#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 10 _journal_issue 2 _journal_year 2019 _journal_page_first 175 _journal_page_last 179 #=============================================================================== data_shelx _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H18 N2 O4' _chemical_formula_sum 'C19 H18 N2 O4' _chemical_formula_weight 338.35 _chemical_absolute_configuration 'rm' 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 triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _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, -z' _cell_length_a 8.2506(17) _cell_length_b 11.934(2) _cell_length_c 17.461(4) _cell_angle_alpha 102.89(3) _cell_angle_beta 94.62(3) _cell_angle_gamma 96.68(3) _cell_volume 1654.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5290 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 24.04 _exptl_crystal_description 'needle' _exptl_crystal_colour 'yellow' _exptl_crystal_density_meas 1.357 _exptl_crystal_density_method none _exptl_crystal_density_diffrn 1.358 _exptl_crystal_F_000 712 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.050 _exptl_absorpt_coefficient_mu 0.096 _shelx_estimated_absorpt_T_min 0.976 _shelx_estimated_absorpt_T_max 0.995 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.976 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_process_details 'SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 0 _diffrn_reflns_number 7227 _diffrn_reflns_av_unetI/netI 0.0662 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.361 _diffrn_reflns_theta_max 26.998 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_point_group_measured_fraction_full 0.997 _reflns_number_total 7227 _reflns_number_gt 5031 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; _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 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refined as a 2-component 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^)+(0.0996P)^2^+0.1345P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 7227 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0561 _refine_ls_wR_factor_ref 0.1658 _refine_ls_wR_factor_gt 0.1390 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 C1A C 0.0578(4) 0.5675(2) 0.41544(18) 0.0269(6) Uani 1 1 d . . . . . H1A H -0.0274 0.5176 0.4267 0.032 Uiso 1 1 calc R U . . . C1B C 0.1512(4) -0.8179(3) -0.0415(2) 0.0389(8) Uani 1 1 d . . . . . H1B H 0.2037 -0.8493 -0.0037 0.047 Uiso 1 1 calc R U . . . C2A C 0.2093(4) 0.5334(2) 0.40875(18) 0.0274(6) Uani 1 1 d . . . . . C2B C 0.0525(4) -0.8886(3) -0.1027(2) 0.0376(8) Uani 1 1 d . . . . . C3A C 0.3400(4) 0.6073(2) 0.39082(19) 0.0320(7) Uani 1 1 d . . . . . H3A H 0.4431 0.5836 0.3867 0.038 Uiso 1 1 calc R U . . . C3B C -0.0301(4) -0.8425(3) -0.1603(2) 0.0376(8) Uani 1 1 d . . . . . H3B H -0.0969 -0.8921 -0.2027 0.045 Uiso 1 1 calc R U . . . C4A C 0.3143(4) 0.7136(2) 0.3795(2) 0.0325(7) Uani 1 1 d . . . . . H4A H 0.4003 0.7614 0.3669 0.039 Uiso 1 1 calc R U . . . C4B C -0.0118(4) -0.7258(3) -0.1538(2) 0.0352(7) Uani 1 1 d . . . . . H4B H -0.0686 -0.6962 -0.1913 0.042 Uiso 1 1 calc R U . . . C5A C 0.1315(4) 0.8645(2) 0.37899(18) 0.0284(6) Uani 1 1 d . . . . . H5A H 0.2156 0.9126 0.3652 0.034 Uiso 1 1 calc R U . . . C5B C 0.1150(4) -0.5273(3) -0.08250(19) 0.0317(7) Uani 1 1 d . . . . . H5B H 0.0578 -0.4958 -0.1188 0.038 Uiso 1 1 calc R U . . . C6A C -0.0163(3) 0.9045(2) 0.39121(17) 0.0251(6) Uani 1 1 d . . . . . C6B C 0.2200(4) -0.4542(3) -0.02196(18) 0.0311(7) Uani 1 1 d . . . . . C7A C -0.1472(4) 0.8284(2) 0.40854(19) 0.0291(7) Uani 1 1 d . . . . . H7A H -0.2491 0.8530 0.4152 0.035 Uiso 1 1 calc R U . . . C7B C 0.3063(4) -0.5029(3) 0.0338(2) 0.0364(7) Uani 1 1 d . . . . . H7B H 0.3786 -0.4547 0.0747 0.044 Uiso 1 1 calc R U . . . C8A C -0.1240(4) 0.7200(2) 0.41536(19) 0.0305(7) Uani 1 1 d . . . . . H8A H -0.2109 0.6717 0.4268 0.037 Uiso 1 1 calc R U . . . C8B C 0.2834(5) -0.6195(3) 0.0276(2) 0.0407(8) Uani 1 1 d . . . . . H8B H 0.3401 -0.6496 0.0648 0.049 Uiso 1 1 calc R U . . . C9A C 0.0292(3) 0.6786(2) 0.40546(17) 0.0236(6) Uani 1 1 d . . . . . C9B C 0.1759(4) -0.6960(3) -0.03395(18) 0.0316(7) Uani 1 1 d . . . . . C10A C 0.1600(4) 0.7526(2) 0.38663(17) 0.0256(6) Uani 1 1 d . . . . . C10B C 0.0919(4) -0.6490(3) -0.09107(19) 0.0306(7) Uani 1 1 d . . . . . C11A C -0.0315(4) 1.0240(2) 0.38839(18) 0.0277(6) Uani 1 1 d . . . . . H11A H 0.0604 1.0645 0.3744 0.033 Uiso 1 1 calc R U . . . C11B C 0.2382(4) -0.3299(2) -0.01708(19) 0.0323(7) Uani 1 1 d . . . . . H11B H 0.1786 -0.3080 -0.0575 0.039 Uiso 1 1 calc R U . . . C12A C -0.1572(3) 1.0850(2) 0.40285(17) 0.0252(6) Uani 1 1 d . . . . . C12B C 0.3282(4) -0.2419(2) 0.03718(19) 0.0329(7) Uani 1 1 d . . . . . C13A C -0.1476(3) 1.2074(2) 0.39778(17) 0.0256(6) Uani 1 1 d . . . . . C13B C 0.3235(4) -0.1193(2) 0.03424(19) 0.0325(7) Uani 1 1 d . . . . . C14A C -0.3955(4) 1.1359(2) 0.42344(17) 0.0262(6) Uani 1 1 d . . . . . C14B C 0.4868(4) -0.1394(3) 0.1392(2) 0.0365(7) Uani 1 1 d . . . . . C15A C -0.5684(4) 1.1385(3) 0.4396(2) 0.0325(7) Uani 1 1 d . . . . . H15A H -0.6357 1.1351 0.3915 0.049 Uiso 1 1 calc R U . . . H15B H -0.5770 1.2090 0.4774 0.049 Uiso 1 1 calc R U . . . H15C H -0.6047 1.0731 0.4605 0.049 Uiso 1 1 calc R U . . . C15B C 0.6031(5) -0.1013(3) 0.2116(2) 0.0519(10) Uani 1 1 d . . . . . H15D H 0.5473 -0.0650 0.2546 0.078 Uiso 1 1 calc R U . . . H15E H 0.6915 -0.0469 0.2034 0.078 Uiso 1 1 calc R U . . . H15F H 0.6463 -0.1674 0.2238 0.078 Uiso 1 1 calc R U . . . C16A C -0.3578(4) 1.3394(2) 0.39739(18) 0.0282(6) Uani 1 1 d . . . . . H16A H -0.2873 1.4060 0.4308 0.034 Uiso 1 1 calc R U . . . H16B H -0.4687 1.3425 0.4116 0.034 Uiso 1 1 calc R U . . . C16B C 0.4520(4) 0.0667(3) 0.1251(2) 0.0386(8) Uani 1 1 d . . . . . H16C H 0.4266 0.0991 0.0800 0.046 Uiso 1 1 calc R U . . . H16D H 0.5667 0.0929 0.1447 0.046 Uiso 1 1 calc R U . . . C17A C -0.3542(4) 1.3438(2) 0.31161(18) 0.0283(6) Uani 1 1 d . . . . . C17B C 0.3460(4) 0.1103(3) 0.1893(2) 0.0359(7) Uani 1 1 d . . . . . C18A C -0.3747(6) 1.4660(3) 0.2228(2) 0.0535(10) Uani 1 1 d . . . . . H18A H -0.4642 1.4139 0.1889 0.064 Uiso 1 1 calc R U . . . H18B H -0.2725 1.4488 0.2021 0.064 Uiso 1 1 calc R U . . . C18B C 0.1790(5) 0.2520(3) 0.2370(2) 0.0517(10) Uani 1 1 d . . . . . H18C H 0.0960 0.1908 0.2428 0.062 Uiso 1 1 calc R U . . . H18D H 0.2427 0.2845 0.2880 0.062 Uiso 1 1 calc R U . . . C19A C -0.3957(5) 1.5870(3) 0.2242(2) 0.0536(10) Uani 1 1 d . . . . . H19A H -0.3970 1.5988 0.1716 0.080 Uiso 1 1 calc R U . . . H19B H -0.4974 1.6032 0.2445 0.080 Uiso 1 1 calc R U . . . H19C H -0.3063 1.6380 0.2576 0.080 Uiso 1 1 calc R U . . . C19B C 0.1011(6) 0.3423(4) 0.2098(3) 0.0739(14) Uani 1 1 d . . . . . H19D H 0.0302 0.3741 0.2475 0.111 Uiso 1 1 calc R U . . . H19E H 0.1840 0.4027 0.2046 0.111 Uiso 1 1 calc R U . . . H19F H 0.0379 0.3093 0.1596 0.111 Uiso 1 1 calc R U . . . N1A N -0.3155(3) 1.04862(19) 0.42080(15) 0.0272(5) Uani 1 1 d . . . . . N1B N 0.4332(3) -0.2457(2) 0.10366(17) 0.0378(6) Uani 1 1 d . . . . . N2A N -0.3023(3) 1.23333(19) 0.41013(15) 0.0261(5) Uani 1 1 d . . . . . N2B N 0.4258(3) -0.0589(2) 0.10023(16) 0.0332(6) Uani 1 1 d . . . . . O1A O 0.2456(3) 0.42916(16) 0.42075(14) 0.0349(5) Uani 1 1 d . . . . . H1A1 H 0.1603 0.3852 0.4184 0.052 Uiso 1 1 calc R U . . . O1B O 0.0260(4) -1.00598(18) -0.11411(16) 0.0526(7) Uani 1 1 d . . . . . H1B1 H 0.0913 -1.0264 -0.0838 0.079 Uiso 1 1 calc R U . . . O2A O -0.0345(3) 1.27477(16) 0.38554(13) 0.0333(5) Uani 1 1 d . . . . . O2B O 0.2529(3) -0.07523(18) -0.01344(14) 0.0412(6) Uani 1 1 d . . . . . O3A O -0.3384(3) 1.26412(19) 0.25872(14) 0.0444(6) Uani 1 1 d . . . . . O3B O 0.3194(3) 0.06496(19) 0.24338(14) 0.0430(6) Uani 1 1 d . . . . . O4A O -0.3729(3) 1.44968(17) 0.30334(13) 0.0380(5) Uani 1 1 d . . . . . O4B O 0.2862(3) 0.20495(18) 0.17879(13) 0.0391(6) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1A 0.0239(15) 0.0225(13) 0.0331(17) 0.0057(12) 0.0039(13) -0.0014(11) C1B 0.047(2) 0.0313(16) 0.040(2) 0.0110(14) 0.0013(16) 0.0067(14) C2A 0.0296(16) 0.0214(13) 0.0305(16) 0.0035(11) 0.0043(13) 0.0053(11) C2B 0.044(2) 0.0284(16) 0.0406(19) 0.0082(14) 0.0076(16) 0.0044(14) C3A 0.0264(16) 0.0322(15) 0.0383(18) 