data_7 _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic 7 _chemical_name_common 7 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H22 N2 O' _chemical_formula_weight 282.37 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _diffrn_refln_scan_width 2.0 _diffrn_refln_scan_rate 10 _space_group.centring_type primitive _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.3071(3) _cell_length_b 4.73520(10) _cell_length_c 19.7305(4) _cell_angle_alpha 90 _cell_angle_beta 97.8660(10) _cell_angle_gamma 90 _cell_volume 1509.20(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9938 _cell_measurement_theta_min 4.52 _cell_measurement_theta_max 68.28 _exptl_crystal_description rod _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.243 _exptl_crystal_F_000 608 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.020 _exptl_crystal_size_min 0.020 _exptl_absorpt_coefficient_mu 0.605 _shelx_estimated_absorpt_T_min 0.970 _shelx_estimated_absorpt_T_max 0.988 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.815 _exptl_absorpt_correction_T_max 0.929 _exptl_absorpt_process_details SADABS _exptl_absorpt_special_details ? _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source 'microfocus rotating anode' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 8.366 _diffrn_reflns_number 44320 _diffrn_reflns_av_unetI/netI 0.0263 _diffrn_reflns_av_R_equivalents 0.0513 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -5 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.260 _diffrn_reflns_theta_max 68.425 _diffrn_reflns_theta_full 67.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_point_group_measured_fraction_full 0.995 _reflns_number_total 5518 _reflns_number_gt 5232 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.757 _reflns_Friedel_fraction_max 0.983 _reflns_Friedel_fraction_full 0.988 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXT' _computing_structure_refinement 'SHELXL-2014' _computing_molecular_graphics 'ORTEP-32' _computing_publication_material 'WinGX' _refine_special_details ? _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0410P)^2^+0.2258P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary iterative _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 x determined using 2175 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.00(9) _chemical_absolute_configuration ad _refine_ls_number_reflns 5518 _refine_ls_number_parameters 381 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0323 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0738 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.048 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.75348(11) 0.9506(4) 0.91571(9) 0.0197(4) Uani 1 1 d . . . . . H1 H 0.7576 1.1587 0.9083 0.024 Uiso 1 1 calc R U . . . C2 C 0.80768(11) 0.8628(4) 0.98141(10) 0.0205(4) Uani 1 1 d . . . . . C3 C 0.80162(13) 0.9489(5) 1.04769(11) 0.0261(4) Uani 1 1 d . . . . . H3 H 0.7617 1.0854 1.0565 0.031 Uiso 1 1 calc R U . . . C4 C 0.85526(13) 0.8307(5) 1.10080(10) 0.0285(5) Uani 1 1 d . . . . . H4 H 0.8526 0.8897 1.1465 0.034 Uiso 1 1 calc R U . . . C5 C 0.91276(12) 0.6275(5) 1.08823(10) 0.0267(5) Uani 1 1 d . . . . . H5 H 0.9478 0.5455 1.1255 0.032 Uiso 1 1 calc R U . . . C6 C 0.91968(12) 0.5428(5) 1.02194(10) 0.0251(4) Uani 1 1 d . . . . . H6 H 0.9593 0.4050 1.0133 0.030 Uiso 1 1 calc R U . . . C7 C 0.86712(11) 0.6645(5) 0.96832(10) 0.0209(4) Uani 1 1 d . . . . . C8 C 0.85987(12) 0.6286(4) 0.89428(10) 0.0208(4) Uani 1 1 d . . . . . C9 C 0.89223(12) 0.5085(5) 0.84056(10) 0.0249(4) Uani 1 1 d . . . . . H9 H 0.9376 0.3811 0.8446 0.030 Uiso 1 1 calc R U . . . C10 C 0.79096(12) 0.7729(4) 0.79696(10) 0.0219(4) Uani 1 1 d . . . . . H10 H 0.7517 0.8690 0.7651 0.026 Uiso 1 1 calc R U . . . C11 C 0.66323(11) 0.8638(4) 0.91640(9) 0.0212(4) Uani 1 1 d . . . . . H11A H 0.6615 0.6591 0.9263 0.025 Uiso 1 1 calc R U . . . H11B H 0.6417 0.9648 0.9542 0.025 Uiso 1 1 calc R U . . . C12 C 0.60606(12) 0.9229(4) 0.85023(10) 0.0192(4) Uani 1 1 d . . . . . H12 H 0.6242 0.8008 0.8137 0.023 Uiso 1 1 calc R U . . . C13 C 0.51511(11) 0.8499(4) 0.85595(9) 0.0200(4) Uani 1 1 d . . . . . H13 H 0.5120 0.6411 0.8628 0.024 Uiso 1 1 calc R U . . . C14 C 0.48086(12) 0.9916(5) 0.91593(10) 0.0236(4) Uani 1 1 d . . . . . H14A H 0.4851 1.1992 0.9116 0.028 Uiso 1 1 calc R U . . . H14B H 0.5145 0.9345 0.9594 0.028 Uiso 1 1 calc R U . . . C15 C 0.39037(12) 0.9099(5) 0.91786(10) 0.0277(5) Uani 1 1 d . . . . . H15A H 0.3869 0.7046 0.9265 0.033 Uiso 1 1 calc R U . . . H15B H 0.3695 1.0104 0.9561 0.033 Uiso 1 1 calc R U . . . C16 C 0.33592(13) 0.9828(5) 0.85097(11) 0.0294(5) Uani 1 1 d . . . . . H16A H 0.2787 0.9171 0.8530 