# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_footnote _publ_author_address "Xavier Company\'o" . ; Department Qu\'imica Org\`anica Universitat de Barcelona Mart\'i i Franqu\'es 1-11 E-08028-Barcelona Spain ; 'Guillem Valero' . ; Department Qu\'imica Org\`anica Universitat de Barcelona Mart\'i i Franqu\'es 1-11 E-08028-Barcelona Spain ; 'Victor Ceban' . ; Department Qu\'imica Org\`anica Universitat de Barcelona Mart\'i i Franqu\'es 1-11 E-08028-Barcelona Spain ; 'Teresa Calvet' . ; Departament de Cristal.lografia Universitat de Barcelona Mart\'i i Franqu\`es, sn E-08028 Barcelona Spain ; 'Font-Bardia, Merc\`e' . ; Departament de Cristal.lografia Universitat de Barcelona Mart\'i i Franqu\`es, sn E-08028 Barcelona Spain ; 'Albert Moyano' . ; Department Qu\'imica Org\`anica Universitat de Barcelona Mart\'i i Franqu\'es 1-11 E-08028-Barcelona Spain ; 'Ramon Rios' . ; Department Qu\'imica Org\`anica Universitat de Barcelona Mart\'i i Franqu\'es 1-11 E-08028-Barcelona Spain ICREA, Passeig Lluis Companys 23, 08010 Barcelona Spain ; #TrackingRef 'xcpm80.cif' # 3. TITLE AND AUTHOR LIST _publ_section_title ; Enantioselective Organocatalytic Asymmetric Allylic Alkylation. Bis(phenylsulfonyl)methane addition to MBH carbonates ; _publ_contact_author_name 'Merce Font-Bardia' _publ_contact_author_email mercef@sct.ub.es data_xcpm80 _database_code_depnum_ccdc_archive 'CCDC 844907' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H22 O6 S2' _chemical_formula_sum 'C24 H22 O6 S2' _chemical_formula_weight 470.54 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 5.919(3) _cell_length_b 14.531(5) _cell_length_c 25.735(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2213.4(17) _cell_formula_units_Z 4 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 185 _cell_measurement_theta_min 3 _cell_measurement_theta_max 31 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 0.280 _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 105(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 'MAR345 with image plate detector' _diffrn_measurement_method 'phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16387 _diffrn_reflns_av_R_equivalents 0.0768 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 32.35 _reflns_number_total 5891 _reflns_number_gt 5116 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MARXDS (Claudio Klein, 2005)' _computing_cell_refinement 'AUTOMAR (Claudio Klein, 2007)' _computing_data_reduction 'MARSCALE (Claudio Klein, 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Brueggermann and Smith, 1990)' _computing_publication_material 'PLATON (Spek, 1990)' _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^)+(0.0785P)^2^+5.2849P] 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 SHELXL _refine_ls_extinction_coef 0.016(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.09(13) _chemical_absolute_configuration rm _refine_ls_number_reflns 5891 _refine_ls_number_parameters 351 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0965 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.2035 _refine_ls_wR_factor_gt 