0.0056(13) 0.0090(13) 0.0090(12) C3B 0.042(2) 0.0354(17) 0.0322(18) 0.0047(14) 0.0008(15) 0.0006(14) C4A 0.0286(17) 0.0274(15) 0.0434(19) 0.0111(13) 0.0098(14) 0.0015(12) C4B 0.0384(18) 0.0340(16) 0.0322(18) 0.0075(13) 0.0022(14) 0.0028(13) C5A 0.0276(16) 0.0267(14) 0.0308(16) 0.0078(12) 0.0055(13) 0.0001(12) C5B 0.0317(17) 0.0336(15) 0.0313(18) 0.0093(13) 0.0066(14) 0.0052(13) C6A 0.0249(15) 0.0235(13) 0.0271(16) 0.0059(11) 0.0038(12) 0.0038(11) C6B 0.0347(18) 0.0296(15) 0.0290(17) 0.0046(12) 0.0095(14) 0.0049(12) C7A 0.0203(15) 0.0295(15) 0.0384(18) 0.0099(13) 0.0036(13) 0.0023(11) C7B 0.043(2) 0.0301(16) 0.0331(18) 0.0039(13) -0.0022(15) 0.0050(14) C8A 0.0224(15) 0.0293(14) 0.0399(18) 0.0109(13) 0.0057(14) -0.0025(12) C8B 0.052(2) 0.0353(17) 0.0347(19) 0.0099(14) -0.0032(16) 0.0095(15) C9A 0.0210(14) 0.0237(13) 0.0247(15) 0.0040(11) 0.0013(12) 0.0018(11) C9B 0.0331(17) 0.0336(16) 0.0279(16) 0.0062(13) 0.0049(14) 0.0047(13) C10A 0.0249(15) 0.0271(14) 0.0249(15) 0.0054(12) 0.0042(12) 0.0043(11) C10B 0.0283(16) 0.0342(15) 0.0308(17) 0.0088(13) 0.0096(14) 0.0045(12) C11A 0.0248(15) 0.0272(14) 0.0323(17) 0.0107(12) 0.0034(13) 0.0004(11) C11B 0.0369(18) 0.0310(15) 0.0299(17) 0.0066(12) 0.0079(14) 0.0060(13) C12A 0.0239(15) 0.0266(14) 0.0247(15) 0.0070(11) 0.0008(12) 0.0009(11) C12B 0.0405(19) 0.0281(15) 0.0318(17) 0.0062(13) 0.0084(15) 0.0097(13) C13A 0.0229(15) 0.0268(14) 0.0278(16) 0.0088(12) 0.0007(12) 0.0036(11) C13B 0.0388(19) 0.0271(15) 0.0334(18) 0.0051(13) 0.0142(15) 0.0084(13) C14A 0.0257(15) 0.0259(13) 0.0272(16) 0.0091(12) 0.0022(13) -0.0006(11) C14B 0.0341(18) 0.0343(17) 0.0395(19) 0.0044(14) 0.0036(15) 0.0076(13) C15A 0.0263(16) 0.0332(16) 0.0395(19) 0.0134(13) 0.0046(14) 0.0005(12) C15B 0.054(2) 0.045(2) 0.052(2) 0.0024(17) -0.0056(19) 0.0094(17) C16A 0.0307(16) 0.0235(13) 0.0334(17) 0.0105(12) 0.0067(13) 0.0072(12) C16B 0.045(2) 0.0272(15) 0.041(2) 0.0014(13) 0.0129(16) 0.0017(14) C17A 0.0236(15) 0.0297(15) 0.0325(17) 0.0098(13) 0.0011(13) 0.0037(12) C17B 0.0384(19) 0.0307(16) 0.0349(19) 0.0023(13) 0.0031(15) 0.0007(14) C18A 0.077(3) 0.057(2) 0.037(2) 0.0232(17) 0.015(2) 0.022(2) C18B 0.062(3) 0.059(2) 0.037(2) 0.0032(17) 0.0119(19) 0.029(2) C19A 0.074(3) 0.054(2) 0.043(2) 0.0262(18) 0.011(2) 0.021(2) C19B 0.076(3) 0.098(4) 0.067(3) 0.030(3) 0.025(3) 0.055(3) N1A 0.0268(13) 0.0254(12) 0.0306(14) 0.0096(10) 0.0023(11) 0.0027(10) N1B 0.0405(16) 0.0293(14) 0.0430(17) 0.0052(12) 0.0034(13) 0.0090(11) N2A 0.0231(13) 0.0224(11) 0.0366(14) 0.0129(10) 0.0070(11) 0.0047(9) N2B 0.0394(16) 0.0263(12) 0.0338(15) 0.0054(11) 0.0076(13) 0.0049(11) O1A 0.0293(12) 0.0233(10) 0.0527(14) 0.0091(10) 0.0044(11) 0.0052(8) O1B 0.0680(19) 0.0279(12) 0.0568(18) 0.0074(11) -0.0072(14) 0.0004(11) O2A 0.0279(12) 0.0260(10) 0.0482(14) 0.0136(10) 0.0095(10) -0.0010(9) O2B 0.0555(16) 0.0329(12) 0.0389(14) 0.0129(10) 0.0060(11) 0.0124(11) O3A 0.0619(17) 0.0370(12) 0.0325(13) 0.0031(10) 0.0007(12) 0.0123(11) O3B 0.0512(16) 0.0410(13) 0.0378(14) 0.0089(10) 0.0099(11) 0.0081(11) O4A 0.0540(15) 0.0323(11) 0.0356(13) 0.0163(9) 0.0128(11) 0.0171(10) O4B 0.0470(15) 0.0371(12) 0.0346(13) 0.0058(9) 0.0086(11) 0.0145(10) _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 C1A C2A 1.365(4) . ? C1A C9A 1.418(4) . ? C1A H1A 0.9300 . ? C1B C2B 1.347(5) . ? C1B C9B 1.421(4) . ? C1B H1B 0.9300 . ? C2A O1A 1.369(3) . ? C2A C3A 1.413(4) . ? C2B O1B 1.359(4) . ? C2B C3B 1.415(5) . ? C3A C4A 1.364(4) . ? C3A H3A 0.9300 . ? C3B C4B 1.362(4) . ? C3B H3B 0.9300 . ? C4A C10A 1.410(4) . ? C4A H4A 0.9300 . ? C4B C10B 1.410(5) . ? C4B H4B 0.9300 . ? C5A C6A 1.376(4) . ? C5A C10A 1.416(4) . ? C5A H5A 0.9300 . ? C5B C6B 1.376(5) . ? C5B C10B 1.416(4) . ? C5B H5B 0.9300 . ? C6A C7A 1.425(4) . ? C6A C11A 1.458(4) . ? C6B C7B 1.425(5) . ? C6B C11B 1.457(4) . ? C7A C8A 1.359(4) . ? C7A H7A 0.9300 . ? C7B C8B 1.360(4) . ? C7B H7B 0.9300 . ? C8A C9A 1.419(4) . ? C8A H8A 0.9300 . ? C8B C9B 1.412(5) . ? C8B H8B 0.9300 . ? C9A C10A 1.421(4) . ? C9B C10B 1.420(4) . ? C11A C12A 1.344(4) . ? C11A H11A 0.9300 . ? C11B C12B 1.347(4) . ? C11B H11B 0.9300 . ? C12A N1A 