0.035 Uiso 1 1 calc R U . . . H16B H 0.3345 1.1903 0.8447 0.035 Uiso 1 1 calc R U . . . C17 C 0.36891(12) 0.8450(5) 0.79079(10) 0.0285(5) Uani 1 1 d . . . . . H17A H 0.3354 0.9072 0.7477 0.034 Uiso 1 1 calc R U . . . H17B H 0.3635 0.6374 0.7941 0.034 Uiso 1 1 calc R U . . . C18 C 0.45980(12) 0.9209(5) 0.78880(10) 0.0253(4) Uani 1 1 d . . . . . H18A H 0.4640 1.1254 0.7795 0.030 Uiso 1 1 calc R U . . . H18B H 0.4800 0.8169 0.7508 0.030 Uiso 1 1 calc R U . . . C19 C 0.74277(11) 0.2719(4) 0.54673(9) 0.0184(4) Uani 1 1 d . . . . . H19 H 0.7424 0.4810 0.5396 0.022 Uiso 1 1 calc R U . . . C20 C 0.69361(11) 0.1229(4) 0.48612(9) 0.0189(4) Uani 1 1 d . . . . . C21 C 0.70626(12) 0.1278(5) 0.41830(10) 0.0241(4) Uani 1 1 d . . . . . H21 H 0.7488 0.2409 0.4040 0.029 Uiso 1 1 calc R U . . . C22 C 0.65536(13) -0.0364(5) 0.37134(10) 0.0272(5) Uani 1 1 d . . . . . H22 H 0.6635 -0.0355 0.3246 0.033 Uiso 1 1 calc R U . . . C23 C 0.59300(12) -0.2014(5) 0.39207(11) 0.0288(5) Uani 1 1 d . . . . . H23 H 0.5587 -0.3107 0.3592 0.035 Uiso 1 1 calc R U . . . C24 C 0.58005(12) -0.2091(5) 0.46022(10) 0.0254(4) Uani 1 1 d . . . . . H24 H 0.5377 -0.3235 0.4744 0.031 Uiso 1 1 calc R U . . . C25 C 0.63073(11) -0.0450(4) 0.50696(10) 0.0195(4) Uani 1 1 d . . . . . C26 C 0.63190(11) -0.0008(4) 0.58020(10) 0.0197(4) Uani 1 1 d . . . . . C27 C 0.59429(12) -0.0547(5) 0.63700(10) 0.0226(4) Uani 1 1 d . . . . . H27 H 0.5501 -0.1839 0.6389 0.027 Uiso 1 1 calc R U . . . C28 C 0.68997(11) 0.2548(5) 0.66697(10) 0.0216(4) Uani 1 1 d . . . . . H28 H 0.7255 0.3855 0.6931 0.026 Uiso 1 1 calc R U . . . C29 C 0.83178(11) 0.1593(4) 0.56019(9) 0.0193(4) Uani 1 1 d . . . . . H29A H 0.8302 -0.0487 0.5550 0.023 Uiso 1 1 calc R U . . . H29B H 0.8631 0.2361 0.5247 0.023 Uiso 1 1 calc R U . . . C30 C 0.87842(11) 0.2305(4) 0.63014(9) 0.0175(4) Uani 1 1 d . . . . . H30 H 0.8506 0.1301 0.6653 0.021 Uiso 1 1 calc R U . . . C31 C 0.96829(11) 0.1286(4) 0.63725(9) 0.0179(4) Uani 1 1 d . . . . . H31 H 0.9667 -0.0745 0.6232 0.021 Uiso 1 1 calc R U . . . C32 C 1.02225(11) 0.2829(4) 0.59119(10) 0.0204(4) Uani 1 1 d . . . . . H32A H 0.9967 0.2662 0.5429 0.024 Uiso 1 1 calc R U . . . H32B H 1.0251 0.4859 0.6033 0.024 Uiso 1 1 calc R U . . . C33 C 1.10974(12) 0.1604(5) 0.59901(10) 0.0247(4) Uani 1 1 d . . . . . H33A H 1.1438 0.2704 0.5705 0.030 Uiso 1 1 calc R U . . . H33B H 1.1073 -0.0370 0.5824 0.030 Uiso 1 1 calc R U . . . C34 C 1.15061(12) 0.1669(5) 0.67353(10) 0.0258(4) Uani 1 1 d . . . . . H34A H 1.2055 0.0741 0.6773 0.031 Uiso 1 1 calc R U . . . H34B H 1.1592 0.3654 0.6886 0.031 Uiso 1 1 calc R U . . . C35 C 1.09708(12) 0.0164(5) 0.71973(10) 0.0252(4) Uani 1 1 d . . . . . H35A H 1.1229 0.0346 0.7680 0.030 Uiso 1 1 calc R U . . . H35B H 1.0940 -0.1871 0.7081 0.030 Uiso 1 1 calc R U . . . C36 C 1.00974(11) 0.1395(4) 0.71190(9) 0.0214(4) Uani 1 1 d . . . . . H36A H 1.0124 0.3380 0.7278 0.026 Uiso 1 1 calc R U . . . H36B H 0.9759 0.0318 0.7409 0.026 Uiso 1 1 calc R U . . . N1 N 0.84875(10) 0.6013(4) 0.77986(9) 0.0254(4) Uani 1 1 d . . . . . N2 N 0.79511(9) 0.7937(4) 0.86529(8) 0.0191(3) Uani 1 1 d . . . . . N3 N 0.63073(10) 0.1083(4) 0.69089(8) 0.0228(4) Uani 1 1 d . . . . . N4 N 0.69309(9) 0.1937(4) 0.60101(8) 0.0188(3) Uani 1 1 d . . . . . O1 O 0.61626(8) 1.2098(3) 0.83127(7) 0.0219(3) Uani 1 1 d . . . . . H1A H 0.6182 1.2193 0.7890 0.033 Uiso 1 1 calc R U . . . O2 O 0.87176(8) 0.5268(3) 0.64154(6) 0.0194(3) Uani 1 1 d . . . . . H2 H 0.8697 0.5566 0.6832 0.029 Uiso 1 1 calc R U . . . 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 0.0227(9) 0.0209(10) 0.0161(9) -0.0014(8) 0.0050(7) 0.0007(8) C2 0.0197(9) 0.0224(10) 0.0196(9) 0.0003(8) 0.0039(7) -0.0037(8) C3 0.0280(10) 0.0284(11) 0.0226(10) -0.0038(8) 0.0063(8) -0.0016(8) C4 0.0313(11) 0.0367(12) 0.0175(10) -0.0032(9) 0.0031(8) -0.0072(9) C5 0.0236(10) 0.0350(12) 0.0200(10) 0.0060(9) -0.0028(7) -0.0069(9) C6 0.0191(9) 0.0317(11) 0.0238(10) 0.0023(9) 0.0009(7) -0.0005(8) C7 0.0193(9) 0.0240(10) 0.0197(9) -0.0008(8) 0.0041(7) -0.0041(8) C8 0.0191(9) 0.0233(10) 0.0201(9) 0.0019(8) 0.0033(7) 0.0000(8) C9 0.0238(10) 0.0297(11) 0.0215(10) -0.0002(9) 0.0047(7) 0.0057(9) C10 0.0227(9) 0.0264(10) 0.0171(9) 0.0012(8) 0.0046(7) 0.0007(8) C11 0.0221(9) 0.0251(10) 0.0175(9) -0.0003(8) 0.0072(7) 0.0006(8) C12 0.0236(9) 0.0190(10) 0.0164(9) 0.0006(7) 0.0070(7) 0.0010(7) C13 0.0226(9) 0.0212(9) 0.0167(9) 0.0016(8) 0.0053(7) 0.0015(8) C14 0.0248(10) 0.0284(11) 0.0187(9) -0.0021(8) 0.0070(7) 0.0004(8) C15 0.0254(10) 0.0362(12) 0.0234(10) -0.0007(9) 0.0104(8) -0.0015(9) C16 0.0227(10) 0.0348(12) 0.0316(11) 0.0033(10) 0.0069(8) 0.0025(9) C17 0.0243(10) 0.0374(12) 0.0230(10) 0.0037(9) 0.0001(8) -0.0006(9) C18 