data_SCSKNCN _audit_creation_method 'SHELXL-2014/7' _shelx_SHELXL_version_number '2014/7' _chemical_name_systematic '(4aS,4bR,6S,10bR)-8,9-dimethoxy-1,1,4a,10b-tetramethyl-7-nitro-1,2,3,4,4a,4b,5,6,10b,11,12,12a,-dodecahydrochrysene-6-carbonitrile' _chemical_name_common ? _chemical_melting_point 513K _chemical_formula_moiety 'C25 H34 N2 O4' _chemical_formula_sum 'C25 H34 N2 O4' _chemical_formula_weight 426.54 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' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.0956(2) _cell_length_b 15.5691(7) _cell_length_c 24.6358(11) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2338.01(17) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3204 _cell_measurement_theta_min 2.744 _cell_measurement_theta_max 25.023 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.212 _exptl_crystal_F_000 920 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_absorpt_coefficient_mu 0.082 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type 'none' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 26551 _diffrn_reflns_av_unetI/netI 0.0328 _diffrn_reflns_av_R_equivalents 0.0525 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.744 _diffrn_reflns_theta_max 25.023 _diffrn_reflns_theta_full 25.023 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measured_fraction_theta_full 0.994 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_Laue_measured_fraction_full 0.994 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_point_group_measured_fraction_full 0.996 _reflns_number_total 4117 _reflns_number_gt 3204 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.724 _reflns_Friedel_fraction_max 0.999 _reflns_Friedel_fraction_full 0.999 _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 ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion twin. ; _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^)+(0.0675P)^2^+0.7882P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 2(3) _chemical_absolute_configuration rm _refine_ls_number_reflns 4117 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0874 _refine_ls_R_factor_gt 0.0590 _refine_ls_wR_factor_ref 0.1581 _refine_ls_wR_factor_gt 0.1397 _refine_ls_goodness_of_fit_ref 1.185 _refine_ls_restrained_S_all 1.185 _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_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 O1 O 0.3482(12) 0.8421(3) 0.6197(2) 0.127(2) Uani 1 1 d . . . . . O2 O 0.6786(13) 0.8643(3) 0.5893(2) 0.136(2) Uani 1 1 d . . . . . O3 O 0.3970(7) 0.6844(3) 0.55366(14) 0.0729(11) Uani 1 1 d . . . . . O4 O 0.4722(6) 0.5197(2) 0.58775(13) 0.0637(10) Uani 1 1 d . . . . . N2 N 0.5274(9) 0.8887(3) 0.7532(2) 0.0754(13) Uani 1 1 d . . . . . N1 N 0.5409(13) 0.8212(3) 0.6109(2) 0.0850(16) Uani 1 1 d . . . . . C10 C 0.9612(7) 0.5373(3) 0.82890(17) 0.0440(10) Uani 1 1 d . . . . . H10A H 0.8981 0.4889 0.8482 0.053 Uiso 1 1 calc R U . . . H10B H 1.1158 0.5256 0.8233 0.053 Uiso 1 1 calc R U . . . C15 C 0.6959(7) 0.5726(3) 0.66252(16) 0.0426(10) Uani 1 1 d . . . . . H15 H 0.7242 0.5170 0.6744 0.051 Uiso 1 1 calc R U . . . C4 C 0.9806(7) 0.6073(3) 0.92487(18) 0.0493(11) Uani 1 1 d . . . . . C8 C 0.9373(6) 0.6232(2) 0.74059(16) 0.0378(9) Uani 1 1 d . . . . . C9 C 0.8480(7) 0.5470(2) 0.77397(16) 0.0414(10) Uani 1 1 d . . . . . H9A H 0.6920 0.5550 0.7798 0.050 Uiso 1 1 calc R U . . . H9B H 0.8676 0.4945 0.7534 0.050 Uiso 1 1 calc R U . . . C12 C 0.8359(8) 0.8039(3) 0.7019(2) 0.0494(11) Uani 1 1 d . . . . . C7 C 0.9367(6) 0.7040(2) 0.77699(17) 0.0368(9) Uani 1 1 d . . . . . C14 C 0.7878(7) 0.6416(3) 0.69140(16) 0.0380(9) Uani 1 1 d . . . . . C23 C 0.6610(8) 0.8521(3) 0.7297(2) 0.0520(12) Uani 1 1 d . . . . . C16 C 0.5661(8) 0.5839(3) 0.61753(16) 0.0464(11) Uani 1 1 d . . . . . C20 C 0.8316(9) 0.5367(4) 0.9476(2) 0.0687(15) Uani 1 1 d . . . . . H20A H 0.8309 0.5397 0.9865 0.103 Uiso 1 1 calc R U . . . H20B H 0.8855 0.4816 0.9364 0.103 Uiso 1 1 calc R U . . . H20C H 0.6852 0.5446 0.9342 0.103 Uiso 1 1 calc R U . . . C11 C 1.0136(8) 0.7812(3) 0.7436(2) 0.0530(12) Uani 1 1 d . . . . . H11A H 1.1496 0.7674 0.7251 0.064 Uiso 1 1 calc R U . . . H11B H 1.0399 0.8299 0.7673 0.064 Uiso 