1.410(4) . ? C12A C13A 1.476(4) . ? C12B N1B 1.404(4) . ? C12B C13B 1.480(4) . ? C13A O2A 1.223(3) . ? C13A N2A 1.371(4) . ? C13B O2B 1.224(4) . ? C13B N2B 1.375(4) . ? C14A N1A 1.291(4) . ? C14A N2A 1.392(3) . ? C14A C15A 1.479(4) . ? C14B N1B 1.290(4) . ? C14B N2B 1.410(4) . ? C14B C15B 1.474(5) . ? C15A H15A 0.9600 . ? C15A H15B 0.9600 . ? C15A H15C 0.9600 . ? C15B H15D 0.9600 . ? C15B H15E 0.9600 . ? C15B H15F 0.9600 . ? C16A N2A 1.451(3) . ? C16A C17A 1.513(4) . ? C16A H16A 0.9700 . ? C16A H16B 0.9700 . ? C16B N2B 1.449(4) . ? C16B C17B 1.515(5) . ? C16B H16C 0.9700 . ? C16B H16D 0.9700 . ? C17A O3A 1.196(4) . ? C17A O4A 1.328(3) . ? C17B O3B 1.211(4) . ? C17B O4B 1.326(4) . ? C18A O4A 1.461(4) . ? C18A C19A 1.469(5) . ? C18A H18A 0.9700 . ? C18A H18B 0.9700 . ? C18B C19B 1.463(5) . ? C18B O4B 1.461(4) . ? C18B H18C 0.9700 . ? C18B H18D 0.9700 . ? C19A H19A 0.9600 . ? C19A H19B 0.9600 . ? C19A H19C 0.9600 . ? C19B H19D 0.9600 . ? C19B H19E 0.9600 . ? C19B H19F 0.9600 . ? O1A H1A1 0.8200 . ? O1B H1B1 0.8200 . ? 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 C2A C1A C9A 120.6(2) . . ? C2A C1A H1A 119.7 . . ? C9A C1A H1A 119.7 . . ? C2B C1B C9B 120.8(3) . . ? C2B C1B H1B 119.6 . . ? C9B C1B H1B 119.6 . . ? C1A C2A O1A 123.1(2) . . ? C1A C2A C3A 120.7(2) . . ? O1A C2A C3A 116.2(3) . . ? C1B C2B O1B 123.7(3) . . ? C1B C2B C3B 120.5(3) . . ? O1B C2B C3B 115.8(3) . . ? C4A C3A C2A 119.7(3) . . ? C4A C3A H3A 120.2 . . ? C2A C3A H3A 120.2 . . ? C4B C3B C2B 120.1(3) . . ? C4B C3B H3B 119.9 . . ? C2B C3B H3B 119.9 . . ? C3A C4A C10A 121.4(3) . . ? C3A C4A H4A 119.3 . . ? C10A C4A H4A 119.3 . . ? C3B C4B C10B 121.0(3) . . ? C3B C4B H4B 119.5 . . ? C10B C4B H4B 119.5 . . ? C6A C5A C10A 122.3(3) . . ? C6A C5A H5A 118.8 . . ? C10A C5A H5A 118.8 . . ? C6B C5B C10B 121.8(3) . . ? C6B C5B H5B 119.1 . . ? C10B C5B H5B 119.1 . . ? C5A C6A C7A 118.6(2) . . ? C5A C6A C11A 118.9(2) . . ? C7A C6A C11A 122.5(3) . . ? C5B C6B C7B 118.8(3) . . ? C5B C6B C11B 118.8(3) . . ? C7B C6B C11B 122.4(3) . . ? C8A C7A C6A 120.4(3) . . ? C8A C7A H7A 119.8 . . ? C6A C7A H7A 119.8 . . ? C8B C7B C6B 120.4(3) . . ? C8B C7B H7B 119.8 . . ? C6B C7B H7B 119.8 . . ? C7A C8A C9A 121.8(2) . . ? C7A C8A H8A 119.1 . . ? C9A C8A H8A 119.1 . . ? C7B C8B C9B 121.7(3) . . ? C7B C8B H8B 119.1 . . ? C9B C8B H8B 119.1 . . ? C1A C9A C10A 118.8(2) . . ? C1A C9A C8A 122.7(2) . . ? C10A C9A C8A 118.5(2) . . ? C8B C9B C1B 122.4(3) . . ? C8B C9B C10B 118.6(3) . . ? C1B C9B C10B 119.0(3) . . ? C4A C10A C5A 122.7(3) . . ? C4A C10A C9A 118.9(2) . . ? C5A C10A C9A 118.3(3) . . ? C4B C10B C5B 122.7(3) . . ? C4B C10B C9B 118.6(3) . . ? C5B C10B C9B 118.7(3) . . ? C12A C11A C6A 130.2(3) . . ? C12A C11A H11A 114.9 . . ? C6A C11A H11A 114.9 . . ? C12B C11B C6B 129.7(3) . . ? C12B C11B H11B 115.1 . . ? C6B C11B H11B 115.1 . . ? C11A C12A N1A 129.4(2) . . ? C11A C12A C13A 122.0(3) . . ? N1A C12A C13A 108.6(2) . . ? C11B C12B N1B 129.2(3) . . ? C11B C12B C13B 121.6(3) . . ? N1B C12B C13B 109.1(3) . . ? O2A C13A N2A 125.1(2) . . ? O2A C13A C12A 131.4(3) . . ? N2A C13A C12A 103.4(2) . . ? O2B C13B N2B 125.0(3) . . ? O2B C13B C12B 131.9(3) . . ? N2B C13B C12B 103.1(3) . . ? N1A C14A N2A 113.5(3) . . ? N1A C14A C15A 125.8(2) . . ? N2A C14A C15A 120.7(2) . . ? N1B C14B N2B 113.0(3) . . ? N1B C14B C15B 125.5(3) . . ? N2B C14B C15B 121.5(3) . . ? C14A C15A H15A 109.5 . . ? C14A C15A H15B 109.5 . . ? H15A C15A H15B 109.5 . . ? C14A C15A H15C 109.5 . . ? H15A C15A H15C 109.5 . . ? H15B C15A H15C 109.5 . . ? C14B C15B H15D 109.5 . . ? C14B C15B H15E 109.5 . . ? H15D C15B H15E 109.5 . . ? C14B C15B H15F 109.5 . . ? H15D C15B H15F 109.5 . . ? H15E C15B H15F 109.5 . . ? N2A C16A C17A 110.1(2) . . ? N2A C16A H16A 109.6 . . ? C17A C16A H16A 109.6 . . ? N2A C16A H16B 109.6 . . ? C17A C16A H16B 109.6 . . ? H16A C16A H16B 108.1 . . ? N2B C16B C17B 111.5(2) . . ? N2B C16B H16C 109.3 . . ? C17B C16B H16C 109.3 . . ? N2B C16B H16D 109.3 . . ? C17B C16B H16D 109.3 . . ? H16C C16B H16D 108.0 . . ? O3A C17A O4A 124.7(3) . . ? O3A C17A C16A 125.5(3) . . ? O4A C17A C16A 109.8(2) . . ? O3B C17B O4B 