0.0261(10) 0.0338(11) 0.0166(9) 0.0027(8) 0.0053(8) 0.0008(9) C19 0.0204(9) 0.0203(9) 0.0153(9) 0.0027(7) 0.0050(7) -0.0006(8) C20 0.0183(9) 0.0201(10) 0.0178(9) 0.0019(8) 0.0006(7) 0.0029(8) C21 0.0231(9) 0.0300(11) 0.0197(10) 0.0042(8) 0.0043(7) 0.0007(8) C22 0.0265(10) 0.0397(12) 0.0154(9) 0.0000(9) 0.0033(7) 0.0017(9) C23 0.0234(10) 0.0395(13) 0.0224(10) -0.0064(9) -0.0010(8) -0.0005(9) C24 0.0193(9) 0.0321(12) 0.0249(10) -0.0012(9) 0.0028(7) -0.0026(8) C25 0.0166(9) 0.0245(10) 0.0173(9) 0.0033(8) 0.0026(7) 0.0038(7) C26 0.0173(9) 0.0216(10) 0.0198(9) 0.0019(8) 0.0009(7) 0.0018(8) C27 0.0187(9) 0.0294(11) 0.0202(9) 0.0037(8) 0.0041(7) 0.0005(8) C28 0.0200(9) 0.0279(10) 0.0167(9) -0.0008(8) 0.0018(7) 0.0040(8) C29 0.0191(9) 0.0221(9) 0.0172(9) -0.0001(8) 0.0041(7) -0.0020(8) C30 0.0206(9) 0.0168(9) 0.0163(9) 0.0009(8) 0.0065(7) -0.0017(7) C31 0.0199(9) 0.0175(9) 0.0164(9) -0.0014(7) 0.0025(7) -0.0008(7) C32 0.0196(9) 0.0225(10) 0.0199(9) 0.0004(8) 0.0054(7) -0.0010(8) C33 0.0199(9) 0.0309(11) 0.0245(10) -0.0043(9) 0.0074(7) 0.0007(8) C34 0.0174(9) 0.0313(11) 0.0286(11) -0.0071(9) 0.0025(8) 0.0021(8) C35 0.0244(10) 0.0310(11) 0.0189(10) -0.0044(9) -0.0009(7) 0.0043(9) C36 0.0220(9) 0.0252(10) 0.0174(9) -0.0018(8) 0.0041(7) -0.0006(8) N1 0.0254(9) 0.0310(10) 0.0206(8) -0.0013(7) 0.0062(7) 0.0029(7) N2 0.0193(8) 0.0224(8) 0.0163(8) -0.0003(6) 0.0049(6) 0.0013(6) N3 0.0212(8) 0.0316(10) 0.0163(8) 0.0029(7) 0.0048(6) 0.0032(7) N4 0.0172(7) 0.0225(8) 0.0169(8) 0.0018(7) 0.0034(6) 0.0012(6) O1 0.0292(7) 0.0205(7) 0.0168(7) 0.0012(6) 0.0056(5) -0.0004(6) O2 0.0248(7) 0.0180(7) 0.0160(7) -0.0007(5) 0.0049(5) 0.0001(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 C1 N2 1.479(2) . ? C1 C2 1.523(3) . ? C1 C11 1.530(3) . ? C1 H1 1.0000 . ? C2 C3 1.386(3) . ? C2 C7 1.399(3) . ? C3 C4 1.388(3) . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C4 H4 0.9500 . ? C5 C6 1.387(3) . ? C5 H5 0.9500 . ? C6 C7 1.392(3) . ? C6 H6 0.9500 . ? C7 C8 1.459(3) . ? C8 C9 1.370(3) . ? C8 N2 1.374(2) . ? C9 N1 1.378(3) . ? C9 H9 0.9500 . ? C10 N1 1.323(3) . ? C10 N2 1.344(2) . ? C10 H10 0.9500 . ? C11 C12 1.523(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 O1 1.425(2) . ? C12 C13 1.542(3) . ? C12 H12 1.0000 . ? C13 C14 1.531(3) . ? C13 C18 1.535(3) . ? C13 H13 1.0000 . ? C14 C15 1.531(3) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.526(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.517(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.531(3) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 N4 1.476(2) . ? C19 C20 1.519(3) . ? C19 C29 1.535(2) . ? C19 H19 1.0000 . ? C20 C21 1.382(3) . ? C20 C25 1.403(3) . ? C21 C22 1.393(3) . ? C21 H21 0.9500 . ? C22 C23 1.387(3) . ? C22 H22 0.9500 . ? C23 C24 1.390(3) . ? C23 H23 0.9500 . ? C24 C25 1.389(3) . ? C24 H24 0.9500 . ? C25 C26 1.458(3) . ? C26 C27 1.373(3) . ? C26 N4 1.378(3) . ? C27 N3 1.381(3) . ? C27 H27 0.9500 . ? C28 N3 1.327(3) . ? C28 N4 1.341(2) . ? C28 H28 0.9500 . ? C29 C30 1.520(2) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 O2 1.427(2) . ? C30 C31 1.531(2) . ? C30 H30 1.0000 . ? C31 C32 1.534(2) . ? C31 C36 1.535(2) . ? C31 H31 1.0000 . ? C32 C33 1.528(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.529(3) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.523(3) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.527(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O1 H1A 0.8400 . ? O2 H2 0.8400 . ? 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 N2 C1 C2 99.73(15) . . ? N2 C1 C11 113.69(16) . . ? C2 C1 C11 111.47(15) . . ? N2 C1 H1 110.5 . . ? C2 C1 H1 110.5 . . ? C11 C1 H1 110.5 . . ? C3 C2 C7 120.82(19) . . ? C3 C2 C1 127.92(18) . . ? C7 C2 C1 111.23(16) . . ? C2 C3 C4 118.3(2) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C3 C4 C5 121.05(19) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 120.82(19) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 118.4(2) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C6 C7 C2 120.52(18) . . ? C6 C7 C8 132.03(19) . . ? C2 C7 C8 107.45(17) . . ? C9 C8 N2 105.63(17) . . ? C9 C8 C7 146.67(19) . . ? N2 C8 C7 107.62(16) . . ? C8 C9 N1 109.46(18) . . ? C8 C9 H9 125.3 . . ? N1 C9 H9 125.3 . . ? N1 C10 N2 111.16(17) . . ? N1 C10 H10 124.4 . . ? N2 C10 H10 124.4 . . ? C12 C11 C1 114.83(15) . . ? C12 C11 H11A 108.6 . . ? C1 C11 H11A 108.6 . . ? C12 C11 H11B 108.6 . . ? C1 C11 H11B 108.6 . . ? H11A C11 H11B 107.5 . . ? O1 C12 C11 108.68(16) . . ? O1 C12 C13 112.39(16) . . ? C11 C12 C13 112.22(15) . . ? O1 C12 H12 107.8 . . ? C11 C12 H12 107.8 . . ? C13 C12 H12 107.8 . . ? C14 C13 C18 109.76(16) . . ? C14 C13 C12 