1 1 calc R U . . . C17 C 0.5172(8) 0.6670(3) 0.59978(17) 0.0529(12) Uani 1 1 d . . . . . C6 C 1.0432(6) 0.6970(3) 0.83480(18) 0.0420(10) Uani 1 1 d . . . . . C22 C 1.1632(8) 0.5981(3) 0.7176(2) 0.0576(13) Uani 1 1 d . . . . . H22A H 1.2275 0.6467 0.6998 0.086 Uiso 1 1 calc R U . . . H22B H 1.1460 0.5520 0.6920 0.086 Uiso 1 1 calc R U . . . H22C H 1.2570 0.5797 0.7467 0.086 Uiso 1 1 calc R U . . . C13 C 0.7421(7) 0.7247(3) 0.67397(17) 0.0429(10) Uani 1 1 d . . . . . C5 C 0.9358(7) 0.6184(3) 0.86310(18) 0.0404(10) Uani 1 1 d . . . . . C21 C 1.2961(7) 0.6934(3) 0.8308(2) 0.0601(13) Uani 1 1 d . . . . . H21A H 1.3411 0.6358 0.8223 0.090 Uiso 1 1 calc R U . . . H21B H 1.3592 0.7105 0.8648 0.090 Uiso 1 1 calc R U . . . H21C H 1.3450 0.7315 0.8027 0.090 Uiso 1 1 calc R U . . . C18 C 0.6050(8) 0.7339(3) 0.62895(18) 0.0523(12) Uani 1 1 d . . . . . C1 C 0.9777(9) 0.7775(3) 0.8671(2) 0.0600(13) Uani 1 1 d . . . . . H1A H 1.0551 0.8268 0.8524 0.072 Uiso 1 1 calc R U . . . H1B H 0.8218 0.7876 0.8625 0.072 Uiso 1 1 calc R U . . . C19 C 1.2170(8) 0.5821(4) 0.9388(2) 0.0627(14) Uani 1 1 d . . . . . H19A H 1.2243 0.5637 0.9760 0.094 Uiso 1 1 calc R U . . . H19B H 1.3117 0.6307 0.9337 0.094 Uiso 1 1 calc R U . . . H19C H 1.2633 0.5361 0.9155 0.094 Uiso 1 1 calc R U . . . C2 C 1.0281(10) 0.7704(3) 0.9277(2) 0.0704(16) Uani 1 1 d . . . . . H2A H 1.1856 0.7673 0.9328 0.084 Uiso 1 1 calc R U . . . H2B H 0.9756 0.8216 0.9460 0.084 Uiso 1 1 calc R U . . . C3 C 0.9227(9) 0.6928(3) 0.9526(2) 0.0638(14) Uani 1 1 d . . . . . H3A H 0.7647 0.7002 0.9516 0.077 Uiso 1 1 calc R U . . . H3B H 0.9662 0.6895 0.9905 0.077 Uiso 1 1 calc R U . . . C24 C 0.1702(13) 0.6625(5) 0.5546(3) 0.107(3) Uani 1 1 d . . . . . H24A H 0.0965 0.6966 0.5815 0.161 Uiso 1 1 calc R U . . . H24B H 0.1543 0.6027 0.5634 0.161 Uiso 1 1 calc R U . . . H24C H 0.1068 0.6734 0.5196 0.161 Uiso 1 1 calc R U . . . C25 C 0.5074(14) 0.4343(3) 0.6049(2) 0.087(2) Uani 1 1 d . . . . . H25A H 0.4645 0.4285 0.6422 0.131 Uiso 1 1 calc R U . . . H25B H 0.6601 0.4203 0.6012 0.131 Uiso 1 1 calc R U . . . H25C H 0.4217 0.3961 0.5829 0.131 Uiso 1 1 calc R U . . . H7 H 0.779(6) 0.715(2) 0.7863(14) 0.027(9) Uiso 1 1 d . . . . . H5 H 0.782(7) 0.631(2) 0.8624(16) 0.037(11) Uiso 1 1 d . . . . . H12 H 0.908(7) 0.842(3) 0.6756(17) 0.042(11) 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 O1 0.153(5) 0.095(4) 0.134(4) 0.014(3) -0.032(4) 0.066(4) O2 0.203(6) 0.081(3) 0.124(4) 0.060(3) -0.031(4) -0.044(4) O3 0.097(3) 0.074(2) 0.0468(19) 0.0089(18) -0.0124(19) 0.006(2) O4 0.090(3) 0.054(2) 0.0474(18) -0.0088(15) -0.0091(19) -0.0006(18) N2 0.076(3) 0.055(3) 0.095(3) -0.014(2) -0.014(3) 0.012(2) N1 0.135(5) 0.054(3) 0.066(3) 0.011(2) -0.028(3) 0.015(4) C10 0.046(2) 0.039(2) 0.047(2) 0.0042(19) -0.002(2) 0.003(2) C15 0.052(3) 0.036(2) 0.040(2) 0.0002(18) 0.009(2) 0.0070(19) C4 0.041(3) 0.059(3) 0.049(3) -0.006(2) -0.008(2) 0.001(2) C8 0.033(2) 0.038(2) 0.043(2) 0.0027(18) 0.0051(18) 0.0057(17) C9 0.049(2) 0.029(2) 0.046(2) -0.0028(18) 0.001(2) -0.0016(18) C12 0.054(3) 0.033(2) 0.062(3) 0.009(2) 0.002(2) -0.011(2) C7 0.026(2) 0.031(2) 0.054(2) -0.0013(18) -0.0008(18) -0.0002(16) C14 0.036(2) 0.035(2) 0.043(2) 0.0029(18) 0.0117(18) 0.0029(17) C23 0.062(3) 0.030(2) 0.065(3) -0.001(2) -0.011(3) -0.003(2) C16 0.056(3) 0.046(2) 0.037(2) -0.0037(19) 0.005(2) -0.002(2) C20 0.064(3) 0.092(4) 0.050(3) 0.005(3) -0.002(3) -0.002(3) C11 0.047(3) 0.041(2) 0.072(3) 0.006(2) -0.001(2) -0.0117(19) C17 0.065(3) 0.059(3) 0.035(2) 0.005(2) -0.002(2) 0.012(2) C6 0.027(2) 0.040(2) 0.059(3) -0.006(2) -0.0069(19) -0.0002(18) C22 0.042(2) 0.069(3) 0.062(3) -0.001(2) 0.011(2) 0.014(2) C13 0.047(3) 0.041(2) 0.041(2) 0.0027(19) 0.0064(19) 0.0019(18) C5 0.026(2) 0.045(2) 0.050(2) -0.0056(19) -0.0041(19) 0.0037(19) C21 0.033(2) 0.069(3) 0.078(3) 0.010(3) -0.009(2) -0.010(2) C18 0.072(3) 0.040(2) 0.045(3) 0.009(2) 0.007(2) 0.008(2) C1 0.065(3) 0.043(3) 0.072(3) -0.017(2) -0.019(3) 0.000(2) C19 0.053(3) 0.068(3) 0.067(3) 0.004(3) -0.024(3) 0.007(3) C2 0.083(4) 0.059(3) 0.069(3) -0.026(3) -0.024(3) 0.012(3) C3 0.063(3) 0.078(4) 0.051(3) -0.020(3) -0.008(2) 0.016(3) C24 0.091(5) 0.148(7) 0.083(5) 