# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'Asa Sjoholm' ; Organic Chemistry Royal Institute of Technology 100 44 Stockholm Sweden ; 'Andreas Fischer' ; Inorganic Chemistry Royal Institute of Technology 100 44 Stockholm Sweden ; 'Peter Somfai' ; Organic Chemistry Royal Institute of Technology 100 44 Stockholm Sweden ; _publ_contact_author_address ; Organic Chemistry Royal Institute of Technology 100 44 Stockholm Sweden ; _publ_contact_author_email somfai@kth.se _publ_contact_author_fax +46(8)791-2333 _publ_contact_author_phone +46(8)790-6960 _publ_contact_author_name 'Peter Somfai' data_1 _database_code_CSD 201523 _audit_creation_method maXus _publ_section_title ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_synopsis ; ; _publ_section_exptl_prep ; ; _publ_section_exptl_refinement ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; _chemical_compound_source 'Local laboratory' _exptl_crystal_description Irregular _exptl_crystal_colour Colourless _cell_measurement_temperature 100 _refine_ls_hydrogen_treatment constr _diffrn_measurement_device KappaCCD _computing_data_collection KappaCCD _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 loop_ _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_wavelength_id all _diffrn_orient_matrix_type X=UH _diffrn_orient_matrix_UB_11 0.09438 _diffrn_orient_matrix_UB_12 0.10165 _diffrn_orient_matrix_UB_13 -0.06237 _diffrn_orient_matrix_UB_21 -0.03831 _diffrn_orient_matrix_UB_22 0.06618 _diffrn_orient_matrix_UB_23 0.04989 _diffrn_orient_matrix_UB_31 0.02178 _diffrn_orient_matrix_UB_32 -0.00549 _diffrn_orient_matrix_UB_33 0.02401 _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_special_details ; ? ; _chemical_formula_weight 446.429 _diffrn_radiation_type ' MoK\a' 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' _symmetry_space_group_name_H-M 'P 21 21 21 ' _symmetry_cell_setting Orthorhombic _chemical_formula_moiety 'C24 H32 Br N O2 ' _chemical_formula_sum 'C24 H32 Br N O2 ' _chemical_name_systematic ; ? ; _cell_length_a 6.5565(12) _cell_length_b 10.915(2) _cell_length_c 30.422(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2177.1(7) _diffrn_reflns_number 17434 _diffrn_reflns_theta_max 27.52 _diffrn_reflns_theta_min 4.51 _diffrn_reflns_theta_full 27.52 _cell_measurement_reflns_used 131 _cell_measurement_theta_min 3.75 _cell_measurement_theta_max 20.02 _diffrn_measurement_method CCD _computing_cell_refinement 'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_crystal_size_min 0.15 #_exptl_crystal_size_med 0.20 _exptl_crystal_size_max 0.25 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' Br Br -0.2901 2.4595 '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' _exptl_absorpt_coefficient_mu 1.907 _reflns_number_total 4969 _reflns_number_gt 3812 _reflns_threshold_expression >2sigma(I) _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^)+(0.0365P)^2^+1.3486P] where P=(Fo^2^+2Fc^2^)/3' _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 -0.007(10) _refine_ls_number_reflns 4969 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0794 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.0931 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _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 0.0358(6) 0.2706(3) 0.15638(11) 0.0143(8) Uani 1 1 d . . . C2 C 0.1878(6) 0.3611(3) 0.17520(11) 0.0162(8) Uani 1 1 d . . . C3 C 0.2519(5) 0.3284(4) 0.22193(11) 0.0183(8) Uani 1 1 d . . . C4 C 0.4098(6) 0.4166(3) 0.23987(12) 0.0252(9) Uani 1 1 d . . . C5 C 0.3296(6) 0.1962(3) 0.22287(12) 0.0198(9) Uani 1 1 d . . . C6 C 0.1798(6) 0.1077(3) 0.20188(12) 0.0206(9) Uani 1 1 d . . . C7 C 0.1241(6) 0.1420(3) 0.15396(10) 0.0140(7) Uani 1 1 d . . . C8 C -0.0075(6) 0.0422(3) 0.13094(12) 0.0152(8) Uani 1 1 d . . . C9 C -0.2294(6) 0.0475(4) 0.14750(14) 0.0240(9) Uani 1 1 d . . . C10 C -0.0148(6) 0.0579(3) 0.08059(12) 0.0214(9) Uani 1 1 d . . . C11 C 0.0902(6) -0.0822(3) 0.14024(11) 0.0140(8) Uani 1 1 d . . . C12 C 0.0000(6) -0.1727(4) 0.16619(11) 0.0211(8) Uani 1 1 d . . . C13 C 0.0988(7) -0.2811(3) 0.17555(12) 0.0233(9) Uani 1 1 d . . . C14 C 0.2946(7) -0.3027(3) 0.15927(12) 0.0241(9) Uani 1 1 d . . . C15 C 0.3836(7) -0.2151(3) 0.13304(11) 0.0188(8) Uani 1 1 d . . . C16 C 0.2837(6) -0.1078(3) 0.12380(12) 0.0171(8) Uani 1 1 d . . . C17 C -0.1542(6) 0.4034(3) 0.10985(11) 0.0151(8) Uani 1 1 d . . . C18 C -0.1812(5) 0.4466(3) 0.06228(12) 0.0145(8) Uani 1 1 d . . . C19 C 0.0181(5) 0.4450(3) 0.03605(13) 0.0177(8) Uani 1 1 d . . . C20 C -0.0135(6) 0.5039(4) -0.00891(13) 0.0245(9) Uani 1 1 d . . . C21 C 0.0051(6) 0.6242(4) -0.00591(14) 0.0269(10) Uani 1 1 d . . . C22 C 0.1536(6) 0.5425(3) 0.05757(12) 0.0237(9) Uani 1 1 d . . . C23 C -0.2874(6) 0.5732(3) 0.05967(13) 0.0197(9) Uani 1 1 d . . . C24 C 0.0472(6) 0.6590(3) 0.04119(14) 0.0248(9) Uani 1 1 d . . . Br1 Br -0.37798(6) 0.32644(3) 0.037300(13) 0.02399(11) Uani 1 1 d . . . O1 O -0.2421(4) 0.4477(2) 0.14059(8) 0.0240(6) Uani 1 1 d . . . O2 O -0.0186(3) 0.3125(2) 0.11234(7) 0.0142(5) Uani 1 1 d . . . N1 N -0.1461(5) 0.6751(3) 0.06504(10) 0.0235(7) Uani 1 1 d . . . H1 H -0.0891 0.2696 0.1752 0.017 Uiso 1 1 calc R . . H2A H 0.1264 0.4440 0.1752 0.019 Uiso 1 1 calc R . . H2B H 0.3102 0.3633 0.1562 0.019 Uiso 1 1 calc R . . H3 H 0.1283 0.3332 0.2411 0.022 Uiso 1 1 calc R . . H4A H 0.3520 0.4994 0.2409 0.030 Uiso 