114.50(16) . . ? C18 C13 C12 110.20(15) . . ? C14 C13 H13 107.4 . . ? C18 C13 H13 107.4 . . ? C12 C13 H13 107.4 . . ? C13 C14 C15 111.30(17) . . ? C13 C14 H14A 109.4 . . ? C15 C14 H14A 109.4 . . ? C13 C14 H14B 109.4 . . ? C15 C14 H14B 109.4 . . ? H14A C14 H14B 108.0 . . ? C16 C15 C14 111.71(17) . . ? C16 C15 H15A 109.3 . . ? C14 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? C14 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C17 C16 C15 110.67(17) . . ? C17 C16 H16A 109.5 . . ? C15 C16 H16A 109.5 . . ? C17 C16 H16B 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? C16 C17 C18 111.57(18) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C17 C18 C13 112.53(16) . . ? C17 C18 H18A 109.1 . . ? C13 C18 H18A 109.1 . . ? C17 C18 H18B 109.1 . . ? C13 C18 H18B 109.1 . . ? H18A C18 H18B 107.8 . . ? N4 C19 C20 99.89(14) . . ? N4 C19 C29 112.79(15) . . ? C20 C19 C29 111.06(15) . . ? N4 C19 H19 110.9 . . ? C20 C19 H19 110.9 . . ? C29 C19 H19 110.9 . . ? C21 C20 C25 120.35(18) . . ? C21 C20 C19 128.47(17) . . ? C25 C20 C19 111.13(16) . . ? C20 C21 C22 118.71(19) . . ? C20 C21 H21 120.6 . . ? C22 C21 H21 120.6 . . ? C23 C22 C21 120.81(18) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 120.96(19) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C25 C24 C23 118.19(19) . . ? C25 C24 H24 120.9 . . ? C23 C24 H24 120.9 . . ? C24 C25 C20 120.99(17) . . ? C24 C25 C26 131.64(18) . . ? C20 C25 C26 107.36(17) . . ? C27 C26 N4 105.50(17) . . ? C27 C26 C25 146.69(19) . . ? N4 C26 C25 107.57(16) . . ? C26 C27 N3 109.35(17) . . ? C26 C27 H27 125.3 . . ? N3 C27 H27 125.3 . . ? N3 C28 N4 111.01(18) . . ? N3 C28 H28 124.5 . . ? N4 C28 H28 124.5 . . ? C30 C29 C19 115.07(15) . . ? C30 C29 H29A 108.5 . . ? C19 C29 H29A 108.5 . . ? C30 C29 H29B 108.5 . . ? C19 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? O2 C30 C29 108.78(15) . . ? O2 C30 C31 112.82(15) . . ? C29 C30 C31 111.53(15) . . ? O2 C30 H30 107.8 . . ? C29 C30 H30 107.8 . . ? C31 C30 H30 107.8 . . ? C30 C31 C32 114.53(15) . . ? C30 C31 C36 111.57(15) . . ? C32 C31 C36 109.85(15) . . ? C30 C31 H31 106.8 . . ? C32 C31 H31 106.8 . . ? C36 C31 H31 106.8 . . ? C33 C32 C31 111.27(16) . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32B 109.4 . . ? C31 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C32 C33 C34 111.56(16) . . ? C32 C33 H33A 109.3 . . ? C34 C33 H33A 109.3 . . ? C32 C33 H33B 109.3 . . ? C34 C33 H33B 109.3 . . ? H33A C33 H33B 108.0 . . ? C35 C34 C33 110.85(16) . . ? C35 C34 H34A 109.5 . . ? C33 C34 H34A 109.5 . . ? C35 C34 H34B 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 108.1 . . ? C34 C35 C36 111.33(17) . . ? C34 C35 H35A 109.4 . . ? C36 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C36 C35 H35B 109.4 . . ? H35A C35 H35B 108.0 . . ? C35 C36 C31 111.49(15) . . ? C35 C36 H36A 109.3 . . ? C31 C36 H36A 109.3 . . ? C35 C36 H36B 109.3 . . ? C31 C36 H36B 109.3 . . ? H36A C36 H36B 108.0 . . ? C10 N1 C9 105.91(16) . . ? C10 N2 C8 107.83(16) . . ? C10 N2 C1 138.30(17) . . ? C8 N2 C1 113.78(15) . . ? C28 N3 C27 106.00(16) . . ? C28 N4 C26 108.12(16) . . ? C28 N4 C19 138.39(17) . . ? C26 N4 C19 113.48(15) . . ? C12 O1 H1A 109.5 . . ? C30 O2 H2 109.5 . . ? _refine_diff_density_max 0.164 _refine_diff_density_min -0.165 _refine_diff_density_rms 0.031 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in P2(1) CELL 1.54178 16.3071 4.7352 19.7305 90.000 97.866 90.000 ZERR 4.00 0.0003 0.0001 0.0004 0.000 0.001 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O UNIT 72 88 8 4 MERG 2 FMAP 2 PLAN 20 SIZE 0.020 0.020 0.050 ACTA 134.00 BOND $H LIST 4 WPDB -2 L.S. 10 TEMP -173.00 WGHT 0.041000 0.225800 FVAR 0.24909 C1 1 0.753476 0.950602 0.915714 11.00000 0.02273 0.02086 = 0.01610 -0.00138 0.00503 0.00070 AFIX 13 H1 2 0.757624 1.158741 0.908308 11.00000 -1.20000 AFIX 0 C2 1 0.807676 0.862806 0.981414 11.00000 0.01973 0.02244 = 0.01964 0.00033 0.00391 -0.00369 C3 1 0.801618 0.948883 1.047692 11.00000 0.02805 0.02840 = 0.02263 -0.00379 0.00626 -0.00160 AFIX 43 H3 2 0.761732 1.085404 1.056539 11.00000 -1.20000 AFIX 0 C4 1 0.855263 0.830684 1.100798 11.00000 0.03127 0.03670 = 0.01748 -0.00317 0.00309 -0.00722 AFIX 43 H4 2 0.852630 0.889657 1.146472 11.00000 -1.20000 AFIX 0 C5 1 0.912763 0.627464 1.088235 11.00000 0.02359 0.03498 = 0.02001 0.00599 -0.00284 -0.00686 AFIX 43 H5 2 0.947779 0.545482 1.125502 11.00000 -1.20000 AFIX 0 C6 1 0.919679 0.542771 1.021944 11.00000 0.01913 0.03170 = 0.02384 0.00231 0.00090 -0.00048 AFIX 43 H6 2 0.959328 0.404988 1.013346 11.00000 -1.20000 AFIX 0 C7 1 0.867120 0.664546 0.968323 11.00000 0.01927 0.02400 = 0.01972 -0.00077 0.00413 -0.00411 C8 1 0.859869 0.628571 0.894279 