0.012(5) -0.031(4) 0.011(5) C25 0.147(6) 0.050(3) 0.065(3) -0.006(3) -0.022(4) -0.019(4) _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 N1 1.238(8) . ? O2 N1 1.199(8) . ? O3 C17 1.379(6) . ? O3 C24 1.424(9) . ? O4 C16 1.365(5) . ? O4 C25 1.411(6) . ? N2 C23 1.151(7) . ? N1 C18 1.483(7) . ? C10 C5 1.526(6) . ? C10 C9 1.526(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C15 C16 1.373(6) . ? C15 C14 1.405(6) . ? C15 H15 0.9300 . ? C4 C20 1.532(7) . ? C4 C19 1.533(7) . ? C4 C3 1.538(6) . ? C4 C5 1.556(6) . ? C8 C22 1.539(6) . ? C8 C9 1.542(5) . ? C8 C14 1.543(6) . ? C8 C7 1.546(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C12 C23 1.473(7) . ? C12 C13 1.523(6) . ? C12 C11 1.534(7) . ? C12 H12 0.98(4) . ? C7 C11 1.530(6) . ? C7 C6 1.569(6) . ? C7 H7 1.00(4) . ? C14 C13 1.392(6) . ? C16 C17 1.399(6) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C17 C18 1.374(7) . ? C6 C1 1.538(6) . ? C6 C21 1.546(6) . ? C6 C5 1.554(6) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C13 C18 1.396(6) . ? C5 H5 0.96(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C1 C2 1.526(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C2 C3 1.501(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 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 C17 O3 C24 117.1(5) . . ? C16 O4 C25 117.7(4) . . ? O2 N1 O1 126.5(6) . . ? O2 N1 C18 117.5(7) . . ? O1 N1 C18 116.0(6) . . ? C5 C10 C9 111.2(3) . . ? C5 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C5 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C16 C15 C14 122.7(4) . . ? C16 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? C20 C4 C19 106.9(4) . . ? C20 C4 C3 108.8(4) . . ? C19 C4 C3 109.7(4) . . ? C20 C4 C5 109.5(4) . . ? C19 C4 C5 114.4(4) . . ? C3 C4 C5 107.4(4) . . ? C22 C8 C9 108.5(3) . . ? C22 C8 C14 106.6(3) . . ? C9 C8 C14 110.7(3) . . ? C22 C8 C7 115.0(4) . . ? C9 C8 C7 108.4(3) . . ? C14 C8 C7 107.6(3) . . ? C10 C9 C8 112.9(3) . . ? C10 C9 H9A 109.0 . . ? C8 C9 H9A 109.0 . . ? C10 C9 H9B 109.0 . . ? C8 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? C23 C12 C13 110.5(4) . . ? C23 C12 C11 108.4(4) . . ? C13 C12 C11 112.4(4) . . ? C23 C12 H12 109(2) . . ? C13 C12 H12 111(2) . . ? C11 C12 H12 105(2) . . ? C11 C7 C8 109.1(3) . . ? C11 C7 C6 114.6(3) . . ? C8 C7 C6 118.0(3) . . ? C11 C7 H7 107(2) . . ? C8 C7 H7 106(2) . . ? C6 C7 H7 102(2) . . ? C13 C14 C15 118.3(4) . . ? C13 C14 C8 122.2(4) . . ? C15 C14 C8 119.4(3) . . ? N2 C23 C12 177.5(5) . . ? O4 C16 C15 125.6(4) . . ? O4 C16 C17 114.8(4) . . ? C15 C16 C17 119.6(4) . . ? C4 C20 H20A 109.5 . . ? C4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C7 C11 C12 109.0(4) . . ? C7 C11 H11A 109.9 . . ? C12 C11 H11A 109.9 . . ? C7 C11 H11B 109.9 . . ? C12 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C18 C17 O3 119.3(4) . . ? C18 C17 C16 117.1(4) . . ? O3 C17 C16 123.5(4) . . ? C1 C6 C21 108.8(4) . . ? C1 C6 C5 107.5(4) . . ? C21 C6 C5 114.8(4) . . ? C1 C6 C7 107.9(3) . . ? C21 C6 C7 110.9(4) . . ? C5 C6 C7 106.7(3) . . ? C8 C22 H22A 109.5 . . ? C8 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C8 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C14 C13 C18 117.4(4) . . ? C14 C13 C12 122.6(4) . . ? C18 C13 C12 120.0(4) . . ? C10 C5 C6 111.2(3) . . ? C10 C5 C4 115.5(3) . . ? C6 C5 C4 116.9(3) . . ? C10 C5 H5 105(2) . . ? C6 C5 H5 104(2) . . ? C4 C5 H5 102(2) . . ? C6 C21 H21A 109.5 . . ? C6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C18 C13 124.8(4) . . ? C17 C18 N1 115.8(4) . . ? C13 C18 N1 119.4(4) . . ? C2 C1 C6 113.3(4) . . ? C2 C1 H1A 108.9 . . ? C6 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? C6 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? C4 C19 H19A 109.5 . . ? C4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C3 C2 C1 111.9(4) . . ? C3 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? C3 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? C2 C3 C4 114.6(4) . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? O3 C24 H24A 109.5 . . ? O3 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O3 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O4 C25 H25A 109.5 . . ? O4 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O4 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 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 C5 C10 C9 C8 58.6(5) . . . . ? C22 C8 C9 C10 75.0(4) . . . . ? C14 C8 C9 C10 -168.3(3) . . . . ? C7 C8 C9 C10 -50.5(4) . . . . ? C22 C8 C7 C11 61.4(5) . . . . ? C9 C8 C7 C11 -177.1(3) . . . . ? C14 C8 C7 C11 -57.3(4) . . . . ? C22 C8 C7 C6 -71.7(5) . . . . ? C9 C8 C7 C6 49.9(4) . . . . ? C14 C8 C7 C6 169.7(3) . . . . ? C16 C15 C14 C13 1.0(6) . . . . ? C16 C15 C14 C8 -178.3(4) . . . . ? C22 C8 C14 C13 -100.6(4) . . . . ? C9 C8 C14 C13 141.6(4) . . . . ? C7 C8 C14 C13 23.3(5) . . . . ? C22 C8 C14 C15 78.6(5) . . . . ? C9 C8 C14 C15 -39.2(5) . . . . ? C7 C8 C14 C15 -157.5(4) . . . . ? C25 O4 C16 C15 1.2(7) . . . . ? C25 O4 C16 C17 -177.4(5) . . . . ? C14 C15 C16 O4 180.0(4) . . . . ? C14 C15 C16 C17 -1.5(6) . . . . ? C8 C7 C11 C12 70.0(4) . . . . ? C6 C7 C11 C12 -155.2(4) . . . . ? C23 C12 C11 C7 78.7(4) . . . . ? C13 C12 C11 C7 -43.7(5) . . . . ? C24 O3 C17 C18 -115.0(6) . . . . ? C24 O3 C17 C16 68.6(7) . . . . ? O4 C16 C17 C18 179.0(4) . . . . ? C15 C16 C17 C18 0.3(7) . . . . ? O4 C16 C17 O3 -4.5(7) . . . . ? C15 C16 C17 O3 176.9(4) . . . . ? C11 C7 C6 C1 61.8(5) . . . . ? C8 C7 C6 C1 -167.7(4) . . . . ? C11 C7 C6 C21 -57.3(5) . . . . ? C8 C7 C6 C21 73.3(5) . . . . ? C11 C7 C6 C5 177.0(3) . . . . ? C8 C7 C6 C5 -52.4(4) . . . . ? C15 C14 C13 C18 0.7(6) . . . . ? C8 C14 C13 C18 179.9(4) . . . . ? C15 C14 C13 C12 -179.1(4) . . . . ? C8 C14 C13 C12 0.1(6) . . . . ? C23 C12 C13 C14 -111.2(5) . . . . ? C11 C12 C13 C14 10.1(6) . . . . ? C23 C12 C13 C18 69.0(5) . . . . ? C11 C12 C13 C18 -169.7(4) . . . . ? C9 C10 C5 C6 -61.4(5) . . . . ? C9 C10 C5 C4 162.3(4) . . . . ? C1 C6 C5 C10 170.9(4) . . . . ? C21 C6 C5 C10 -67.9(5) . . . . ? C7 C6 C5 C10 55.5(4) . . . . ? C1 C6 C5 C4 -53.4(5) . . . . ? C21 C6 C5 C4 67.8(5) . . . . ? C7 C6 C5 C4 -168.9(3) . . . . ? C20 C4 C5 C10 -56.0(5) . . . . ? C19 C4 C5 C10 63.9(5) . . . . ? C3 C4 C5 C10 -174.0(4) . . . . ? C20 C4 C5 C6 170.2(4) . . . . ? C19 C4 C5 C6 -69.8(5) . . . . ? C3 C4 C5 C6 52.3(5) . . . . ? O3 C17 C18 C13 -175.3(4) . . . . ? C16 C17 C18 C13 1.4(7) . . . . ? O3 C17 C18 N1 6.4(7) . . . . ? C16 C17 C18 N1 -177.0(5) . . . . ? C14 C13 C18 C17 -1.9(7) . . . . ? C12 C13 C18 C17 177.9(4) . . . . ? C14 C13 C18 N1 176.4(5) . . . . ? C12 C13 C18 N1 -3.8(7) . . . . ? O2 N1 C18 C17 -109.3(6) . . . . ? O1 N1 C18 C17 70.6(7) . . . . ? O2 N1 C18 C13 72.2(7) . . . . ? O1 N1 C18 C13 -107.9(6) . . . . ? C21 C6 C1 C2 -72.1(6) . . . . ? C5 C6 C1 C2 52.8(6) . . . . ? C7 C6 C1 C2 167.6(4) . . . . ? C6 C1 C2 C3 -55.7(6) . . . . ? C1 C2 C3 C4 55.2(6) . . . . ? C20 C4 C3 C2 -169.9(4) . . . . ? C19 C4 C3 C2 73.4(5) . . . . ? C5 C4 C3 C2 -51.5(5) . . . . ? _refine_diff_density_max 0.251 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.075 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL RN16ANVR_a.res in P1 New: P212121 CELL 0.71073 6.0956 15.5691 24.6358 90.000 90.000 90.000 ZERR 4.00 0.0002 0.0007 0.0011 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O UNIT 100 136 8 16 MERG 2 TWIN SHEL 0.84 840 FMAP 2 PLAN 5 ACTA BOND $H CONF L.S. 10 WGHT 0.067500 0.788200 BASF 1.97936 FVAR 0.85745 O1 4 0.348177 0.842075 0.619670 11.00000 0.15327 0.09499 = 0.13355 0.01381 -0.03201 0.06574 O2 4 0.678562 0.864316 0.589260 11.00000 0.20335 0.08056 = 0.12446 0.06040 -0.03076 -0.04450 O3 4 0.396952 0.684370 0.553665 11.00000 0.09736 0.07450 = 0.04681 0.00886 -0.01242 0.00577 O4 4 0.472248 0.519707 0.587753 11.00000 0.08971 0.05407 = 0.04743 -0.00875 -0.00910 -0.00059 N2 3 0.527400 0.888667 0.753231 11.00000 0.07604 0.05502 = 0.09522 -0.01446 -0.01381 0.01199 N1 3 0.540889 0.821202 0.610862 11.00000 0.13497 0.05359 = 0.06636 0.01092 -0.02840 0.01461 C10 1 0.961153 0.537319 0.828900 11.00000 0.04581 0.03868 = 0.04743 0.00417 -0.00205 0.00310 AFIX 23 H10A 2 0.898061 0.488941 0.848184 11.00000 -1.20000 H10B 2 1.115822 0.525631 0.823319 11.00000 -1.20000 AFIX 0 C15 1 0.695916 0.572589 0.662515 11.00000 0.05183 0.03556 = 0.04036 0.00024 0.00903 0.00699 AFIX 43 H15 2 0.724204 0.516960 0.674354 11.00000 -1.20000 