# Electronic Supplementary Material (ESI) for Organic & Biomolecular Chemistry # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Org.Biomol.Chem. _journal_coden_cambridge 0177 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email lulingwu@zju.edu.cn _publ_contact_author_name 'Luling Wu' loop_ _publ_author_name 'Jianfeng Xu' 'Luling Wu' 'An Xian Huang' data_101110_jeff_086 _database_code_depnum_ccdc_archive 'CCDC 821931' #TrackingRef 'web_deposit_cif_file_0_jianfengxu_1302849326.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H21 I O Se' _chemical_formula_sum 'C25 H21 I O Se' _chemical_formula_weight 543.28 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' I I -0.4742 1.8119 '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' Se Se -0.0929 2.2259 '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 21/n' _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 16.1185(6) _cell_length_b 5.7251(2) _cell_length_c 24.3065(9) _cell_angle_alpha 90.00 _cell_angle_beta 106.365(4) _cell_angle_gamma 90.00 _cell_volume 2152.12(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3569 _cell_measurement_theta_min 2.7142 _cell_measurement_theta_max 29.3475 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.677 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 3.192 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.638 _exptl_absorpt_correction_T_max 0.727 _exptl_absorpt_process_details ; CrysAlis PRO (Oxford Diffraction, 2009) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3592 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9508 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_sigmaI/netI 0.0424 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.35 _reflns_number_total 3928 _reflns_number_gt 2996 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrysAlis PRO (Oxford Diffraction, 2009)' _computing_data_collection 'CrysAlis PRO' _computing_data_reduction 'CrysAlis PRO' _computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)' _computing_publication_material OLEX2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement '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^)+(0.0375P)^2^+1.5711P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3928 _refine_ls_number_parameters 262 _refine_ls_number_restraints 187 _refine_ls_R_factor_all 0.0564 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0921 _refine_ls_wR_factor_gt 0.0816 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _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 I1 I 0.26563(2) -0.14805(6) 0.141077(13) 0.05415(14) Uani 1 1 d . . . Se1 Se 0.39762(3) -0.07881(10) 0.36117(2) 0.05567(17) Uani 1 1 d . A . O1 O 0.4627(2) 0.3330(5) 0.13087(12) 0.0443(7) Uani 1 1 d . . . C1 C 0.3533(4) -0.0856(9) 0.0212(2) 0.0609(14) Uani 1 1 d . . . H1 H 0.3369 -0.1997 0.0433 0.073 Uiso 1 1 calc R . . C2 C 0.3422(4) -0.1243(10) -0.0365(2) 0.0753(17) Uani 1 1 d . . . H2 H 0.3180 -0.2641 -0.0530 0.090 Uiso 1 1 calc R . . C3 C 0.3661(4) 0.0391(11) -0.0695(2) 0.0707(16) Uani 1 1 d . . . H3 H 0.3582 0.0115 -0.1083 0.085 Uiso 1 1 calc R . . C4 C 0.4015(4) 0.2427(11) -0.0456(2) 