############################################################################## # # # This CIF contains the data in a paper accepted for publication in # # Acta Crystallographica Section E. It conforms to the requirements of # # Notes for Authors for Acta Crystallographica Section E, and has been # # peer reviewed under the auspices of the IUCr Commission on Journals. # # # # Full details of the Crystallographic Information File format # # are given in the paper "The Crystallographic Information File (CIF): # # a New Standard Archive File for Crystallography" by S. R. Hall, F. H. # # Allen and I. D. Brown [Acta Cryst. (1991), A47, 655-685]. # # # # The current version of the core CIF dictionary is obtainable from # # ftp://ftp.iucr.org/pub/cif_core.dic. # # # # Software is freely available for graphical display of the structure(s) # # in this CIF. For information consult the CIF software page # # http://www.iucr.org/resources/cif/software. # # # # This file may be used for bona fide research purposes within the # # scientific community so long as proper attribution is given to the journal # # article from which it was obtained. # # # ############################################################################## data_I _audit_creation_method 'SHELXL-2016/6' _chemical_name_systematic 'Bis[pyridin-2(1H)-one] 2,5-dichloro-3,6-dihydroxy-1,4-bebzoquinone' _chemical_name_common 'bis(2-pyridone) chloranilic acid' _chemical_formula_moiety '2(C5 H5 N O) , C6 H2 Cl2 O4' _chemical_formula_sum 'C16 H12 Cl2 N2 O6' _chemical_formula_iupac '2C5 H5 N O , C6 H2 Cl2 O4' _chemical_formula_weight 399.19 _chemical_melting_point ? _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. ; _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 2/c' _space_group_name_Hall '-P 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' _cell_length_a 11.9402(7) _cell_length_b 3.7005(2) _cell_length_c 21.7919(13) _cell_angle_alpha 90.0000 _cell_angle_beta 121.278(2) _cell_angle_gamma 90.0000 _cell_volume 822.92(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 20111 _cell_measurement_theta_min 3.29 _cell_measurement_theta_max 30.07 _cell_measurement_temperature 120.0(10) _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.390 _exptl_crystal_size_mid 0.360 _exptl_crystal_size_min 0.210 _exptl_crystal_density_diffrn 1.611 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408.00 _exptl_absorpt_coefficient_mu 0.432 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (ABSCOR; Higashi, 1995) ; _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.913 _diffrn_ambient_temperature 120(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPIDII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 22767 _diffrn_reflns_av_R_equivalents 0.0129 _diffrn_reflns_theta_min 3.415 _diffrn_reflns_theta_max 29.998 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? _reflns_number_total 2401 _reflns_number_gt 2316 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.0763 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_number_reflns 2401 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0443P)^2^+0.3557P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.489 _refine_diff_density_min -0.244 _refine_ls_extinction_method none _refine_ls_extinction_coef . 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' 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; RAPID-AUTO (Rigaku, 2006) ; _computing_cell_refinement ; RAPID-AUTO (Rigaku, 2006) ; _computing_data_reduction ; RAPID-AUTO (Rigaku, 2006) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2016 (Sheldrick, 2015) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; CrystalStructure (Rigaku, 2010), PLATON (Spek, 2009) ; loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl Cl1 0.60869(2) 0.78653(6) 0.40403(2) 0.01704(8) Uani d 1 . . O O1 0.33921(7) 0.8229(2) 0.37552(4) 0.02149(16) Uani d 1 . . O O2 0.75999(6) 0.4050(2) 0.54453(4) 0.01794(15) Uani d 1 . . H H2 0.8039(15) 0.289(4) 0.5870(8) 0.027 Uiso d 1 . . O O3 0.92219(7) 