# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2002 _database_code_CSD 181904 _journal_coden_Cambridge 182 loop_ _publ_author_name _publ_author_address 'Ian R. Cooper' ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Ronald E. Grigg' ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; 'William S. Maclachlan' ; GlaxoSmithKline New Frontiers Science Park (North) Third Avenue Harlow CM19 5AW UK ; 'Mark Thornton-Pett' ; Department of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Visuvanathar Sridharan' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; # 1. SUBMISSION DETAILS _publ_contact_author_name 'Prof Ronald Grigg' _publ_contact_author_address ; School of Chemistry University of Leeds Woodhouse Lane Leeds West Yorkshire LS2 9JT UNITED KINGDOM ; _publ_contact_author_phone '+44 (0)113 2336423' _publ_contact_author_fax '+44 (0)113 2336565' _publ_contact_author_email marktp@chem.leeds.ac.uk _publ_requested_journal 'J Chem Soc., Chem. Commun.' _publ_contact_letter ; The following set of data is supplementary data for the the crystal structure included in the paper, details of which are given below ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; 3-component palladium-indium mediated cascade allylation of imines with allenes and aryl iodides ; #================================================================= _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H27 N O3 S' _chemical_formula_weight 385.51 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 0 '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' O O 0.0106 0.006 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 6.2460(1) _cell_length_b 16.5619(3) _cell_length_c 20.0492(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2079.98(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.177 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9106 _exptl_absorpt_correction_T_max 0.9825 _exptl_absorpt_process_details ; Using multiple and symmetry-related data measurements via the program SORTAV See R.H. Blessing, Acta Cryst (1995), A51, 33-38 ; _exptl_special_details ; PLEASE NOTE cell_measurement_ fields are not relevant to area detector data, the entire data set is used to refine the cell, which is indexed from all observed reflections in a 15 degree phi range. ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD area detector diffractometer' _diffrn_measurement_method ; Detector set at 30mm from sample with different 2theta offsets 1 degree phi exposures for chi=0 degree settings 1 degree omega exposures for chi=90 degree settings ; _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14791 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0454 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4073 _reflns_number_gt 3667 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ; ORTEP3 for Windows (Farrugia, 1997) XSeed (Barbour, 2001) ; _computing_publication_material 'WC (Thornton-Pett, 2000)' _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^)+(0.0375P)^2^+0.3392P] 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 0.0090(18) _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 