0.0679(15) Uani 1 1 d . . . H4 H 0.4178 0.3556 -0.0680 0.081 Uiso 1 1 calc R . . C5 C 0.4132(3) 0.2824(10) 0.0119(2) 0.0587(14) Uani 1 1 d . . . H5 H 0.4385 0.4216 0.0280 0.070 Uiso 1 1 calc R . . C6 C 0.3885(3) 0.1209(8) 0.04622(19) 0.0434(11) Uani 1 1 d . . . C7 C 0.4003(3) 0.1675(8) 0.10705(18) 0.0431(11) Uani 1 1 d . . . C8 C 0.3647(3) 0.0945(8) 0.14801(18) 0.0422(11) Uani 1 1 d . . . C9 C 0.4061(3) 0.2142(8) 0.20053(18) 0.0410(10) Uani 1 1 d . . . C10 C 0.4661(3) 0.3542(8) 0.18812(18) 0.0421(10) Uani 1 1 d . . . C11 C 0.5317(3) 0.5162(8) 0.22102(18) 0.0436(11) Uani 1 1 d . . . C12 C 0.5525(3) 0.7204(8) 0.19670(19) 0.0457(11) Uani 1 1 d . . . H12 H 0.5231 0.7582 0.1590 0.055 Uiso 1 1 calc R . . C13 C 0.6159(3) 0.8659(8) 0.2278(2) 0.0495(12) Uani 1 1 d . . . H13 H 0.6290 1.0007 0.2106 0.059 Uiso 1 1 calc R . . C14 C 0.6614(3) 0.8185(8) 0.2845(2) 0.0492(12) Uani 1 1 d . . . C15 C 0.6392(3) 0.6192(8) 0.3084(2) 0.0562(13) Uani 1 1 d . . . H15 H 0.6678 0.5838 0.3464 0.067 Uiso 1 1 calc R . . C16 C 0.5756(3) 0.4698(8) 0.2777(2) 0.0522(12) Uani 1 1 d . . . H16 H 0.5622 0.3364 0.2953 0.063 Uiso 1 1 calc R . . C17 C 0.7318(4) 0.9770(10) 0.3177(3) 0.0737(16) Uani 1 1 d . . . H17B H 0.7277 0.9930 0.3562 0.111 Uiso 1 1 calc R . . H17A H 0.7257 1.1276 0.2997 0.111 Uiso 1 1 calc R . . H17C H 0.7870 0.9119 0.3186 0.111 Uiso 1 1 calc R . . C18 C 0.3856(3) 0.1912(8) 0.25650(18) 0.0455(11) Uani 1 1 d . . . H18A H 0.3234 0.1967 0.2499 0.055 Uiso 1 1 calc R . . H18B H 0.4105 0.3220 0.2809 0.055 Uiso 1 1 calc R . . C19 C 0.4204(3) -0.0366(8) 0.28700(18) 0.0502(12) Uani 1 1 d . . . H19B H 0.4824 -0.0420 0.2927 0.060 Uiso 1 1 calc R . . H19A H 0.3950 -0.1662 0.2623 0.060 Uiso 1 1 calc R . . C20 C 0.4995(3) 0.0567(8) 0.40975(19) 0.0557(12) Uani 1 1 d DU . . C21 C 0.4921(6) 0.2185(14) 0.4508(3) 0.072(2) Uani 0.514(4) 1 d PDU A 1 H21 H 0.4377 0.2683 0.4520 0.087 Uiso 0.514(4) 1 calc PRU A 1 C22 C 0.5658(5) 0.3060(19) 0.4900(5) 0.100(3) Uani 0.514(4) 1 d PDU A 1 H22 H 0.5612 0.4150 0.5174 0.120 Uiso 0.514(4) 1 calc PRU A 1 C23 C 0.6463(5) 0.2278(14) 0.4877(3) 0.122(3) Uani 1 1 d DU . . H23A H 0.6846 0.2837 0.5212 0.146 Uiso 0.486(4) 1 calc PRU A 2 H23 H 0.6943 0.2665 0.5178 0.146 Uiso 0.514(4) 1 calc PRU A 1 C24 C 0.6596(8) 0.095(2) 0.4430(5) 0.118(4) Uiso 0.514(4) 1 d PDU A 1 H24 H 0.7134 0.0719 0.4369 0.142 Uiso 0.514(4) 1 calc PRU A 1 C25 C 0.5829(4) 0.002(2) 0.4085(5) 0.087(3) Uani 0.514(4) 1 d PDU A 1 H25 H 0.5880 -0.1085 0.3817 0.104 Uiso 0.514(4) 1 calc PRU A 1 C24A C 0.6340(9) -0.0097(15) 0.4763(6) 0.118(4) Uiso 0.486(4) 1 d PDU A 2 H24A H 0.6786 -0.1109 0.4941 0.142 Uiso 0.486(4) 1 calc PRU A 2 C25A C 0.5592(7) -0.1056(18) 0.4401(5) 0.087(3) Uani 0.486(4) 1 d PDU A 2 H25A H 0.5498 -0.2658 0.4365 0.104 Uiso 0.486(4) 1 calc PRU A 2 C21A C 0.5203(7) 0.2922(10) 0.4099(5) 0.072(2) Uani 0.486(4) 1 d PDU A 2 H21A H 0.4820 0.3949 0.3858 0.087 Uiso 0.486(4) 1 calc PRU A 2 C22A C 0.5978(7) 0.3761(19) 0.4456(4) 0.100(3) Uani 0.486(4) 1 d PDU A 2 H22A H 0.6165 0.5269 0.4414 0.120 Uiso 0.486(4) 1 calc PRU 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 I1 0.0406(2) 0.0694(2) 0.0493(2) 0.00306(16) 