0.1199(2) 0.66164(4) 0.02094(16) Uani d 1 . . N N1 1.13199(8) -0.0736(2) 0.72858(4) 0.01604(16) Uani d 1 . . H H1 1.1281(13) -0.016(4) 0.7672(8) 0.024 Uiso d 1 . . C C1 0.41591(9) 0.6765(2) 0.43248(5) 0.01361(17) Uani d 1 . . C C2 0.55361(8) 0.6274(3) 0.45806(5) 0.01311(16) Uani d 1 . . C C3 0.63639(8) 0.4587(2) 0.52136(5) 0.01342(17) Uani d 1 . . C C4 1.02174(9) -0.0153(3) 0.66317(5) 0.01563(17) Uani d 1 . . C C5 1.02800(9) -0.1116(3) 0.60168(5) 0.01779(18) Uani d 1 . . H H5 0.953363 -0.080221 0.554948 0.021 Uiso calc 1 . . C C6 1.14171(10) -0.2497(3) 0.60990(5) 0.01837(19) Uani d 1 . . H H6 1.145376 -0.312374 0.568705 0.022 Uiso calc 1 . . C C7 1.25330(10) -0.2995(3) 0.67902(5) 0.01870(19) Uani d 1 . . H H7 1.332337 -0.392760 0.684778 0.022 Uiso calc 1 . . C C8 1.24515(9) -0.2109(3) 0.73732(5) 0.01775(18) Uani d 1 . . H H8 1.318846 -0.245048 0.784277 0.021 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl1 0.02123(12) 0.01778(12) 0.01883(12) 0.00121(8) 0.01512(10) 0.00259(7) O1 0.0172(3) 0.0304(4) 0.0166(3) 0.0046(3) 0.0086(3) 0.0080(3) O2 0.0124(3) 0.0244(4) 0.0172(3) 0.0022(3) 0.0079(2) 0.0040(3) O3 0.0149(3) 0.0307(4) 0.0184(3) 0.0048(3) 0.0095(3) 0.0034(3) N1 0.0158(3) 0.0189(4) 0.0145(3) 0.0021(3) 0.0086(3) 0.0000(3) C1 0.0150(4) 0.0138(4) 0.0134(4) 0.0000(3) 0.0083(3) -0.0005(3) C2 0.0150(4) 0.0139(4) 0.0139(4) 0.0000(3) 0.0098(3) 0.0002(3) C3 0.0139(4) 0.0137(4) 0.0143(4) -0.0005(3) 0.0084(3) -0.0010(3) C4 0.0142(4) 0.0170(4) 0.0162(4) -0.0005(3) 0.0083(3) 0.0012(3) C5 0.0178(4) 0.0207(4) 0.0146(4) -0.0011(3) 0.0082(3) 0.0004(3) C6 0.0221(4) 0.0189(4) 0.0179(4) -0.0015(3) 0.0131(4) -0.0018(3) C7 0.0184(4) 0.0190(4) 0.0211(4) 0.0023(3) 0.0119(4) -0.0009(3) C8 0.0157(4) 0.0191(4) 0.0174(4) 0.0033(3) 0.0078(3) 0.0002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 C2 . 1.7233(9) ? O1 C1 . 1.2217(11) ? O2 C3 . 1.3033(10) ? O2 H2 . 0.901(16) ? O3 C4 . 1.2739(11) ? N1 C8 . 1.3611(12) ? N1 C4 . 1.3648(11) ? N1 H1 . 0.892(15) ? C1 C2 . 1.4475(12) ? C1 C3 3_666 1.5182(12) ? C2 C3 . 1.3614(12) ? C4 C5 . 1.4256(13) ? C5 C6 . 1.3726(14) ? C5 H5 . 0.9500 ? C6 C7 . 1.4120(14) ? C6 H6 . 0.9500 ? C7 C8 . 1.3636(14) ? C7 H7 . 0.9500 ? C8 H8 . 0.9500 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C3 O2 H2 . . 114.1(10) ? C8 N1 C4 . . 123.66(8) ? C8 N1 H1 . . 119.5(9) ? C4 N1 H1 . . 116.9(9) ? O1 C1 C2 . . 123.32(8) ? O1 C1 C3 . 3_666 118.05(8) ? C2 C1 C3 . 3_666 118.63(7) ? C3 C2 C1 . . 121.99(8) ? C3 C2 Cl1 . . 121.00(7) ? C1 C2 Cl1 . . 117.01(7) ? O2 C3 C2 . . 122.88(8) ? O2 C3 C1 . 3_666 117.75(8) ? C2 C3 C1 . 3_666 119.37(8) ? O3 C4 N1 . . 118.06(8) ? O3 C4 C5 . . 125.24(8) ? N1 C4 C5 . . 116.69(8) ? C6 C5 C4 . . 120.10(9) ? C6 C5 H5 . . 120.0 ? C4 C5 H5 . . 120.0 ? C5 C6 C7 . . 120.62(9) ? C5 C6 H6 . . 119.7 ? C7 C6 H6 . . 119.7 ? C8 C7 C6 . . 118.57(9) ? C8 C7 H7 . . 120.7 ? C6 C7 H7 . . 120.7 ? N1 C8 C7 . . 120.35(9) ? N1 C8 H8 . . 119.8 ? C7 C8 H8 . . 119.8 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1 C1 C2 C3 . . . . -179.08(9) ? C3 C1 C2 C3 3_666 . . . 1.18(15) ? O1 C1 C2 Cl1 . . . . -0.05(13) ? C3 C1 C2 Cl1 3_666 . . . -179.79(6) ? C1 C2 C3 O2 . . . . 178.46(9) ? Cl1 C2 C3 O2 . . . . -0.53(14) ? C1 C2 C3 C1 . . . 3_666 -1.19(15) ? Cl1 C2 C3 C1 . . . 3_666 179.82(7) ? C8 N1 C4 O3 . . . . -178.90(9) ? C8 N1 C4 C5 . . . . 1.04(15) ? O3 C4 C5 C6 . . . . 178.84(10) ? N1 C4 C5 C6 . . . . -1.09(15) ? C4 C5 C6 C7 . . . . 0.28(16) ? C5 C6 C7 C8 . . . . 0.64(16) ? C4 N1 C8 C7 . . . . -0.13(16) ? C6 C7 C8 N1 . . . . -0.73(15) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O2 H2 O3 . 0.901(15) 1.627(16) 2.4989(11) 161.9(19) y N1 H1 O3 2_756 0.893(16) 1.996(17) 2.8743(12) 167.6(16) y C7 H7 Cl1 3_756 0.95 2.79 3.5122(13) 134 y _shelx_hkl_file ; 0 0 -3 37.51 3.72 0 0 -3 80.69 5.80 0 0 3 30.37 3.27 0 0 3 28.74 3.41 -2 0 2 8020.32 81.05 2 0 -2 8078.62 78.53 2 0 -2 7824.40 77.13 2 0 -2 8069.59 78.18 -2 0 2 8149.49 77.22 -2 0 2 8067.65 76.24 -2 0 1 42.14 4.27 -2 0 1 49.08 6.79 2 0 -1 105.88 8.06 2 0 -1 104.85 4.59 -2 0 1 53.69 4.13 2 0 -3 99.37 6.23 2 0 -3 62.63 5.66 2 0 -3 83.37 5.31 -2 0 3 96.05 8.42 -2 0 3 92.75 6.10 -1 0 -2 175314. 