# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name _publ_author_address 'J. Clayden' ; FIRST AUTHORS ADDRESS ; 'James Clayton' '' 'Madeleine Helliwell' '' 'Lluis Vallverdu' '' _publ_contact_author_name 'J. Clayden' _publ_contact_author_address ; School of Chemistry University of Manchester Oxford Road MANCHESTER M13 9PL UNITED KINGDOM ; _publ_contact_author_email J.P.CLAYDEN@MAN.AC.UK _publ_section_title ; Conformational switching between diastereoisomeric atropisomers of arenedicarboxamides induced by complexation with Lewis acids ; _publ_contact_author ; Madeleine Helliwell ; _publ_contact_author_fax ' ENTER FAX NUMBER ' _publ_contact_author_phone ' ENTER PHONE NUMBER ' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_coeditor_name ? data_s2456n _database_code_depnum_ccdc_archive 'CCDC 658995' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H34 I2 N2 O2' _chemical_formula_sum 'C26 H34 I2 N2 O2' _chemical_formula_weight 660.35 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 _symmetry_space_group_name_Hall P22ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 13.0880(10) _cell_length_b 13.5460(10) _cell_length_c 7.5320(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1335.35(18) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5908 _cell_measurement_theta_min 3.006 _cell_measurement_theta_max 28.1695 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 652 _exptl_absorpt_coefficient_mu 2.379 _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 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11386 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_sigmaI/netI 0.0380 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.27 _reflns_number_total 3165 _reflns_number_gt 2935 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR2004 (Burla et al, 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0420P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_ls_number_reflns 3165 _refine_ls_number_parameters 149 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _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 C1 C 0.4761(3) 0.0503(3) 0.1321(5) 0.0144(7) Uani 1 1 d . . . C2 C 0.5306(3) 0.1359(3) 0.1813(4) 0.0153(7) Uani 1 1 d . . . C3 C 0.4806(3) 0.2269(3) 0.1742(5) 0.0186(8) Uani 1 1 d . . . C4 C 0.3793(3) 0.2358(3) 0.1192(5) 0.0199(8) Uani 1 1 d . . . H4 H 0.3469 0.2986 0.1163 0.024 Uiso 1 1 calc R . . C5 C 0.3270(3) 0.1520(3) 0.0691(5) 0.0216(8) Uani 1 1 d . . . H5 H 0.2580 0.1568 0.0310 0.026 Uiso 1 1 calc R . . C6 C 0.3743(3) 0.0614(3) 0.0739(5) 0.0176(8) Uani 1 1 d . . . H6 H 0.3373 0.0046 0.0370 0.021 Uiso 1 1 calc R . . C7 C 0.6451(3) 0.1393(3) 0.2186(4) 0.0165(7) Uani 1 1 d . . . C8 C 0.7912(3) 0.1267(3) 0.4203(6) 0.0230(8) Uani 1 1 d . . . H8 H 0.8000 0.1089 0.5482 0.028 Uiso 1 1 calc R . . C9 C 0.8279(3) 0.2313(3) 0.4010(6) 0.0272(9) Uani 1 1 d . . . H9A H 0.8269 0.2500 0.2754 0.041 Uiso 1 1 calc R . . H9B H 0.8977 0.2366 0.4469 0.041 Uiso 1 1 calc R . . H9C H 0.7829 0.2754 0.4682 0.041 Uiso 1 1 calc R . . C10 C 0.8532(3) 0.0528(3) 0.3151(6) 0.0314(10) Uani 1 1 d . . . H10A H 0.8260 -0.0137 0.3347 0.047 Uiso 1 1 calc R . . H10B H 0.9247 0.0553 0.3538 0.047 Uiso 1 1 calc R . . H10C H 0.8492 0.0690 0.1884 0.047 Uiso 1 1 calc R . . C11 C 0.6121(3) 0.0901(3) 0.5297(5) 0.0196(8) Uani 1 1 d . . . H11 H 0.5411 0.0847 0.4814 0.023 Uiso 1 1 calc R . . C12 C 0.6105(3) 0.1694(3) 0.6723(6) 0.0286(10) Uani 1 1 d . . . H12A H 0.6771 0.1718 0.7315 0.043 Uiso 1 1 calc R . . H12B H 0.5573 0.1540 0.7596 0.043 Uiso 1 1 calc R . . H12C H 0.5960 0.2336 0.6176 0.043 Uiso 1 1 calc R . . C13 C 0.6414(3) -0.0114(3) 0.6021(6) 0.0306(10) Uani 1 1 d . . . H13A H 0.6294 -0.0616 0.5107 0.046 Uiso 1 1 calc R . . H13B H 0.5997 -0.0263 0.7069 0.046 Uiso 1 1 calc R . . H13C H 0.7138 -0.0114 0.6352 0.046 Uiso 1 1 calc R . . I1 I 0.553652(17) 0.360085(16) 0.24215(3) 0.02416(9) Uani 1 1 d . . . N1 N 0.6794(2) 0.1173(2) 0.3808(4) 0.0169(7) Uani 1 1 d . . . O1 O 0.7001(2) 0.16403(19) 0.0953(3) 0.0192(6) Uani 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 C1 0.0167(17) 0.0187(19) 0.0079(16) 0.0030(13) 0.0002(13) 0.0019(14) C2 0.0170(17) 0.0189(18) 0.0101(14) 0.0023(14) 0.0019(12) -0.0006(15) C3 0.0213(18) 0.0206(19) 0.0138(17) 0.0040(14) 0.0000(15) -0.0023(15) C4 0.0201(19) 0.0188(19) 0.0206(19) 0.0032(15) 0.0012(15) 0.0059(16) C5 0.0156(17) 0.027(2) 0.0227(19) 0.0033(16) -0.0020(15) -0.0002(17) C6 0.0197(18) 0.0188(19) 0.0143(18) 0.0009(14) -0.0018(14) -0.0017(15) C7 0.0172(15) 0.0128(15) 0.0196(18) -0.0030(16) 0.0001(13) 0.0009(14) C8 0.0191(18) 0.026(2) 0.0236(19) 0.0020(17) -0.0036(15) -0.0044(17) C9 0.023(2) 0.030(2) 0.029(2) 0.0035(17) -0.0045(18) -0.0073(18) C10 0.0186(19) 0.036(2) 0.040(2) -0.0001(19) -0.0040(17) 0.0097(19) C11 0.0181(18) 0.025(2) 0.0151(18) 0.0034(15) -0.0019(14) -0.0039(17) C12 0.029(2) 0.041(3) 0.0163(18) -0.0027(17) -0.0041(17) 0.0009(19) C13 0.031(3) 0.030(2) 0.030(2) 0.0145(19) -0.0055(19) -0.005(2) I1 0.02528(13) 0.01516(12) 0.03205(14) -0.00131(14) 0.00151(14) -0.00137(9) N1 0.0142(15) 0.0154(17) 0.0212(16) 0.0044(12) -0.0008(12) -0.0006(12) O1 0.0180(13) 0.0213(15) 0.0184(13) 0.0002(10) 0.0032(10) -0.0032(11) _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 C1 C2 1.411(5) . ? C1 