1 1 calc R . . H4B H 0.5300 0.4163 0.2207 0.030 Uiso 1 1 calc R . . H4C H 0.4495 0.3912 0.2696 0.030 Uiso 1 1 calc R . . H5A H 0.4614 0.1917 0.2071 0.024 Uiso 1 1 calc R . . H5B H 0.3539 0.1714 0.2537 0.024 Uiso 1 1 calc R . . H6A H 0.0536 0.1056 0.2197 0.025 Uiso 1 1 calc R . . H6B H 0.2395 0.0244 0.2022 0.025 Uiso 1 1 calc R . . H7 H 0.2550 0.1479 0.1372 0.017 Uiso 1 1 calc R . . H9A H -0.2899 0.1265 0.1395 0.029 Uiso 1 1 calc R . . H9B H -0.2314 0.0383 0.1795 0.029 Uiso 1 1 calc R . . H9C H -0.3082 -0.0190 0.1340 0.029 Uiso 1 1 calc R . . H10A H -0.0911 -0.0103 0.0676 0.026 Uiso 1 1 calc R . . H10B H 0.1244 0.0585 0.0689 0.026 Uiso 1 1 calc R . . H10C H -0.0825 0.1353 0.0734 0.026 Uiso 1 1 calc R . . H12 H -0.1329 -0.1592 0.1777 0.025 Uiso 1 1 calc R . . H13 H 0.0334 -0.3413 0.1931 0.028 Uiso 1 1 calc R . . H14 H 0.3648 -0.3763 0.1662 0.029 Uiso 1 1 calc R . . H15 H 0.5157 -0.2291 0.1212 0.023 Uiso 1 1 calc R . . H16 H 0.3487 -0.0489 0.1056 0.021 Uiso 1 1 calc R . . H19 H 0.0833 0.3622 0.0346 0.021 Uiso 1 1 calc R . . H20 H -0.0425 0.4605 -0.0352 0.029 Uiso 1 1 calc R . . H21 H -0.0063 0.6800 -0.0297 0.032 Uiso 1 1 calc R . . H22A H 0.1511 0.5366 0.0900 0.028 Uiso 1 1 calc R . . H22B H 0.2963 0.5375 0.0471 0.028 Uiso 1 1 calc R . . H23A H -0.3563 0.5808 0.0308 0.024 Uiso 1 1 calc R . . H23B H -0.3932 0.5780 0.0828 0.024 Uiso 1 1 calc R . . H24 H 0.1371 0.7328 0.0435 0.030 Uiso 1 1 calc R . . H1N H -0.1739 0.7402 0.0810 0.028 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 C1 0.017(2) 0.0117(18) 0.0145(18) -0.0011(14) 0.0011(16) 0.0013(15) C2 0.020(2) 0.0089(18) 0.0195(18) 0.0003(14) -0.0001(16) -0.0008(14) C3 0.022(2) 0.0125(17) 0.0204(18) -0.0025(17) -0.0005(16) 0.0018(19) C4 0.029(3) 0.022(2) 0.025(2) -0.0039(16) 0.000(2) -0.0005(19) C5 0.023(2) 0.016(2) 0.0199(18) -0.0008(15) -0.0048(16) 0.0030(16) C6 0.028(2) 0.0139(19) 0.0199(19) -0.0006(15) -0.0032(18) 0.0019(16) C7 0.0125(17) 0.0128(18) 0.0167(16) -0.0013(12) -0.0019(18) 0.0026(16) C8 0.010(2) 0.0128(19) 0.023(2) -0.0014(16) -0.0007(17) -0.0006(15) C9 0.013(2) 0.018(2) 0.041(3) 0.0002(18) -0.0031(19) 0.0019(17) C10 0.021(2) 0.016(2) 0.027(2) -0.0041(16) -0.0050(18) 0.0054(17) C11 0.014(2) 0.0123(17) 0.0152(17) -0.0036(13) -0.0014(16) -0.0031(15) C12 0.023(2) 0.0168(18) 0.0234(19) -0.0051(18) 0.0031(17) -0.004(2) C13 0.034(3) 0.0126(18) 0.023(2) 0.0015(14) 0.006(2) -0.0049(19) C14 0.038(2) 0.011(2) 0.023(2) -0.0030(15) -0.0085(19) 0.0028(17) C15 0.017(2) 0.0162(18) 0.0229(19) -0.0048(14) -0.001(2) 0.0026(18) C16 0.020(2) 0.0112(19) 0.0196(19) 0.0020(15) -0.0011(18) -0.0026(16) C17 0.014(2) 0.0103(17) 0.0208(18) -0.0017(14) -0.0024(17) -0.0009(15) C18 