2434. -1 0 -2 191001. 2647. 1 0 2 195902. 2720. 1 0 2 174905. 2437. 1 0 2 194562. 2676. -1 0 -2 196258. 2701. -1 0 434194.01 367.46 -1 0 434689.30 374.24 1 0 -434059.99 368.02 1 0 -434613.89 373.04 1 0 -434244.65 367.84 -1 0 434239.67 370.07 2 0 0 137.92 5.88 -2 0 0 128.42 6.08 -2 0 0 145.39 5.35 -2 0 0 136.51 9.68 2 0 0 136.06 10.11 -2 0 483074.93 1009.29 2 0 -480208.57 985.25 2 0 -482800.39 1007.20 2 0 -483343.25 1013.44 -2 0 482321.74 999.99 -2 0 479564.15 976.24 0 0 -477872.67 954.93 0 0 481893.78 1001.14 0 0 478181.15 960.02 0 0 -481910.02 1002.37 1 0 3 1.64 6.75 1 0 3 -1.02 6.47 -1 0 -3 0.15 4.60 -1 0 -3 -2.65 7.99 -1 0 -3 6.12 2.85 -2 0 -1 8.02 9.22 -2 0 -1 42.15 9.13 -2 0 -1 9.10 6.91 2 0 1 12.43 9.30 2 0 1 19.21 8.26 2 0 1 6.98 3.84 1 0 -5 78.18 5.00 1 0 -5 76.83 7.83 1 0 -5 90.60 8.22 -1 0 5 110.28 7.87 -1 0 5 67.10 7.79 2 0 -5 114.30 4.60 2 0 -5 110.77 7.44 2 0 -5 120.89 4.76 -2 0 5 107.38 6.26 -2 0 5 106.62 7.56 2 0 -5 118.41 10.88 -2 0 5 116.18 4.71 -2 0 5 94.30 7.31 3 0 -3 13.89 9.91 3 0 -3 9.40 4.46 -3 0 3 14.51 6.03 3 0 -3 8.77 6.95 -3 0 3 12.68 4.48 -3 0 3 13.79 7.52 3 0 -259246.58 700.85 3 0 -258271.21 693.73 -3 0 258497.77 696.55 3 0 -259368.32 710.64 -3 0 259100.64 702.22 -3 0 259525.21 703.87 3 0 -412187.39 126.79 3 0 -411790.93 123.80 -3 0 411922.14 130.50 3 0 -412168.70 121.91 -3 0 411827.47 122.63 -3 0 412080.88 121.55 -2 0 -216385.93 167.17 -2 0 -215700.72 166.03 2 0 216040.52 176.37 -2 0 -216022.45 169.85 2 0 216273.03 165.96 2 0 215926.21 168.48 0 0 -5 9.90 4.52 0 0 -5 2.60 5.35 0 0 5 -1.77 4.23 0 0 -5 -0.13 4.76 0 0 5 5.48 4.37 3 0 -1 8.01 8.77 3 0 -1 1.61 8.94 3 0 -1 33.42 9.95 -3 0 1 17.39 8.65 -3 0 1 11.59 8.46 -3 0 1 -2.67 5.20 0 1 027475.94 297.49 0 -1 027252.55 291.98 0 1 027187.82 291.09 0 1 027697.86 295.27 0 1 026889.32 290.77 0 1 027215.13 295.12 0 -1 027398.87 292.58 0 1 -1 2200.08 24.79 0 -1 -1 2179.82 24.19 0 -1 1 2263.53 25.76 0 1 1 2218.54 25.24 0 1 -1 2189.16 28.85 0 1 -1 2150.06 24.92 0 1 -1 2249.47 25.02 0 -1 -1 2237.72 28.87 0 1 1 2322.71 29.33 0 -1 -1 2239.73 25.77 0 1 1 2190.26 25.74 0 1 1 2200.42 28.53 0 -1 1 2188.91 28.98 3 0 -5 5.68 3.57 -3 0 5 28.79 6.49 3 0 -5 11.28 6.29 3 0 -5 8.63 9.58 -3 0 5 8.75 3.96 -3 0 5 5.44 9.84 2 0 -6 3805.76 41.18 -2 0 6 3763.88 40.88 2 0 -6 3804.99 37.68 -2 0 6 3851.13 41.66 2 0 -6 3820.89 41.38 -2 0 6 3751.99 44.05 2 0 -6 3751.11 44.72 -2 0 6 3875.52 41.44 -1 0 -410056.61 104.57 1 0 410140.40 105.23 1 0 410225.29 106.23 -1 0 -410388.20 108.12 -1 0 -410417.03 105.41 -1 -1 1 2980.14 37.21 -1 1 1 2864.75 31.30 1 -1 -1 2989.06 36.83 1 1 -1 2955.79 30.90 -1 1 1 2954.16 28.90 -1 1 1 2940.46 35.61 -1 1 1 2970.91 29.05 -1 -1 1 2945.24 30.80 1 1 -1 2859.98 31.51 1 1 -1 2977.73 34.57 1 1 -1 3037.88 31.61 1 -1 -1 2956.76 31.58 -1 0 624269.37 262.42 -1 0 624452.16 264.45 -1 0 624511.24 266.68 1 0 -624488.95 265.62 1 0 -624612.09 263.21 1 0 -624725.01 268.45 -1 -1 0 124000. 1627. -1 1 0 122335. 1596. -1 1 0 122267. 1602. 1 1 0 128125. 1668. 1 -1 0 124158. 1635. 1 1 0 126587. 1650. -1 1 0 122669. 1620. -1 -1 0 124773. 1624. 1 1 0 124883. 1628. 1 -1 0 122779. 1614. 1 -1 0 123246. 1616. 1 1 0 122486. 1609. 1 -1 -2 146.34 7.55 1 1 -2 164.47 7.36 -1 -1 2 140.98 12.17 1 -1 -2 141.33 9.48 -1 1 2 136.02 5.69 1 1 -2 132.99 5.68 -1 1 2 124.84 12.00 -1 1 2 141.18 3.85 1 1 -2 127.15 7.48 -1 1 2 129.91 7.69 1 1 -2 124.71 12.43 -1 1 2 140.02 6.07 1 1 -2 128.32 5.40 0 1 -2 124394. 1648. 0 1 -2 124965. 1625. 0 1 -2 124094. 1638. 0 1 2 125545. 1660. 0 -1 -2 123434. 1607. 0 1 -2 126098. 1664. 0 -1 -2 125781. 1664. 0 1 2 124580. 1640. 0 -1 2 123756. 1610. 0 1 2 123961. 1602. 0 1 2 124354. 1617. 0 -1 2 124520. 1641. 3 0 053517.72 634.81 3 0 054880.29 651.50 3 0 056236.57 659.57 -3 0 056499.90 664.27 -3 0 053792.73 638.31 -3 0 054632.84 648.77 1 -1 1 139813. 1890. 1 -1 1 138054. 1848. -1 1 -1 139532. 1877. -1 -1 -1 139304. 1868. 1 1 1 138727. 1855. -1 1 -1 138367. 1848. -1 1 -1 138495. 