C6 1.412(5) . ? C1 C1 1.499(7) 2_655 ? C2 C3 1.396(5) . ? C2 C7 1.525(5) . ? C3 C4 1.394(5) . ? C3 I1 2.106(4) . ? C4 C5 1.379(6) . ? C4 H4 0.9500 . ? C5 C6 1.375(5) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 O1 1.223(4) . ? C7 N1 1.335(4) . ? C8 N1 1.498(5) . ? C8 C9 1.503(6) . ? C8 C10 1.512(6) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N1 1.474(5) . ? C11 C12 1.519(6) . ? C11 C13 1.528(6) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? 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 C2 C1 C6 118.1(3) . . ? C2 C1 C1 122.5(4) . 2_655 ? C6 C1 C1 119.3(4) . 2_655 ? C3 C2 C1 118.6(3) . . ? C3 C2 C7 116.2(3) . . ? C1 C2 C7 124.7(3) . . ? C4 C3 C2 122.3(3) . . ? C4 C3 I1 115.4(3) . . ? C2 C3 I1 122.2(3) . . ? C5 C4 C3 118.8(4) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C6 C5 C4 120.3(3) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 121.9(3) . . ? C5 C6 H6 119.1 . . ? C1 C6 H6 119.1 . . ? O1 C7 N1 123.9(3) . . ? O1 C7 C2 116.5(3) . . ? N1 C7 C2 119.5(3) . . ? N1 C8 C9 111.9(3) . . ? N1 C8 C10 111.4(3) . . ? C9 C8 C10 113.7(4) . . ? N1 C8 H8 106.5 . . ? C9 C8 H8 106.5 . . ? C10 C8 H8 106.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 111.6(3) . . ? N1 C11 C13 110.3(3) . . ? C12 C11 C13 112.8(3) . . ? N1 C11 H11 107.3 . . ? C12 C11 H11 107.3 . . ? C13 C11 H11 107.3 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C7 N1 C11 123.4(3) . . ? C7 N1 C8 119.4(3) . . ? C11 N1 C8 117.1(3) . . ? 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 C6 C1 C2 C3 1.6(5) . . . . ? C1 C1 C2 C3 178.8(3) 2_655 . . . ? C6 C1 C2 C7 -169.8(3) . . . . ? C1 C1 C2 C7 7.4(4) 2_655 . . . ? C1 C2 C3 C4 -0.5(5) . . . . ? C7 C2 C3 C4 171.6(3) . . . . ? C1 C2 C3 I1 -179.5(3) . . . . ? C7 C2 C3 I1 -7.4(4) . . . . ? C2 C3 C4 C5 -0.4(6) . . . . ? I1 C3 C4 C5 178.7(3) . . . . ? C3 C4 C5 C6 0.1(6) . . . . ? C4 C5 C6 C1 1.0(6) . . . . ? C2 C1 C6 C5 -1.9(5) . . . . ? C1 C1 C6 C5 -179.2(3) 2_655 . . . ? C3 C2 C7 O1 -76.2(4) . . . . ? C1 C2 C7 O1 95.4(4) . . . . ? C3 C2 C7 N1 102.7(4) . . . . ? C1 C2 C7 N1 -85.7(4) . . . . ? O1 C7 N1 C11 178.3(3) . . . . ? C2 C7 N1 C11 -0.4(5) . . . . ? O1 C7 N1 C8 2.5(5) . . . . ? C2 C7 N1 C8 -176.3(3) . . . . ? C12 C11 N1 C7 -111.3(4) . . . . ? C13 C11 N1 C7 122.5(4) . . . . ? C12 C11 N1 C8 64.7(4) . . . . ? C13 C11 N1 C8 -61.6(4) . . . . ? C9 C8 N1 C7 62.5(5) . . . . ? C10 C8 N1 C7 -66.0(5) . . . . ? C9 C8 N1 C11 -113.6(4) . . . . ? C10 C8 N1 C11 117.