124.3(3) . . ? O3B C17B C16B 124.4(3) . . ? O4B C17B C16B 111.3(3) . . ? O4A C18A C19A 108.7(3) . . ? O4A C18A H18A 109.9 . . ? C19A C18A H18A 109.9 . . ? O4A C18A H18B 109.9 . . ? C19A C18A H18B 109.9 . . ? H18A C18A H18B 108.3 . . ? C19B C18B O4B 108.5(3) . . ? C19B C18B H18C 110.0 . . ? O4B C18B H18C 110.0 . . ? C19B C18B H18D 110.0 . . ? O4B C18B H18D 110.0 . . ? H18C C18B H18D 108.4 . . ? C18A C19A H19A 109.5 . . ? C18A C19A H19B 109.5 . . ? H19A C19A H19B 109.5 . . ? C18A C19A H19C 109.5 . . ? H19A C19A H19C 109.5 . . ? H19B C19A H19C 109.5 . . ? C18B C19B H19D 109.5 . . ? C18B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C18B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C14A N1A C12A 106.0(2) . . ? C14B N1B C12B 106.4(3) . . ? C13A N2A C14A 108.5(2) . . ? C13A N2A C16A 122.6(2) . . ? C14A N2A C16A 128.2(2) . . ? C13B N2B C14B 108.4(2) . . ? C13B N2B C16B 123.3(3) . . ? C14B N2B C16B 128.2(3) . . ? C2A O1A H1A1 109.5 . . ? C2B O1B H1B1 109.5 . . ? C17A O4A C18A 115.7(3) . . ? C17B O4B C18B 115.2(3) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C3A H3A O4A 0.93 2.62 3.438(4) 147.1 1_645 C3B H3B O3B 0.93 2.53 3.331(4) 144.9 2_545 C15A H15A O3B 0.96 2.52 3.366(4) 147.5 1_465 C15B H15D O3B 0.96 2.60 3.244(5) 125.1 . C16B H16D O3A 0.97 2.51 3.151(4) 123.3 1_645 C18B H18D O1A 0.97 2.56 3.389(5) 143.5 . O1A H1A1 O2A 0.82 1.92 2.718(3) 165.9 1_545 O1B H1B1 O2B 0.82 1.97 2.785(4) 178.2 1_545 _refine_diff_density_max 0.284 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.066 _shelxl_version_number 2014-3 _shelx_res_file ; TITL newtwin in P-1 CELL 0.71073 8.2506 11.9341 17.4612 102.892 94.622 96.683 ZERR 4.00 0.0017 0.0024 0.0035 0.030 0.030 0.030 LATT 1 SFAC C H N O UNIT 76 72 8 16 MERG 0 OMIT -3.00 54.00 EQIV $1 x+1, y-1, z HTAB C3A O4A_$1 EQIV $2 -x, -y-1, -z HTAB C3B O3B_$2 EQIV $3 x-1, y+1, z HTAB C15A O3B_$3 HTAB C15B O3B HTAB C16B O3A_$1 HTAB C18B O1A EQIV $4 x, y-1, z HTAB O1A O2A_$4 HTAB O1B O2B_$4 OMIT 1 0 2 OMIT 3 0 0 OMIT 0 1 0 OMIT 1 -7 10 OMIT 0 0 1 OMIT 2 -8 10 FMAP 2 PLAN 5 SIZE 0.050 0.100 0.250 ACTA HTAB 2.00000 BOND $H L.S. 15 TEMP -100.00 WGHT 0.099600 0.134500 BASF 0.35512 FVAR 0.56482 C1A 1 0.057793 0.567541 0.415445 11.00000 0.02390 0.02245 = 0.03306 0.00568 0.00385 -0.00144 AFIX 43 H1A 2 -0.027406 0.517561 0.426654 11.00000 -1.20000 AFIX 0 C1B 1 0.151159 -0.817896 -0.041457 11.00000 0.04664 0.03126 = 0.03972 0.01098 0.00129 0.00667 AFIX 43 H1B 2 0.203683 -0.849261 -0.003680 11.00000 -1.20000 AFIX 0 C2A 1 0.209273 0.533380 0.408746 11.00000 0.02964 0.02144 = 0.03049 0.00346 0.00428 0.00527 C2B 1 0.052505 -0.888620 -0.102669 11.00000 0.04408 0.02845 = 0.04061 0.00819 0.00763 0.00438 C3A 1 0.339988 0.607319 0.390822 11.00000 0.02639 0.03218 = 0.03827 0.00555 0.00899 0.00896 AFIX 43 H3A 2 0.443060 0.583631 0.386742 11.00000 -1.20000 AFIX 0 C3B 1 -0.030052 -0.842536 -0.160323 11.00000 0.04193 0.03543 = 0.03215 0.00466 0.00082 0.00058 AFIX 43 H3B 2 -0.096857 -0.892081 -0.202739 11.00000 -1.20000 AFIX 0 C4A 1 0.314298 0.713626 0.379528 11.00000 0.02863 0.02736 = 0.04339 0.01115 0.00985 0.00147 AFIX 43 H4A 2 0.400306 0.761420 0.366881 11.00000 -1.20000 AFIX 0 C4B 1 -0.011832 -0.725758 -0.153793 11.00000 0.03836 0.03401 = 0.03216 0.00752 0.00221 0.00279 AFIX 43 H4B 2 -0.068637 -0.696163 -0.191272 11.00000 -1.20000 AFIX 0 C5A 1 0.131456 0.864480 0.378989 11.00000 0.02758 0.02673 = 0.03076 0.00776 0.00547 0.00010 AFIX 43 H5A 2 0.215555 0.912609 0.365220 11.00000 -1.20000 AFIX 0 C5B 1 0.115046 -0.527292 -0.082501 11.00000 0.03169 0.03365 = 0.03134 0.00927 0.00656 0.00515 AFIX 43 H5B 2 0.057791 -0.495833 -0.118794 11.00000 -1.20000 AFIX 0 C6A 1 -0.016315 0.904529 0.391213 11.00000 0.02493 0.02350 = 0.02712 0.00586 0.00382 0.00375 C6B 1 0.219956 -0.454231 -0.021959 11.00000 0.03472 0.02963 = 0.02897 0.00460 0.00948 0.00486 C7A 1 -0.147201 0.828410 0.408545 11.00000 0.02032 0.02948 = 0.03835 0.00994 0.00363 0.00234 AFIX 43 H7A 2 -0.249097 0.853048 0.415232 11.00000 -1.20000 AFIX 0 C7B 1 0.306258 -0.502906 0.033816 11.00000 0.04321 0.03014 = 0.03315 0.00394 -0.00216 0.00498 AFIX 43 H7B 2 