1853. -1 -1 -1 142479. 1910. 1 1 1 144078. 1896. 1 1 1 143697. 1928. 1 -1 1 139683. 1871. -3 0 6 2138.91 26.33 -3 0 6 2102.09 31.54 3 0 -6 2115.37 26.12 3 0 -6 2105.11 32.22 -3 0 6 2134.98 26.21 3 0 -6 2175.01 26.85 1 1 -3 256220. 3796. -1 1 3 256940. 3712. -1 1 3 249888. 3658. -1 -1 3 260779. 3854. -1 1 3 251749. 3734. 1 1 -3 263659. 3817. 1 1 -3 265925. 3933. 1 -1 -3 250979. 3732. -1 -1 3 251902. 3729. -1 1 3 250475. 3704. -1 1 3 255382. 3690. 1 1 -3 254591. 3785. 1 -1 -3 250100. 3669. -2 0 -3 -2.38 6.16 -2 0 -3 13.37 3.91 2 0 3 10.84 10.45 2 0 3 14.29 9.91 -2 0 -3 1.45 9.61 0 1 -3 217510. 3157. 0 -1 3 220743. 3189. 0 -1 3 220522. 3146. 0 1 3 217559. 3065. 0 1 3 219483. 3171. 0 -1 -3 219554. 3183. 0 1 -3 220581. 3147. 0 1 3 216861. 3091. 0 1 -3 226205. 3271. 0 -1 -3 216909. 3058. 0 -1 -3 218631. 3112. 0 1 3 220619. 3197. 2 1 -2 37.87 2.96 2 -1 -2 22.39 6.35 -2 -1 2 19.99 8.80 -2 -1 2 47.31 5.08 -2 1 2 31.92 10.53 2 1 -2 31.40 6.53 -2 1 2 101.55 11.23 -2 -1 2 44.91 11.27 2 -1 -2 24.08 9.80 2 1 -2 27.34 8.59 2 -1 -2 23.63 5.52 -2 1 2 63.03 5.80 -2 0 7 2.68 6.46 -2 0 7 3.39 6.35 2 0 -7 1.43 6.31 2 0 -7 6.42 3.71 2 0 -7 3.60 3.79 -2 0 7 5.14 3.73 2 0 -7 7.95 7.67 -2 0 7 9.19 4.63 -2 -1 1 141685. 1888. -2 1 1 134826. 1824. -2 -1 1 141749. 1882. 2 1 -1 141761. 1890. 2 -1 -1 137569. 1853. -2 1 1 136743. 1840. -2 1 1 136253. 1816. 2 -1 -1 137824. 1864. 2 -1 -1 137894. 1839. 2 1 -1 135951. 1832. 2 1 -1 142447. 1891. -2 -1 1 138999. 1880. 0 0 654910.04 657.59 0 0 -655165.04 660.05 0 0 -655437.77 648.82 0 0 656044.16 667.79 0 0 -656574.26 675.68 2 1 -348594.20 538.22 2 1 -349612.63 577.04 -2 -1 348404.13 534.22 -2 1 347155.10 553.24 -2 1 347545.58 551.12 -2 -1 348228.77 567.04 2 -1 -348519.67 540.88 -2 -1 348350.27 562.52 2 1 -348865.12 539.88 2 -1 -347882.84 563.22 2 -1 -347962.63 562.05 2 1 -347390.82 564.02 -2 1 347668.47 529.81 -1 -1 -2 2513.47 27.68 1 1 2 2551.65 23.48 1 1 2 2495.15 29.42 -1 1 -2 2501.57 32.27 -1 1 -2 2444.86 30.31 1 -1 2 2537.39 35.98 -1 1 -2 2525.26 36.24 -1 -1 -2 2521.40 35.10 1 -1 2 2544.09 32.50 1 -1 2 2453.15 30.24 1 1 2 2434.94 31.77 -3 0 -1 3.84 5.97 3 0 1 4.78 4.48 3 0 1 6.35 5.81 3 0 1 11.98 10.32 -3 0 -1 0.25 9.49 -3 0 -1 8.22 7.67 1 1 -439057.51 449.57 1 1 -438699.84 415.71 -1 1 438809.79 415.36 1 -1 -438496.83 443.22 -1 1 438860.54 452.91 -1 1 438969.70 447.95 -1 1 438243.82 422.70 -1 -1 439038.21 448.68 1 -1 -439560.21 461.73 1 1 -438682.32 446.19 1 1 -438851.79 454.14 1 -1 -439309.44 434.90 -1 0 -5 5.31 9.69 1 0 5 14.02 9.42 1 0 5 5.46 5.50 -1 0 -5 9.84 5.53 -1 0 -5 8.29 3.64 -2 1 045844.27 534.00 -2 -1 046392.99 537.22 -2 -1 046852.96 531.01 2 1 046093.44 543.79 2 -1 046704.29 538.33 -2 1 045846.70 543.68 -2 1 045785.26 533.16 -2 -1 045937.59 536.07 2 -1 046350.15 543.10 2 -1 045674.32 533.48 2 1 047000.10 539.31 2 1 047226.03 532.82 -4 0 447764.45 562.09 -4 0 447984.07 562.88 -4 0 447267.42 565.00 4 0 -447404.32 558.32 4 0 -447666.46 553.98 4 0 -447444.33 552.94 -1 0 7 13.90 4.47 1 0 -7 2.02 4.15 -1 0 7 10.41 4.11 -1 0 7 2.20 4.64 1 0 -7 8.25 4.46 1 0 -7 2.92 7.23 -3 0 7 20.84 6.87 3 0 -7 13.07 6.36 -3 0 7 17.71 6.98 -3 0 7 11.93 5.88 3 0 -7 12.51 6.78 3 0 -7 39.75 6.99 3 0 -7 10.69 6.93 -3 0 7 23.44 4.39 2 -1 -427217.91 311.07 2 -1 -427907.08 279.95 2 1 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113.71 10 3 -2 -11.34 37.04 -7 -4 5 5169.59 93.31 10 -3 -2 3.12 22.72 -10 3 2 -8.60 38.07 -10 3 2 4.17 23.33 7 -4 -5 5025.21 94.43 7 4 -5 5176.13 120.99 -7 4 5 5118.47 92.42 7 4 -5 5222.20 90.23 10 3 -2 4.27 20.69 -7 4 5 5243.75 95.93 10 -3 -2 19.82 22.32 7 -4 -5 5100.96 91.21 -10 -3 2 19.26 22.99 10 3 -2 3.71 15.94 7 4 -5 5213.65 92.20 10 -3 -2 5.61 37.89 -10 -3 2 -4.47 15.39 -10 -3 2 21.41 21.00 -10 3 2 11.91 37.96 -10 2 23 2297.45 82.60 10 2 -23 2363.01 59.57 10 2 -23 2354.09 89.30 -10 2 23 2355.02 49.04 -10 2 23 2471.03 59.40 10 2 -23 2244.33 80.61 -10 -2 23 2249.34 61.08 10 -2 -23 2394.02 66.81 -9 1 26 1587.58 43.11 1 -4 10 1971.94 42.81 1 4 10 2009.61 72.72 -1 4 -10 2078.15 76.12 9 1 -26 1568.19 60.52 9 -1 -26 