0.0091(19) 0.0124(18) 0.0220(19) -0.0026(15) -0.0043(15) -0.0040(14) C19 0.0135(18) 0.0199(19) 0.0198(17) -0.0007(18) -0.0030(19) 0.0070(15) C20 0.015(2) 0.034(2) 0.025(2) 0.0062(18) 0.0001(18) 0.0032(19) C21 0.019(2) 0.030(2) 0.032(2) 0.0128(18) 0.001(2) -0.0028(18) C22 0.012(2) 0.031(2) 0.028(2) 0.0062(17) -0.0010(18) 0.0005(18) C23 0.014(2) 0.017(2) 0.028(2) -0.0027(17) -0.0062(18) 0.0012(17) C24 0.0177(18) 0.019(2) 0.038(2) 0.009(2) -0.0090(19) -0.0058(15) Br1 0.0241(2) 0.01624(17) 0.03166(19) 0.00030(18) -0.0108(2) -0.00392(18) O1 0.0235(16) 0.0248(15) 0.0236(14) -0.0011(12) 0.0056(13) 0.0087(12) O2 0.0136(13) 0.0111(13) 0.0180(12) 0.0013(11) -0.0010(11) 0.0045(11) N1 0.0244(19) 0.0109(14) 0.0354(17) -0.0070(15) -0.0026(16) 0.0038(17) _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 O2 1.460(4) . ? C1 C2 1.515(5) . ? C1 C7 1.520(5) . ? C2 C3 1.525(5) . ? C3 C4 1.516(5) . ? C3 C5 1.530(5) . ? C5 C6 1.519(5) . ? C6 C7 1.549(5) . ? C7 C8 1.556(5) . ? C8 C11 1.528(5) . ? C8 C9 1.541(5) . ? C8 C10 1.542(5) . ? C11 C16 1.392(5) . ? C11 C12 1.396(5) . ? C12 C13 1.379(5) . ? C13 C14 1.396(6) . ? C14 C15 1.375(5) . ? C15 C16 1.371(5) . ? C17 O1 1.200(4) . ? C17 O2 1.335(4) . ? C17 C18 1.532(5) . ? C18 C19 1.531(5) . ? C18 C23 1.549(5) . ? C18 Br1 1.991(3) . ? C19 C20 1.526(5) . ? C19 C22 1.533(5) . ? C20 C21 1.321(6) . ? C21 C24 1.508(6) . ? C22 C24 1.533(5) . ? C23 N1 1.456(5) . ? C24 N1 1.471(5) . ? C1 H1 1.0000 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3 1.0000 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 H7 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 . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C19 H19 1.0000 . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24 1.0000 . ? N1 H1N 0.8800 . ? 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 O2 C1 C2 107.7(3) . . ? O2 C1 C7 109.7(3) . . ? C2 C1 C7 111.7(3) . . ? C1 C2 C3 112.4(3) . . ? C4 C3 C2 112.0(3) . . ? C4 C3 C5 111.4(3) . . ? C2 C3 C5 109.3(3) . . ? C6 C5 C3 112.1(3) . . ? C5 C6 C7 113.2(3) . . ? C1 C7 C6 105.5(3) . . ? C1 C7 C8 117.2(3) . . ? C6 C7 C8 112.6(3) . . ? C11 C8 C9 111.6(3) . . ? C11 C8 C10 107.2(3) . . ? C9 C8 C10 106.9(3) . . ? C11 C8 C7 107.9(3) . . ? C9 C8 C7 110.5(3) . . ? C10 C8 C7 112.7(3) . . ? C16 C11 C12 116.6(3) . . ? C16 C11 C8 119.6(3) . . ? C12 C11 C8 123.8(3) . . ? C13 C12 C11 121.6(4) . . ? C12 C13 C14 120.3(3) . . ? C15 C14 C13 118.6(4) . . ? C16 C15 C14 120.7(4) . . ? C15 C16 C11 122.2(4) . . ? O1 C17 O2 125.1(3) . . ? O1 C17 C18 123.8(3) . . ? O2 C17 C18 111.1(3) . . ? C19 C18 C17 113.0(3) . . ? C19 C18 C23 111.6(3) . . ? C17 C18 C23 112.0(3) . . ? C19 C18 Br1 110.3(2) . . ? C17 