 1_555 1_555 yes C(7) C(8) H(3) 117(1) 1_555 1_555 1_555 no C(9) C(8) H(3) 118(1) 1_555 1_555 1_555 no C(7') C(8') H(20) 106(1) 1_555 1_555 1_555 no C(7') C(8') H(21) 106(1) 1_555 1_555 1_555 no C(7') C(8') H(22) 117(1) 1_555 1_555 1_555 no H(20) C(8') H(21) 108(1) 1_555 1_555 1_555 no H(20) C(8') H(22) 109(1) 1_555 1_555 1_555 no H(21) C(8') H(22) 107(1) 1_555 1_555 1_555 no C(4) C(9) C(8) 120.1(7) 1_555 1_555 1_555 yes C(4) C(9) H(4) 120(1) 1_555 1_555 1_555 no C(8) C(9) H(4) 119(1) 1_555 1_555 1_555 no C(7') C(9') H(24) 113(1) 1_555 1_555 1_555 no C(7') C(9') H(25) 112(1) 1_555 1_555 1_555 no C(7') C(9') H(26) 103.5(10) 1_555 1_555 1_555 no H(24) C(9') H(25) 109(1) 1_555 1_555 1_555 no H(24) C(9') H(26) 107(1) 1_555 1_555 1_555 no H(25) C(9') H(26) 110(1) 1_555 1_555 1_555 no C(7) C(10) H(5) 120(1) 1_555 1_555 1_555 no C(7) C(10) H(6) 104(1) 1_555 1_555 1_555 no C(7) C(10) H(7) 103(1) 1_555 1_555 1_555 no H(5) C(10) H(6) 109(1) 1_555 1_555 1_555 no H(5) C(10) H(7) 109(1) 1_555 1_555 1_555 no H(6) C(10) H(7) 109(1) 1_555 1_555 1_555 no C(5') C(10') H(17) 111(1) 1_555 1_555 1_555 no C(5') C(10') H(18) 114(1) 1_555 1_555 1_555 no C(5') C(10') H(19) 109(1) 1_555 1_555 1_555 no H(17) C(10') H(18) 109(1) 1_555 1_555 1_555 no H(17) C(10') H(19) 103(1) 1_555 1_555 1_555 no H(18) C(10') H(19) 108(1) 1_555 1_555 1_555 no #------------------------------------------------------------------------------ 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 F(1) C(2) C(1) O(1) -27.3(10) 1_555 1_555 1_555 1_555 yes F(1) C(2) C(1) O(2) 158.9(5) 1_555 1_555 1_555 1_555 yes F(1) C(2) C(3) N(1) 29(29) 1_555 1_555 1_555 1_555 yes F(1) C(2) C(4) C(5) -157.0(6) 1_555 1_555 1_555 1_555 yes F(1) C(2) C(4) C(9) 29.6(9) 1_555 1_555 1_555 1_555 yes O(1) C(1) O(2) C(1') 1(1) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(2) C(3) -141.0(8) 1_555 1_555 1_555 1_555 yes O(1) C(1) C(2) C(4) 93.3(8) 1_555 1_555 1_555 1_555 yes O(2) C(1) C(2) C(3) 45.2(7) 1_555 1_555 1_555 1_555 yes O(2) C(1) C(2) C(4) -80.5(7) 1_555 1_555 1_555 1_555 yes O(2) C(1') C(2') C(3') -69.3(6) 1_555 1_555 1_555 1_555 yes O(2) C(1') C(2') C(7') 57.5(7) 1_555 1_555 1_555 1_555 yes O(2) C(1') C(6') C(5') 63.1(6) 1_555 1_555 1_555 1_555 yes N(1) C(3) C(2) C(1) 142(28) 1_555 1_555 1_555 1_555 yes N(1) C(3) C(2) C(4) -93(28) 1_555 1_555 1_555 1_555 yes C(1) O(2) C(1') C(2') -150.4(5) 1_555 1_555 1_555 1_555 yes C(1) O(2) C(1') C(6') 87.7(6) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(4) C(5) 86.5(8) 1_555 1_555 1_555 1_555 yes C(1) C(2) C(4) C(9) -86.8(7) 1_555 1_555 1_555 1_555 yes C(1') O(2) C(1) C(2) 175.5(6) 1_555 