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 1.518 _refine_diff_density_min -0.950 _refine_diff_density_rms 0.121 # Attachment 's2461_=_anti-2c.cif' data_s2461abs _database_code_depnum_ccdc_archive 'CCDC 658996' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _publ_section_exptl_refinement ; The structure was solved by the direct methods. All non-H atoms were refined anisotropically. H atoms were included in calculated positions. ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H34 I2 N2 O2' _chemical_formula_sum 'C26 H34 I2 N2 O2' _chemical_formula_weight 660.35 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' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall -P2yn 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 7.7369(6) _cell_length_b 19.5591(14) _cell_length_c 17.9914(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.4260(10) _cell_angle_gamma 90.00 _cell_volume 2668.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5733 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 26.32 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.644 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 2.381 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6474 _exptl_absorpt_correction_T_max 0.8324 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15228 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0337 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.40 _reflns_number_total 5440 _reflns_number_gt 4687 _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 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0463P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5440 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0754 _refine_ls_wR_factor_gt 0.0719 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.002 _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 0.72415(3) 0.705566(10) 0.821499(12) 0.02284(7) Uani 1 1 d . . . I2 I 1.29140(3) 1.105105(10) 0.744542(12) 0.02527(7) Uani 1 1 d . . . O1 O 1.1507(3) 0.81495(11) 0.85098(11) 0.0192(4) Uani 1 1 d . . . O2 O 0.8349(3) 1.06055(10) 0.72725(11) 0.0208(5) Uani 1 1 d . . . N1 N 1.0778(3) 0.79008(12) 0.96402(14) 0.0168(5) Uani 1 1 d . . . N2 N 0.9372(3) 0.96255(12) 0.68375(13) 0.0151(5) Uani 1 1 d . . . C1 C 0.7146(4) 0.81133(15) 0.84008(17) 0.0184(6) Uani 1 1 d . . . C2 C 0.8655(4) 0.85021(14) 0.86513(15) 0.0152(6) Uani 1 1 d . . . C3 C 0.8546(4) 0.92198(14) 0.85766(15) 0.0141(6) Uani 1 1 d . . . C4 C 0.6905(4) 0.95253(16) 0.83359(16) 0.0174(6) Uani 1 1 d . . . H4 H 0.6823 1.0009 0.8289 0.021 Uiso 1 1 calc R . . C5 C 0.5391(4) 0.91304(16) 0.81636(17) 0.0205(6) Uani 1 1 d . . . H5 H 0.4269 0.9345 0.8042 0.025 Uiso 1 1 calc R . . C6 C 0.5508(4) 0.84227(16) 0.81677(17) 0.0207(6) Uani 1 1 d . . . H6 H 0.4480 0.8152 0.8013 