C18 Br1 103.4(2) . . ? C23 C18 Br1 106.1(2) . . ? C20 C19 C18 110.2(3) . . ? C20 C19 C22 99.7(3) . . ? C18 C19 C22 105.3(3) . . ? C21 C20 C19 110.2(4) . . ? C20 C21 C24 109.5(4) . . ? C24 C22 C19 100.0(3) . . ? N1 C23 C18 112.9(3) . . ? N1 C24 C21 109.9(3) . . ? N1 C24 C22 109.3(3) . . ? C21 C24 C22 100.5(3) . . ? C17 O2 C1 116.6(3) . . ? C23 N1 C24 113.7(3) . . ? O2 C1 H1 109.2 . . ? C2 C1 H1 109.2 . . ? C7 C1 H1 109.2 . . ? C1 C2 H2A 109.1 . . ? C3 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? C3 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C4 C3 H3 108.0 . . ? C2 C3 H3 108.0 . . ? C5 C3 H3 108.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 H5A 109.2 . . ? C3 C5 H5A 109.2 . . ? C6 C5 H5B 109.2 . . ? C3 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? C5 C6 H6A 108.9 . . ? C7 C6 H6A 108.9 . . ? C5 C6 H6B 108.9 . . ? C7 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? C1 C7 H7 107.0 . . ? C6 C7 H7 107.0 . . ? C8 C7 H7 107.0 . . ? 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 . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 H14 120.7 . . ? C13 C14 H14 120.7 . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C15 C16 H16 118.9 . . ? C11 C16 H16 118.9 . . ? C20 C19 H19 113.5 . . ? C18 C19 H19 113.5 . . ? C22 C19 H19 113.5 . . ? C21 C20 H20 124.9 . . ? C19 C20 H20 124.9 . . ? C20 C21 H21 125.3 . . ? C24 C21 H21 125.3 . . ? C24 C22 H22A 111.8 . . ? C19 C22 H22A 111.8 . . ? C24 C22 H22B 111.8 . . ? C19 C22 H22B 111.8 . . ? H22A C22 H22B 109.5 . . ? N1 C23 H23A 109.0 . . ? C18 C23 H23A 109.0 . . ? N1 C23 H23B 109.0 . . ? C18 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? N1 C24 H24 112.2 . . ? C21 C24 H24 112.2 . . ? C22 C24 H24 112.2 . . ? C23 N1 H1N 123.2 . . ? C24 N1 H1N 123.2 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.552 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.100 _publ_section_references ; Mackay, S., Gilmore, C. J.,Edwards, C., Stewart, N. & Shankland, K. (1999). maXus Computer Program for the Solution and Refinement of Crystal Structures. Bruker Nonius, The Netherlands, MacScience, Japan & The University of Glasgow. Johnson, C. K. (1976). ORTEP-II. A Fortran Thermal-Ellipsoid Plot Program. Report ORNL-5138. Oak Ridge National Laboratory, Oak Ridge, Tennessee, USA. Otwinowski, Z. and Minor, W, (1997). In Methods in Enzymology, 276, edited by C.W. Carter, Jr. & R.M. Sweet pp. 307-326, New York:Academic Press. Sheldrick, G.M. (1997). SHELXS-97. Program for Crystal Structure Solution. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL97. Program for the Refinement of Crystal Structures. University of G\"ottingen, Germany. ;