11.00000 0.01907 0.02332 = 0.02007 0.00194 0.00333 -0.00003 C9 1 0.892234 0.508522 0.840562 11.00000 0.02383 0.02972 = 0.02151 -0.00017 0.00474 0.00575 AFIX 43 H9 2 0.937629 0.381060 0.844566 11.00000 -1.20000 AFIX 0 C10 1 0.790962 0.772916 0.796964 11.00000 0.02269 0.02639 = 0.01708 0.00118 0.00463 0.00069 AFIX 43 H10 2 0.751650 0.868968 0.765112 11.00000 -1.20000 AFIX 0 C11 1 0.663226 0.863846 0.916400 11.00000 0.02213 0.02514 = 0.01746 -0.00030 0.00724 0.00063 AFIX 23 H11A 2 0.661484 0.659143 0.926307 11.00000 -1.20000 H11B 2 0.641660 0.964824 0.954193 11.00000 -1.20000 AFIX 0 C12 1 0.606064 0.922871 0.850230 11.00000 0.02356 0.01896 = 0.01637 0.00062 0.00697 0.00100 AFIX 13 H12 2 0.624191 0.800752 0.813686 11.00000 -1.20000 AFIX 0 C13 1 0.515105 0.849908 0.855952 11.00000 0.02264 0.02124 = 0.01673 0.00165 0.00529 0.00151 AFIX 13 H13 2 0.511999 0.641133 0.862797 11.00000 -1.20000 AFIX 0 C14 1 0.480865 0.991626 0.915928 11.00000 0.02480 0.02844 = 0.01873 -0.00213 0.00702 0.00037 AFIX 23 H14A 2 0.485087 1.199239 0.911602 11.00000 -1.20000 H14B 2 0.514534 0.934528 0.959359 11.00000 -1.20000 AFIX 0 C15 1 0.390371 0.909942 0.917865 11.00000 0.02544 0.03624 = 0.02337 -0.00068 0.01037 -0.00154 AFIX 23 H15A 2 0.386909 0.704583 0.926451 11.00000 -1.20000 H15B 2 0.369528 1.010393 0.956069 11.00000 -1.20000 AFIX 0 C16 1 0.335924 0.982846 0.850965 11.00000 0.02273 0.03481 = 0.03164 0.00333 0.00695 0.00247 AFIX 23 H16A 2 0.278679 0.917137 0.853002 11.00000 -1.20000 H16B 2 0.334465 1.190297 0.844678 11.00000 -1.20000 AFIX 0 C17 1 0.368914 0.844998 0.790792 11.00000 0.02428 0.03736 = 0.02299 0.00374 0.00007 -0.00058 AFIX 23 H17A 2 0.335411 0.907183 0.747727 11.00000 -1.20000 H17B 2 0.363468 0.637404 0.794126 11.00000 -1.20000 AFIX 0 C18 1 0.459796 0.920851 0.788798 11.00000 0.02607 0.03379 = 0.01663 0.00270 0.00532 0.00075 AFIX 23 H18A 2 0.464049 1.125362 0.779454 11.00000 -1.20000 H18B 2 0.480039 0.816904 0.750831 11.00000 -1.20000 AFIX 0 C19 1 0.742770 0.271920 0.546732 11.00000 0.02035 0.02034 = 0.01534 0.00273 0.00497 -0.00060 AFIX 13 H19 2 0.742354 0.481034 0.539613 11.00000 -1.20000 AFIX 0 C20 1 0.693611 0.122947 0.486119 11.00000 0.01828 0.02009 = 0.01777 0.00186 0.00056 0.00293 C21 1 0.706256 0.127790 0.418297 11.00000 0.02307 0.03001 = 0.01966 0.00425 0.00433 0.00072 AFIX 43 H21 2 0.748824 0.240898 0.403959 11.00000 -1.20000 AFIX 0 C22 1 0.655360 -0.036445 0.371344 11.00000 0.02651 0.03967 = 0.01544 -0.00001 0.00331 0.00167 AFIX 43 H22 2 0.663451 -0.035465 0.324569 11.00000 -1.20000 AFIX 0 C23 1 0.593004 -0.201403 0.392069 11.00000 0.02342 0.03952 = 0.02245 -0.00639 -0.00099 -0.00046 AFIX 43 H23 2 0.558666 -0.310681 0.359199 11.00000 -1.20000 AFIX 0 C24 1 0.580049 -0.209092 0.460220 11.00000 0.01930 0.03206 = 0.02492 -0.00115 0.00282 -0.00263 AFIX 43 H24 2 0.537683 -0.323483 0.474441 11.00000 -1.20000 AFIX 0 C25 1 0.630733 -0.044976 0.506963 11.00000 0.01662 0.02449 = 0.01734 0.00333 0.00264 0.00377 C26 1 0.631895 -0.000752 0.580205 11.00000 0.01733 0.02160 = 0.01979 0.00189 0.00093 0.00179 C27 1 0.594293 -0.054670 0.637002 11.00000 0.01869 0.02935 = 0.02016 0.00367 0.00411 0.00049 AFIX 43 H27 2 0.550112 -0.183916 0.638921 11.00000 -1.20000 AFIX 0 C28 1 0.689974 0.254783 0.666971 11.00000 0.01998 0.02787 = 0.01674 -0.00075 0.00182 0.00404 AFIX 43 H28 2 0.725463 0.385512 0.693115 11.00000 -1.20000 AFIX 0 C29 1 0.831782 0.159252 0.560190 11.00000 0.01914 0.02211 = 0.01722 -0.00006 0.00406 -0.00200 AFIX 23 H29A 2 0.830212 -0.048708 0.555004 11.00000 -1.20000 H29B 2 0.863114 0.236050 0.524749 11.00000 -1.20000 AFIX 0 C30 1 0.878422 0.230514 0.630139 11.00000 0.02065 0.01683 = 0.01625 0.00094 0.00648 -0.00166 AFIX 13 H30 2 0.850582 0.130114 0.665313 11.00000 -1.20000 AFIX 0 C31 1 0.968289 0.128624 0.637252 11.00000 0.01985 0.01751 = 0.01636 -0.00136 0.00252 -0.00082 AFIX 13 H31 2 0.966688 -0.074451 0.623223 11.00000 -1.20000 AFIX 0 C32 1 1.022254 0.282890 0.591185 11.00000 0.01957 0.02252 = 0.01988 0.00041 0.00539 -0.00097 AFIX 23 H32A 2 0.996652 0.266155 0.542878 11.00000 -1.20000 H32B 2 1.025105 0.485920 0.603254 11.00000 -1.20000 AFIX 0 C33 1 1.109742 0.160398 0.599015 11.00000 0.01988 0.03087 = 0.02449 -0.00431 0.00737 0.00070 AFIX 23 H33A 2 1.143756 0.270428 0.570538 11.00000 -1.20000 H33B 2 1.107328 -0.037032 0.582350 11.00000 -1.20000 AFIX 0 C34 1 1.150615 0.166928 0.673534 11.00000 0.01741 0.03130 = 0.02858 -0.00714 0.00250 0.00215 AFIX 23 H34A 2 1.205454 0.074142 0.677289 11.00000 -1.20000 H34B 2 1.159184 0.365409 0.688624 11.00000 -1.20000 AFIX 0 C35 1 1.097085 0.016362 0.719731 11.00000 0.02444 0.03102 = 0.01892 -0.00439 -0.00089 0.00431 AFIX 23 H35A 2 1.122872 0.034592 