0.025 Uiso 1 1 calc R . . C7 C 1.0443(4) 0.81684(14) 0.89294(16) 0.0143(6) Uani 1 1 d . . . C8 C 0.9579(5) 0.79539(18) 1.01876(19) 0.0305(8) Uani 1 1 d . . . H8 H 0.8524 0.8225 0.9942 0.037 Uiso 1 1 calc R . . C9 C 1.0443(6) 0.83248(19) 1.0910(2) 0.0443(11) Uani 1 1 d . . . H9A H 1.1522 0.8083 1.1147 0.067 Uiso 1 1 calc R . . H9B H 0.9626 0.8337 1.1262 0.067 Uiso 1 1 calc R . . H9C H 1.0736 0.8793 1.0786 0.067 Uiso 1 1 calc R . . C10 C 0.8942(5) 0.7254(2) 1.0387(2) 0.0428(10) Uani 1 1 d . . . H10A H 0.8360 0.7021 0.9922 0.064 Uiso 1 1 calc R . . H10B H 0.8105 0.7309 1.0726 0.064 Uiso 1 1 calc R . . H10C H 0.9951 0.6982 1.0640 0.064 Uiso 1 1 calc R . . C11 C 1.2492(4) 0.75516(16) 0.99171(17) 0.0211(7) Uani 1 1 d . . . H11 H 1.2447 0.7372 1.0433 0.025 Uiso 1 1 calc R . . C12 C 1.2745(5) 0.69317(17) 0.9436(2) 0.0314(8) Uani 1 1 d . . . H12A H 1.1670 0.6653 0.9348 0.047 Uiso 1 1 calc R . . H12B H 1.3738 0.6658 0.9702 0.047 Uiso 1 1 calc R . . H12C H 1.2988 0.7085 0.8948 0.047 Uiso 1 1 calc R . . C13 C 1.4037(5) 0.8049(2) 1.0022(2) 0.0339(8) Uani 1 1 d . . . H13A H 1.4171 0.8225 0.9527 0.051 Uiso 1 1 calc R . . H13B H 1.5119 0.7812 1.0263 0.051 Uiso 1 1 calc R . . H13C H 1.3813 0.8430 1.0344 0.051 Uiso 1 1 calc R . . C14 C 1.0156(4) 0.96555(14) 0.87170(16) 0.0142(6) Uani 1 1 d . . . C15 C 1.0590(4) 1.00482(14) 0.81288(16) 0.0145(6) Uani 1 1 d . . . C16 C 1.2121(4) 1.04505(15) 0.82872(16) 0.0172(6) Uani 1 1 d . . . C17 C 1.3179(4) 1.04739(15) 0.90045(17) 0.0195(6) Uani 1 1 d . . . H17 H 1.4210 1.0750 0.9099 0.023 Uiso 1 1 calc R . . C18 C 1.2715(4) 1.00891(15) 0.95837(17) 0.0197(6) Uani 1 1 d . . . H18 H 1.3415 1.0109 1.0081 0.024 Uiso 1 1 calc R . . C19 C 1.1240(4) 0.96776(15) 0.94376(16) 0.0167(6) Uani 1 1 d . . . H19 H 1.0955 0.9404 0.9833 0.020 Uiso 1 1 calc R . . C20 C 0.9351(4) 1.01079(15) 0.73702(16) 0.0157(6) Uani 1 1 d . . . C21 C 1.0559(4) 0.90285(14) 0.69590(16) 0.0168(6) Uani 1 1 d . . . H21 H 1.1159 0.9028 0.7505 0.020 Uiso 1 1 calc R . . C22 C 1.1990(4) 0.90860(17) 0.64863(18) 0.0238(7) Uani 1 1 d . . . H22A H 1.1446 0.9070 0.5946 0.036 Uiso 1 1 calc R . . H22B H 1.2821 0.8705 0.6609 0.036 Uiso 1 1 calc R . . H22C H 1.2621 0.9520 0.6600 0.036 Uiso 1 1 calc R . . C23 C 0.9555(5) 0.83584(16) 0.68024(18) 0.0270(7) Uani 1 1 d . . . H23A H 0.8559 0.8358 0.7065 0.040 Uiso 1 1 calc R . . H23B H 1.0344 0.7976 0.6986 0.040 Uiso 1 1 calc R . . H23C H 0.9114 0.8309 0.6256 0.040 Uiso 1 1 calc R . . C24 C 0.8197(4) 0.96945(16) 0.60814(16) 0.0208(6) Uani 1 1 d . . . H24 H 0.8461 0.9298 0.5772 0.025 Uiso 1 1 calc R . . C25 C 0.6259(4) 0.9632(2) 0.61354(19) 0.0322(8) Uani 1 1 d . . . H25A H 0.6089 0.9216 0.6417 0.048 Uiso 1 1 calc R . . H25B H 0.5531 0.9607 0.5624 0.048 Uiso 1 1 calc R . . H25C H 0.5912 1.0031 0.6400 0.048 Uiso 1 1 calc R . . C26 C 0.8585(5) 1.03362(17) 0.56655(18) 0.0290(8) Uani 1 1 d . . . H26A H 0.8244 1.0740 0.5925 0.043 Uiso 1 1 calc R . . H26B H 0.7912 1.0325 0.5143 0.043 Uiso 1 1 calc R . . H26C H 0.9848 1.0357 0.5660 0.043 Uiso 1 1 calc R . . 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 0.02309(12) 0.01561(11) 0.03037(12) -0.00042(8) 0.00663(9) -0.00438(8) I2 0.02537(13) 0.02149(12) 0.03130(13) 0.00607(8) 0.01133(9) -0.00485(8) O1 0.0150(11) 0.0222(11) 0.0222(11) 0.0016(9) 0.0079(9) 0.0012(9) O2 0.0217(11) 0.0188(11) 0.0232(11) 0.0046(9) 0.0079(9) 0.0055(9) N1 0.0180(13) 0.0158(12) 0.0172(12) 0.0014(9) 0.0049(10) 0.0053(10) N2 0.0140(12) 0.0176(12) 0.0142(11) 0.0009(9) 0.0040(9) 0.0008(10) C1 0.0189(15) 0.0159(14) 0.0217(15) 0.0020(12) 0.0075(12) -0.0025(12) C2 0.0167(15) 0.0166(14) 0.0141(13) 0.0008(11) 0.0074(11) -0.0005(12) C3 0.0162(15) 0.0157(14) 0.0123(13) 0.0000(10) 0.0074(11) -0.0005(11) C4 0.0179(15) 0.0188(15) 0.0161(14) 0.0006(11) 0.0051(12) 0.0022(12) C5 0.0142(15) 0.0250(16) 0.0233(15) 0.0011(13) 0.0064(12) 0.0032(13) C6 0.0145(15) 0.0250(16) 0.0239(15) 0.0006(12) 0.0070(12) -0.0038(13) C7 0.0159(14) 0.0103(13) 0.0173(14) -0.0011(11) 0.0043(11) 0.0001(11) C8 0.0297(19) 0.039(2) 0.0268(17) 0.0163(14) 0.0165(15) 0.0176(16) C9 0.083(3) 0.0301(19) 0.0276(19) 0.0071(15) 0.030(2) 0.024(2) C10 0.033(2) 0.063(3) 0.035(2) 0.0186(19) 0.0113(17) -0.007(2) C11 0.0197(16) 0.0244(16) 0.0195(15) 0.0026(12) 0.0049(12) 0.0076(13) C12 0.038(2) 0.0270(17) 0.0305(18) 0.0019(14) 0.0097(16) 0.0157(16) C13 0.0200(18) 0.045(2) 0.0325(19) 0.0031(16) -0.0036(15) -0.0044(16) C14 0.0132(14) 0.0117(13) 0.0189(14) -0.0012(11) 0.0060(11) 0.0017(11) C15 0.0147(14) 0.0120(13) 0.0179(14) -0.0010(11) 0.0056(11) 0.0037(11) C16 0.0195(15) 0.0130(14) 0.0210(15) 0.0018(11) 0.0081(12) 0.0013(12) C17 0.0144(15) 0.0168(14) 0.0281(16) -0.0055(12) 0.0064(12) -0.0025(12) C18 0.0183(15) 0.0222(15) 0.0176(15) -0.0044(12) 0.0011(12) 0.0034(12) C19 0.0191(15) 0.0169(14) 0.0166(14) -0.0002(11) 0.0093(12) 0.0038(12) C20 0.0130(14) 0.0167(14) 0.0192(14) 0.0026(11) 0.0080(11) -0.0004(11) C21 0.0221(16) 0.0130(14) 0.0152(14) 0.0001(11) 0.0038(12) 0.0033(12) C22 0.0232(17) 0.0263(16) 0.0237(16) -0.0021(13) 0.0094(13) 0.0072(14) C23 0.043(2) 0.0169(15) 0.0201(16) -0.0016(12) 0.0051(14) -0.0038(15) C24 0.0205(16) 0.0269(16) 0.0145(14) -0.0013(12) 0.0026(12) 0.0029(13) C25 0.0183(17) 0.049(2) 0.0272(18) -0.0008(16) -0.0002(14) -0.0017(16) C26 0.038(2) 