0.05(6) _refine_ls_number_reflns 4073 _refine_ls_number_parameters 353 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 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 S3 S 0.60991(7) 0.87320(3) 0.82953(2) 0.03003(14) Uani 1 1 d . . . O240 O 0.9040(2) 1.00696(9) 0.51201(6) 0.0342(3) Uani 1 1 d . . . O3 O 0.3765(2) 0.88193(9) 0.84082(8) 0.0444(4) Uani 1 1 d . . . O241 O 1.2354(2) 1.01200(10) 0.55469(6) 0.0356(3) Uani 1 1 d . . . C21 C 0.8023(3) 1.01833(11) 0.76133(8) 0.0238(4) Uani 1 1 d . . . C240 C 1.0224(3) 1.01011(11) 0.55983(9) 0.0275(4) Uani 1 1 d . . . C1 C 0.7248(3) 1.02609(11) 0.83286(9) 0.0258(4) Uani 1 1 d . . . H1 H 0.583(3) 1.0436(11) 0.8330(8) 0.018(4) Uiso 1 1 d . . . C22 C 0.6749(3) 1.04559(12) 0.70926(9) 0.0253(4) Uani 1 1 d . . . H22 H 0.533(3) 1.0674(11) 0.7188(8) 0.019(4) Uiso 1 1 d . . . N2 N 0.7431(3) 0.94750(10) 0.86809(8) 0.0265(4) Uani 1 1 d . . . H2 H 0.709(3) 0.9495(12) 0.9087(10) 0.022(5) Uiso 1 1 d . . . C26 C 1.0041(3) 0.98693(12) 0.74724(9) 0.0281(4) Uani 1 1 d . . . H26 H 1.093(4) 0.9674(12) 0.7823(10) 0.035(5) Uiso 1 1 d . . . C23 C 0.7469(3) 1.04168(11) 0.64408(9) 0.0258(4) Uani 1 1 d . . . H23 H 0.659(3) 1.0614(13) 0.6097(10) 0.036(6) Uiso 1 1 d . . . C24 C 0.9501(3) 1.01276(11) 0.63039(8) 0.0248(4) Uani 1 1 d . . . C25 C 1.0793(3) 0.98532(12) 0.68240(9) 0.0280(4) Uani 1 1 d . . . H25 H 1.225(3) 0.9614(12) 0.6721(10) 0.029(5) Uiso 1 1 d . . . C4 C 0.6990(3) 0.78838(13) 0.88221(10) 0.0303(4) Uani 1 1 d . . . C6 C 0.5854(4) 0.71565(15) 0.85164(14) 0.0454(6) Uani 1 1 d . . . H6A H 0.627(4) 0.6664(17) 0.8770(12) 0.057(7) Uiso 1 1 d . . . H6B H 0.435(4) 0.7219(15) 0.8587(12) 0.053(7) Uiso 1 1 d . . . H6C H 0.625(5) 0.7128(16) 0.8008(14) 0.068(8) Uiso 1 1 d . . . C11 C 0.8608(3) 1.08804(12) 0.87082(9) 0.0292(4) Uani 1 1 d . . . H11B H 1.012(3) 1.0751(12) 0.8664(9) 0.023(5) Uiso 1 1 d . . . H11A H 0.829(3) 1.0827(11) 0.9173(10) 0.023(5) Uiso 1 1 d . . . C242 C 1.3213(4) 1.00574(19) 0.48780(11) 0.0436(6) Uani 1 1 d . . . H242A H 1.264(5) 1.048(2) 0.4601(15) 0.075(10) Uiso 1 1 d . . . H242B H 1.275(4) 0.9492(15) 0.4706(11) 0.044(6) Uiso 1 1 d . . . H242C H 1.469(5) 1.0113(15) 0.4921(11) 0.051(7) Uiso 1 1 d . . . C5 C 0.9395(3) 0.78002(15) 0.87470(11) 0.0352(5) Uani 1 1 d . . . H5A H 0.985(3) 0.7291(14) 0.8952(10) 0.031(5) Uiso 1 1 d . . . H5B H 1.012(4) 0.8246(16) 0.8930(11) 0.043(6) Uiso 1 1 d . . . H5C H 0.976(4) 0.7770(14) 0.8283(12) 0.048(6) Uiso 1 1 d . . . C14 C 0.5079(4) 1.19020(14) 0.92236(10) 0.0402(5) Uani 1 1 d . . . H14 H 0.549(4) 1.1402(15) 0.9443(12) 0.052(7) Uiso 1 1 d . . . C13 C 0.6318(4) 1.21680(12) 0.86819(9) 0.0344(4) Uani 1 1 d . . . C12 C 0.8266(4) 1.17349(13) 0.84682(9) 0.0356(5) Uani 1 1 d . . . C7 C 0.6332(4) 0.80104(15) 0.95440(11) 0.0413(5) Uani 1 1 d . . . H7A H 0.482(5) 0.8176(16) 0.9583(12) 0.061(8) Uiso 1 1 d . . . H7B H 0.642(4) 0.7489(16) 0.9799(11) 0.052(7) Uiso 1 1 d . . . H7C H 0.712(4) 0.8486(17) 0.9769(13) 0.057(7) Uiso 1 1 d . . . C15 C 0.3367(4) 1.23402(15) 0.94589(12) 0.0494(6) Uani 1 1 d . . . H15 H 0.258(4) 1.2162(15) 0.9861(13) 0.055(7) Uiso 1 1 d . . . C16 C 0.2828(5) 1.30560(17) 0.91462(14) 0.0606(8) Uani 1 1 d . . . H16 H 