1566.11 58.42 -9 1 26 1586.81 60.99 -1 4 -10 1983.21 57.76 9 1 -26 1682.85 60.74 -9 1 26 1629.22 56.03 -1 4 -10 2139.30 59.55 -1 4 -10 1981.72 76.41 1 4 10 1979.44 50.78 -9 -1 26 1584.07 47.77 9 1 -26 1615.51 50.77 11 -1 4 43.20 45.39 10 -3 -17 7902.42 159.98 -11 -1 -4 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23.94 21.61 -11 1 25 -1.24 17.68 -11 1 25 11.27 16.68 -11 1 25 9.92 16.79 4 0 -26 52.23 17.02 11 1 -25 7.20 17.96 4 0 -26 58.87 17.90 11 -1 -25 23.50 19.99 11 1 -25 26.15 28.69 -4 0 26 36.01 16.54 -4 0 26 40.01 15.75 4 0 -26 50.83 18.23 4 0 -26 39.14 17.00 -11 0 -5 -7.13 30.57 11 0 5 -1.21 13.86 -11 0 -5 -3.05 20.79 11 0 5 -7.62 36.45 -11 0 -5 5.57 19.07 6 4 -12 1100.62 59.70 -8 0 27 -9.49 11.53 -8 0 27 3.45 13.98 8 0 -27 -2.89 19.04 8 0 -27 0.00 19.40 -6 4 12 992.21 69.99 6 4 -12 1035.40 72.07 6 4 -12 1066.94 45.07 -6 4 12 1137.90 43.07 -8 0 27 13.84 18.92 8 0 -27 -7.80 25.97 6 -4 -12 1141.64 42.25 -6 4 12 1042.58 46.30 -5 2 24 1154.41 46.68 5 2 -24 1182.44 45.99 7 3 7 1616.42 45.87 7 -3 7 1551.95 65.44 -7 -3 -7 1620.12 64.11 7 -3 7 1632.79 68.63 -7 3 -7 1610.48 64.61 5 2 -24 1202.51 68.48 -7 -3 -7 1668.10 47.09 5 2 -24 1154.23 45.92 -7 3 -7 1655.24 70.07 -5 2 24 1236.77 46.54 -7 3 -7 1556.95 53.91 7 3 7 1525.73 65.46 -5 0 -17 -17.26 19.65 5 0 17 -1.96 32.56 -5 0 -17 2.70 16.95 5 0 17 13.72 35.24 -5 0 -17 -6.34 31.40 -5 0 -17 7.70 17.29 -3 -3 -14 573.35 60.19 3 3 14 702.61 36.59 -3 3 -14 604.57 63.04 -3 3 -14 587.09 40.93 -3 -3 -14 693.56 37.65 3 -3 14 589.09 26.36 3 -3 14 607.48 39.68 3 3 14 611.52 60.87 -3 3 -14 606.97 25.09 -2 4 -9 70.16 26.64 2 4 9 34.88 20.56 2 -4 9 42.95 13.31 -2 4 -9 60.01 23.23 -2 4 -9 53.46 27.49 2 4 9 31.00 20.19 -2 -4 -9 42.93 21.09 2 4 9 46.97 35.03 2 -4 9 46.13 37.10 2 4 9 60.79 34.63 -2 4 -9 35.21 21.94 1 0 -24 1854.62 52.05 1 0 -24 1969.74 53.33 -1 0 24 1958.25 50.62 -2 0 -21 -4.74 19.33 -2 0 -21 10.71 19.44 -2 0 -21 2.14 20.39 2 0 21 5.59 20.64 1 0 -24 1908.99 66.38 2 0 21 11.05 30.90 -1 0 24 1953.88 45.83 -2 0 -21 36.56 32.25 1 0 -24 1987.04 67.50 -11 -3 7 893.21 31.48 7 0 -27 11.33 27.60 7 0 -27 -10.68 14.17 11 -3 -7 937.64 43.96 11 -3 -7 893.01 35.45 11 -3 -7 923.02 44.15 7 0 -27 -10.13 13.56 -11 -3 7 957.22 69.50 -11 3 7 963.83 45.40 -11 3 7 916.33 67.76 11 3 -7 959.65 44.34 -11 3 7 961.37 36.00 -7 0 27 -17.18 14.06 -11 -3 7 875.25 29.12 11 3 -7 1032.09 69.81 -7 0 27 7.71 13.13 -5 4 1311117.10 142.30 5 4 -1312090.77 203.20 13 2 -17 1211.15 47.72 13 2 -17 1202.40 49.51 13 2 -17 1103.14 80.25 13 -2 -17 1296.72 48.65 -5 4 1311831.60 203.61 -5 4 1311837.64 203.54 -13 2 17 1258.85 49.48 -13 -2 17 1287.34 48.38 13 -2 -17 1208.72 49.02 5 4 -1311865.32 180.99 -13 2 17 1266.28 72.94 -13 -2 17 1208.46 71.62 5 4 -1312194.58 204.30 5 4 -1311774.67 179.83 -9 3 19 8729.37 140.91 9 3 -19 8753.24 175.02 9 -3 -19 8838.05 142.33 -9 3 19 8972.18 177.82 9 3 -19 9063.61 172.46 -9 3 19 8736.91 144.19 9 3 -19 9009.72 150.55 -14 -1 1912296.53 189.71 -14 -1 1912630.39 205.28 -14 1 1912532.16 189.80 -14 -1 1912718.02 171.13 14 1 -1912576.12 169.76 -14 1 1912676.25 174.73 14 -1 -1912462.91 181.50 -14 1 1912578.84 183.79 14 -1 -1912840.66 195.53 14 1 -1912397.75 216.72 14 -1 -1912590.34 173.49 14 1 -1912784.68 207.34 12 1 -24 4.27 16.62 11 -3 -14 2063.04 53.01 -11 3 14 2014.45 86.17 -11 3 14 1998.25 73.70 -12 1 24 -44.42 28.91 -11 3 14 2085.92 59.59 12 -1 -24 -11.69 30.38 11 3 -14 2092.72 73.18 11 3 -14 2124.62 88.40 12 1 -24 9.26 22.03 -11 -3 14 1962.13 68.04 11 -3 -14 2042.58 58.41 11 3 -14 1953.41 58.29 -12 1 24 0.94 19.41 12 1 -24 0.05 15.56 -11 -3 14 1945.16 58.68 -12 -1 24 -0.10 36.00 -12 1 24 12.87 28.27 -7 4 10 8.07 18.24 -7 4 10 -24.40 29.81 -7 4 10 -2.52 13.51 7 -4 -10 1.88 21.90 7 4 -10 2.63 14.58 7 4 -10 -0.44 18.63 7 -4 -10 16.37 31.17 7 4 -10 -1.59 19.62 -7 -4 10 0.39 18.45 -9 -3 -2 22.87 21.88 9 3 2 30.19 22.32 9 -3 2 60.54 36.49 -9 3 -2 27.95 18.83 -9 -3 -2 18.78 17.11 9 3 2 33.86 17.39 9 -3 2 24.72 25.60 9 -3 2 31.41 18.67 -9 3 -2 36.27 25.33 -9 3 -2 21.31 36.50 -12 0 25 -0.10 11.67 12 0 -25 -3.22 18.85 