data_cd25218 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H29 Cl N2 O2' _chemical_formula_weight 364.90 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' 'Cl' 'Cl' 0.1484 0.1585 '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 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 9.6531(10) _cell_length_b 10.8282(11) _cell_length_c 18.872(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.196(2) _cell_angle_gamma 90.00 _cell_volume 1935.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2609 _cell_measurement_theta_min 4.358 _cell_measurement_theta_max 49.285 _exptl_crystal_description ? _exptl_crystal_colour colorless _exptl_crystal_size_max 0.508 _exptl_crystal_size_mid 0.443 _exptl_crystal_size_min 0.357 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.213 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.88819 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _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 '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 11342 _diffrn_reflns_av_R_equivalents 0.0569 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4389 _reflns_number_gt 3077 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0820P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4389 _refine_ls_number_parameters 266 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0828 _refine_ls_R_factor_gt 0.0577 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _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 Cl Cl 1.01493(6) 0.04452(6) 0.79371(4) 0.0545(2) Uani 1 1 d . . . O1 O 0.71224(17) 0.14728(14) 0.76755(9) 0.0417(4) Uani 1 1 d D . . O2 O 0.1753(3) 0.1853(2) 0.93508(15) 0.0971(8) Uani 1 1 d . . . H2 H 0.1400 0.1405 0.9014 0.146 Uiso 1 1 calc R . . N1 N 0.40359(19) 0.23072(17) 0.66447(9) 0.0320(4) Uani 1 1 d . . . N4 N 0.45105(17) -0.08688(15) 0.74036(9) 0.0326(4) Uani 1 1 d . . . C2 C 0.3865(2) 0.11225(18) 0.68779(11) 0.0284(4) Uani 1 1 d . . . C3 C 0.5430(3) -0.1426(2) 0.80695(14) 0.0420(6) Uani 1 1 d . . . C5 C 0.2992(2) -0.1239(2) 0.72950(14) 0.0414(6) Uani 1 1 d . . . H5A H 0.2611 -0.0992 0.7713 0.050 Uiso 1 1 calc R . . H5B H 0.2920 -0.2130 0.7253 0.050 Uiso 1 1 calc R . . C6 C 0.2124(2) -0.0647(2) 0.66194(13) 0.0407(5) Uani 1 1 d . . . H6A H 0.2193 -0.1147 0.6201 0.049 Uiso 1 1 calc R . . H6B H 0.1140 -0.0617 0.6662 0.049 Uiso 1 1 calc R . . C7 C 0.2631(2) 0.06348(19) 0.65122(11) 0.0311(5) Uani 1 1 d . . . C8 C 0.1980(2) 0.15620(19) 0.60177(11) 0.0325(5) Uani 1 1 d . . . C9 C 0.0712(3) 0.1633(3) 0.55094(13) 0.0440(6) Uani 1 1 d . . . C10 C 