0.178(5) 1.339(2) 0.9315(15) 0.079(9) Uiso 1 1 d . . . C17 C 0.3928(5) 1.33050(16) 0.85888(14) 0.0622(7) Uani 1 1 d . . . H17 H 0.342(5) 1.3775(18) 0.8322(14) 0.072(8) Uiso 1 1 d . . . C18 C 0.5656(4) 1.28709(14) 0.83610(12) 0.0489(6) Uani 1 1 d . . . H18 H 0.645(4) 1.3023(15) 0.7947(11) 0.049(7) Uiso 1 1 d . . . C120 C 0.9762(5) 1.20790(18) 0.80911(13) 0.0546(6) Uani 1 1 d . . . H120A H 1.108(5) 1.1774(16) 0.7945(12) 0.061(8) Uiso 1 1 d . . . H120B H 0.971(5) 1.266(2) 0.7942(15) 0.089(10) 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 S3 0.0277(2) 0.0321(3) 0.0302(2) 0.0052(2) -0.00606(19) -0.0057(2) O240 0.0343(7) 0.0467(9) 0.0215(6) -0.0009(6) -0.0019(6) -0.0019(7) O3 0.0252(7) 0.0430(9) 0.0649(10) 0.0137(7) -0.0107(7) -0.0052(7) O241 0.0278(7) 0.0537(9) 0.0254(7) -0.0037(7) 0.0046(5) -0.0003(7) C21 0.0257(10) 0.0249(10) 0.0210(9) 0.0028(7) -0.0006(7) -0.0025(7) C240 0.0299(9) 0.0272(10) 0.0254(9) -0.0009(8) -0.0002(8) -0.0003(8) C1 0.0245(10) 0.0303(10) 0.0225(9) 0.0023(8) 0.0002(7) 0.0001(7) C22 0.0242(10) 0.0266(10) 0.0251(9) 0.0014(7) -0.0021(7) 0.0025(8) N2 0.0290(8) 0.0323(9) 0.0182(8) 0.0043(7) 0.0002(6) -0.0026(7) C26 0.0241(9) 0.0357(11) 0.0245(9) 0.0045(8) -0.0057(7) 0.0014(9) C23 0.0279(9) 0.0269(10) 0.0226(9) 0.0013(8) -0.0045(8) 0.0038(8) C24 0.0272(9) 0.0246(10) 0.0227(9) 0.0001(8) -0.0004(7) -0.0021(7) C25 0.0233(10) 0.0326(10) 0.0281(9) 0.0020(8) -0.0004(7) 0.0011(8) C4 0.0247(9) 0.0308(11) 0.0353(10) 0.0047(9) -0.0021(8) -0.0020(8) C6 0.0411(13) 0.0336(13) 0.0616(15) 0.0060(11) -0.0091(11) -0.0074(10) C11 0.0316(11) 0.0351(11) 0.0210(9) 0.0009(8) -0.0015(8) -0.0038(9) C242 0.0341(12) 0.0658(18) 0.0310(11) -0.0078(11) 0.0088(9) -0.0039(12) C5 0.0312(11) 0.0384(13) 0.0360(12) 0.0034(10) 0.0022(8) 0.0019(9) C14 0.0512(13) 0.0370(12) 0.0322(11) 0.0035(9) 0.0002(9) 0.0037(11) C13 0.0496(12) 0.0270(10) 0.0266(10) -0.0029(8) -0.0059(9) -0.0041(9) C12 0.0472(12) 0.0352(12) 0.0245(10) 0.0009(8) -0.0016(8) -0.0081(9) C7 0.0438(14) 0.0412(13) 0.0390(11) 0.0152(10) 0.0105(10) 0.0074(11) C15 0.0617(16) 0.0467(14) 0.0397(13) 0.0001(11) 0.0058(11) 0.0072(12) C16 0.078(2) 0.0423(15) 0.0611(17) -0.0032(13) 0.0089(14) 0.0201(14) C17 0.0865(19) 0.0365(14) 0.0637(16) 0.0094(12) 0.0119(16) 0.0153(15) C18 0.0675(16) 0.0359(12) 0.0433(13) 0.0064(10) 0.0041(11) -0.0021(11) C120 0.0651(17) 0.0465(15) 0.0522(15) 0.0115(12) 0.0129(12) -0.0041(13) _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 S3 O3 1.4867(15) . ? S3 N2 1.6757(16) . ? S3 C4 1.844(2) . ? O240 C240 1.213(2) . ? O241 C240 1.339(2) . ? O241 C242 1.449(2) . ? C21 C22 1.389(2) . ? C21 C26 1.396(3) . ? C21 C1 1.520(2) . ? C240 C24 1.486(2) . ? C1 N2 1.485(2) . ? C1 C11 1.535(3) . ? C1 H1 0.932(19) . ? C22 C23 1.384(3) . ? C22 H22 0.978(19) . ? N2 H2 0.84(2) . ? C26 C25 1.383(3) . ? C26 H26 0.95(2) . ? C23 C24 1.388(3) . ? C23 H23 0.94(2) . ? C24 C25 1.396(2) . ? C25 H25 1.02(2) . ? C4 C7 1.520(3) . ? C4 C5 1.520(3) . ? C4 C6 1.527(3) . ? C6 H6A 1.00(3) . ? C6 H6B 0.96(3) . ? C6 H6C 1.05(3) . ? C11 C12 1.510(3) . ? C11 H11B 0.97(2) . ? C11 H11A 0.958(19) . ? C242 H242A 0.96(3) . ? C242 H242B 1.04(3) . ? C242 H242C 0.94(3) . ? C5 H5A 