12 0 -25 -4.35 19.47 -12 0 25 2.25 19.42 -12 0 25 18.85 19.34 12 0 -25 -4.07 20.43 -5 -3 -11 132.82 33.22 -5 3 -11 173.37 29.98 5 -3 11 162.17 36.05 -5 3 -11 137.35 33.80 5 3 11 166.87 34.34 5 3 11 214.37 28.59 -5 3 -11 161.19 30.81 -5 -3 -11 141.40 27.54 5 -3 11 185.78 47.73 -14 0 21 -9.83 24.04 14 0 -21 -3.06 38.66 14 0 -21 18.06 13.22 -14 0 21 -9.23 14.23 -14 0 21 17.06 13.86 14 0 -21 11.61 13.59 -14 0 21 7.47 14.43 11 0 -26 1480.84 47.81 -11 0 26 1481.52 46.11 11 0 -26 1481.73 45.16 -11 0 26 1376.98 33.31 -11 0 26 1576.51 47.24 11 0 -26 1452.30 33.67 6 4 1 786.91 38.77 -6 4 -1 786.22 43.04 -6 4 -1 855.09 39.93 -6 4 -1 913.10 50.33 6 -4 1 838.12 28.08 -6 -4 -1 825.27 26.88 -6 -4 -1 800.32 50.42 6 -4 1 816.44 51.49 6 4 1 855.63 33.35 -7 4 3 7507.25 123.58 7 4 -3 7561.16 112.83 7 4 -3 7581.58 111.88 7 4 -3 7671.40 153.84 7 4 -3 7696.35 126.51 -7 4 3 7661.79 116.04 7 -4 -3 7674.52 129.37 7 -4 -3 7668.32 115.89 -7 -4 3 7510.01 153.32 -7 4 3 7527.36 153.83 8 3 -20 838.65 71.82 8 3 -20 841.28 69.39 9 2 -24 100.31 28.14 9 -2 -24 125.06 18.92 8 -3 -20 874.75 38.96 8 3 -20 865.90 46.41 9 2 -24 116.40 26.95 9 2 -24 114.63 30.69 -9 2 24 128.17 27.64 -9 2 24 107.19 29.01 -9 2 24 69.43 45.24 -8 3 20 912.29 38.85 -8 3 20 893.46 47.48 -8 3 20 817.34 73.22 -6 2 -13 5508.26 105.74 6 2 13 5371.46 102.92 6 -2 13 5567.68 131.70 -6 2 -13 5483.13 117.62 -6 -2 -13 5475.98 129.89 -6 -2 -13 5423.53 115.95 6 2 13 5444.58 92.40 -6 2 -13 5357.36 123.29 6 -2 13 5482.31 119.95 -5 -1 26 125.45 23.52 -9 0 27 -5.43 20.26 -5 -1 26 98.05 14.53 3 1 -25 1312.49 66.35 -5 -1 26 122.93 15.15 3 1 -25 1298.40 44.34 5 -1 -26 99.09 24.01 -5 1 26 126.24 39.44 3 1 -25 1298.59 41.21 3 -1 -25 1385.47 45.34 5 1 -26 101.30 37.00 9 0 -27 -0.07 17.44 -9 0 27 -9.37 26.61 -3 1 25 1309.81 41.68 3 -1 -25 1343.06 44.50 -3 -1 25 1305.94 34.36 3 1 -25 1305.91 60.59 -3 1 25 1279.96 65.75 -9 0 27 -0.86 20.52 3 1 -25 1267.39 44.87 9 0 -27 0.78 17.40 -3 -1 25 1279.20 43.20 -3 -1 25 1350.91 45.55 5 1 -26 100.86 22.67 -5 1 26 87.20 24.63 5 1 -26 75.22 14.17 5 -1 -26 -9.02 23.09 5 1 -26 110.47 23.52 5 -1 -26 89.07 20.20 9 0 -27 3.27 25.42 5 -1 -26 65.08 21.03 3 -1 -25 1256.40 42.83 2 4 -13 1351.76 48.20 2 4 -13 1309.27 49.53 2 4 -13 1344.34 48.91 -2 4 13 1327.74 70.59 -2 4 13 1414.72 70.81 2 4 -13 1380.63 73.48 4 -1 18 34.71 32.92 4 1 18 5.93 39.19 -4 -1 -18 23.81 19.33 -4 1 -18 15.77 17.43 -4 1 -18 35.59 31.42 -4 1 -18 20.48 39.81 -4 1 -18 17.39 16.61 4 1 18 8.36 29.41 4 -1 18 16.77 22.61 -4 -1 -18 4.27 23.10 13 0 -1 -14.44 26.87 8 0 12 1910.59 56.65 -8 0 -12 1993.83 83.72 -13 0 1 7.83 28.75 8 0 12 1918.35 83.28 13 0 -1 17.54 28.60 -13 0 1 2.74 20.78 -8 0 -12 1858.74 81.30 13 0 -1 -0.44 13.42 -8 0 -12 1848.37 54.15 -9 2 -7 600.08 38.03 -9 -2 -7 641.22 38.02 -9 -2 -7 665.33 38.40 -12 -2 211476.19 179.12 -9 2 -7 737.88 39.40 -9 2 -7 667.14 39.51 9 2 7 634.50 39.05 -12 -2 210869.07 175.44 -12 -2 210785.37 145.30 12 2 -211212.12 178.72 9 2 7 725.36 37.46 9 -2 7 664.65 39.42 -12 2 211535.11 180.38 -12 2 211310.66 208.63 9 -2 7 579.89 36.99 12 -2 -210879.27 160.67 9 -2 7 719.41 60.70 12 2 -211249.20 163.62 -12 2 211213.80 183.43 12 -2 -211524.42 207.87 12 2 -211063.10 159.06 12 -2 -211324.60 206.96 10 -1 7 974.22 45.50 -4 -4 -6 738.73 29.05 -10 1 -7 826.30 44.19 -10 1 -7 876.94 38.57 10 1 7 865.32 68.96 -10 1 -7 894.56 46.13 10 1 7 861.95 34.54 10 -1 7 894.09 36.22 4 -4 6 733.91 45.83 -4 -4 -6 737.43 33.26 10 -1 7 947.22 69.65 4 4 6 772.11 49.66 10 1 7 891.92 44.38 -10 -1 -7 886.94 45.46 -10 -1 -7 949.74 44.57 -4 4 -6 791.27 44.05 4 -4 6 753.18 34.59 -4 4 -6 811.24 43.51 -10 -1 -7 911.32 36.17 -4 4 -6 791.73 34.95 4 4 6 785.33 41.80 -9 0 -10 2108.06 85.16 -9 0 -10 2005.83 57.71 9 0 10 2190.75 84.95 -9 0 -10 2015.86 58.34 6 1 15 3893.73 75.67 6 -1 15 4016.39 80.21 -13 -2 7 307.86 24.38 -13 -2 7 295.87 33.33 6 1 15 4021.34 111.99 13 2 -7 329.58 32.33 13 -2 -7 272.42 58.09 13 2 -7 294.41 38.18 13 2 -7 260.35 58.08 -13 -2 7 275.26 55.45 -6 1 -15 4058.47 72.18 -6 -1 -15 4010.28 82.77 6 -1 15 4017.49 81.77 -13 2 7 338.12 