0.0394(3) 0.2700(3) 0.51198(13) 0.0534(7) Uani 1 1 d . . . C11 C 0.1315(3) 0.3684(3) 0.52138(13) 0.0550(7) Uani 1 1 d . . . H11 H 0.1082 0.4389 0.4934 0.066 Uiso 1 1 calc R . . C12 C 0.2572(3) 0.3662(2) 0.57081(13) 0.0454(6) Uani 1 1 d . . . C13 C 0.2885(2) 0.25902(19) 0.61090(11) 0.0337(5) Uani 1 1 d . . . C14 C 0.6747(3) -0.0595(2) 0.81808(14) 0.0414(6) Uani 1 1 d . . . C15 C 0.6398(2) 0.03492(18) 0.75563(11) 0.0322(5) Uani 1 1 d . . . C16 C 0.4788(2) 0.05178(18) 0.75132(11) 0.0288(4) Uani 1 1 d . . . C17 C 0.4400(3) 0.1042(2) 0.81994(12) 0.0422(6) Uani 1 1 d . . . H17A H 0.4701 0.1887 0.8258 0.063 Uiso 1 1 calc R . . H17B H 0.4858 0.0569 0.8609 0.063 Uiso 1 1 calc R . . H17C H 0.3395 0.1000 0.8163 0.063 Uiso 1 1 calc R . . C18 C 0.6938(4) -0.0336(3) 0.55834(17) 0.0833(11) Uani 1 1 d . . . H18A H 0.7793 -0.0795 0.5742 0.125 Uiso 1 1 calc R . . H18B H 0.7050 0.0200 0.5193 0.125 Uiso 1 1 calc R . . H18C H 0.6173 -0.0898 0.5421 0.125 Uiso 1 1 calc R . . C19 C 0.6621(3) 0.0426(2) 0.62030(13) 0.0500(6) Uani 1 1 d . . . H19A H 0.5732 0.0856 0.6047 0.060 Uiso 1 1 calc R . . H19B H 0.7355 0.1043 0.6335 0.060 Uiso 1 1 calc R . . C20 C 0.6530(2) -0.03559(19) 0.68660(12) 0.0363(5) Uani 1 1 d . . . H20 H 0.7369 -0.0885 0.6973 0.044 Uiso 1 1 calc R . . C21 C 0.5209(2) -0.11827(19) 0.67676(12) 0.0366(5) Uani 1 1 d . . . H21A H 0.4579 -0.1005 0.6313 0.044 Uiso 1 1 calc R . . H21B H 0.5470 -0.2049 0.6777 0.044 Uiso 1 1 calc R . . C22 C 0.1047(6) 0.1680(4) 0.9930(2) 0.1191(17) Uani 1 1 d . . . H20A H 0.1007 0.0814 1.0034 0.179 Uiso 1 1 calc R . . H20B H 0.0106 0.2003 0.9803 0.179 Uiso 1 1 calc R . . H20C H 0.1548 0.2105 1.0349 0.179 Uiso 1 1 calc R . . H1 H 0.465(2) 0.283(2) 0.6821(11) 0.031(6) Uiso 1 1 d . . . H1A H 0.7970(19) 0.128(2) 0.7771(14) 0.058(8) Uiso 1 1 d D . . H3A H 0.485(3) -0.139(2) 0.8433(14) 0.047(7) Uiso 1 1 d . . . H3B H 0.560(3) -0.225(3) 0.7965(13) 0.052(7) Uiso 1 1 d . . . H9 H 0.008(3) 0.093(2) 0.5466(13) 0.050(7) Uiso 1 1 d . . . H10 H -0.048(3) 0.281(2) 0.4789(14) 0.058(7) Uiso 1 1 d . . . H12 H 0.325(3) 0.431(2) 0.5748(12) 0.044(7) Uiso 1 1 d . . . H14A H 0.695(2) -0.0195(19) 0.8639(12) 0.034(6) Uiso 1 1 d . . . H14B H 0.756(3) -0.106(2) 0.8134(13) 0.053(7) 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 Cl 0.0358(3) 0.0513(4) 0.0733(5) -0.0012(3) 0.0027(3) 0.0083(3) O1 0.0309(9) 0.0333(9) 0.0561(10) 0.0002(7) -0.0032(7) -0.0028(7) O2 0.103(2) 0.0838(19) 0.0931(19) -0.0010(14) -0.0103(16) -0.0127(14) N1 0.0304(9) 0.0262(9) 0.0364(10) 0.0012(8) -0.0011(7) -0.0030(7) N4 0.0328(9) 0.0260(9) 0.0387(10) 