AFIX 0 C4 1 0.980596 0.607308 0.924869 11.00000 0.04080 0.05859 = 0.04861 -0.00579 -0.00807 0.00100 C8 1 0.937309 0.623167 0.740591 11.00000 0.03252 0.03752 = 0.04332 0.00269 0.00507 0.00570 C9 1 0.848050 0.547016 0.773973 11.00000 0.04932 0.02895 = 0.04582 -0.00279 0.00058 -0.00157 AFIX 23 H9A 2 0.691977 0.555021 0.779754 11.00000 -1.20000 H9B 2 0.867561 0.494494 0.753352 11.00000 -1.20000 AFIX 0 C12 1 0.835889 0.803907 0.701867 11.00000 0.05416 0.03260 = 0.06155 0.00885 0.00202 -0.01059 C7 1 0.936748 0.704016 0.776993 11.00000 0.02579 0.03064 = 0.05386 -0.00129 -0.00082 -0.00023 C14 1 0.787791 0.641563 0.691403 11.00000 0.03614 0.03459 = 0.04321 0.00293 0.01173 0.00290 C23 1 0.660989 0.852055 0.729706 11.00000 0.06158 0.02968 = 0.06465 -0.00056 -0.01090 -0.00262 C16 1 0.566092 0.583869 0.617531 11.00000 0.05650 0.04611 = 0.03656 -0.00368 0.00499 -0.00226 C20 1 0.831634 0.536704 0.947620 11.00000 0.06376 0.09212 = 0.05014 0.00501 -0.00205 -0.00248 AFIX 137 H20A 2 0.830885 0.539704 0.986541 11.00000 -1.50000 H20B 2 0.885511 0.481562 0.936377 11.00000 -1.50000 H20C 2 0.685160 0.544601 0.934200 11.00000 -1.50000 AFIX 0 C11 1 1.013597 0.781213 0.743579 11.00000 0.04650 0.04082 = 0.07170 0.00650 -0.00086 -0.01174 AFIX 23 H11A 2 1.149631 0.767419 0.725103 11.00000 -1.20000 H11B 2 1.039929 0.829876 0.767287 11.00000 -1.20000 AFIX 0 C17 1 0.517191 0.667015 0.599775 11.00000 0.06467 0.05926 = 0.03477 0.00517 -0.00177 0.01224 C6 1 1.043207 0.697043 0.834799 11.00000 0.02656 0.04022 = 0.05930 -0.00620 -0.00694 -0.00021 C22 1 1.163218 0.598059 0.717598 11.00000 0.04160 0.06945 = 0.06165 -0.00120 0.01100 0.01398 AFIX 137 H22A 2 1.227545 0.646747 0.699755 11.00000 -1.50000 H22B 2 1.146007 0.552039 0.692015 11.00000 -1.50000 H22C 2 1.256979 0.579732 0.746687 11.00000 -1.50000 AFIX 0 C13 1 0.742122 0.724684 0.673971 11.00000 0.04668 0.04112 = 0.04081 0.00266 0.00642 0.00190 C5 1 0.935812 0.618409 0.863102 11.00000 0.02608 0.04538 = 0.04987 -0.00555 -0.00413 0.00367 C21 1 1.296075 0.693368 0.830763 11.00000 0.03297 0.06936 = 0.07802 0.00966 -0.00908 -0.00993 AFIX 137 H21A 2 1.341061 0.635801 0.822333 11.00000 -1.50000 H21B 2 1.359209 0.710470 0.864787 11.00000 -1.50000 H21C 2 1.345011 0.731549 0.802662 11.00000 -1.50000 AFIX 0 C18 1 0.604993 0.733907 0.628950 11.00000 0.07186 0.03989 = 0.04506 0.00935 0.00725 0.00772 C1 1 0.977711 0.777548 0.867145 11.00000 0.06461 0.04318 = 0.07217 -0.01694 -0.01883 -0.00047 AFIX 23 H1A 2 1.055055 0.826776 0.852443 11.00000 -1.20000 H1B 2 0.821792 0.787584 0.862484 11.00000 -1.20000 AFIX 0 C19 1 1.217045 0.582090 0.938822 11.00000 0.05325 0.06825 = 0.06660 0.00386 -0.02351 0.00728 AFIX 137 H19A 2 1.224262 0.563685 0.975971 11.00000 -1.50000 H19B 2 1.311651 0.630713 0.933693 11.00000 -1.50000 H19C 2 1.263305 0.536079 0.915542 11.00000 -1.50000 AFIX 0 C2 1 1.028050 0.770450 0.927670 11.00000 0.08285 0.05937 = 0.06901 -0.02584 -0.02389 0.01182 AFIX 23 H2A 2 1.185628 0.767275 0.932778 11.00000 -1.20000 H2B 2 0.975614 0.821611 0.946016 11.00000 -1.20000 AFIX 0 C3 1 0.922679 0.692786 0.952644 11.00000 0.06263 0.07823 = 0.05064 -0.01995 -0.00806 0.01587 AFIX 23 H3A 2 0.764716 0.700157 0.951649 11.00000 -1.20000 H3B 2 0.966183 0.689506 0.990460 11.00000 -1.20000 AFIX 0 C24 1 0.170167 0.662501 0.554638 11.00000 0.09119 0.14771 = 0.08302 0.01219 -0.03057 0.01091 AFIX 137 H24A 2 0.096539 0.696581 0.581521 11.00000 -1.50000 H24B 2 0.154300 0.602743 0.563404 11.00000 -1.50000 H24C 2 0.106764 0.673435 0.519643 11.00000 -1.50000 AFIX 0 C25 1 0.507425 0.434342 0.604864 11.00000 0.14689 0.05040 = 0.06457 -0.00575 -0.02210 -0.01927 AFIX 137 H25A 2 0.464484 0.428540 0.642175 11.00000 -1.50000 H25B 2 0.660066 0.420320 0.601182 11.00000 -1.50000 H25C 2 0.421664 0.396075 0.582879 11.00000 -1.50000 AFIX 0 H7 2 0.778718 0.714706 0.786297 11.00000 0.02679 H5 2 0.781675 0.631274 0.862386 11.00000 0.03744 H12 2 0.908287 0.841893 0.675644 11.00000 0.04210 HKLF 4 REM RN16ANVR_a.res in P1 New: P212121 REM R1 = 0.0590 for 3204 Fo > 4sig(Fo) and 0.0874 for all 4117 data REM 299 parameters refined using 0 restraints END WGHT 0.0675 0.7882 REM Highest difference peak 0.251, deepest hole -0.244, 1-sigma level 0.075 Q1 1 0.9306 0.8353 0.8248 11.00000 0.05 0.25 Q2 1 1.2802 0.8828 0.8310 11.00000 0.05 0.23 Q3 1 0.5104 0.8852 0.6329 11.00000 0.05 0.22 Q4 1 1.0956 0.8541 0.8233 11.00000 0.05 0.21 Q5 1 0.9876 0.8585 0.7813 11.00000 0.05 0.21 ; _shelx_res_checksum 18088 _shelx_hkl_file ; 1 0 0 -6.80 0.80 1 0 0 -6.80 0.80 -1 0 0 -6.30 0.90 -1 0 0 -6.30 0.90 -2 0 0 4051.79 54.39 2 0 0 4030.10 54.19 -2 0 0 4051.39 54.39 2 0 0 4030.70 54.29 -3 0 0 -3.00 2.80 3 0 0 -5.50 2.50 -3 0 0 -3.00 2.80 3 0 0 -5.50 2.50 4 0 0 562.94 16.20 4 0 0 563.94 16.20 -4 0 0 535.95 16.00 -4 0 0 535.95 16.00 -5 0 0 9.60 7.30 -5 0 0 9.60 7.30 -6 0 0 37.80 10.70 -6 0 0 37.80 10.70 -1 -1 0 112.49 3.40 1 -1 0 110.99 3.80 1 -1 0 110.89 3.80 1 1 0 116.59 2.40 -1 -1 0 112.49 3.40 -1 -1 0 116.39 2.20 -1 1 0 108.89 3.80 -1 -1 0 116.49 2.20 1 1 0 116.69 2.40 -1 1 0 108.89 3.80 1 1 0 104.49 3.20 1 1 0 104.59 3.30 -2 1 0 247.68 7.90 2 1 0 270.07 7.40 -2 -1 0 252.07 7.40 -2 -1 0 252.07 7.40 2 1 0 270.07 7.40 -2 1 0 247.68 7.90 3 1 0 336.37 10.40 3 -1 0 336.37 11.10 -3 -1 0 326.97 10.60 -3 -1 0 327.07 10.60 3 -1 0 336.27 11.00 3 1 0 336.47 10.40 -3 1 0 334.47 10.90 3 -1 0 339.87 7.20 -3 1 0 335.17 10.90 3 -1 0 339.77 7.20 -4 1 0 9.60 4.70 4 -1 0 10.90 2.50 4 -1 0 10.90 2.40 -4 -1 0 9.50 4.50 4 -1 0 15.50 1.90 -4 -1 0 9.50 4.50 -4 1 0 9.60 4.70 4 -1 0 15.50 1.90 4 -1 0 12.40 4.60 4 -1 0 12.30 4.60 -5 -1 0 101.09 10.20 -5 1 0 84.79 11.70 -5 -1 0 100.99 10.20 5 -1 0 99.59 11.20 5 -1 0 99.59 11.20 -5 1 0 84.89 11.80 -6 -1 0 10.80 10.30 -6 1 0 15.60 10.10 -6 -1 0 10.80 10.30 -6 1 0 15.70 10.10 1 -2 0 9998.30 122.39 1 -2 0 9999.00 122.39 -2 2 0 491.45 11.40 2 -2 0 448.36 11.10 -2 -2 0 464.35 7.00 2 -2 0 467.55 9.50 2 -2 0 467.55 9.50 2 -2 0 448.36 11.10 2 2 0 471.85 7.80 -2 -2 0 479.45 10.40 -2 -2 0 479.55 10.40 -2 2 0 491.55 11.40 2 2 0 472.05 7.90 -2 -2 0 465.05 7.00 3 -2 0 82.39 6.70 -3 -2 0 91.29 6.30 3 -2 0 82.39 6.70 -3 2 0 85.59 6.80 -3 -2 0 91.29 6.30 -3 2 0 85.49 6.80 -4 -2 0 60.59 7.30 4 -2 0 64.99 7.80 -4 2 0 58.29 7.40 -4 -2 0 60.79 7.40 4 -2 0 62.79 5.00 4 -2 0 64.89 7.80 -4 2 0 58.59 7.40 4 -2 0 62.69 4.90 -5 2 0 24.40 8.60 5 -2 0 13.60 2.60 5 -2 0 13.60 2.60 5 -2 0 -2.50 6.10 5 -2 0 -2.40 6.10 -5 -2 0 17.60 7.20 5 -2 0 15.90 3.60 -5 -2 0 17.60 7.20 5 -2 0 15.80 3.60 -5 2 0 24.30 8.70 -6 -2 0 20.70 9.80 -6 -2 0 20.70 9.80 0 3 0 1.60 1.40 0 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2025.60 30.70 0 4 0 2115.29 30.80 -1 -4 0 1663.33 25.20 1 -4 0 1671.43 26.40 1 -4 0 1652.23 24.70 1 4 0 1687.43 25.40 1 4 0 1687.23 25.50 1 -4 0 1671.53 26.50 1 -4 0 1652.63 24.70 -1 -4 0 1663.73 25.10 2 4 0 204.68 6.60 2 -4 0 213.88 7.60 -2 -4 0 217.98 6.50 -2 -4 0 221.18 6.20 2 -4 0 213.88 7.70 -2 -4 0 221.18 6.20 2 4 0 204.58 6.70 2 -4 0 205.08 7.80 -2 -4 0 218.08 6.50 -2 4 0 218.48 7.80 -2 4 0 218.48 7.80 2 -4 0 205.08 7.80 -3 -4 0 10.70 1.80 3 -4 0 17.40 4.40 3 4 0 13.40 2.70 3 -4 0 18.80 3.80 3 4 0 13.40 2.70 -3 -4 0 10.80 1.90 -3 4 0 14.70 4.40 3 -4 0 17.40 4.40 -3 -4 0 14.30 3.60 -3 4 0 14.80 4.50 -3 -4 0 14.30 3.60 3 -4 0 18.80 3.80 -4 -4 0 19.10 5.20 -4 -4 0 19.20 5.20 4 -4 0 19.70 4.30 4 -4 0 28.40 6.50 4 -4 0 19.70 4.30 -4 4 0 14.40 5.40 4 -4 0 28.40 6.50 -4 4 0 14.10 5.40 -5 -4 0 108.59 11.40 5 -4 0 114.59 11.80 -5 -4 0 108.69 11.40 5 -4 0 114.49 11.80 6 -4 0 0.70 5.70 -6 -4 0 2.20 9.20 6 -4 0 2.40 4.70 6 -4 0 2.60 4.80 -6 -4 0 2.20 9.30 6 -4 0 0.70 5.80 0 -5 0 13.70 2.60 0 5 0 16.10 3.40 0 5 0 16.10 3.30 0 -5 0 13.80 2.60 1 5 0 22.70 3.40 -1 -5 0 24.90 3.70 1 -5 0 20.90 2.90 1 5 0 22.70 3.50 -1 -5 0 24.90 3.70 1 -5 0 23.50 3.40 1 -5 0 21.00 2.90 1 -5 0 23.50 3.40 -2 -5 0 117.19 5.50 2 -5 0 124.79 6.40 2 -5 0 124.79 6.40 2 -5 0 121.49 6.60 2 5 0 118.49 6.00 2 -5 0 121.49 6.70 -2 -5 0 124.89 5.10 -2 -5 0 117.09 5.40 2 5 0 118.49 6.10 -2 -5 0 124.99 5.10 3 -5 0 231.38 9.40 3 -5 0 231.48 9.50 -3 -5 0 232.48 8.70 -3 -5 0 232.58 6.70 3 5 0 236.78 8.20 -3 -5 0 232.38 8.60 3 -5 0 236.58 10.30 3 5 0 236.88 8.10 3 -5 0 236.38 10.30 -3 -5 0 232.58 6.60 -4 -5 0 0.10 4.80 4 -5 0 -0.60 4.20 4 -5 0 1.20 5.10 -4 -5 0 1.90 1.70 4 -5 0 1.20 5.10 4 -5 0 -0.70 4.10 -4 -5 0 0.10 4.80 -5 -5 0 36.20 7.90 -5 -5 0 36.20 