0.1815 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 S1 S 0.86548(18) 0.46297(8) 0.80146(4) 0.0278(2) Uani 1 1 d . . . S2 S 1.02906(19) 0.41301(8) 0.90672(4) 0.0286(2) Uani 1 1 d . . . O1 O 0.6249(7) 0.8109(2) 0.83489(13) 0.0378(8) Uani 1 1 d . . . O2 O 0.9733(7) 0.7753(2) 0.86302(14) 0.0389(8) Uani 1 1 d . . . O3 O 1.1039(5) 0.4712(2) 0.79171(12) 0.0307(7) Uani 1 1 d . . . O4 O 0.7140(6) 0.5216(2) 0.77314(12) 0.0329(7) Uani 1 1 d . . . O5 O 1.2410(5) 0.4614(2) 0.91037(12) 0.0313(7) Uani 1 1 d . . . O6 O 1.0277(6) 0.3241(2) 0.88222(12) 0.0328(7) Uani 1 1 d . . . C1 C 1.0478(8) 0.6472(3) 0.96748(17) 0.0298(9) Uani 1 1 d . . . C2 C 1.0411(9) 0.6668(3) 1.02078(18) 0.0326(9) Uani 1 1 d . . . C3 C 0.8517(9) 0.6458(3) 1.04986(17) 0.0323(9) Uani 1 1 d . . . C4 C 0.6640(8) 0.6054(3) 1.02589(18) 0.0324(9) Uani 1 1 d . . . C5 C 0.6672(7) 0.5883(3) 0.97231(16) 0.0285(8) Uani 1 1 d . . . H5 H 0.5400 0.5640 0.9561 0.034 Uiso 1 1 calc R . . C6 C 0.8617(7) 0.6075(3) 0.94290(16) 0.0265(8) Uani 1 1 d . . . C7 C 0.8628(8) 0.5896(3) 0.88404(15) 0.0273(8) Uani 1 1 d . . . C8 C 0.6908(8) 0.6561(3) 0.85996(16) 0.0278(9) Uani 1 1 d . . . C9 C 0.7802(8) 0.7516(3) 0.85306(17) 0.0314(9) Uani 1 1 d . . . C10 C 0.6910(12) 0.9067(4) 0.8303(2) 0.0467(14) Uani 1 1 d . . . H10 H 0.5588 0.9441 0.8257 0.056 Uiso 1 1 calc R . . H10A H 0.7892 0.9140 0.8009 0.056 Uiso 1 1 calc R . . H10B H 0.7688 0.9253 0.8613 0.056 Uiso 1 1 calc R . . C11 C 0.4767(8) 0.6365(4) 0.84909(17) 0.0333(10) Uani 1 1 d . . . C12 C 0.8249(8) 0.4870(3) 0.87157(16) 0.0282(9) Uani 1 1 d . . . C13 C 0.7802(7) 0.3476(3) 0.79202(16) 0.0290(9) Uani 1 1 d . . . C14 C 0.5607(8) 0.3200(3) 0.8053(2) 0.0338(10) Uani 1 1 d . . . C15 C 0.5043(9) 0.2276(4) 0.7984(2) 0.0384(10) Uani 1 1 d . . . C16 C 0.6591(9) 0.1645(4) 0.77799(19) 0.0377(11) Uani 1 1 d . . . H16 H 0.6188 0.1030 0.7738 0.045 Uiso 1 1 calc R . . C17 C 0.8711(10) 0.1941(3) 0.76418(18) 0.0354(10) Uani 1 1 d . . . C18 C 0.9345(8) 0.2856(3) 0.77087(17) 0.0314(9) Uani 1 1 d . . . C19 C 0.9159(8) 0.3977(3) 0.96990(17) 0.0298(9) Uani 1 1 d . . . C20 C 1.0492(8) 0.4205(3) 1.01229(17) 0.0315(9) Uani 1 1 d . . . H20 H 1.1875 0.4498 1.0078 0.038 Uiso 1 1 calc R . . C21 C 0.9708(10) 0.3983(4) 1.06196(18) 0.0404(11) Uani 1 1 d . . . C22 C 0.7618(10) 0.3567(4) 1.0682(2) 0.0428(12) Uani 1 1 d . . . C23 C 0.6317(10) 0.3344(4) 1.0250(2) 0.0388(11) Uani 1 1 d . . . H23 H 0.4921 0.3061 1.0294 0.08(2) Uiso 1 1 calc R . . C24 C 0.7081(8) 0.3540(4) 0.97533(19) 0.0343(10) Uani 1 1 d . . . H1 H 1.197(9) 0.661(4) 0.9453(19) 0.028(13) Uiso 1 1 d . . . H2 H 1.172(11) 0.695(4) 1.035(2) 0.048(17) Uiso 1 1 d . . . H3 H 0.849(9) 0.655(4) 1.0906(19) 0.030(13) Uiso 1 1 d . . . H4 H 0.521(9) 0.588(3) 1.0487(18) 0.025(12) Uiso 1 1 d . . . H7 H 1.019(9) 0.611(3) 0.8696(17) 0.021(11) Uiso 1 1 d . . . H11 H 0.389(12) 0.687(5) 0.838(2) 0.052(19) Uiso 1 1 d . . . H11A H 0.410(10) 0.574(4) 0.855(2) 0.040(16) Uiso 1 1 d . . . H12 H 0.673(9) 0.463(4) 0.8807(18) 0.023(12) Uiso 1 1 d . . . H14 H 0.448(9) 0.369(4) 0.8170(19) 0.028(13) Uiso 1 1 d . . . H15 H 0.348(14) 0.204(5) 