35.92 13 -2 -7 250.62 22.98 -13 2 7 272.84 57.93 -13 2 7 303.02 36.08 -6 -1 -15 4128.34 102.20 13 -2 -7 284.92 55.66 -6 1 -15 4197.23 114.64 14 -1 -7 8646.83 141.07 -14 -1 7 8620.95 152.44 -14 -1 7 8689.30 167.20 -14 1 7 8598.84 150.53 -14 -1 7 8283.34 125.04 14 1 -7 8730.40 148.11 -14 1 7 8707.40 166.71 14 1 -7 8660.27 169.86 -14 1 7 8737.74 142.33 14 -1 -7 8465.90 163.08 14 1 -7 8787.49 132.87 14 -1 -7 8397.06 129.41 10 -1 -26 38.30 21.17 -10 1 26 79.23 35.01 -10 1 26 59.60 20.69 -10 -1 26 58.64 25.78 10 1 -26 46.40 33.78 10 1 -26 69.52 20.46 10 1 -26 83.71 43.45 -10 1 26 56.90 35.15 -6 0 27 -0.51 21.89 6 0 -27 -4.88 24.38 -11 -3 6 809.77 66.44 11 -3 -6 751.39 42.10 -11 3 6 769.22 67.70 6 0 -27 -1.73 27.74 -11 -3 6 785.15 32.50 11 3 -6 756.95 32.23 11 -3 -6 714.98 36.32 -11 3 6 767.10 36.18 11 3 -6 722.37 66.76 -6 0 27 -1.50 12.86 -11 3 6 723.49 43.20 6 0 -27 23.29 14.82 11 3 -6 727.80 39.71 11 -3 -6 766.37 66.80 -11 -3 6 738.96 26.34 8 -3 5 2662.52 60.04 8 -3 5 2576.66 61.97 -8 3 -5 2643.74 85.93 -8 -3 -5 2688.82 62.28 -8 -3 -5 2692.71 77.75 8 3 5 2668.50 58.43 8 3 5 2683.07 60.98 -8 3 -5 2773.86 95.52 -8 3 -5 2728.28 61.02 0 2 21 10.80 24.53 0 2 21 12.26 24.05 0 -2 21 21.99 21.60 0 2 -21 16.90 21.78 0 2 21 13.33 18.18 0 2 -21 8.99 24.84 0 -2 -21 26.81 12.53 0 -2 -21 20.35 24.48 0 -2 21 8.71 23.12 0 2 -21 19.26 21.91 0 2 -21 18.86 13.09 0 2 -21 13.86 25.63 5 4 4 258.14 34.56 -5 -4 -4 234.82 21.77 -5 4 -4 218.46 22.16 5 4 4 238.46 34.35 -5 4 -4 216.81 50.38 -5 4 -4 214.64 36.84 5 -4 4 181.61 36.72 5 -4 4 165.87 35.81 -5 -4 -4 208.13 22.07 -1 2 -20 46.41 37.53 1 2 20 68.22 27.69 1 -2 20 48.46 16.50 -1 2 -20 22.48 14.86 -1 2 -20 49.26 36.55 1 2 20 56.97 27.20 1 2 20 7.44 22.91 -1 -2 -20 24.30 23.18 -1 2 -20 44.85 26.29 -1 -2 -20 41.60 25.97 1 -2 20 52.50 26.57 -13 1 2 338.32 54.62 13 -1 -2 369.20 57.74 -13 -1 2 384.24 58.28 13 1 -2 388.47 25.38 -13 -1 2 369.26 30.55 13 -1 -2 401.05 32.29 -13 1 2 430.55 36.91 13 1 -2 428.96 37.75 13 -1 -2 400.22 52.15 -13 -1 2 403.72 40.63 13 1 -2 380.22 47.33 10 3 -1 5055.81 94.51 10 -3 -1 5291.82 129.33 -10 -3 1 5302.87 121.93 -10 3 1 5170.22 100.03 10 3 -1 5264.19 122.13 -10 -3 1 5050.74 94.83 10 -3 -1 5088.65 95.18 -10 3 1 5086.19 122.43 10 -3 -1 5051.82 98.50 -10 3 1 5038.04 82.32 -11 -3 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2037.04 83.55 -7 0 -17 -31.79 43.50 2 5 4 2029.82 66.54 -2 5 -4 2059.04 68.08 -7 0 -17 -1.29 27.25 -3 4 -13 4922.04 143.35 14 -1 0 72.49 50.76 -14 -1 0 88.28 57.51 -3 -4 -13 4415.08 124.03 -14 -1 0 89.98 47.13 14 -1 0 75.39 55.95 14 -1 0 86.00 47.56 -14 -1 0 76.48 22.03 -14 1 0 84.50 50.52 -3 4 -13 4449.93 138.98 14 1 0 99.92 21.79 -3 4 -13 4557.62 97.95 -14 1 0 78.35 30.80 3 4 13 4644.55 95.77 -14 1 0 111.12 56.66 14 1 0 43.93 58.77 3 -4 13 4586.97 96.74 -5 -3 -15 797.74 35.09 -5 -3 -15 737.37 74.94 -5 3 -15 829.59 35.76 -5 3 -15 737.95 78.08 -5 3 -15 779.85 51.27 5 3 15 790.49 34.66 5 3 15 827.16 48.31 5 -3 15 706.68 54.62 5 -3 15 819.24 49.43 -10 4 4 346.95 61.01 -3 5 -2 7376.14 130.92 10 4 -4 357.51 60.42 3 5 2 7411.57 109.39 -3 5 -2 7488.45 130.44 3 5 2 7204.66 124.54 -10 4 4 337.72 37.35 3 5 2 7565.48 113.68 10 -4 -4 292.50 60.76 -3 5 -2 7817.26 154.48 -3 5 -2 7534.16 132.17 -3 5 -2 7801.66 131.58 -3 5 -2 7423.91 130.03 -10 -4 4 304.85 37.67 10 -4 -4 348.22 37.66 3 5 2 7372.26 129.58 6 0 -30 5320.76 106.01 -4 -1 -21 494.88 68.39 -4 1 -21 415.15 31.41 4 1 21 396.73 72.82 6 0 -30 5437.89 111.96 -6 0 30 5449.19 93.16 4 -1 21 447.72 38.24 -4 1 -21 384.57 45.46 -4 1 -21 475.45 46.98 -6 0 30 5400.35 90.83 -4 -1 -21 434.40 57.40 6 0 -30 5572.17 108.60 13 -3 -6 38.87 27.65 4 2 -27 1976.46 61.96 -4 -2 27 1916.72 62.21 4 2 -27 1865.28 63.56 13 3 -6 9.22 31.84 13 -3 -6 24.91 50.17 4 2 -27 1867.60 61.26 -4 2 27 2000.63 93.93 -13 3 6 23.32 49.59 -4 2 27 1958.97 64.03 -13 3 6 24.09 27.10 13 -3 -6 30.38 30.69 -13 -3 6 40.57 25.73 -13 -3 6 -4.91 30.07 4 2 -27 1933.51 88.63 -13 3 6 13.90 30.42 13 3 -6 32.80 16.82 -5 2 -18 2050.18 70.02 10 -4 -15 184.71 38.07 -10 4 15 207.40 37.74 10 