0.378608 -0.454731 0.074705 11.00000 -1.20000 AFIX 0 C8A 1 -0.124018 0.720016 0.415362 11.00000 0.02244 0.02926 = 0.03995 0.01092 0.00565 -0.00251 AFIX 43 H8A 2 -0.210887 0.671681 0.426826 11.00000 -1.20000 AFIX 0 C8B 1 0.283402 -0.619479 0.027583 11.00000 0.05236 0.03534 = 0.03473 0.00986 -0.00324 0.00951 AFIX 43 H8B 2 0.340065 -0.649598 0.064819 11.00000 -1.20000 AFIX 0 C9A 1 0.029150 0.678571 0.405465 11.00000 0.02105 0.02375 = 0.02474 0.00400 0.00129 0.00179 C9B 1 0.175889 -0.695958 -0.033948 11.00000 0.03310 0.03362 = 0.02786 0.00618 0.00494 0.00471 C10A 1 0.160034 0.752551 0.386630 11.00000 0.02487 0.02707 = 0.02493 0.00537 0.00422 0.00434 C10B 1 0.091852 -0.649050 -0.091070 11.00000 0.02833 0.03423 = 0.03077 0.00877 0.00958 0.00446 C11A 1 -0.031494 1.024048 0.388387 11.00000 0.02477 0.02718 = 0.03230 0.01068 0.00337 0.00045 AFIX 43 H11A 2 0.060365 1.064494 0.374361 11.00000 -1.20000 AFIX 0 C11B 1 0.238158 -0.329881 -0.017081 11.00000 0.03694 0.03101 = 0.02985 0.00662 0.00786 0.00603 AFIX 43 H11B 2 0.178629 -0.307952 -0.057524 11.00000 -1.20000 AFIX 0 C12A 1 -0.157231 1.085020 0.402846 11.00000 0.02392 0.02660 = 0.02472 0.00699 0.00076 0.00088 C12B 1 0.328221 -0.241901 0.037183 11.00000 0.04050 0.02812 = 0.03178 0.00623 0.00836 0.00973 C13A 1 -0.147565 1.207431 0.397776 11.00000 0.02292 0.02675 = 0.02784 0.00878 0.00072 0.00365 C13B 1 0.323525 -0.119302 0.034241 11.00000 0.03881 0.02708 = 0.03337 0.00507 0.01418 0.00841 C14A 1 -0.395473 1.135900 0.423443 11.00000 0.02574 0.02586 = 0.02717 0.00913 0.00215 -0.00063 C14B 1 0.486827 -0.139375 0.139172 11.00000 0.03412 0.03432 = 0.03954 0.00441 0.00358 0.00757 C15A 1 -0.568404 1.138493 0.439627 11.00000 0.02628 0.03318 = 0.03951 0.01341 0.00456 0.00049 AFIX 137 H15A 2 -0.635743 1.135056 0.391465 11.00000 -1.50000 H15B 2 -0.576992 1.208983 0.477404 11.00000 -1.50000 H15C 2 -0.604712 1.073123 0.460517 11.00000 -1.50000 AFIX 0 C15B 1 0.603117 -0.101350 0.211570 11.00000 0.05352 0.04473 = 0.05195 0.00240 -0.00556 0.00939 AFIX 137 H15D 2 0.547320 -0.065039 0.254619 11.00000 -1.50000 H15E 2 0.691462 -0.046878 0.203441 11.00000 -1.50000 H15F 2 0.646322 -0.167362 0.223811 11.00000 -1.50000 AFIX 0 C16A 1 -0.357808 1.339371 0.397388 11.00000 0.03074 0.02354 = 0.03342 0.01055 0.00675 0.00718 AFIX 23 H16A 2 -0.287287 1.405955 0.430780 11.00000 -1.20000 H16B 2 -0.468708 1.342533 0.411620 11.00000 -1.20000 AFIX 0 C16B 1 0.452046 0.066701 0.125104 11.00000 0.04468 0.02715 = 0.04141 0.00138 0.01295 0.00166 AFIX 23 H16C 2 0.426599 0.099078 0.080025 11.00000 -1.20000 H16D 2 0.566702 0.092921 0.144680 11.00000 -1.20000 AFIX 0 C17A 1 -0.354238 1.343790 0.311614 11.00000 0.02362 0.02966 = 0.03245 0.00977 0.00108 0.00365 C17B 1 0.345966 0.110332 0.189277 11.00000 0.03843 0.03069 = 0.03486 0.00230 0.00307 0.00068 C18A 1 -0.374717 1.466046 0.222806 11.00000 0.07718 0.05663 = 0.03719 0.02319 0.01534 0.02205 AFIX 23 H18A 2 -0.464223 1.413927 0.188910 11.00000 -1.20000 H18B 2 -0.272502 1.448832 0.202067 11.00000 -1.20000 AFIX 0 C18B 1 0.179047 0.251967 0.237036 11.00000 0.06163 0.05870 = 0.03713 0.00318 0.01187 0.02936 AFIX 23 H18C 2 0.095977 0.190776 0.242829 11.00000 -1.20000 H18D 2 0.242685 0.284469 0.287984 11.00000 -1.20000 AFIX 0 C19A 1 -0.395669 1.587021 0.224223 11.00000 0.07400 0.05423 = 0.04327 0.02625 0.01127 0.02084 AFIX 33 H19A 2 -0.397029 1.598838 0.171578 11.00000 -1.50000 H19B 2 -0.497383 1.603248 0.244453 11.00000 -1.50000 H19C 2 -0.306290 1.638039 0.257566 11.00000 -1.50000 AFIX 0 C19B 1 0.101080 0.342274 0.209847 11.00000 0.07611 0.09760 = 0.06665 0.03049 0.02468 0.05470 AFIX 33 H19D 2 0.030189 0.374076 0.247542 11.00000 -1.50000 H19E 2 0.184048 0.402679 0.204580 11.00000 -1.50000 H19F 2 0.037851 0.309313 0.159582 11.00000 -1.50000 AFIX 0 N1A 3 -0.315506 1.048622 0.420800 11.00000 0.02677 0.02535 = 0.03055 0.00962 0.00229 0.00274 N1B 3 0.433242 -0.245745 0.103665 11.00000 0.04046 0.02925 = 0.04303 0.00519 0.00339 0.00897 N2A 3 -0.302294 1.233333 0.410130 11.00000 0.02313 0.02241 = 0.03658 0.01293 0.00705 0.00472 N2B 3 0.425834 -0.058873 0.100227 11.00000 0.03943 0.02633 = 