0.809(3) 0.08(2) Uiso 1 1 d . . . H17 H 0.991(11) 0.149(4) 0.750(2) 0.039(15) Uiso 1 1 d . . . H18 H 1.099(12) 0.309(5) 0.762(3) 0.055(19) Uiso 1 1 d . . . H21 H 1.064(12) 0.413(5) 1.094(2) 0.055(19) Uiso 1 1 d . . . H22 H 0.702(10) 0.340(4) 1.106(2) 0.036(15) Uiso 1 1 d . . . H24 H 0.619(10) 0.335(4) 0.942(2) 0.041(15) Uiso 1 1 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 S1 0.0283(5) 0.0247(6) 0.0302(4) -0.0002(4) 0.0006(4) 0.0004(4) S2 0.0282(5) 0.0267(6) 0.0310(5) 0.0003(4) -0.0018(4) 0.0017(4) O1 0.045(2) 0.0255(18) 0.0429(18) 0.0038(13) 0.0014(15) 0.0071(16) O2 0.0389(19) 0.0307(19) 0.0469(19) 0.0003(14) -0.0021(15) -0.0067(16) O3 0.0284(15) 0.0271(17) 0.0365(15) -0.0051(12) 0.0055(11) -0.0030(13) O4 0.0374(17) 0.0297(19) 0.0316(15) 0.0018(12) -0.0003(12) 0.0028(14) O5 0.0275(15) 0.0317(18) 0.0346(15) 0.0040(13) 0.0000(11) -0.0005(14) O6 0.0400(18) 0.0256(17) 0.0329(15) -0.0020(11) -0.0055(13) 0.0054(14) C1 0.0257(19) 0.023(2) 0.040(2) 0.0023(16) -0.0013(16) 0.0014(18) C2 0.035(2) 0.026(3) 0.037(2) -0.0023(16) -0.0080(18) -0.0020(19) C3 0.038(2) 0.028(2) 0.031(2) -0.0050(16) -0.0050(17) 0.006(2) C4 0.032(2) 0.029(3) 0.036(2) -0.0011(16) 0.0016(16) 0.0082(19) C5 0.027(2) 0.028(2) 0.0310(18) -0.0013(16) -0.0002(14) 0.0018(17) C6 0.0219(18) 0.024(2) 0.0332(18) 0.0029(14) -0.0010(14) 0.0036(16) C7 0.027(2) 0.025(2) 0.0300(17) -0.0002(15) 0.0021(14) -0.0006(18) C8 0.032(2) 0.025(2) 0.0268(18) -0.0022(15) 0.0022(14) 0.0012(17) C9 0.036(2) 0.025(3) 0.032(2) -0.0002(16) 0.0021(16) 0.0042(19) C10 0.071(4) 0.025(3) 0.044(3) 0.007(2) 0.009(2) 0.009(3) C11 0.030(2) 0.037(3) 0.033(2) 0.0013(17) 0.0033(16) 0.006(2) C12 0.028(2) 0.025(2) 0.0308(19) 0.0017(15) -0.0010(14) 0.0049(17) C13 0.029(2) 0.027(2) 0.0307(19) 0.0018(15) -0.0041(15) -0.0014(18) C14 0.031(2) 0.027(3) 0.044(2) -0.0020(18) -0.0028(18) -0.0008(18) C15 0.035(3) 0.034(3) 0.046(3) 0.0016(19) -0.005(2) -0.006(2) C16 0.049(3) 0.025(3) 0.039(2) -0.0012(18) -0.008(2) -0.005(2) C17 0.046(3) 0.024(2) 0.036(2) -0.0054(16) -0.0037(19) 0.001(2) C18 0.033(2) 0.029(3) 0.032(2) -0.0022(16) -0.0019(16) 0.0017(18) C19 0.031(2) 0.024(2) 0.035(2) -0.0011(15) 0.0013(15) 0.0016(17) C20 0.033(2) 0.023(2) 0.039(2) 0.0007(16) -0.0043(16) 0.0010(19) C21 0.051(3) 0.037(3) 0.033(2) 0.0033(18) -0.005(2) -0.002(2) C22 0.054(3) 0.039(3) 0.035(2) 0.005(2) 0.004(2) -0.005(3) C23 0.041(3) 0.028(3) 0.047(3) 0.0050(19) 0.003(2) -0.003(2) C24 0.034(2) 0.027(3) 0.041(2) 0.0015(18) 0.0001(18) 0.001(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 S1 O4 1.436(3) . ? S1 O3 1.439(3) . ? S1 C13 1.768(5) . ? S1 C12 1.853(4) . ? S2 O6 1.437(3) . ? S2 O5 1.442(3) . ? S2 C19 1.773(5) . ? S2 C12 1.853(4) . ? O1 C9 1.344(6) . ? O1 C10 1.450(7) . ? O2 C9 1.221(6) . ? C1 C6 1.395(6) . ? C1 C2 1.401(6) . ? C1 H1 1.07(5) . ? C2 C3 1.382(7) . ? C2 H2 0.95(7) . ? C3 C4 1.400(7) . ? C3 H3 1.06(5) . ? C4 C5 1.401(6) . ? C4 H4 1.06(5) . ? C5 C6 1.406(6) . ? C5 H5 0.9300 . ? C6 C7 1.537(6) . ? C7 C8 1.534(6) . ? C7 C12 1.542(6) . ? C7 H7 1.04(5) . ? C8 C11 1.328(7) . ? C8 C9 1.496(7) . ? C10 H10 