0.0040(7) 0.0063(8) -0.0004(7) C2 0.0259(10) 0.0260(11) 0.0328(11) -0.0004(8) 0.0044(8) 0.0018(8) C3 0.0435(14) 0.0371(14) 0.0446(14) 0.0147(11) 0.0063(11) 0.0064(10) C5 0.0330(12) 0.0332(12) 0.0590(15) 0.0042(10) 0.0117(10) -0.0078(9) C6 0.0310(11) 0.0358(13) 0.0535(14) -0.0048(10) 0.0036(10) -0.0063(9) C7 0.0270(10) 0.0309(11) 0.0343(11) -0.0036(9) 0.0034(8) -0.0005(8) C8 0.0306(11) 0.0346(12) 0.0307(11) -0.0069(9) 0.0018(8) 0.0025(9) C9 0.0369(13) 0.0522(16) 0.0392(13) -0.0111(11) -0.0022(10) 0.0026(11) C10 0.0476(15) 0.0679(19) 0.0371(14) -0.0007(12) -0.0105(11) 0.0150(13) C11 0.0674(18) 0.0539(17) 0.0384(14) 0.0098(12) -0.0029(12) 0.0184(14) C12 0.0520(15) 0.0396(14) 0.0410(13) 0.0074(11) 0.0005(11) 0.0052(12) C13 0.0346(11) 0.0358(12) 0.0290(11) 0.0004(9) 0.0021(8) 0.0059(9) C14 0.0349(12) 0.0416(14) 0.0438(14) 0.0082(11) -0.0023(10) 0.0080(10) C15 0.0270(10) 0.0296(11) 0.0379(12) 0.0016(9) 0.0010(8) 0.0023(8) C16 0.0290(10) 0.0249(10) 0.0316(11) 0.0007(8) 0.0036(8) 0.0003(8) C17 0.0453(13) 0.0447(14) 0.0355(12) -0.0023(10) 0.0052(10) 0.0090(11) C18 0.099(3) 0.099(3) 0.062(2) -0.0095(18) 0.0401(19) 0.006(2) C19 0.0530(15) 0.0525(16) 0.0494(15) 0.0007(12) 0.0219(12) -0.0042(12) C20 0.0312(11) 0.0332(12) 0.0455(13) 0.0005(9) 0.0102(9) 0.0045(9) C21 0.0380(12) 0.0284(11) 0.0434(12) -0.0050(9) 0.0076(10) 0.0031(9) C22 0.191(5) 0.092(3) 0.083(3) -0.011(2) 0.046(3) 0.033(3) _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 O1 C15 1.400(2) . ? O1 H1A 0.830(17) . ? O2 C22 1.409(5) . ? O2 H2 0.8200 . ? N1 C2 1.376(3) . ? N1 C13 1.383(3) . ? N1 H1 0.84(2) . ? N4 C5 1.495(3) . ? N4 C3 1.516(3) . ? N4 C21 1.525(3) . ? N4 C16 1.532(3) . ? C2 C7 1.362(3) . ? C2 C16 1.498(3) . ? C3 C14 1.538(3) . ? C3 H3A 0.97(3) . ? C3 H3B 0.93(3) . ? C5 C6 1.524(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C7 1.498(3) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.430(3) . ? C8 C9 1.403(3) . ? C8 C13 1.405(3) . ? C9 C10 1.371(4) . ? C9 H9 0.96(3) . ? C10 C11 1.378(4) . ? C10 H10 0.95(3) . ? C11 C12 1.380(3) . ? C11 H11 0.9300 . ? C12 C13 1.387(3) . ? C12 H12 0.95(2) . ? C14 C15 1.547(3) . ? C14 H14A 0.95(2) . ? C14 H14B 0.95(3) . ? C15 C20 1.537(3) . ? C15 C16 1.551(3) . ? C16 C17 1.526(3) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.510(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.527(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C21 1.540(3) . ? C20 H20 0.9800 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H20A 0.9600 . ? C22 H20B 0.9600 . ? C22 H20C 0.9600 . ? 