0.767955 11.00000 -1.20000 H35B 2 1.094036 -0.187087 0.708099 11.00000 -1.20000 AFIX 0 C36 1 1.009742 0.139514 0.711898 11.00000 0.02196 0.02519 = 0.01739 -0.00176 0.00411 -0.00059 AFIX 23 H36A 2 1.012378 0.337965 0.727837 11.00000 -1.20000 H36B 2 0.975887 0.031798 0.740948 11.00000 -1.20000 AFIX 0 N1 3 0.848752 0.601287 0.779862 11.00000 0.02539 0.03102 = 0.02058 -0.00128 0.00624 0.00289 N2 3 0.795113 0.793692 0.865288 11.00000 0.01931 0.02240 = 0.01633 -0.00025 0.00487 0.00129 N3 3 0.630729 0.108325 0.690892 11.00000 0.02122 0.03159 = 0.01631 0.00294 0.00483 0.00316 N4 3 0.693085 0.193737 0.601007 11.00000 0.01717 0.02251 = 0.01695 0.00177 0.00340 0.00125 O1 4 0.616265 1.209777 0.831274 11.00000 0.02921 0.02047 = 0.01680 0.00116 0.00561 -0.00041 AFIX 147 H1A 2 0.618246 1.219276 0.789016 11.00000 -1.50000 AFIX 0 O2 4 0.871756 0.526806 0.641537 11.00000 0.02478 0.01800 = 0.01604 -0.00069 0.00485 0.00015 AFIX 147 H2 2 0.869680 0.556563 0.683238 11.00000 -1.50000 AFIX 0 HKLF 4 REM shelxt_a.res in P2(1) REM R1 = 0.0299 for 5232 Fo > 4sig(Fo) and 0.0323 for all 5518 data REM 381 parameters refined using 1 restraints END WGHT 0.0410 0.2259 REM Highest difference peak 0.164, deepest hole -0.165, 1-sigma level 0.031 Q1 1 0.5033 0.9598 0.8824 11.00000 0.05 0.16 Q2 1 0.7208 0.2044 0.5113 11.00000 0.05 0.15 Q3 1 0.8640 0.6037 0.9296 11.00000 0.05 0.15 Q4 1 0.5602 0.8745 0.8524 11.00000 0.05 0.14 Q5 1 0.8452 0.7698 0.8796 11.00000 0.05 0.14 Q6 1 0.6182 0.1393 0.7276 11.00000 0.05 0.13 Q7 1 0.8971 0.6497 0.8736 11.00000 0.05 0.13 Q8 1 0.3957 0.7094 0.9084 11.00000 0.05 0.13 Q9 1 0.6183 -0.0413 0.5446 11.00000 0.05 0.13 Q10 1 0.6794 -0.0534 0.5001 11.00000 0.05 0.13 Q11 1 0.7058 0.8818 0.9123 11.00000 0.05 0.12 Q12 1 0.5877 0.0289 0.5962 11.00000 0.05 0.12 Q13 1 0.8201 0.7047 0.9743 11.00000 0.05 0.12 Q14 1 0.7851 0.1951 0.5536 11.00000 0.05 0.12 Q15 1 0.8761 0.5424 0.9902 11.00000 0.05 0.12 Q16 1 0.7779 0.9139 0.9540 11.00000 0.05 0.12 Q17 1 0.9243 0.1640 0.6280 11.00000 0.05 0.12 Q18 1 1.0543 0.1007 0.7183 11.00000 0.05 0.12 Q19 1 1.0662 0.2215 0.5981 11.00000 0.05 0.11 Q20 1 0.9924 0.2380 0.6203 11.00000 0.05 0.11 ; _shelx_res_checksum 71365 _shelx_hkl_file ; 1 0 0 0.19 0.13 1 0 0 0.34 0.13 1 0 0 0.43 0.13 -1 0 0 0.28 0.12 -1 0 0 0.24 0.07 -1 0 0 0.44 0.16 -1 0 0 0.51 0.13 -1 0 0 0.45 0.13 2 0 0 34.67 1.58 -2 0 0 35.17 1.47 2 0 0 33.58 1.51 -2 0 0 34.86 1.54 -2 0 0 31.51 1.40 -2 0 0 33.58 1.48 -3 0 0 0.43 0.35 -3 0 0 0.08 0.27 3 0 0 0.41 0.39 -3 0 0 0.24 0.16 3 0 0 0.18 0.33 -3 0 0 0.62 0.38 4 0 0 829.70 33.59 -4 0 0 856.82 33.60 4 0 0 910.77 33.80 -4 0 0 840.27 33.46 -4 0 0 819.20 33.71 -4 0 0 832.64 33.58 4 0 0 907.61 33.66 5 0 0 2.02 0.69 -5 0 0 1.48 0.59 5 0 0 1.26 0.50 5 0 0 1.52 0.47 -5 0 0 2.09 0.61 5 0 0 1.06 0.57 -6 0 0 111.63 4.70 -6 0 0 110.43 4.89 -6 0 0 105.84 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107.00 4.54 -8 -2 0 11.82 0.93 8 -2 0 11.68 0.92 8 -2 0 12.86 1.02 -8 -2 0 12.01 0.94 -8 -2 0 12.40 0.92 8 -2 0 11.97 0.77 8 -2 0 11.68 0.89 -8 -2 0 12.57 1.06 8 -2 0 9.63 1.11 8 2 0 10.96 0.93 8 2 0 11.42 0.86 -8 2 0 11.76 0.90 8 2 0 13.01 1.34 8 2 0 11.28 1.02 -8 2 0 11.90 0.93 -8 2 0 10.04 0.96 9 -2 0 0.98 0.57 -9 -2 0 0.99 0.45 -9 -2 0 1.66 0.74 9 -2 0 0.96 0.31 -9 -2 0 1.42 0.54 -9 -2 0 0.54 0.62 9 -2 0 1.23 0.66 9 -2 0 0.95 0.51 9 -2 0 0.55 0.71 -9 -2 0 0.47 0.48 9 -2 0 0.81 0.45 9 2 0 0.78 0.41 -9 2 0 1.07 0.54 9 2 0 1.70 0.85 9 2 0 1.26 0.55 -9 2 0 0.92 0.47 9 2 0 2.12 0.54 9 2 0 1.33 0.66 -9 2 0 1.28 0.52 -9 2 0 0.70 0.47 10 -2 0 8.94 0.86 10 -2 0 9.39 1.16 10 -2 0 7.02 0.62 10 -2 0 8.04 1.11 -10 -2 0 7.63 0.69 10 -2 0 7.90 0.63 -10 -2 0 8.85 1.03 -10 -2 0 7.41 0.78 -10 -2 0 7.90 1.09 -10 -2 0 7.73 0.96 10 -2 0 5.68 0.93 -10 -2 0 6.93 0.84 10 -2 0 8.49 0.89 10 2 0 7.42 0.83 10 2 0 6.28 1.18 -10 2 0 8.82 0.96 -10 2 0 7.75 0.94 10 2 0 7.51 0.97 10 2 0 7.07 0.89 -10 2 0 7.11 0.84 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17.63 1.55 13 -2 0 18.67 1.18 -13 -2 0 18.62 1.30 13 -2 0 18.24 0.96 13 -2 0 18.11 0.99 13 -2 0 18.00 1.23 13 -2 0 18.20 1.61 13 -2 0 18.70 1.26 -13 -2 0 17.63 1.24 -13 -2 0 16.32 1.19 13 -2 0 17.82 1.40 -13 2 0 17.76 1.10 13 2 0 17.52 1.05 13 2 0 17.26 1.02 13 2 0 16.95 1.00 -13 2 0 18.74 1.37 13 2 0 19.10 1.24 13 2 0 18.24 1.52 -13 2 0 12.58 1.21 -13 2 0 17.42 1.22 13 2 0 16.29 0.98 13 2 0 19.10 1.32 -13 2 0 18.65 1.20 -13 2 0 17.82 1.02 -13 2 0 16.68 1.24 -13 2 0 16.64 1.07 13 2 0 17.92 1.16 -14 -2 0 4.85 1.03 14 -2 0 4.23 0.81 14 -2 0 4.86 0.82 14 -2 0 5.10 1.15 -14 -2 0 3.99 0.64 14 -2 0 5.35 0.92 14 -2 0 4.58 1.15 14 -2 0 4.71 0.86 -14 -2 0 4.83 1.09 -14 -2 0 4.22 0.80 14 -2 0 4.61 0.88 14 -2 0 4.70 0.48 -14 -2 0 5.37 