data_4c _audit_creation_method SHELXL-97 _chemical_name_systematic ; '1-(para-methoxybenzyl)-3’-pyrrolidinocarbonylspiro[3H-indole-3,2’ -oxiran]-2(1H)-one' ; _chemical_name_common ? _chemical_melting_point 175-178\%C _chemical_formula_moiety 'C22 H22 N2 O4' _chemical_formula_sum 'C22 H22 N2 O4' _chemical_formula_weight 378.42 _chemical_compound_source synthetised _chemical_absolute_configuration 'ad' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn ' 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 11.4610(3) _cell_length_b 9.3131(2) _cell_length_c 18.6652(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.4583(11) _cell_angle_gamma 90.00 _cell_volume 1910.64(8) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 53613 _cell_measurement_theta_min 1.88 _cell_measurement_theta_max 31.62 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.5 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.316 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 53613 _diffrn_reflns_av_R_equivalents 0.0272 _diffrn_reflns_av_sigmaI/netI 0.0168 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 31.62 _reflns_number_total 6417 _reflns_number_gt 4736 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1027P)^2^+0.2132P] 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 6417 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0692 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1694 _refine_ls_wR_factor_gt 0.1418 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 N1 N 0.32938(8) 0.76107(10) 0.21771(5) 0.03459(19) Uani 1 1 d . . . O2 O 0.50954(8) 0.99845(9) 0.14508(5) 0.0442(2) Uani 1 1 d . . . C3 C 0.44356(9) 0.69190(11) 0.24242(6) 0.0331(2) Uani 1 1 d . . . N4 N 0.51749(8) 0.76200(11) -0.01087(5) 0.0411(2) Uani 1 1 d . A . O5 O 0.24945(8) 0.95012(9) 0.13918(5) 0.0443(2) Uani 1 1 d . . . C6 C 0.52497(9) 0.75171(11) 0.20728(6) 0.0335(2) Uani 1 1 d . . . C7 C 0.45712(9) 0.86406(11) 0.15645(6) 0.0327(2) Uani 1 1 d . . . C8 C 0.33193(9) 0.86877(11) 0.16884(5) 0.0330(2) Uani 1 1 d . . . C9 C 0.46574(10) 0.90742(12) 0.08165(6) 0.0375(2) Uani 1 1 d . . . H9 H 0.3913(12) 0.9385(14) 0.0468(8) 0.037(3) Uiso 1 1 d . . . C10 C 0.47749(11) 0.58276(13) 0.29439(7) 0.0421(2) Uani 1 1 d . . . H10 H 0.4173(15) 0.5395(18) 0.3206(9) 0.056(4) Uiso 1 1 d . . . C11 C 0.13960(10) 0.61846(13) 0.18707(6) 0.0390(2) Uani 1 1 d . . . C12 C 0.22101(10) 0.72408(13) 0.23924(7) 0.0399(2) Uani 1 1 d . . . H12A H 0.2433(15) 0.6840(18) 0.2910(10) 0.057(4) Uiso 1 1 d . . . H12B H 0.1786(15) 0.8165(18) 0.2415(9) 0.054(4) Uiso 1 1 d . . . O13 O 0.66927(9) 0.87042(14) 0.07608(6) 0.0631(3) Uani 1 1 d . . . C14 C 0.56099(10) 0.84438(13) 0.04931(6) 0.0401(2) Uani 1 1 d . . . C15 C 0.64418(10) 