0.0292(18) 0.0199(16) 0.0060(13) 0.0075(14) 0.0105(15) _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 C1 2.099(3) . ? I2 C16 2.102(3) . ? O1 C7 1.223(4) . ? O2 C20 1.235(3) . ? N1 C7 1.358(4) . ? N1 C8 1.484(4) . ? N1 C11 1.488(4) . ? N2 C20 1.347(4) . ? N2 C21 1.475(4) . ? N2 C24 1.485(4) . ? C1 C2 1.391(4) . ? C1 C6 1.392(4) . ? C2 C3 1.411(4) . ? C2 C7 1.522(4) . ? C3 C4 1.392(4) . ? C3 C14 1.489(4) . ? C4 C5 1.386(4) . ? C4 H4 0.9500 . ? C5 C6 1.387(4) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C8 C10 1.521(5) . ? C8 C9 1.522(5) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.523(5) . ? C11 C12 1.525(4) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C19 1.398(4) . ? C14 C15 1.401(4) . ? C15 C16 1.404(4) . ? C15 C20 1.509(4) . ? C16 C17 1.385(4) . ? C17 C18 1.389(4) . ? C17 H17 0.9500 . ? C18 C19 1.379(4) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C21 C23 1.521(4) . ? C21 C22 1.528(4) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C26 1.521(5) . ? C24 C25 1.527(5) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 C7 N1 C8 124.8(2) . . ? C7 N1 C11 118.9(2) . . ? C8 N1 C11 116.3(2) . . ? C20 N2 C21 123.0(2) . . ? C20 N2 C24 119.8(2) . . ? C21 N2 C24 117.3(2) . . ? C2 C1 C6 121.0(3) . . ? C2 C1 I1 122.4(2) . . ? C6 C1 I1 116.0(2) . . ? C1 C2 C3 118.8(3) . . ? C1 C2 C7 121.5(3) . . ? C3 C2 C7 119.4(2) . . ? C4 C3 C2 119.3(3) . . ? C4 C3 C14 119.2(3) . . ? C2 C3 C14 121.4(3) . . ? C5 C4 C3 120.6(3) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.2(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C5 C6 C1 119.3(3) . . ? C5 C6 H6 120.3 . . ? C1 C6 H6 120.3 . . ? O1 C7 N1 122.9(3) . . ? O1 C7 C2 119.3(2) . . ? N1 C7 C2 117.8(2) . . ? N1 C8 C10 111.5(3) . . ? N1 C8 C9 111.9(3) . . ? C10 C8 C9 109.6(3) . . ? N1 C8 H8 107.9 . . ? C10 C8 H8 107.9 . . ? C9 C8 H8 107.9 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C13 112.0(3) . . ? N1 C11 C12 112.4(3) . . ? C13 C11 C12 113.1(3) . . ? N1 C11 H11 106.2 . . ? C13 C11 H11 106.2 . . ? C12 C11 H11 106.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C19 C14 C15 119.6(3) . . ? C19 C14 C3 120.2(3) . . ? C15 C14 C3 120.2(2) . . ? C14 C15 C16 118.2(3) . . ? C14 C15 C20 121.4(3) . . ? C16 C15 C20 120.0(2) . . ? C17 C16 C15 121.8(3) . . ? C17 C16 I2 116.7(2) . . ? C15 C16 I2 121.5(2) . . ? C16 C17 C18 119.2(3) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 120.0(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C14 121.1(3) . . ? C18 C19 H19 119.4 . . ? C14 C19 H19 119.4 . . ? O2 C20 N2 123.1(3) . . ? O2 C20 C15 117.3(3) . . ? N2 C20 C15 119.6(2) . . ? N2 C21 C23 112.0(3) . . ? N2 C21 C22 111.0(2) . . ? C23 C21 C22 111.1(3) . . ? N2 C21 H21 107.5 . . ? C23 C21 H21 107.5 . . ? C22 C21 H21 107.