0.67 14 -2 0 5.27 0.88 14 -2 0 4.34 1.13 -14 -2 0 4.12 0.87 -14 -2 0 3.79 0.86 -14 2 0 4.90 0.89 14 2 0 4.32 0.63 14 2 0 4.41 0.72 14 2 0 5.69 0.78 14 2 0 3.80 0.55 14 2 0 4.62 0.63 -14 2 0 4.79 0.70 -14 2 0 4.17 0.83 -14 2 0 5.05 0.80 -14 2 0 4.27 0.92 14 2 0 3.94 0.71 -14 2 0 4.42 0.73 15 -2 0 17.64 1.20 -15 -2 0 16.75 0.94 -15 -2 0 18.49 1.52 -15 -2 0 18.70 1.22 15 -2 0 18.35 1.21 15 -2 0 17.21 1.44 -15 -2 0 16.45 1.20 15 -2 0 18.35 1.19 -15 -2 0 17.56 1.14 -15 -2 0 18.15 0.97 -15 -2 0 17.26 1.26 15 -2 0 16.29 1.45 15 -2 0 16.13 1.14 -15 2 0 15.99 1.04 -15 2 0 18.65 1.12 -15 2 0 19.42 1.21 -15 2 0 17.94 1.18 -15 2 0 17.52 1.09 15 2 0 18.81 1.07 -15 2 0 19.10 1.17 -15 2 0 16.63 1.10 15 2 0 17.56 1.00 15 2 0 18.60 0.98 16 -2 0 0.71 0.63 -16 -2 0 3.54 0.78 16 -2 0 1.75 0.55 16 -2 0 0.99 0.74 -16 -2 0 2.17 0.54 16 -2 0 2.12 0.51 16 -2 0 2.64 0.79 -16 -2 0 2.58 0.67 16 -2 0 1.25 0.49 -16 -2 0 1.33 0.76 -16 -2 0 1.80 0.60 -16 -2 0 1.86 0.41 -16 -2 0 2.11 0.38 -16 2 0 1.04 0.44 -16 2 0 1.13 0.43 16 2 0 2.00 0.49 16 2 0 2.66 0.66 -16 2 0 3.15 0.93 -16 2 0 2.95 0.58 -16 2 0 2.08 0.42 16 2 0 0.90 0.31 16 2 0 2.11 0.60 -16 2 0 1.52 0.52 17 -2 0 0.98 0.40 -17 -2 0 1.65 0.41 17 -2 0 0.55 0.57 17 -2 0 1.14 0.39 17 -2 0 1.43 0.46 -17 -2 0 0.62 0.40 -17 -2 0 2.13 0.55 -17 2 0 1.48 0.37 17 2 0 0.66 0.36 17 2 0 1.50 0.43 -17 2 0 1.74 0.48 17 2 0 0.80 0.26 -17 2 0 1.04 0.43 -17 2 0 1.63 0.76 17 2 0 1.03 0.33 18 -2 0 0.36 0.44 -18 -2 0 0.56 0.28 18 -2 0 1.14 0.34 -18 -2 0 0.91 0.31 -18 2 0 0.26 0.31 18 2 0 0.83 0.37 18 2 0 0.64 0.33 -18 2 0 0.76 0.26 18 2 0 0.80 0.21 -18 2 0 0.82 0.29 -18 2 0 1.03 0.58 0 -3 0 0.06 0.41 0 -3 0 -0.09 0.45 0 -3 0 0.16 0.25 0 -3 0 -0.29 0.39 0 -3 0 -0.13 0.45 0 3 0 -0.09 0.44 0 3 0 -0.26 0.34 0 3 0 -0.15 0.33 0 3 0 0.25 0.56 0 3 0 -0.06 0.66 1 -3 0 62.06 2.93 1 -3 0 62.53 2.61 -1 -3 0 63.92 2.64 1 -3 0 63.34 2.76 -1 -3 0 62.34 2.97 -1 -3 0 60.78 2.83 -1 -3 0 62.89 2.75 -1 -3 0 62.95 2.95 1 -3 0 64.24 2.97 1 -3 0 65.03 2.86 -1 3 0 58.84 2.92 1 3 0 55.71 3.33 1 3 0 64.94 2.80 1 3 0 62.37 2.87 -1 3 0 65.29 2.79 -1 3 0 61.77 2.85 1 3 0 64.23 2.78 -1 3 0 61.32 3.42 -1 3 0 64.43 2.82 1 3 0 62.29 2.92 2 -3 0 14.20 0.94 -2 -3 0 13.90 1.11 2 -3 0 15.22 1.05 2 -3 0 14.64 1.15 2 -3 0 14.02 1.12 2 -3 0 14.47 0.76 -2 -3 0 15.76 1.18 -2 -3 0 12.70 0.80 -2 -3 0 15.98 0.99 -2 -3 0 15.01 1.05 2 3 0 15.73 1.08 2 3 0 13.97 0.92 -2 3 0 13.93 1.00 -2 3 0 14.70 1.17 -2 3 0 12.58 1.39 2 3 0 13.18 1.10 -2 3 0 13.91 0.92 2 3 0 15.62 0.96 2 3 0 12.55 1.36 2 3 0 13.09 1.12 -2 3 0 14.75 0.97 -3 -3 0 5.60 0.77 3 -3 0 5.23 0.43 3 -3 0 4.71 0.67 -3 -3 0 6.30 0.97 -3 -3 0 4.63 0.69 3 -3 0 5.26 0.82 -3 -3 0 5.29 0.58 3 -3 0 5.09 0.67 -3 -3 0 4.86 0.67 3 -3 0 5.93 0.85 3 3 0 4.99 0.71 3 3 0 5.23 0.69 3 3 0 4.68 0.61 -3 3 0 5.20 1.03 3 3 0 4.26 0.97 3 3 0 5.71 1.01 -3 3 0 4.90 0.61 -3 3 0 4.94 0.77 -3 3 0 6.38 0.68 -3 3 0 4.26 0.98 3 3 0 4.69 0.75 3 3 0 5.71 0.59 -4 -3 0 1.55 0.53 4 -3 0 1.15 0.52 -4 -3 0 1.31 0.35 4 -3 0 1.33 0.58 -4 -3 0 1.18 0.47 4 -3 0 1.27 0.61 -4 -3 0 1.26 0.58 -4 -3 0 2.89 0.78 4 -3 0 1.33 0.46 4 -3 0 1.83 0.58 4 -3 0 1.12 0.27 -4 3 0 1.31 0.48 4 3 0 0.83 0.41 -4 3 0 2.06 0.53 4 3 0 1.54 0.47 4 3 0 1.67 0.46 -4 3 0 1.49 0.67 -4 3 0 -0.08 0.71 -4 3 0 1.26 0.54 4 3 0 -0.09 0.59 4 3 0 1.59 0.60 4 3 0 2.51 0.64 -4 3 0 0.97 0.50 5 -3 0 16.89 1.26 -5 -3 0 19.23 1.23 -5 -3 0 18.59 1.12 5 -3 0 17.65 1.08 5 -3 0 16.79 1.24 5 -3 0 17.38 1.28 -5 -3 0 16.99 1.33 -5 -3 0 18.48 1.30 -5 -3 0 16.35 0.95 5 -3 0 17.14 1.15 5 3 0 14.82 1.17 -5 3 0 19.94 1.20 -5 3 0 16.51 1.23 -5 3 0 17.31 1.76 -5 3 0 17.75 1.14 5 3 0 15.73 1.56 5 3 0 17.56 1.31 5 3 0 15.80 1.11 5 3 0 17.42 1.10 5 3 0 18.75 1.10 5 3 0 15.73 1.31 -5 3 0 15.06 1.10 -6 -3 0 9.65 0.90 -6 -3 0 8.63 0.98 6 -3 0 7.25 0.98 -6 -3 0 9.60 0.89 -6 -3 0 8.69 0.96 -6 -3 0 8.11 0.66 6 -3 0 10.19 1.02 6 -3 0 9.36 1.04 6 -3 0 8.69 0.82 6 -3 0 9.35 0.94 6 -3 0 8.43 0.59 -6 -3 0 9.27 0.68 -6 3 0 8.38 1.36 6 3 0 7.36 1.22 6 3 0 8.70 0.97 -6 3 0 10.09 0.90 6 3 0 9.28 0.99 6 3 0 8.48 0.82 -6 3 0 7.82 1.01 6 3 0 8.86 0.75 6 3 0 9.52 1.11 -6 3 0 9.37 0.82 6 3 0 7.97 0.81 7 -3 0 28.54 1.53 7 -3 0 33.91 1.78 7 -3 0 31.13 1.38 -7 -3 0 29.56 1.75 -7 -3 0 31.79 1.65 -7 -3 0 31.38 1.74 -7 -3 0 30.61 1.88 7 -3 0 32.06 1.88 -7 -3 0 31.04 1.43 -7 -3 0 29.48 1.41 7 -3 0 29.08 1.76 7 3 0 30.20 1.70 7 3 0 31.86 1.63 -7 3 0 22.19 2.19 -7 3 0 32.85 1.74 -7 3 0 29.43 1.64 -7 3 0 30.20 1.69 7 3 0 29.75 1.58 -7 3 0 30.33 1.62 7 3 0 26.60 2.22 7 3 0 31.75 1.65 7 3 0 31.37 1.82 -8 -3 0 -0.14 0.48 8 -3 0 0.11 0.31 -8 -3 0 -0.05 0.53 8 -3 0 0.59 0.50 -8 -3 0 0.26 0.36 -8 -3 0 0.97 0.76 8 -3 0 -0.30 0.66 8 -3 0 -0.06 0.63 8 -3 0 0.43 0.71 8 -3 0 0.49 0.64 -8 -3 0 -0.23 0.57 -8 3 0 -0.24 0.52 -8 3 0 -0.36 0.58 8 3 0 -0.21 0.68 8 3 0 -0.08 0.54 -8 3 0 0.23 0.50 8 3 0 0.09 0.48 -8 3 0 0.90 0.61 8 3 0 -0.48 0.44 9 -3 0 16.91 1.41 -9 -3 0 17.10 1.21 -9 -3 0 17.90 1.38 -9 -3 0 15.10 1.18 9 -3 0 17.10 1.37 -9 -3 0 18.13 1.33 -9 -3 0 17.00 0.94 9 -3 0 17.47 1.30 -9 -3 0 17.38 1.43 -9 3 0 17.89 1.33 -9 3 0 18.23 1.20 -9 3 0 18.36 1.32 9 3 0 15.94 1.27 -9 3 0 12.96 1.15 9 3 0 17.64 1.27 9 3 0 14.50 1.33 9 3 0 17.39 1.19 -10 -3 0 1.74 0.75 10 -3 0 1.78 0.80 10 -3 0 1.15 0.63 10 -3 0 2.29 0.87 -10 -3 0 1.65 0.75 -10 -3 0 0.84 0.54 -10 -3 0 1.43 0.61 -10 -3 0 1.87 0.80 -10 -3 0 1.97 0.53 -10 3 0 1.56 0.64 10 3 0 0.01 0.66 -10 3 0 1.61 0.58 10 3 0 2.90 0.71 10 3 0 1.88 0.61 10 3 0 2.44 0.67 -10 3 0 1.77 0.79 10 3 0 3.19 0.73 -10 3 0 1.81 0.64 -11 -3 0 15.06 1.32 11 -3 0 17.04 1.44 11 -3 0 15.67 0.91 -11 -3 0 14.81 1.08 -11 -3 0 12.48 1.12 -11 -3 0 15.72 1.02 11 -3 0 13.86 1.13 11 -3 0 14.47 1.41 11 -3 0 15.71 1.10 11 -3 0 17.02 1.15 -11 -3 0 15.09 0.87 -11 -3 0 14.43 1.40 -11 -3 0 15.46 1.25 11 -3 0 12.24 1.16 -11 -3 0 14.92 0.79 -11 -3 0 14.64 1.13 11 -3 0 14.68 1.36 -11 -3 0 14.16 0.95 -11 -3 0 14.49 0.86 -11 3 0 14.66 1.09 -11 3 0 14.14 1.01 -11 3 0 10.96 1.17 11 3 0 15.47 1.08 11 3 0 15.26 1.17 -11 3 0 13.69 0.93 11 3 0 15.05 1.12 -11 3 0 15.14 1.27 11 3 0 11.14 1.24 11 3 0 14.52 0.86 11 3 0 15.20 1.01 -11 3 0 12.90 1.13 11 3 0 17.74 1.00 11 3 0 13.95 0.90 -11 3 0 15.00 1.13 -12 -3 0 2.84 0.48 -12 -3 0 3.24 0.78 -12 -3 0 2.90 0.85 12 -3 0 2.15 0.64 -12 -3 0 3.78 1.04 12 -3 0 3.10 0.88 12 -3 0 3.03 1.12 12 -3 0 2.45 0.89 -12 -3 0 3.35 0.62 12 -3 0 4.37 0.78 -12 -3 0 2.59 0.66 12 -3 0 4.43 0.87 -12 -3 0 2.88 0.57 12 -3 0 3.86 1.08 -12 -3 0 1.53 0.41 12 -3 0 2.50 0.56 12 3 0 3.14 0.54 12 3 0 3.27 0.69 12 3 0 2.29 0.57 -12 3 0 2.01 0.58 12 3 0 4.10 0.71 12 3 0 2.67 0.62 -12 3 0 3.06 0.54 -12 3 0 2.36 0.67 12 3 0 3.09 0.83 -12 3 0 2.55 0.61 -12 3 0 3.63 1.27 -12 3 0 2.87 0.65 -12 3 0 3.17 0.80 12 3 0 2.64 0.60 -13 -3 0 7.09 0.72 13 -3 0 6.88 0.83 -13 -3 0 8.26 0.91 13 -3 0 6.08 1.09 13 -3 0 7.99 0.94 -13 -3 0 6.90 0.97 -13 -3 0 7.94 0.86 13 -3 0 6.57 1.11 -13 -3 0 8.73 1.11 13 -3 0 7.61 1.08 13 -3 0 7.07 0.91 13 -3 0 7.31 0.89 13 -3 0 7.10 0.62 -13 -3 0 7.99 0.45 13 3 0 6.74 0.75 -13 3 0 6.71 0.97 13 3 0 7.53 0.68 -13 3 0 7.46 0.81 13 3 0 8.01 0.67 -13 3 0 7.60 0.88 13 3 0 6.58 0.77 -13 3 0 8.25 0.81 13 3 0 7.60 0.61 -13 3 0 8.28 0.75 -13 3 0 7.03 1.26 13 3 0 7.84 0.77 -13 3 0 7.47 0.71 14 -3 0 1.87 0.46 -14 -3 0 2.70 0.78 -14 -3 0 2.39 0.70 14 -3 0 2.62 0.69 14 -3 0 1.20 0.45 14 -3 0 1.54 0.70 -14 -3 0 3.50 0.72 14 -3 0 2.03 0.52 -14 -3 0 1.18 0.65 14 -3 0 2.93 0.91 14 -3 0 3.59 0.88 -14 3 0 3.69 1.10 -14 3 0 3.09 0.69 14 3 0 3.06 0.54 14 3 0 3.10 0.61 14 3 0 3.00 0.49 -14 3 0 2.48 0.61 14 3 0 3.16 0.45 -14 3 0 2.96 0.64 -14 3 0 3.05 0.76 -15 -3 0 1.90 0.55 15 -3 0 2.85 0.56 15 -3 0 3.02 0.60 -15 -3 0 2.60 0.62 15 -3 0 3.59 0.67 15 -3 0 1.58 0.49 -15 -3 0 3.10 0.63 15 3 0 3.15 0.56 15 3 0 2.85 0.45 -15 3 0 2.30 0.66 -15 3 0 2.56 0.52 -15 3 0 3.21 0.57 -15 3 0 2.56 0.82 -16 -3 0 2.88 0.47 -16 -3 0 2.73 0.50 16 -3 0 2.76 0.54 -16 3 0 2.59 0.55 -16 3 0 2.40 0.75 -16 3 0 2.46 0.48 -16 3 0 1.44 0.40 16 3 0 2.55 0.39 16 3 0 2.69 0.36 16 3 0 2.89 0.44 0 -4 0 8.51 0.99 0 -4 0 9.25 1.14 0 -4 0 8.66 1.13 0 4 0 8.22 1.02 0 4 0 8.95 0.91 0 4 0 10.14 1.25 0 4 0 8.60 0.98 0 4 0 8.56 1.05 1 -4 0 8.63 0.97 -1 -4 0 8.01 1.11 1 -4 0 8.25 1.11 -1 -4 0 7.66 1.11 -1 -4 0 9.22 0.99 1 -4 0 7.07 1.03 1 4 0 6.94 0.99 1 4 0 8.82 1.23 -1 4 0 9.93 0.99 1 4 0 8.84 0.94 -1 4 0 10.84 1.36 1 4 0 9.43 0.96 -1 4 0 7.48 1.02 1 4 0 7.51 0.79 -1 4 0 8.43 0.88 1 4 0 7.28 0.96 -1 4 0 6.61 1.00 2 -4 0 1.54 0.65 -2 -4 0 2.17 0.76 -2 -4 0 1.06 0.74 2 -4 0 1.48 0.77 2 -4 0 1.93 0.77 -2 -4 0 1.31 0.63 2 4 0 1.34 0.62 -2 4 0 0.59 0.58 2 4 0 1.66 0.78 2 4 0 1.79 0.60 2 4 0 0.99 0.60 2 4 0 1.97 0.67 -2 4 0 1.80 0.64 -2 4 0 1.97 0.83 -2 4 0 1.41 0.55 -2 4 0 1.42 0.53 2 4 0 2.05 0.57 3 -4 0 4.09 1.00 3 -4 0 2.53 0.87 -3 -4 0 4.13 0.96 3 -4 0 2.94 0.75 -3 -4 0 4.16 0.89 -3 -4 0 3.94 0.84 3 4 0 4.49 1.17 -3 4 0 3.65 0.89 -3 4 0 4.46 1.10 3 4 0 3.04 0.84 3 4 0 3.51 0.69 3 4 0 4.50 0.88 3 4 0 2.55 0.74 -3 4 0 4.10 0.91 3 4 0 3.75 0.90 -3 4 0 4.60 0.89 -3 4 0 2.62 0.71 -4 -4 0 4.33 0.85 4 -4 0 4.70 0.87 4 -4 0 4.63 0.92 4 -4 0 5.61 1.06 -4 -4 0 4.30 1.00 4 4 0 4.38 0.79 -4 4 0 5.77 0.87 4 4 0 3.46 0.81 -4 4 0 3.91 0.86 -4 4 0 5.72 1.27 4 4 0 2.97 0.89 4 4 0 3.83 0.84 4 4 0 3.50 0.83 4 4 0 5.40 0.93 -4 4 0 3.71 0.92 -4 4 0 4.28 0.77 -5 -4 0 0.33 0.62 -5 -4 0 0.41 0.69 5 -4 0 0.52 0.78 -5 -4 0 0.85 0.35 5 -4 0 -0.12 0.69 -5 -4 0 0.40 0.46 5 -4 0 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