0.70408(14) 0.22525(7) 0.0435(3) Uani 1 1 d . . . H15 H 0.6971(15) 0.7478(17) 0.2001(10) 0.055(4) Uiso 1 1 d . . . C18 C 0.18044(12) 0.52755(16) 0.14132(8) 0.0512(3) Uani 1 1 d . . . H18 H 0.2639(17) 0.5350(19) 0.1415(10) 0.066(5) Uiso 1 1 d . . . C19 C 0.67948(12) 0.59482(16) 0.27781(8) 0.0505(3) Uani 1 1 d . . . H19 H 0.7633(17) 0.5601(19) 0.2935(11) 0.067(5) Uiso 1 1 d . . . C20 C 0.59772(12) 0.53573(15) 0.31152(7) 0.0487(3) Uani 1 1 d . . . H20 H 0.6218(14) 0.4637(18) 0.3491(10) 0.056(4) Uiso 1 1 d . . . C21 C 0.10406(14) 0.42710(18) 0.09544(9) 0.0591(4) Uani 1 1 d . . . H21 H 0.1353(18) 0.363(2) 0.0650(11) 0.078(6) Uiso 1 1 d . . . O22 O -0.09712(14) 0.32336(18) 0.05337(8) 0.0949(5) Uani 1 1 d . . . C23 C -0.01514(14) 0.4183(2) 0.09564(8) 0.0635(4) Uani 1 1 d . . . C24 C 0.01874(13) 0.6080(2) 0.18564(9) 0.0652(4) Uani 1 1 d . . . H24 H -0.010(2) 0.672(2) 0.2190(13) 0.093(7) Uiso 1 1 d . . . C27 C -0.05748(15) 0.5097(3) 0.14046(12) 0.0823(6) Uani 1 1 d . . . H27 H -0.140(2) 0.499(3) 0.1429(14) 0.105(8) Uiso 1 1 d . . . C28 C -0.0542(3) 0.2208(3) 0.01192(14) 0.1055(9) Uani 1 1 d . . . H28A H 0.015(3) 0.153(3) 0.0442(16) 0.118(9) Uiso 1 1 d . . . H28B H -0.018(2) 0.258(3) -0.0250(14) 0.094(7) Uiso 1 1 d . . . H28C H -0.116(3) 0.153(3) -0.0125(17) 0.125(9) Uiso 1 1 d . . . C16 C 0.59838(13) 0.69915(17) -0.05099(8) 0.0514(3) Uani 1 1 d . . . H16A H 0.6582(17) 0.633(2) -0.0197(10) 0.069(5) Uiso 1 1 d . . . H16B H 0.6523(17) 0.774(2) -0.0631(11) 0.073(5) Uiso 1 1 d . . . C17 C 0.38891(12) 0.72674(16) -0.04627(8) 0.0500(3) Uani 1 1 d . . . H17A H 0.3414(15) 0.8182(19) -0.0686(9) 0.059(5) Uiso 1 1 d . . . H17B H 0.3517(18) 0.686(2) -0.0092(12) 0.080(6) Uiso 1 1 d . . . C25A C 0.4025(9) 0.6542(13) -0.1184(7) 0.066(2) Uani 0.311(10) 1 d P A 1 H25A H 0.3403 0.5814 -0.1356 0.079 Uiso 0.311(10) 1 calc PR A 1 H25B H 0.3938 0.7250 -0.1577 0.079 Uiso 0.311(10) 1 calc PR A 1 C26A C 0.5230(6) 0.5893(11) -0.1001(5) 0.0585(18) Uani 0.311(10) 1 d P A 1 H26A H 0.5493 0.5739 -0.1446 0.070 Uiso 0.311(10) 1 calc PR A 1 H26B H 0.5250 0.4987 -0.0741 0.070 Uiso 0.311(10) 1 calc PR A 1 C25B C 0.3923(4) 0.6089(5) -0.1017(2) 0.0522(7) Uani 0.689(10) 1 d P A 2 H25C H 0.3204 0.6114 -0.1444 0.063 Uiso 0.689(10) 1 calc PR A 2 H25D H 0.3990 0.5149 -0.0785 0.063 Uiso 0.689(10) 1 calc PR A 2 C26B C 0.5073(3) 0.6469(4) -0.12431(19) 0.0534(8) Uani 0.689(10) 1 d P A 2 H26C H 0.4907 0.7221 -0.1618 0.064 Uiso 0.689(10) 1 calc PR A 2 H26D H 0.5385 0.5634 -0.1439 0.064 Uiso 0.689(10) 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 N1 0.0330(4) 0.0354(4) 0.0366(4) 0.0017(3) 0.0119(3) -0.0006(3) O2 0.0563(5) 0.0340(4) 0.0441(4) -0.0044(3) 0.0171(4) -0.0136(3) C3 0.0341(4) 0.0322(5) 