0.00758(14) -0.00894(15) Se1 0.0526(3) 0.0695(4) 0.0452(3) 0.0077(2) 0.0144(2) -0.0068(3) O1 0.0467(19) 0.0488(18) 0.0359(16) -0.0006(14) 0.0090(14) -0.0050(15) C1 0.079(4) 0.057(3) 0.050(3) -0.006(3) 0.022(3) -0.011(3) C2 0.099(5) 0.068(4) 0.057(3) -0.019(3) 0.018(3) -0.025(3) C3 0.075(4) 0.096(4) 0.042(3) -0.015(3) 0.018(3) -0.014(3) C4 0.082(4) 0.082(4) 0.045(3) 0.002(3) 0.026(3) -0.022(3) C5 0.060(4) 0.067(3) 0.047(3) -0.005(3) 0.012(3) -0.014(3) C6 0.033(2) 0.053(3) 0.041(2) 0.001(2) 0.006(2) 0.002(2) C7 0.036(3) 0.050(3) 0.039(2) -0.001(2) 0.004(2) 0.001(2) C8 0.035(3) 0.051(3) 0.037(2) 0.003(2) 0.006(2) 0.001(2) C9 0.036(3) 0.046(3) 0.040(2) 0.000(2) 0.009(2) 0.008(2) C10 0.043(3) 0.046(3) 0.035(2) -0.001(2) 0.007(2) 0.006(2) C11 0.043(3) 0.046(3) 0.041(2) -0.003(2) 0.011(2) 0.005(2) C12 0.048(3) 0.050(3) 0.041(2) -0.002(2) 0.015(2) 0.003(2) C13 0.054(3) 0.044(3) 0.056(3) -0.003(2) 0.025(3) -0.001(2) C14 0.044(3) 0.047(3) 0.053(3) -0.009(2) 0.007(2) -0.003(2) C15 0.060(3) 0.051(3) 0.044(3) 0.000(2) -0.007(2) 0.001(3) C16 0.054(3) 0.048(3) 0.049(3) 0.005(2) 0.005(2) -0.006(2) C17 0.064(4) 0.065(3) 0.082(4) -0.003(3) 0.003(3) -0.014(3) C18 0.043(3) 0.055(3) 0.039(2) -0.003(2) 0.011(2) 0.002(2) C19 0.054(3) 0.056(3) 0.040(2) -0.001(2) 0.011(2) 0.005(2) C20 0.055(3) 0.069(3) 0.040(2) 0.008(2) 0.008(2) 0.003(2) C21 0.079(5) 0.067(4) 0.064(5) -0.007(4) 0.009(4) -0.003(4) C22 0.113(6) 0.103(7) 0.071(5) -0.006(5) 0.006(5) -0.034(5) C23 0.075(4) 0.159(7) 0.111(5) 0.009(5) -0.007(4) -0.046(5) C25 0.067(5) 0.099(6) 0.087(6) 0.000(4) 0.010(4) 0.012(4) C25A 0.067(5) 0.099(6) 0.087(6) 0.000(4) 0.010(4) 0.012(4) C21A 0.079(5) 0.067(4) 0.064(5) -0.007(4) 0.009(4) -0.003(4) C22A 0.113(6) 0.103(7) 0.071(5) -0.006(5) 0.006(5) -0.034(5) _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 I1 C8 2.087(4) . ? Se1 C20 1.897(5) . ? Se1 C19 1.954(4) . ? O1 C10 1.382(5) . ? O1 C7 1.384(5) . ? C1 C6 1.376(6) . ? C1 C2 1.383(7) . ? C1 H1 0.9300 . ? C2 C3 1.356(8) . ? C2 H2 0.9300 . ? C3 C4 1.355(8) . ? C3 H3 0.9300 . ? C4 C5 1.376(7) . ? C4 H4 0.9300 . ? C5 C6 1.377(6) . ? C5 H5 0.9300 . ? C6 C7 1.461(6) . ? C7 C8 1.348(6) . ? C8 C9 1.437(6) . ? C9 C10 1.354(6) . ? C9 C18 1.494(6) . ? C10 C11 1.463(6) . ? C11 C16 1.387(6) . ? C11 C12 1.393(6) . ? C12 C13 1.369(6) . ? C12 H12 0.9300 . ? C13 C14 1.392(7) . ? C13 H13 0.9300 . ? C14 C15 1.373(7) . ? C14 C17 1.499(7) . ? C15 C16 1.381(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 H17B 0.9600 . ? C17 H17A 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.527(6) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 H19B 0.9700 . ? C19 H19A 0.9700 . ? C20 C21A 1.3892(10) . ? C20 C25 1.3893(10) . ? C20 C25A 1.3904(10) . ? C20 C21 1.3907(10) . ? C21 C22 1.3902(10) . ? C21 H21 0.9300 . ? C22 C23 1.3905(10) . ? C22 H22 0.9300 . ? C23 C24 1.3888(10) . ? C23 C22A 1.3891(10) . ? C23 C24A 1.3905(10) . ? C23 H23A 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.3897(10) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C24A C25A 1.3903(10) . ? C24A H24A 0.9300 . ? C25A H25A 0.9300 . ? C21A C22A 1.3895(10) . ? C21A H21A 0.9300 . ? C22A H22A 0.9300 . ? 