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 C15 O1 H1A 104.7(18) . . ? C22 O2 H2 109.5 . . ? C2 N1 C13 108.12(17) . . ? C2 N1 H1 128.3(15) . . ? C13 N1 H1 123.0(15) . . ? C5 N4 C3 114.06(17) . . ? C5 N4 C21 113.85(17) . . ? C3 N4 C21 106.66(17) . . ? C5 N4 C16 114.97(16) . . ? C3 N4 C16 102.66(16) . . ? C21 N4 C16 103.43(15) . . ? C7 C2 N1 110.29(17) . . ? C7 C2 C16 124.18(18) . . ? N1 C2 C16 124.99(17) . . ? N4 C3 C14 102.47(18) . . ? N4 C3 H3A 104.1(14) . . ? C14 C3 H3A 117.1(14) . . ? N4 C3 H3B 107.6(15) . . ? C14 C3 H3B 114.3(17) . . ? H3A C3 H3B 110(2) . . ? N4 C5 C6 111.52(18) . . ? N4 C5 H5A 109.3 . . ? C6 C5 H5A 109.3 . . ? N4 C5 H5B 109.3 . . ? C6 C5 H5B 109.3 . . ? H5A C5 H5B 108.0 . . ? C7 C6 C5 111.21(18) . . ? C7 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? C7 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C2 C7 C8 106.77(18) . . ? C2 C7 C6 124.56(19) . . ? C8 C7 C6 128.65(18) . . ? C9 C8 C13 118.6(2) . . ? C9 C8 C7 134.4(2) . . ? C13 C8 C7 107.00(17) . . ? C10 C9 C8 119.2(2) . . ? C10 C9 H9 123.0(14) . . ? C8 C9 H9 117.7(14) . . ? C9 C10 C11 120.7(2) . . ? C9 C10 H10 122.5(16) . . ? C11 C10 H10 116.7(16) . . ? C10 C11 C12 122.3(2) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C11 C12 C13 117.0(2) . . ? C11 C12 H12 122.7(14) . . ? C13 C12 H12 120.1(14) . . ? N1 C13 C12 130.0(2) . . ? N1 C13 C8 107.81(18) . . ? C12 C13 C8 122.2(2) . . ? C3 C14 C15 103.32(17) . . ? C3 C14 H14A 114.3(14) . . ? C15 C14 H14A 111.5(13) . . ? C3 C14 H14B 110.6(15) . . ? C15 C14 H14B 110.0(15) . . ? H14A C14 H14B 107.2(19) . . ? O1 C15 C20 116.54(18) . . ? O1 C15 C14 115.08(17) . . ? C20 C15 C14 106.01(18) . . ? O1 C15 C16 111.74(16) . . ? C20 C15 C16 105.16(16) . . ? C14 C15 C16 100.70(17) . . ? C2 C16 C17 108.09(16) . . ? C2 C16 N4 105.01(15) . . ? C17 C16 N4 114.43(17) . . ? C2 C16 C15 121.85(17) . . ? C17 C16 C15 114.08(17) . . ? N4 C16 C15 92.23(14) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C18 C19 C20 112.6(2) . . ? C18 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? C18 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C19 C20 C15 116.52(19) . . ? C19 C20 C21 113.67(19) . . ? C15 C20 C21 100.82(17) . . ? C19 C20 H20 108.5 . . ? C15 C20 H20 108.5 . . ? C21 C20 H20 108.5 . . ? N4 C21 C20 104.96(16) . . ? N4 C21 H21A 110.8 . . ? C20 C21 H21A 110.8 . . ? N4 C21 H21B 110.8 . . ? C20 C21 H21B 110.8 . . ? H21A C21 H21B 108.8 . . ? O2 C22 H20A 109.5 . . ? O2 C22 H20B 109.5 . . ? H20A C22 H20B 109.5 . . ? O2 C22 H20C 109.5 . . ? H20A C22 H20C 109.5 . . ? H20B C22 H20C 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 