0.0313(4) -0.0024(4) 0.0066(4) -0.0020(4) N4 0.0360(4) 0.0492(5) 0.0404(5) -0.0042(4) 0.0147(4) -0.0021(4) O5 0.0466(4) 0.0444(5) 0.0422(4) 0.0028(3) 0.0132(3) 0.0128(3) C6 0.0324(4) 0.0340(5) 0.0328(4) -0.0033(4) 0.0068(3) -0.0034(4) C7 0.0349(4) 0.0306(4) 0.0332(4) -0.0026(3) 0.0105(4) -0.0042(4) C8 0.0369(5) 0.0320(5) 0.0305(4) -0.0036(3) 0.0105(4) 0.0001(4) C9 0.0418(5) 0.0372(5) 0.0343(5) -0.0008(4) 0.0121(4) -0.0056(4) C10 0.0465(6) 0.0386(5) 0.0386(5) 0.0031(4) 0.0076(4) -0.0016(4) C11 0.0327(5) 0.0462(6) 0.0378(5) 0.0084(4) 0.0095(4) -0.0015(4) C12 0.0385(5) 0.0443(6) 0.0414(6) 0.0000(4) 0.0186(4) -0.0013(4) O13 0.0401(5) 0.0949(8) 0.0550(6) -0.0149(5) 0.0147(4) -0.0177(5) C14 0.0393(5) 0.0472(6) 0.0355(5) 0.0017(4) 0.0133(4) -0.0070(4) C15 0.0332(5) 0.0495(6) 0.0454(6) -0.0045(5) 0.0072(4) -0.0015(4) C18 0.0356(5) 0.0553(7) 0.0597(8) -0.0091(6) 0.0084(5) -0.0024(5) C19 0.0386(6) 0.0533(7) 0.0514(7) -0.0026(5) -0.0005(5) 0.0081(5) C20 0.0502(6) 0.0450(6) 0.0435(6) 0.0044(5) 0.0011(5) 0.0062(5) C21 0.0547(8) 0.0571(8) 0.0573(8) -0.0074(7) 0.0024(6) -0.0077(6) O22 0.0834(9) 0.1143(11) 0.0710(8) -0.0059(8) -0.0044(7) -0.0575(9) C23 0.0553(8) 0.0762(10) 0.0477(7) 0.0113(7) -0.0040(6) -0.0283(7) C24 0.0392(6) 0.1000(13) 0.0613(8) -0.0067(8) 0.0222(6) -0.0121(7) C27 0.0440(7) 0.1306(18) 0.0734(11) -0.0095(11) 0.0184(7) -0.0330(9) C28 0.133(2) 0.0932(17) 0.0639(12) -0.0042(12) -0.0152(13) -0.0520(16) C16 0.0462(6) 0.0594(8) 0.0542(7) -0.0055(6) 0.0236(6) 0.0036(6) C17 0.0389(6) 0.0576(8) 0.0532(7) -0.0147(6) 0.0123(5) -0.0054(5) C25A 0.059(4) 0.064(5) 0.072(6) -0.028(4) 0.015(3) -0.015(4) C26A 0.064(3) 0.057(4) 0.055(3) -0.009(3) 0.018(3) 0.012(3) C25B 0.0535(13) 0.0499(17) 0.0549(16) -0.0142(12) 0.0178(11) -0.0140(13) C26B 0.0688(15) 0.0488(15) 0.0485(14) -0.0077(11) 0.0264(12) -0.0001(12) _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 C8 1.3616(14) . ? N1 C3 1.4136(13) . ? N1 C12 1.4511(13) . ? O2 C9 1.4268(13) . ? O2 C7 1.4299(12) . ? C3 C10 1.3826(15) . ? C3 C6 1.3993(15) . ? N4 C14 1.3347(15) . ? N4 C16 1.4683(15) . ? N4 C17 1.4712(15) . ? O5 C8 1.2156(13) . ? C6 C15 1.3843(15) . ? C6 C7 1.4770(15) . ? C7 C9 1.4833(14) . ? C7 C8 1.5173(14) . ? C9 C14 1.5080(16) . ? C9 H9 0.960(14) . ? C10 C20 1.3939(18) . ? C10 H10 1.035(17) . ? C11 C18 1.3753(19) . ? C11 C24 1.3812(17) . ? C11 C12 1.5072(16) . ? C12 H12A 1.000(17) . ? C12 H12B 0.995(17) . ? O13 C14 1.2237(14) . ? C15 C19 1.3916(19) . ? C15 H15 0.956(17) . ? C18 C21 1.3964(19) . ? C18 H18 0.959(18) . ? C19 C20 1.382(2) . ? C19 H19 0.977(18) . ? C20 H20 0.953(17) . ? C21 C23 1.370(2) . ? C21 H21 0.96(2) . ? O22 C23 1.3663(18) . ? O22 C28 1.403(4) . ? C23 C27 1.375(3) . ? C24 C27 1.377(3) . ? C24 H24 