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 C20 Se1 C19 99.7(2) . . ? C10 O1 C7 107.5(3) . . ? C6 C1 C2 120.3(5) . . ? C6 C1 H1 119.8 . . ? C2 C1 H1 119.8 . . ? C3 C2 C1 120.8(5) . . ? C3 C2 H2 119.6 . . ? C1 C2 H2 119.6 . . ? C4 C3 C2 119.7(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 119.9(5) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 121.6(5) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C1 C6 C5 117.6(4) . . ? C1 C6 C7 121.6(4) . . ? C5 C6 C7 120.8(4) . . ? C8 C7 O1 108.2(4) . . ? C8 C7 C6 136.8(4) . . ? O1 C7 C6 114.9(4) . . ? C7 C8 C9 108.7(4) . . ? C7 C8 I1 128.5(3) . . ? C9 C8 I1 122.8(3) . . ? C10 C9 C8 105.4(4) . . ? C10 C9 C18 127.6(4) . . ? C8 C9 C18 126.9(4) . . ? C9 C10 O1 110.1(4) . . ? C9 C10 C11 134.8(4) . . ? O1 C10 C11 115.1(4) . . ? C16 C11 C12 117.8(4) . . ? C16 C11 C10 120.6(4) . . ? C12 C11 C10 121.5(4) . . ? C13 C12 C11 120.5(4) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 122.1(4) . . ? C12 C13 H13 118.9 . . ? C14 C13 H13 118.9 . . ? C15 C14 C13 116.9(4) . . ? C15 C14 C17 121.5(5) . . ? C13 C14 C17 121.5(5) . . ? C14 C15 C16 121.9(5) . . ? C14 C15 H15 119.0 . . ? C16 C15 H15 119.0 . . ? C15 C16 C11 120.7(5) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? C14 C17 H17B 109.5 . . ? C14 C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? C14 C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? C9 C18 C19 111.8(4) . . ? C9 C18 H18A 109.2 . . ? C19 C18 H18A 109.2 . . ? C9 C18 H18B 109.2 . . ? C19 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? C18 C19 Se1 114.5(3) . . ? C18 C19 H19B 108.6 . . ? Se1 C19 H19B 108.6 . . ? C18 C19 H19A 108.6 . . ? Se1 C19 H19A 108.6 . . ? H19B C19 H19A 107.6 . . ? C21A C20 C25 89.0(8) . . ? C21A C20 C25A 121.1(8) . . ? C25 C20 C25A 48.1(7) . . ? C21A C20 C21 54.7(6) . . ? C25 C20 C21 116.4(8) . . ? C25A C20 C21 104.5(7) . . ? C21A C20 Se1 124.4(5) . . ? C25 C20 Se1 124.6(6) . . ? C25A C20 Se1 113.9(6) . . ? C21 C20 Se1 119.0(5) . . ? C22 C21 C20 120.2(9) . . ? C22 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? C21 C22 C23 118.9(9) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22A 86.4(10) . . ? C24 C23 C22 124.0(9) . . ? C22A C23 C22 59.6(8) . . ? C24 C23 C24A 49.9(9) . . ? C22A C23 C24A 115.6(10) . . ? C22 C23 C24A 103.9(9) . . ? C24 C23 H23A 131.6 . . ? C22A C23 H23A 122.2 . . ? C22 C23 H23A 104.4 . . ? C24A C23 H23A 122.2 . . ? C24 C23 H23 118.0 . . ? C22A C23 H23 127.3 . . ? C22 C23 H23 118.0 . . ? C24A C23 H23 115.5 . . ? H23A C23 H23 13.6 . . ? C23 C24 C25 112.0(11) . . ? C23 C24 H24 124.0 . . ? C25 C24 H24 124.0 . . ? C20 C25 C24 127.1(11) . . ? C20 C25 H25 116.5 . . ? C24 C25 H25 116.5 . . ? C25A C24A C23 124.2(12) . . ? C25A C24A H24A 117.9 . . ? C23 C24A H24A 117.9 . . ? C24A C25A C20 114.8(11) . . ? C24A C25A H25A 122.6 . . ? C20 C25A H25A 122.6 . . ? C20 C21A C22A 120.7(9) . . ? C20 C21A H21A 119.6 . . ? C22A C21A H21A 119.6 . . ? C23 C22A C21A 118.0(9) . . ? C23 C22A H22A 121.0 . . ? C21A C22A H22A 121.0 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.732 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.084