1_555 1_555 1_555 yes C(1') C(2') C(3') C(4') -50.0(7) 1_555 1_555 1_555 1_555 yes C(1') C(2') C(7') C(8') 168.2(6) 1_555 1_555 1_555 1_555 yes C(1') C(2') C(7') C(9') 46.1(8) 1_555 1_555 1_555 1_555 yes C(1') C(6') C(5') C(4') 55.0(7) 1_555 1_555 1_555 1_555 yes C(1') C(6') C(5') C(10') -179.9(6) 1_555 1_555 1_555 1_555 yes C(2) C(4) C(5) C(6) -172.6(7) 1_555 1_555 1_555 1_555 yes C(2) C(4) C(9) C(8) 173.9(7) 1_555 1_555 1_555 1_555 yes C(2') C(1') C(6') C(5') -54.0(7) 1_555 1_555 1_555 1_555 yes C(2') C(3') C(4') C(5') 54.8(8) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(4) C(5) -36.9(10) 1_555 1_555 1_555 1_555 yes C(3) C(2) C(4) C(9) 149.7(6) 1_555 1_555 1_555 1_555 yes C(3') C(2') C(1') C(6') 49.4(7) 1_555 1_555 1_555 1_555 yes C(3') C(2') C(7') C(8') -65.9(8) 1_555 1_555 1_555 1_555 yes C(3') C(2') C(7') C(9') 172.1(6) 1_555 1_555 1_555 1_555 yes C(3') C(4') C(5') C(6') -55.2(8) 1_555 1_555 1_555 1_555 yes C(3') C(4') C(5') C(10') -179.3(7) 1_555 1_555 1_555 1_555 yes C(4) C(5) C(6) C(7) 0(1) 1_555 1_555 1_555 1_555 yes C(4) C(9) C(8) C(7) -2(1) 1_555 1_555 1_555 1_555 yes C(4') C(3') C(2') C(7') -178.2(6) 1_555 1_555 1_555 1_555 yes C(5) C(4) C(9) C(8) 0(1) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(8) -3.3(10) 1_555 1_555 1_555 1_555 yes C(5) C(6) C(7) C(10) 178.7(8) 1_555 1_555 1_555 1_555 yes C(6) C(5) C(4) C(9) 0(1) 1_555 1_555 1_555 1_555 yes C(6) C(7) C(8) C(9) 4(1) 1_555 1_555 1_555 1_555 yes C(6') C(1') C(2') C(7') 176.2(6) 1_555 1_555 1_555 1_555 yes C(9) C(8) C(7) C(10) -177.6(7) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ _publ_contact_author_name ' ENTER NAME' _publ_contact_author_address ; ENTER ADDRESS ; _publ_contact_author_email ' ENTER EMAIL ADDRESS ' _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ' ENTER JOURNAL NAME HERE' _publ_requested_category ' CHOOSE FI FM FO CI CM CO or AD' _publ_requested_coeditor_name ? _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; _publ_section_synopsis ; ENTER SYNOPSIS ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_comment ; ENTER TEXT ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_experimental ; ENTER EXPERIMENTAL SECTION ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1998). teXsan. Single Crystal Structure Analysis Software. Version 1.9. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. North, A.C.T., Phillips, D. C. & Mathews, F. S. (1968). Acta Cryst. A24, 351-359. ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _publ_section_exptl_prep ; ENTER COMPOUND PREPARATION DETAILS ; _publ_section_exptl_refinement ; ENTER SPECIAL DETAILS OF THE REFINEMENT ;