0.98(2) . ? C5 H5B 0.94(3) . ? C5 H5C 0.96(2) . ? C14 C15 1.378(3) . ? C14 C13 1.405(3) . ? C14 H14 0.97(3) . ? C13 C18 1.393(3) . ? C13 C12 1.479(3) . ? C12 C120 1.332(3) . ? C7 H7A 0.99(3) . ? C7 H7B 1.01(3) . ? C7 H7C 1.03(3) . ? C15 C16 1.383(4) . ? C15 H15 0.99(3) . ? C16 C17 1.376(4) . ? C16 H16 0.92(3) . ? C17 C18 1.378(4) . ? C17 H17 1.00(3) . ? C18 H18 1.00(2) . ? C120 H120A 1.01(3) . ? C120 H120B 1.00(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 O3 S3 N2 110.37(9) . . ? O3 S3 C4 106.53(8) . . ? N2 S3 C4 98.31(8) . . ? C240 O241 C242 116.07(16) . . ? C22 C21 C26 119.30(16) . . ? C22 C21 C1 119.87(16) . . ? C26 C21 C1 120.78(16) . . ? O240 C240 O241 123.35(17) . . ? O240 C240 C24 124.56(17) . . ? O241 C240 C24 112.10(15) . . ? N2 C1 C21 110.48(15) . . ? N2 C1 C11 107.88(14) . . ? C21 C1 C11 110.31(15) . . ? N2 C1 H1 110.2(11) . . ? C21 C1 H1 109.4(11) . . ? C11 C1 H1 108.6(11) . . ? C23 C22 C21 120.46(17) . . ? C23 C22 H22 119.9(10) . . ? C21 C22 H22 119.6(10) . . ? C1 N2 S3 112.69(12) . . ? C1 N2 H2 113.9(14) . . ? S3 N2 H2 110.4(14) . . ? C25 C26 C21 120.38(16) . . ? C25 C26 H26 119.2(13) . . ? C21 C26 H26 120.4(13) . . ? C22 C23 C24 120.13(17) . . ? C22 C23 H23 119.1(13) . . ? C24 C23 H23 120.7(13) . . ? C23 C24 C25 119.76(16) . . ? C23 C24 C240 118.55(16) . . ? C25 C24 C240 121.67(16) . . ? C26 C25 C24 119.91(17) . . ? C26 C25 H25 120.3(12) . . ? C24 C25 H25 119.7(12) . . ? C7 C4 C5 112.07(18) . . ? C7 C4 C6 111.38(19) . . ? C5 C4 C6 110.50(19) . . ? C7 C4 S3 111.00(15) . . ? C5 C4 S3 108.21(14) . . ? C6 C4 S3 103.30(14) . . ? C4 C6 H6A 108.5(15) . . ? C4 C6 H6B 108.2(15) . . ? H6A C6 H6B 106(2) . . ? C4 C6 H6C 108.4(16) . . ? H6A C6 H6C 113(2) . . ? H6B C6 H6C 112(2) . . ? C12 C11 C1 112.93(16) . . ? C12 C11 H11B 108.3(12) . . ? C1 C11 H11B 110.3(11) . . ? C12 C11 H11A 111.6(11) . . ? C1 C11 H11A 107.7(12) . . ? H11B C11 H11A 105.8(15) . . ? O241 C242 H242 110.0(18) . . ? O241 C242 H242 105.5(13) . . ? H242 C242 H242 111(2) . . ? O241 C242 H242 105.9(15) . . ? H242 C242 H242 111(2) . . ? H242 C242 H242 113(2) . . ? C4 C5 H5A 109.1(13) . . ? C4 C5 H5B 111.7(15) . . ? H5A C5 H5B 111.5(19) . . ? C4 C5 H5C 109.6(14) . . ? H5A C5 H5C 107.0(19) . . ? H5B C5 H5C 108(2) . . ? C15 C14 C13 121.9(2) . . ? C15 C14 H14 120.1(15) . . ? C13 C14 H14 118.0(14) . . ? C18 C13 C14 117.0(2) . . ? C18 C13 C12 121.12(19) . . ? C14 C13 C12 121.82(18) . . ? C120 C12 C13 122.5(2) . . ? C120 C12 C11 118.8(2) . . ? C13 C12 C11 118.63(18) . . ? C4 C7 H7A 111.9(14) . . ? C4 C7 H7B 110.6(13) . . ? H7A C7 H7B 105(2) . . ? C4 C7 H7C 113.1(15) . . ? H7A C7 H7C 102(2) . . ? H7B C7 H7C 113.9(19) . . ? C14 C15 C16 119.1(2) . . ? C14 C15 H15 120.5(15) . . ? C16 C15 H15 120.3(15) . . ? C17 C16 C15 120.2(3) . . ? C17 C16 H16 119(2) . . ? C15 C16 H16 121(2) . . ? C16 C17 C18 120.4(3) . . ? C16 C17 H17 120.9(17) . . ? C18 C17 H17 118.5(17) . . ? C17 C18 C13 121.1(2) . . ? C17 C18 H18 122.4(14) . . ? C13 C18 H18 116.4(15) . . ? C12 C120 H120 121.7(15) . . ? C12 C120 H120 123.8(19) . . ? H120 C120 H120 115(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.202 _refine_diff_density_min -0.21 _refine_diff_density_rms 0.035