0.98(2) . ? C27 H27 0.97(2) . ? C28 H28A 1.05(3) . ? C28 H28B 0.96(3) . ? C28 H28C 0.96(3) . ? C16 C26A 1.478(7) . ? C16 C26B 1.546(3) . ? C16 H16A 0.982(19) . ? C16 H16B 1.00(2) . ? C17 C25B 1.516(4) . ? C17 C25A 1.553(11) . ? C17 H17A 1.033(17) . ? C17 H17B 0.99(2) . ? C25A C26A 1.457(13) . ? C25A H25A 0.9700 . ? C25A H25B 0.9700 . ? C26A H26A 0.9700 . ? C26A H26B 0.9700 . ? C25B C26B 1.535(5) . ? C25B H25C 0.9700 . ? C25B H25D 0.9700 . ? C26B H26C 0.9700 . ? C26B H26D 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 C8 N1 C3 111.14(8) . . ? C8 N1 C12 122.89(9) . . ? C3 N1 C12 125.96(9) . . ? C9 O2 C7 62.56(7) . . ? C10 C3 C6 121.95(10) . . ? C10 C3 N1 127.90(10) . . ? C6 C3 N1 110.13(9) . . ? C14 N4 C16 121.27(10) . . ? C14 N4 C17 126.44(10) . . ? C16 N4 C17 112.26(10) . . ? C15 C6 C3 120.15(10) . . ? C15 C6 C7 133.36(10) . . ? C3 C6 C7 106.47(9) . . ? O2 C7 C6 123.26(9) . . ? O2 C7 C9 58.62(7) . . ? C6 C7 C9 129.36(9) . . ? O2 C7 C8 116.91(9) . . ? C6 C7 C8 105.73(8) . . ? C9 C7 C8 116.98(9) . . ? O5 C8 N1 127.06(10) . . ? O5 C8 C7 126.56(10) . . ? N1 C8 C7 106.35(8) . . ? O2 C9 C7 58.82(6) . . ? O2 C9 C14 116.04(9) . . ? C7 C9 C14 121.30(10) . . ? O2 C9 H9 114.8(8) . . ? C7 C9 H9 115.9(8) . . ? C14 C9 H9 116.8(8) . . ? C3 C10 C20 117.08(11) . . ? C3 C10 H10 121.7(9) . . ? C20 C10 H10 121.2(9) . . ? C18 C11 C24 117.42(13) . . ? C18 C11 C12 123.07(10) . . ? C24 C11 C12 119.49(12) . . ? N1 C12 C11 113.44(9) . . ? N1 C12 H12A 110.6(10) . . ? C11 C12 H12A 108.8(9) . . ? N1 C12 H12B 105.8(10) . . ? C11 C12 H12B 111.8(9) . . ? H12A C12 H12B 106.0(13) . . ? O13 C14 N4 123.45(11) . . ? O13 C14 C9 121.66(11) . . ? N4 C14 C9 114.87(10) . . ? C6 C15 C19 118.36(12) . . ? C6 C15 H15 117.6(10) . . ? C19 C15 H15 124.0(10) . . ? C11 C18 C21 121.91(13) . . ? C11 C18 H18 117.9(11) . . ? C21 C18 H18 120.2(11) . . ? C20 C19 C15 120.85(11) . . ? C20 C19 H19 117.9(11) . . ? C15 C19 H19 121.2(11) . . ? C19 C20 C10 121.61(12) . . ? C19 C20 H20 121.6(10) . . ? C10 C20 H20 116.8(10) . . ? C23 C21 C18 119.40(16) . . ? C23 C21 H21 120.2(12) . . ? C18 C21 H21 120.4(12) . . ? C23 O22 C28 117.90(19) . . ? O22 C23 C21 124.09(19) . . ? O22 C23 C27 116.65(16) . . ? C21 C23 C27 119.26(14) . . ? C27 C24 C11 121.17(17) . . ? C27 C24 H24 121.8(13) . . ? C11 C24 H24 117.0(13) . . ? C23 C27 C24 120.83(15) . . ? C23 C27 H27 118.9(15) . . ? C24 C27 H27 120.1(15) . . ? O22 C28 H28A 114.4(15) . . ? O22 C28 H28B 116.2(15) . . ? H28A C28 H28B 103(2) . . ? O22 C28 H28C 112.6(18) . . ? H28A C28 H28C 102(2) . . ? H28B C28 H28C 108(2) . . ? N4 C16 C26A 104.5(3) . . ? N4 C16 C26B 102.19(14) . . ? C26A C16 C26B 26.3(3) . . ? N4 C16 H16A 112.4(11) . . ? C26A C16 H16A 97.0(11) . . ? C26B C16 H16A 120.8(11) . . ? N4 