0.03381 0.00538 0.00763 0.00487 O1A 4 0.245638 0.429156 0.420749 11.00000 0.02930 0.02329 = 0.05268 0.00910 0.00440 0.00516 AFIX 147 H1A1 2 0.160255 0.385241 0.418392 11.00000 -1.50000 AFIX 0 O1B 4 0.025954 -1.005979 -0.114110 11.00000 0.06796 0.02794 = 0.05676 0.00743 -0.00721 0.00042 AFIX 147 H1B1 2 0.091284 -1.026376 -0.083776 11.00000 -1.50000 AFIX 0 O2A 4 -0.034474 1.274774 0.385543 11.00000 0.02791 0.02596 = 0.04818 0.01359 0.00946 -0.00097 O2B 4 0.252899 -0.075225 -0.013440 11.00000 0.05553 0.03294 = 0.03887 0.01294 0.00596 0.01244 O3A 4 -0.338433 1.264118 0.258725 11.00000 0.06185 0.03696 = 0.03245 0.00309 0.00068 0.01234 O3B 4 0.319422 0.064964 0.243376 11.00000 0.05124 0.04096 = 0.03780 0.00894 0.00991 0.00812 O4A 4 -0.372934 1.449681 0.303338 11.00000 0.05399 0.03232 = 0.03564 0.01634 0.01277 0.01707 O4B 4 0.286161 0.204952 0.178793 11.00000 0.04702 0.03710 = 0.03462 0.00582 0.00857 0.01451 HKLF 5 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM newtwin in P-1 REM R1 = 0.0561 for 5031 Fo > 4sig(Fo) and 0.0947 for all 7227 data REM 456 parameters refined using 0 restraints END WGHT 0.0716 0.1836 REM Instructions for potential hydrogen bonds HTAB C3A O4A_$1 HTAB C3B O3B_$2 HTAB C15A O3B_$3 HTAB C15B O3B HTAB C16B O3A_$1 HTAB C18B O1A HTAB O1A O2A_$4 HTAB O1B O2B_$4 REM Highest difference peak 0.284, deepest hole -0.317, 1-sigma level 0.066 Q1 1 -0.3686 1.6644 0.2917 11.00000 0.05 0.28 Q2 1 -0.2827 1.5000 0.3286 11.00000 0.05 0.25 Q3 1 0.1865 -0.3763 -0.1138 11.00000 0.05 0.25 Q4 1 -0.3184 0.5993 0.3470 11.00000 0.05 0.25 Q5 1 0.1935 -0.6609 0.0174 11.00000 0.05 0.23 ; _shelx_res_checksum 28537 _shelx_hkl_file ; -2 0 1 166.806 6.34198 -2 2 0 0 166.806 6.34198 1 -3 0 1 15.9057 3.54848 -2 3 0 0 15.9057 3.54848 1 -4 0 2 268.912 9.91620 -2 4 0 0 268.912 9.91620 1 -5 0 2 22.9084 3.42697 -2 5 0 0 22.9084 3.42697 1 -6 0 3 172.626 7.57860 -2 6 0 0 172.626 7.57860 1 -7 0 3 51.9170 3.41523 -2 7 0 0 51.9170 3.41523 1 8 0 0 0.60918 2.22421 1 -9 0 4 7.53857 3.66312 -2 9 0 0 7.53857 3.66312 1 10 0 0 9.36368 3.37223 1 -10 1 4 23.9927 5.35402 -2 -10 1 0 23.9927 5.35402 1 -9 1 3 30.9145 6.87196 -2 -9 1 0 30.9145 6.87196 1 -8 1 3 13.4698 3.72792 -2 -8 1 0 13.4698 3.72792 1 -7 1 0 7.35644 2.02550 1 -6 1 2 2.84361 1.57216 -2 -6 1 0 2.84361 1.57216 1 -5 1 2 68.3614 5.78092 -2 -5 1 0 68.3614 5.78092 1 -4 1 1 310.543 5.85711 -2 -4 1 0 310.543 5.85711 1 -3 1 1 74.8414 4.78913 -2 -3 1 0 74.8414 4.78913 1 -2 1 0 5172.63 220.850 -2 -2 1 0 5172.63 220.850 1 -1 1 0 154.771 4.00273 1 0 1 0 0.01366 0.03197 1 1 1 0 169.359 2.70991 1 2 1 0 8.30480 0.52660 1 -3 -1 2 152.239 2.46306 -2 3 1 0 152.239 2.46306 1 4 1 0 227.191 4.19936 1 -5 -1 3 4.35026 1.57800 -2 5 1 0 4.35026 1.57800 1 6 1 0 149.229 4.40363 1 -7 -1 4 467.663 10.1682 -2 7 1 0 467.663 10.1682 1 -8 -1 4 7.27943 4.16121 -2 8 1 0 7.27943 4.16121 1 -9 -1 5 4.18236 4.47796 -2 9 1 0 4.18236 4.47796 1 -10 -1 5 21.9939 4.75438 -2 10 1 0 21.9939 4.75438 1 -10 2 3 17.3767 4.98607 -2 -10 2 0 17.3767 4.98607 1 -9 2 3 14.9567 5.77302 -2 -9 2 0 14.9567 5.77302 1 -8 2 2 18.2460 3.08690 -2 -8 2 0 18.2460 3.08690 1 -7 2 2 3.46254 2.53481 -2 -7 2 0 3.46254 2.53481 1 -6 2 1 8.09816 4.52754 -2 -6 2 0 8.09816 4.52754 1 -5 2 1 33.3148 2.16539 -2 -5 2 0 33.3148 2.16539 1 -4 2 0 199.817 10.5639 -2 -4 2 0 199.817 10.5639 1 -3 2 0 389.743 6.93115 -2 -3 2 0 389.743 6.93115 1 -2 2 0 442.950 6.35708 1 -1 2 0 115.887 1.78634 1 0 2 0 67.5991 1.39909 1 -1 -2 2 448.193 11.2297 -2 1 2 0 448.193 11.2297 1 2 2 0 733.862 9.65164 1 3 2 0 1.06955 0.59595 1 -4 -2 3 77.3022 2.65395 -2 4 2 0 77.3022 2.65395 1 -5 -2 4 24.3207 7.51508 -2 5 2 0 24.3207 7.51508 1 -6 -2 4 337.119 7.48898 -2 6 2 0 337.119 7.48898 1 7 2 0 135.957 4.43488 1 -8 -2 5 13.2739 2.80722 -2 8 2 0 13.2739 2.80722 1 9 2 0 0.03651 2.49401 1 -10 -2 6 3.12081 4.57347 -2 10 2 0 3.12081 4.57347 1 -10 3 0 4.72309 3.41720 1 -9 3 2 21.6148 4.22014 -2 -9 3 0 21.6148 4.22014 1 -8 3 0 -2.2637 1.49056 1 -7 3 1 -1.3199 1.30651 -2 -7 3 0 -1.3199 1.30651 1 -6 3 1 56.8966 8.13241 -2 -6 3 0 56.8966 8.13241 1 -5 3 0 37.3217 2.67225 -2 -5 3 0 37.3217 2.67225 1 -4 3 