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N2 C24 C26 112.4(3) . . ? N2 C24 C25 111.4(3) . . ? C26 C24 C25 112.9(3) . . ? N2 C24 H24 106.5 . . ? C26 C24 H24 106.5 . . ? C25 C24 H24 106.5 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? 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 C6 C1 C2 C3 -7.9(4) . . . . ? I1 C1 C2 C3 163.8(2) . . . . ? C6 C1 C2 C7 178.2(3) . . . . ? I1 C1 C2 C7 -10.1(4) . . . . ? C1 C2 C3 C4 7.2(4) . . . . ? C7 C2 C3 C4 -178.8(3) . . . . ? C1 C2 C3 C14 -170.1(3) . . . . ? C7 C2 C3 C14 3.9(4) . . . . ? C2 C3 C4 C5 -0.6(4) . . . . ? C14 C3 C4 C5 176.7(3) . . . . ? C3 C4 C5 C6 -5.4(4) . . . . ? C4 C5 C6 C1 4.7(5) . . . . ? C2 C1 C6 C5 2.0(5) . . . . ? I1 C1 C6 C5 -170.2(2) . . . . ? C8 N1 C7 O1 175.6(3) . . . . ? C11 N1 C7 O1 -1.7(4) . . . . ? C8 N1 C7 C2 -4.7(4) . . . . ? C11 N1 C7 C2 178.0(2) . . . . ? C1 C2 C7 O1 101.8(3) . . . . ? C3 C2 C7 O1 -72.0(4) . . . . ? C1 C2 C7 N1 -77.9(4) . . . . ? C3 C2 C7 N1 108.2(3) . . . . ? C7 N1 C8 C10 117.1(3) . . . . ? C11 N1 C8 C10 -65.5(4) . . . . ? C7 N1 C8 C9 -119.6(3) . . . . ? C11 N1 C8 C9 57.7(3) . . . . ? C7 N1 C11 C13 67.5(3) . . . . ? C8 N1 C11 C13 -110.0(3) . . . . ? C7 N1 C11 C12 -61.2(4) . . . . ? C8 N1 C11 C12 121.3(3) . . . . ? C4 C3 C14 C19 119.6(3) . . . . ? C2 C3 C14 C19 -63.2(4) . . . . ? C4 C3 C14 C15 -60.2(4) . . . . ? C2 C3 C14 C15 117.1(3) . . . . ? C19 C14 C15 C16 0.3(4) . . . . ? C3 C14 C15 C16 -179.9(3) . . . . ? C19 C14 C15 C20 -172.5(3) . . . . ? C3 C14 C15 C20 7.3(4) . . . . ? C14 C15 C16 C17 -0.9(4) . . . . ? C20 C15 C16 C17 172.0(3) . . . . ? C14 C15 C16 I2 179.3(2) . . . . ? C20 C15 C16 I2 -7.8(4) . . . . ? C15 C16 C17 C18 0.0(4) . . . . ? I2 C16 C17 C18 179.8(2) . . . . ? C16 C17 C18 C19 1.5(4) . . . . ? C17 C18 C19 C14 -2.1(4) . . . . ? C15 C14 C19 C18 1.2(4) . . . . ? C3 C14 C19 C18 -178.6(3) . . . . ? C21 N2 C20 O2 -179.4(3) . . . . ? C24 N2 C20 O2 2.3(4) . . . . ? C21 N2 C20 C15 0.3(4) . . . . ? C24 N2 C20 C15 -178.0(3) . . . . ? C14 C15 C20 O2 94.8(3) . . . . ? C16 C15 C20 O2 -77.9(4) . . . . ? C14 C15 C20 N2 -84.9(3) . . . . ? C16 C15 C20 N2 102.4(3) . . . . ? C20 N2 C21 C23 125.7(3) . . . . ? C24 N2 C21 C23 -56.1(3) . . . . ? C20 N2 C21 C22 -109.5(3) . . . . ? C24 N2 C21 C22 68.7(3) . . . . ? C20 N2 C24 C26 61.3(4) . . . . ? C21 N2 C24 C26 -117.0(3) . . . . ? C20 N2 C24 C25 -66.6(4) . . . . ? C21 N2 C24 C25 115.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.574 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.117