7.90 5 -5 0 29.10 6.60 5 -5 0 28.70 8.00 5 -5 0 28.70 7.90 5 -5 0 28.90 6.50 6 -5 0 13.80 7.40 6 -5 0 46.10 11.70 -6 -5 0 15.90 10.30 6 -5 0 13.40 7.50 6 -5 0 46.10 11.70 -6 -5 0 15.90 10.30 7 -5 0 15.50 7.60 7 -5 0 23.80 6.10 7 -5 0 23.90 6.20 7 -5 0 15.20 7.60 0 6 0 578.14 14.40 0 6 0 578.14 14.30 0 -6 0 526.45 14.30 0 -6 0 527.15 14.20 -1 -6 0 3160.08 46.70 1 6 0 3229.48 47.00 1 -6 0 3240.58 44.40 1 -6 0 3207.08 47.90 1 -6 0 3206.98 48.10 1 6 0 3229.68 47.10 1 -6 0 3240.08 44.30 -1 -6 0 3160.58 46.60 2 6 0 -0.40 3.00 -2 -6 0 -1.30 2.10 2 -6 0 -4.80 2.40 2 -6 0 -4.80 2.50 -2 -6 0 -1.30 2.10 -2 -6 0 -2.40 2.30 2 6 0 -0.40 2.90 2 -6 0 -3.50 2.90 2 -6 0 -3.50 2.90 -2 -6 0 -2.40 2.30 -3 -6 0 85.39 6.20 -3 -6 0 85.59 6.20 -4 -6 0 54.79 4.20 4 -6 0 66.39 9.50 4 -6 0 52.69 7.00 4 -6 0 66.49 9.50 -4 -6 0 72.49 8.10 4 -6 0 52.69 7.00 -4 -6 0 72.59 8.10 -4 -6 0 54.79 4.30 -5 -6 0 146.79 11.80 5 -6 0 124.79 13.80 5 -6 0 125.69 11.10 5 -6 0 125.19 11.20 5 -6 0 124.79 13.80 -5 -6 0 145.89 11.80 6 -6 0 28.40 11.10 6 -6 0 28.40 11.10 -6 -6 0 -5.40 9.70 -6 -6 0 -5.80 9.70 7 -6 0 3.00 7.80 7 -6 0 3.10 7.70 1 -7 0 208.58 8.40 1 7 0 204.08 9.40 -1 -7 0 197.88 8.80 1 -7 0 202.08 9.60 1 -7 0 198.48 9.40 1 7 0 204.08 9.30 1 -7 0 208.58 8.40 -1 -7 0 197.78 8.90 -2 -7 0 1586.54 23.00 2 7 0 1592.64 28.30 -2 -7 0 1586.54 23.00 -2 -7 0 1512.75 26.90 -2 -7 0 1513.25 27.10 2 -7 0 1571.34 30.00 2 7 0 1592.24 28.40 2 -7 0 1502.95 27.40 2 -7 0 1570.94 29.80 2 -7 0 1502.55 27.30 3 7 0 35.90 5.70 3 -7 0 34.20 6.70 3 7 0 35.90 5.70 -3 -7 0 36.20 5.00 3 -7 0 36.70 6.40 -3 -7 0 36.20 5.00 -3 -7 0 39.40 4.90 3 -7 0 34.20 6.70 3 -7 0 36.60 6.30 -3 -7 0 39.40 4.90 4 -7 0 148.89 10.30 4 -7 0 149.59 12.00 -4 -7 0 133.39 6.60 -4 -7 0 133.59 6.60 -4 -7 0 149.29 9.80 -4 -7 0 149.29 9.70 4 -7 0 148.89 10.30 4 -7 0 149.59 12.00 5 -7 0 -9.50 6.70 -5 -7 0 7.00 7.00 5 -7 0 -9.20 6.70 5 -7 0 6.00 7.70 -5 -7 0 6.90 7.00 5 -7 0 6.00 7.70 6 -7 0 -10.10 10.60 -6 -7 0 -14.80 9.40 -6 -7 0 -14.70 9.40 6 -7 0 -5.90 8.90 6 -7 0 -5.90 8.90 6 -7 0 -10.10 10.60 0 -8 0 634.74 17.00 0 -8 0 634.54 17.10 0 8 0 657.13 17.60 0 8 0 657.13 17.50 1 -8 0 212.98 10.50 1 8 0 204.48 10.30 1 -8 0 212.58 7.60 1 -8 0 213.08 10.50 1 8 0 204.38 10.40 -1 -8 0 218.08 9.60 -1 -8 0 218.08 9.70 1 -8 0 212.58 7.50 2 -8 0 37.70 6.40 -2 -8 0 38.20 5.50 2 8 0 26.60 5.80 2 8 0 26.60 5.70 -2 -8 0 33.00 3.90 2 -8 0 34.00 5.00 -2 -8 0 38.00 5.40 2 -8 0 34.00 5.10 2 -8 0 37.60 6.30 -2 -8 0 33.10 3.90 3 8 0 507.15 15.50 3 -8 0 485.85 16.10 -3 -8 0 501.45 12.30 -3 -8 0 502.05 12.30 3 -8 0 485.75 16.10 -3 -8 0 480.05 13.80 -3 -8 0 480.55 13.70 3 -8 0 524.35 17.80 3 8 0 507.15 15.40 3 -8 0 523.75 17.60 -4 -8 0 13.10 4.20 -4 -8 0 17.00 5.70 4 -8 0 18.10 7.00 -4 -8 0 13.00 4.20 -4 -8 0 17.00 5.70 4 -8 0 40.50 8.80 4 -8 0 18.00 7.00 4 -8 0 40.50 8.80 -5 -8 0 30.40 8.20 5 -8 0 27.70 10.10 -5 -8 0 27.50 3.90 -5 -8 0 27.10 3.80 5 -8 0 21.90 8.60 -5 -8 0 30.40 8.20 5 -8 0 27.70 10.10 5 -8 0 21.80 8.50 -6 -8 0 37.40 11.10 -6 -8 0 37.10 11.10 6 -8 0 -3.00 11.90 6 -8 0 10.90 10.10 6 -8 0 10.70 10.20 6 -8 0 -3.10 11.80 0 9 0 9.80 4.30 0 -9 0 2.60 4.10 0 -9 0 2.60 4.10 0 9 0 9.80 4.20 1 9 0 17.20 4.90 1 -9 0 29.20 5.80 -1 -9 0 19.90 5.00 1 -9 0 19.30 3.80 1 9 0 17.20 4.90 1 -9 0 29.30 5.80 1 -9 0 19.30 3.80 -1 -9 0 19.90 4.90 -2 -9 0 8.30 2.70 2 -9 0 0.60 3.70 2 -9 0 6.50 4.70 -2 -9 0 5.40 4.10 2 9 0 12.00 5.50 -2 -9 0 5.40 4.00 -2 -9 0 8.30 2.70 2 -9 0 6.50 4.70 2 -9 0 0.60 3.70 2 9 0 12.00 5.50 3 -9 0 57.19 8.00 3 -9 0 64.39 8.60 -3 -9 0 66.89 7.40 -3 -9 0 66.99 7.40 -3 -9 0 63.69 6.20 3 -9 0 64.49 8.70 -3 -9 0 63.49 6.20 3 -9 0 57.09 7.90 4 -9 0 30.90 8.10 4 -9 0 20.00 7.70 -4 -9 0 21.40 6.00 4 -9 0 20.20 7.70 -4 -9 0 21.60 6.00 -4 -9 0 23.50 5.40 -4 -9 0 23.50 5.50 4 -9 0 31.00 8.10 -5 -9 0 113.59 11.00 -5 -9 0 113.89 11.10 -5 -9 0 112.59 7.80 5 -9 0 113.59 13.70 -5 -9 0 112.19 7.70 5 -9 0 141.39 15.30 5 -9 0 141.19 15.40 5 -9 0 113.79 13.60 6 -9 0 64.19 12.90 -6 -9 0 112.29 13.90 6 -9 0 59.99 14.20 -6 -9 0 111.89 13.90 6 -9 0 63.79 12.90 6 -9 0 59.99 14.20 0 -10 0 173.28 10.60 0 -10 0 173.28 10.70 0 -10 0 161.38 6.00 0 -10 0 161.38 6.00 1 10 0 7.80 5.00 1 -10 0 5.30 3.20 1 -10 0 7.90 5.20 -1 -10 0 1.40 4.80 1 10 0 7.80 5.00 1 -10 0 5.30 3.20 -1 -10 0 1.40 4.70 1 -10 0 8.00 5.20 2 10 0 522.05 17.70 2 10 0 522.05 17.80 2 -10 0 512.05 15.10 2 -10 0 508.15 18.30 -2 -10 0 516.65 16.60 2 -10 0 508.55 18.20 -2 -10 0 517.65 16.80 2 -10 0 511.95 15.10 -3 -10 0 63.39 6.40 3 -10 0 70.69 8.60 3 -10 0 70.69 8.60 -3 -10 0 63.49 6.40 -3 -10 0 66.29 7.90 3 -10 0 64.79 9.20 3 -10 0 64.79 9.10 -3 -10 0 66.19 7.90 -4 -10 0 54.29 6.70 4 -10 0 54.29 10.10 -4 -10 0 54.29 6.70 4 -10 0 54.19 10.00 4 -10 0 63.19 9.80 4 -10 0 63.19 9.80 -5 -10 0 -1.70 6.10 5 -10 0 -3.80 9.50 5 -10 0 -5.20 9.70 5 -10 0 -5.30 9.70 -5 -10 0 5.90 7.40 -5 -10 0 -2.10 6.10 -5 -10 0 5.90 7.40 5 -10 0 -3.80 9.60 6 -10 0 20.00 15.50 6 -10 0 2.60 17.30 6 -10 0 2.30 17.50 6 -10 0 19.90 15.50 0 -11 0 8.00 6.00 0 -11 0 10.00 2.80 0 -11 0 10.00 2.80 0 -11 0 7.90 5.90 1 -11 0 554.04 14.10 1 -11 0 554.04 14.10 1 -11 0 575.04 20.10 -1 -11 0 572.94 19.00 1 -11 0 575.04 20.00 -1 -11 0 572.84 18.90 2 -11 0 411.26 17.70 2 -11 0 411.36 17.60 -2 -11 0 446.36 17.00 -2 -11 0 446.96 16.90 2 -11 0 419.26 14.10 2 -11 0 419.26 14.10 3 -11 0 16.90 8.40 3 -11 0 7.00 6.60 3 -11 0 7.10 6.50 -3 -11 0 8.60 6.10 3 -11 0 17.00 8.50 -3 -11 0 8.60 6.20 4 -11 0 36.10 10.40 4 -11 0 38.70 9.10 -4 -11 0 34.00 6.50 4 -11 0 36.00 10.50 -4 -11 0 34.20 6.50 -4 -11 0 35.00 7.40 4 -11 0 38.80 9.10 -4 -11 0 34.90 7.30 5 -11 0 -6.60 11.00 5 -11 0 13.60 12.60 5 -11 0 14.00 12.50 5 -11 0 -6.80 11.00 -5 -11 0 18.80 8.30 -5 -11 0 11.10 6.80 -5 -11 0 11.00 6.90 -5 -11 0 19.00 8.30 6 -11 0 67.99 18.20 6 -11 0 69.09 18.10 0 -12 0 342.97 9.40 0 -12 0 339.37 16.10 0 -12 0 339.57 16.20 0 -12 0 342.87 9.40 1 -12 0 202.38 14.20 1 -12 0 202.08 14.40 1 -12 0 219.88 9.50 1 -12 0 219.88 9.50 -2 -12 0 134.59 12.50 2 -12 0 135.09 10.00 2 -12 0 133.89 13.00 -2 -12 0 134.89 12.60 2 -12 0 133.99 12.90 2 -12 0 135.29 10.00 -3 -12 0 290.37 15.00 3 -12 0 317.67 18.00 3 -12 0 285.37 15.40 -3 -12 0 290.77 14.90 3 -12 0 285.47 15.40 3 -12 0 317.27 18.10 -4 -12 0 19.00 7.70 -4 -12 0 17.40 5.60 4 -12 0 17.60 11.30 -4 -12 0 19.00 7.80 4 -12 0 17.60 11.20 4 -12 0 29.80 9.10 -4 -12 0 17.30 5.60 4 -12 0 29.80 9.10 5 -12 0 15.20 11.50 -5 -12 0 16.20 7.60 5 -12 0 15.10 11.40 5 -12 0 -34.40 12.20 5 -12 0 -33.90 12.30 -5 -12 0 16.40 7.70 -6 -12 0 1.70 7.00 -6 -12 0 2.80 7.00 0 -13 0 -5.80 7.60 0 -13 0 -6.00 7.60 0 -13 0 5.00 4.10 0 -13 0 5.10 4.10 1 -13 0 67.89 7.30 -1 -13 0 75.09 10.20 1 -13 0 67.79 7.30 -1 -13 0 75.19 10.30 2 -13 0 52.79 11.60 -2 -13 0 65.49 9.80 2 -13 0 52.89 11.70 2 -13 0 67.29 8.60 -2 -13 0 65.29 9.90 2 -13 0 67.29 8.60 -3 -13 0 21.00 8.70 3 -13 0 24.00 7.80 3 -13 0 25.40 9.80 -3 -13 0 21.10 8.70 3 -13 0 23.60 7.80 3 -13 0 25.50 9.90 4 -13 0 -13.40 9.50 -4 -13 0 1.60 8.40 4 -13 0 17.20 11.80 4 -13 0 17.10 11.70 -4 -13 0 1.60 8.40 4 -13 0 -13.20 9.50 5 -13 0 -15.40 13.50 5 -13 0 2.80 12.30 5 -13 0 -15.50 13.40 -5 -13 0 -9.00 8.40 -5 -13 0 -8.80 8.30 5 -13 0 2.60 12.30 -6 -13 0 17.60 8.80 -6 -13 0 17.00 8.90 0 -14 0 9.10 8.60 0 -14 0 9.10 8.50 1 -14 0 722.23 17.80 1 -14 0 723.23 17.80 -1 -14 0 769.12 25.80 1 -14 0 756.62 26.80 1 -14 0 756.52 26.60 -1 -14 0 768.92 25.60 2 -14 0 96.49 11.00 -2 -14 0 114.29 13.40 2 -14 0 134.79 14.70 -2 -14 0 114.29 13.20 2 -14 0 96.09 11.00 2 -14 0 134.79 14.90 -3 -14 0 324.87 18.70 3 -14 0 321.87 17.30 -3 -14 0 324.77 18.80 3 -14 0 321.97 22.40 3 -14 0 321.87 22.60 3 -14 0 321.87 17.20 4 -14 0 38.60 10.50 4 -14 0 -9.20 15.50 -4 -14 0 3.70 9.60 4 -14 0 38.30 10.50 4 -14 0 -9.60 15.60 -4 -14 0 3.70 9.60 5 -14 0 -17.50 19.90 5 -14 0 19.10 14.40 5 -14 0 -17.80 19.80 -5 -14 0 1.10 10.50 5 -14 0 19.00 14.30 -5 -14 0 1.20 10.60 0 -15 0 6.60 9.90 0 -15 0 6.80 10.00 1 -15 0 32.10 10.30 1 -15 0 32.10 10.40 -1 -15 0 48.00 10.20 -1 -15 0 48.40 10.20 1 -15 0 39.10 6.40 1 -15 0 39.10 6.40 2 -15 0 117.79 15.40 2 -15 0 127.39 12.00 -2 -15 0 104.99 13.60 -2 -15 0 104.99 13.80 2 -15 0 127.19 12.00 2 -15 0 117.89 15.30 -3 -15 0 10.30 9.80 3 -15 0 -3.50 8.70 3 -15 0 9.70 12.00 -3 -15 0 10.20 9.70 3 -15 0 -3.50 8.70 3 -15 0 9.40 12.10 4 -15 0 -3.30 12.00 -4 -15 0 -1.70 10.30 4 -15 0 13.00 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