C16 H16B 111.0(11) . . ? C26A C16 H16B 129.2(12) . . ? C26B C16 H16B 109.0(11) . . ? H16A C16 H16B 101.5(15) . . ? N4 C17 C25B 104.61(19) . . ? N4 C17 C25A 98.8(4) . . ? C25B C17 C25A 20.8(4) . . ? N4 C17 H17A 110.1(9) . . ? C25B C17 H17A 115.7(10) . . ? C25A C17 H17A 100.3(11) . . ? N4 C17 H17B 110.4(11) . . ? C25B C17 H17B 107.4(12) . . ? C25A C17 H17B 127.5(13) . . ? H17A C17 H17B 108.6(15) . . ? C26A C25A C17 107.4(8) . . ? C26A C25A H25A 110.2 . . ? C17 C25A H25A 110.2 . . ? C26A C25A H25B 110.2 . . ? C17 C25A H25B 110.2 . . ? H25A C25A H25B 108.5 . . ? C25A C26A C16 101.9(6) . . ? C25A C26A H26A 111.4 . . ? C16 C26A H26A 111.4 . . ? C25A C26A H26B 111.4 . . ? C16 C26A H26B 111.4 . . ? H26A C26A H26B 109.2 . . ? C17 C25B C26B 102.2(3) . . ? C17 C25B H25C 111.3 . . ? C26B C25B H25C 111.3 . . ? C17 C25B H25D 111.3 . . ? C26B C25B H25D 111.3 . . ? H25C C25B H25D 109.2 . . ? C25B C26B C16 104.3(2) . . ? C25B C26B H26C 110.9 . . ? C16 C26B H26C 110.9 . . ? C25B C26B H26D 110.9 . . ? C16 C26B H26D 110.9 . . ? H26C C26B H26D 108.9 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 31.62 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.310 _refine_diff_density_min -0.324 _refine_diff_density_rms 0.096 _publ_requested_journal 'Organic Letters' _publ_contact_author_name 'Bri\`ere, Jean-Fran\,cois' _publ_contact_author_address ; Laboratoire de Chimie Mol\'eculaire et Thio-organique, UMR CNRS 6507 ENSICAEN - Universit\'e de Caen 14050 Caen France ; _publ_contact_author_phone '332 31 45 28 86' _publ_contact_author_fax '332 31 45 28 65' _publ_contact_author_email jean-francois.briere@ensicaen.fr loop_ _publ_author_name _publ_author_address 'Schulz, Verena' ; Laboratoire de Chimie Mol\'eculaire et Thio-organique, UMR CNRS 6507 ENSICAEN - Universit\'e de Caen 14050 Caen France ; 'Davoust, Marion' ; Laboratoire de Chimie Mol\'eculaire et Thio-organique, UMR CNRS 6507 ENSICAEN - Universit\'e de Caen 14050 Caen France ; 'Lemari\'e, Margareth' ; Laboratoire de Chimie Mol\'eculaire et Thio-organique, UMR CNRS 6507 ENSICAEN - Universit\'e de Caen 14050 Caen France ; 'Lohier, Jean-Fran\,cois' ; Laboratoire de Chimie Mol\'eculaire et Thio-organique, UMR CNRS 6507 ENSICAEN - Universit\'e de Caen 14050 Caen France ; 'Sopkova-de Oliveira Santos, Jana' ; Centre d'\'Etudes et de Recherche sur le Medicament de Normandie (CERMN) Universit\'e de Caen 5 rue Vaub\'enard 14032 Caen France ; 'Metzner, Patrick' ; Laboratoire de Chimie Mol\'eculaire et Thio-organique, UMR CNRS 6507 ENSICAEN - Universit\'e de Caen 14050 Caen France ; 'Bri\`ere, Jean-Fran\,cois' ; Laboratoire de Chimie Mol\'eculaire et Thio-organique, UMR CNRS 6507 ENSICAEN - Universit\'e de Caen 14050 Caen France ;