C13 N1 C2 C7 -0.5(2) . . . . ? C13 N1 C2 C16 -172.29(19) . . . . ? C5 N4 C3 C14 -162.4(2) . . . . ? C21 N4 C3 C14 71.0(2) . . . . ? C16 N4 C3 C14 -37.4(2) . . . . ? C3 N4 C5 C6 179.8(2) . . . . ? C21 N4 C5 C6 -57.4(2) . . . . ? C16 N4 C5 C6 61.6(2) . . . . ? N4 C5 C6 C7 -36.2(3) . . . . ? N1 C2 C7 C8 0.0(2) . . . . ? C16 C2 C7 C8 171.93(18) . . . . ? N1 C2 C7 C6 178.8(2) . . . . ? C16 C2 C7 C6 -9.3(3) . . . . ? C5 C6 C7 C2 12.2(3) . . . . ? C5 C6 C7 C8 -169.3(2) . . . . ? C2 C7 C8 C9 -178.8(2) . . . . ? C6 C7 C8 C9 2.5(4) . . . . ? C2 C7 C8 C13 0.4(2) . . . . ? C6 C7 C8 C13 -178.3(2) . . . . ? C13 C8 C9 C10 -0.1(3) . . . . ? C7 C8 C9 C10 179.1(2) . . . . ? C8 C9 C10 C11 1.2(4) . . . . ? C9 C10 C11 C12 -1.4(4) . . . . ? C10 C11 C12 C13 0.6(4) . . . . ? C2 N1 C13 C12 -179.9(2) . . . . ? C2 N1 C13 C8 0.7(2) . . . . ? C11 C12 C13 N1 -178.8(2) . . . . ? C11 C12 C13 C8 0.5(4) . . . . ? C9 C8 C13 N1 178.68(19) . . . . ? C7 C8 C13 N1 -0.7(2) . . . . ? C9 C8 C13 C12 -0.8(3) . . . . ? C7 C8 C13 C12 179.9(2) . . . . ? N4 C3 C14 C15 0.4(3) . . . . ? C3 C14 C15 O1 156.2(2) . . . . ? C3 C14 C15 C20 -73.4(2) . . . . ? C3 C14 C15 C16 35.9(2) . . . . ? C7 C2 C16 C17 -94.8(2) . . . . ? N1 C2 C16 C17 76.0(2) . . . . ? C7 C2 C16 N4 27.8(3) . . . . ? N1 C2 C16 N4 -161.48(19) . . . . ? C7 C2 C16 C15 130.2(2) . . . . ? N1 C2 C16 C15 -59.1(3) . . . . ? C5 N4 C16 C2 -53.8(2) . . . . ? C3 N4 C16 C2 -178.25(17) . . . . ? C21 N4 C16 C2 70.92(18) . . . . ? C5 N4 C16 C17 64.5(2) . . . . ? C3 N4 C16 C17 -59.9(2) . . . . ? C21 N4 C16 C17 -170.73(17) . . . . ? C5 N4 C16 C15 -177.67(17) . . . . ? C3 N4 C16 C15 57.89(18) . . . . ? C21 N4 C16 C15 -52.94(17) . . . . ? O1 C15 C16 C2 71.9(2) . . . . ? C20 C15 C16 C2 -55.5(2) . . . . ? C14 C15 C16 C2 -165.47(19) . . . . ? O1 C15 C16 C17 -60.8(2) . . . . ? C20 C15 C16 C17 171.84(17) . . . . ? C14 C15 C16 C17 61.8(2) . . . . ? O1 C15 C16 N4 -178.92(16) . . . . ? C20 C15 C16 N4 53.75(17) . . . . ? C14 C15 C16 N4 -56.25(18) . . . . ? C18 C19 C20 C15 172.5(2) . . . . ? C18 C19 C20 C21 -70.8(3) . . . . ? O1 C15 C20 C19 -34.9(3) . . . . ? C14 C15 C20 C19 -164.46(19) . . . . ? C16 C15 C20 C19 89.4(2) . . . . ? O1 C15 C20 C21 -158.46(17) . . . . ? C14 C15 C20 C21 72.02(19) . . . . ? C16 C15 C20 C21 -34.1(2) . . . . ? C5 N4 C21 C20 160.94(17) . . . . ? C3 N4 C21 C20 -72.4(2) . . . . ? C16 N4 C21 C20 35.49(19) . . . . ? C19 C20 C21 N4 -126.14(19) . . . . ? C15 C20 C21 N4 -0.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.415 _refine_diff_density_min -0.261 _refine_diff_density_rms 0.053