0 327.166 5.59183 1 3 -3 1 611.671 38.0524 -2 -3 3 0 611.671 38.0524 1 -2 3 0 36.0533 1.05612 1 -1 3 0 288.331 4.14630 1 0 -3 2 38.6096 1.03773 -2 0 3 0 38.6096 1.03773 1 1 3 0 85.3013 1.54899 1 -2 -3 3 642.762 9.07998 -2 2 3 0 642.762 9.07998 1 3 3 0 81.3858 1.83461 1 -4 -3 4 10.1416 1.74641 -2 4 3 0 10.1416 1.74641 1 -5 -3 4 105.746 8.27393 -2 5 3 0 105.746 8.27393 1 -6 -3 5 16.5333 2.66796 -2 6 3 0 16.5333 2.66796 1 -7 -3 5 60.9066 3.58585 -2 7 3 0 60.9066 3.58585 1 -8 -3 6 5.57842 5.71710 -2 8 3 0 5.57842 5.71710 1 -9 -3 6 6.14509 3.45633 -2 9 3 0 6.14509 3.45633 1 10 3 0 12.5987 3.55092 1 -10 4 2 6.40390 5.53794 -2 -10 4 0 6.40390 5.53794 1 -9 4 1 6.82846 5.26146 -2 -9 4 0 6.82846 5.26146 1 -8 4 1 100.270 5.39182 -2 -8 4 0 100.270 5.39182 1 -7 4 0 75.6358 8.98991 -2 -7 4 0 75.6358 8.98991 1 -6 4 0 145.123 3.09915 -2 -6 4 0 145.123 3.09915 1 -5 4 0 16.6062 1.47776 1 4 -4 1 27.3262 1.53569 -2 -4 4 0 27.3262 1.53569 1 -3 4 0 330.096 5.52449 1 2 -4 2 181.289 6.95307 -2 -2 4 0 181.289 6.95307 1 -1 4 0 20.2569 0.69078 1 0 -4 3 31.7001 1.83320 -2 0 4 0 31.7001 1.83320 1 -1 -4 3 493.464 11.6359 -2 1 4 0 493.464 11.6359 1 -2 -4 4 49.3083 3.49215 -2 2 4 0 49.3083 3.49215 1 -3 -4 4 33.8331 1.34756 -2 3 4 0 33.8331 1.34756 1 4 4 0 61.1515 1.77451 1 -5 -4 5 22.4770 1.68414 -2 5 4 0 22.4770 1.68414 1 6 4 0 5.58154 1.52392 1 -7 -4 6 18.3969 2.66620 -2 7 4 0 18.3969 2.66620 1 -8 -4 6 0.04805 3.68024 -2 8 4 0 0.04805 3.68024 1 -9 -4 7 28.0865 4.98377 -2 9 4 0 28.0865 4.98377 1 -10 -4 7 31.4854 5.56854 -2 10 4 0 31.4854 5.56854 1 -10 5 1 9.91760 4.76907 -2 -10 5 0 9.91760 4.76907 1 -9 5 1 1.14386 7.64217 -2 -9 5 0 1.14386 7.64217 1 -8 5 0 2.00409 3.86344 -2 -8 5 0 2.00409 3.86344 1 -7 5 0 7.29359 4.74909 -2 -7 5 0 7.29359 4.74909 1 6 -5 1 15.5019 3.21300 -2 -6 5 0 15.5019 3.21300 1 5 -5 1 35.0507 3.11570 -2 -5 5 0 35.0507 3.11570 1 4 -5 2 4.29714 6.34879 -2 -4 5 0 4.29714 6.34879 1 3 -5 2 165.242 3.48556 -2 -3 5 0 165.242 3.48556 1 -2 5 0 3.92892 0.70783 1 1 -5 3 474.163 7.27288 -2 -1 5 0 474.163 7.27288 1 0 5 0 525.707 7.94079 1 -1 -5 4 358.125 5.12791 -2 1 5 0 358.125 5.12791 1 -2 -5 4 180.257 7.54323 -2 2 5 0 180.257 7.54323 1 -3 -5 5 30.5960 2.34333 -2 3 5 0 30.5960 2.34333 1 -4 -5 5 18.8219 2.46880 -2 4 5 0 18.8219 2.46880 1 -5 -5 6 18.1122 6.03312 -2 5 5 0 18.1122 6.03312 1 -6 -5 6 8.55615 2.23214 -2 6 5 0 8.55615 2.23214 1 -7 -5 7 49.6575 7.75539 -2 7 5 0 49.6575 7.75539 1 -8 -5 7 10.5669 2.93656 -2 8 5 0 10.5669 2.93656 1 9 5 0 34.7716 4.44305 1 -10 6 0 10.2906 6.20866 -2 -10 6 0 10.2906 6.20866 1 -9 6 0 -0.6982 4.02007 -2 -9 6 0 -0.6982 4.02007 1 -8 6 0 16.7637 3.01231 1 7 -6 1 36.3906 3.50274 -2 -7 6 0 36.3906 3.50274 1 6 -6 1 3.35612 10.9187 -2 -6 6 0 3.35612 10.9187 1 5 -6 2 70.6957 2.83514 -2 -5 6 0 70.6957 2.83514 1 -4 6 0 10.4631 1.37162 1 3 -6 3 166.351 6.79434 -2 -3 6 0 166.351 6.79434 1 2 -6 3 83.2234 3.90521 -2 -2 6 0 83.2234 3.90521 1 -1 6 0 577.541 11.6247 1 0 -6 4 375.569 7.67114 -2 0 6 0 375.569 7.67114 1 1 6 0 61.2988 1.53318 1 -2 -6 5 184.447 3.62488 -2 2 6 0 184.447 3.62488 1 3 6 0 8.60800 0.70210 1 -4 -6 6 20.2609 1.39948 -2 4 6 0 20.2609 1.39948 1 -5 -6 6 9.09877 6.02881 -2 5 6 0 9.09877 6.02881 1 -6 -6 7 27.2466 2.92209 -2 6 6 0 27.2466 2.92209 1 -7 -6 7 9.88762 3.17447 -2 7 6 0 9.88762 3.17447 1 -8 -6 8 22.1149 3.91519 -2 8 6 0 22.1149 3.91519 1 -9 -6 8 6.92649 4.10856 -2 9 6 0 6.92649 4.10856 1 -10 7 0 1.07953 5.64955 -2 -10 7 0 1.07953 5.64955 1 9 -7 1 17.7267 5.02674 -2 -9 7 0 17.7267 5.02674 1 8 -7 1 6.11248 4.27841 -2 -8 7 0 6.11248 4.27841 1 7 -7 2 7.44259 6.22275 -2 -7 7 0 7.44259 6.22275 1 6 -7 2 210.502 5.49000 -2 -6 7 0 210.502 5.49000 1 -5 7 0 1.57012 1.56567 1 4 -7 3 58.4986 2.49422 -2 -4 7 0 58.4986 2.49422 1 -3 7 0 -0.2886 0.50765 1 2 -7 4 410.801 7.36055 -2 -2 7 0 410.801 7.36055 1 -1 7 0 113.144 2.81712 1 0 -7 5 12.7459 1.26041 -2 0 7 0 12.7459 1.26041 1 -1 -7 5 104.294 3.40968 -2 1 7 0 104.294 3.40968 1 -2 -7 6 60.2454 2.06783 -2 2 7 0 60.2454 2.06783 1 -3 -7 6 7.80460 1.14419 -2 3 7 0 7.80460 1.14419 1 -4 -7 7 17.7564 5.30893 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