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C11 H11 0.94(7) . ? C11 H11A 1.01(6) . ? C12 H12 0.99(5) . ? C13 C18 1.393(7) . ? C13 C14 1.402(7) . ? C14 C15 1.394(7) . ? C14 H14 1.03(5) . ? C15 C16 1.399(8) . ? C15 H15 1.02(9) . ? C16 C17 1.373(8) . ? C16 H16 0.9300 . ? C17 C18 1.392(7) . ? C17 H17 1.04(6) . ? C18 H18 1.05(7) . ? C19 C20 1.387(6) . ? C19 C24 1.391(7) . ? C20 C21 1.397(7) . ? C20 H20 0.9300 . ? C21 C22 1.387(8) . ? C21 H21 1.02(6) . ? C22 C23 1.392(8) . ? C22 H22 1.06(6) . ? C23 C24 1.384(7) . ? C23 H23 0.9300 . ? C24 H24 1.05(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 O4 S1 O3 118.3(2) . . ? O4 S1 C13 108.3(2) . . ? O3 S1 C13 109.6(2) . . ? O4 S1 C12 107.5(2) . . ? O3 S1 C12 106.3(2) . . ? C13 S1 C12 106.0(2) . . ? O6 S2 O5 118.2(2) . . ? O6 S2 C19 106.7(2) . . ? O5 S2 C19 109.3(2) . . ? O6 S2 C12 107.7(2) . . ? O5 S2 C12 108.4(2) . . ? C19 S2 C12 105.9(2) . . ? C9 O1 C10 117.3(5) . . ? C6 C1 C2 120.3(4) . . ? C6 C1 H1 119(3) . . ? C2 C1 H1 120(3) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 H2 123(4) . . ? C1 C2 H2 116(4) . . ? C2 C3 C4 119.9(4) . . ? C2 C3 H3 121(3) . . ? C4 C3 H3 119(3) . . ? C3 C4 C5 119.8(4) . . ? C3 C4 H4 119(3) . . ? C5 C4 H4 121(3) . . ? C4 C5 C6 120.4(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C1 C6 C5 119.0(4) . . ? C1 C6 C7 120.9(4) . . ? C5 C6 C7 120.0(4) . . ? C8 C7 C6 106.8(3) . . ? C8 C7 C12 115.3(4) . . ? C6 C7 C12 111.6(4) . . ? C8 C7 H7 105(3) . . ? C6 C7 H7 108(3) . . ? C12 C7 H7 110(3) . . ? C11 C8 C9 120.8(5) . . ? C11 C8 C7 125.7(5) . . ? C9 C8 C7 113.4(4) . . ? O2 C9 O1 122.2(5) . . ? O2 C9 C8 124.6(4) . . ? O1 C9 C8 113.2(4) . . ? O1 C10 H10 109.5 . . ? O1 C10 H10A 109.5 . . ? H10 C10 H10A 109.5 . . ? O1 C10 H10B 109.5 . . ? H10 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C11 H11 115(4) . . ? C8 C11 H11A 122(3) . . ? H11 C11 H11A 122(5) . . ? C7 C12 S2 111.4(3) . . ? C7 C12 S1 111.5(3) . . ? S2 C12 S1 106.3(2) . . ? C7 C12 H12 115(3) . . ? S2 C12 H12 106(3) . . ? S1 C12 H12 106(3) . . ? C18 C13 C14 121.2(4) . . ? C18 C13 S1 118.7(4) . . ? C14 C13 S1 120.1(4) . . ? C15 C14 C13 117.8(5) . . ? C15 C14 H14 124(3) . . ? C13 C14 H14 118(3) . . ? C14 C15 C16 121.5(5) . . ? C14 C15 H15 120(4) . . ? C16 C15 H15 119(4) . . ? C17 C16 C15 119.3(5) . . ? C17 C16 H16 120.3 . . ? C15 C16 H16 120.3 . . ? C16 C17 C18 120.9(5) . . ? C16 C17 H17 121(3) . . ? C18 C17 H17 118(3) . . ? C17 C18 C13 119.3(5) . . ? C17 C18 H18 122(4) . . ? C13 C18 H18 119(4) . . ? C20 C19 C24 122.2(4) . . ? C20 C19 S2 118.5(4) . . ? C24 C19 S2 118.9(4) . . ? C19 C20 C21 118.4(5) . . ? C19 C20 H20 120.8 . . ? C21 C20 H20 120.8 . . ? C22 C21 C20 120.2(5) . . ? C22 C21 H21 118(4) . . ? C20 C21 H21 121(4) . . ? C21 C22 C23 120.1(5) . . ? C21 C22 H22 120(3) . . ? C23 C22 H22 120(3) . . ? C24 C23 C22 120.6(5) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C23 C24 C19 118.4(5) . . ? C23 C24 H24 123(3) . . ? C19 C24 H24 119(3) . . ? _diffrn_measured_fraction_theta_max 0.809 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 0.562 _refine_diff_density_min -0.767 _refine_diff_density_rms 0.116 #===END