4 -15 157.48 59.67 5 -2 18 2162.35 99.38 5 2 18 2129.39 70.47 10 4 -15 163.45 38.44 -5 2 -18 2055.92 60.62 -5 -2 -18 2012.50 55.25 -10 4 15 173.73 26.70 -10 4 15 155.77 38.22 -5 2 -18 2145.26 86.71 10 4 -15 143.83 29.56 -5 -2 -18 2058.39 68.93 -5 2 -18 2087.23 76.27 5 2 18 1985.17 53.08 5 -2 18 2096.85 57.70 10 -4 -15 148.83 26.11 9 2 11 184.55 35.43 -9 -2 -11 4.26 32.16 -9 2 -11 136.79 36.00 -9 2 -11 4.37 31.58 9 -2 11 147.85 36.48 -9 -2 -11 167.64 53.60 -9 2 -11 174.67 32.20 9 -2 11 138.54 55.19 9 2 11 -1.19 54.12 -3 -1 28 1206.93 51.83 -3 -1 28 1224.51 54.04 4 5 -1 51.98 33.00 4 5 -1 32.76 31.91 3 -1 -28 1393.22 73.15 3 1 -28 1219.33 74.13 3 1 -28 1205.20 66.27 3 1 -28 1188.49 36.19 -3 1 28 1315.13 73.47 -3 1 28 1295.01 75.96 3 1 -28 1232.79 64.95 -4 5 1 -7.03 28.89 -4 5 1 46.37 28.78 3 1 -28 1244.96 48.45 -4 5 1 -9.17 33.34 -3 -1 28 1239.25 46.28 -2 0 -24 3937.73 82.57 -2 5 8 1863.04 78.15 -6 4 -8 749.59 50.71 -6 4 -8 821.96 52.09 2 0 24 3831.10 81.01 2 5 -8 1952.68 79.85 -2 5 8 1996.89 76.68 2 0 24 3917.78 86.79 6 4 8 831.38 33.89 6 4 8 782.81 39.10 -6 -4 -8 767.20 34.88 2 5 -8 2008.02 79.36 2 5 -8 1990.60 79.09 -2 0 -24 4036.88 112.45 -6 -4 -8 800.37 59.20 6 -4 8 801.42 41.48 -6 4 -8 748.57 41.80 2 5 -8 2010.45 56.87 6 -4 8 759.95 36.34 -14 0 -1 -7.80 21.15 14 0 1 0.88 16.09 14 0 1 6.45 34.24 -14 0 -1 -17.81 26.43 14 0 1 -15.05 36.22 -11 3 23 529.73 70.25 -8 2 -13 0.63 50.66 -8 2 -13 144.56 30.39 11 -3 -23 587.38 48.04 11 3 -23 580.56 70.73 11 3 -23 682.35 46.86 -8 2 -13 134.21 37.40 -8 -2 -13 147.90 48.57 -11 3 23 569.10 46.11 -8 -2 -13 128.88 34.57 8 -2 13 143.23 48.80 8 2 13 138.33 34.43 8 2 13 0.22 29.32 8 -2 13 131.30 34.96 -11 3 23 576.27 46.44 11 3 -23 591.55 46.11 -10 3 -5 2385.20 63.74 -10 -3 -5 2325.87 83.16 10 3 5 2365.49 66.05 10 -3 5 2219.91 66.45 10 -3 5 2343.68 62.61 -10 3 -5 2342.84 73.07 -10 -3 -5 2362.49 66.98 -10 3 -5 2413.68 67.46 10 3 5 2300.75 82.32 1 0 -27 9.83 28.83 -1 0 27 7.54 36.26 -1 0 27 20.09 19.47 1 0 -27 -0.22 18.62 1 0 -27 2.50 21.31 3 5 -8 106.34 26.54 -3 5 8 157.08 28.62 3 5 -8 128.40 42.75 3 5 -8 124.18 45.12 3 5 -8 114.56 45.80 -3 5 8 122.80 44.88 -2 -2 -22 1689.19 94.45 -2 2 -22 1826.57 97.39 -2 -2 -22 1693.08 60.94 -2 2 -22 2298.84 84.83 2 2 22 1704.66 57.74 -2 2 -22 1756.91 45.62 2 2 22 1793.52 95.89 2 -2 22 1766.31 92.76 -2 2 -22 1741.51 56.61 2 -2 22 1686.29 64.40 15 2 -20 3711.88 82.46 16 1 -21 4247.89 84.34 -10 3 24 425.71 25.46 -10 3 24 453.19 43.25 -15 2 20 3847.44 113.48 -15 2 20 3715.08 110.29 -10 3 24 463.95 42.62 -16 1 21 4355.79 110.66 10 3 -24 423.78 70.73 10 3 -24 511.38 43.32 1 2 -25 803.48 48.69 10 3 -24 470.45 42.33 15 -2 -20 3606.21 109.63 -16 1 21 4481.45 99.47 -16 1 21 4267.74 84.48 1 2 -25 901.14 43.98 -16 -1 21 4388.70 86.82 0 5 7 57.00 37.44 0 5 7 109.47 38.30 -15 -2 20 3645.53 84.03 1 2 -25 822.22 49.34 -16 -1 21 4413.91 128.61 10 -3 -24 482.70 40.57 16 1 -21 4391.88 129.94 1 -2 -25 796.98 73.98 15 2 -20 3631.44 84.60 15 2 -20 3714.11 85.30 -15 2 20 3655.09 114.62 0 5 -7 31.28 22.23 1 2 -25 795.25 44.38 15 -2 -20 3692.55 85.09 -1 -2 25 870.21 47.89 0 5 -7 34.52 24.54 0 5 -7 19.80 22.81 16 1 -21 4443.84 88.51 -15 -2 20 3583.53 83.49 16 -1 -21 4357.17 109.12 0 5 -7 65.83 24.97 16 -1 -21 4483.82 100.22 -1 2 25 721.35 77.34 -1 2 25 877.73 75.79 -13 1 28 346.23 45.67 13 1 -28 287.05 27.85 13 1 -28 356.45 45.41 13 -1 -28 277.87 54.40 4 5 -7 554.34 49.26 -4 5 7 559.75 41.15 -4 5 7 641.91 56.25 -4 5 7 554.63 36.44 4 5 -7 504.96 57.89 -13 1 28 350.79 29.41 -13 -1 28 294.88 62.22 13 1 -28 240.69 40.47 -13 1 28 325.91 33.15 4 5 -7 559.38 48.12 4 5 -7 555.04 37.26 -2 3 23 58.43 34.15 -2 -3 23 51.77 54.08 2 3 -23 61.36 53.50 -2 3 23 70.63 34.01 2 3 -23 45.33 31.83 2 3 -23 67.50 54.46 2 3 -23 26.66 52.95 -5 -4 -10 743.52 62.39 -5 -4 -10 587.48 47.86 5 -4 10 693.58 49.66 5 4 10 705.35 31.19 5 4 10 725.62 62.21 -5 4 -10 775.90 50.80 5 -4 10 658.73 65.37 -5 4 -10 727.68 49.28 -5 4 -10 750.31 66.85 14 -2 -3 84.87 41.35 -14 -2 3 81.08 23.20 14 -2 -3 90.68 53.73 14 -2 -3 95.76 55.05 9 1 -30 1036.32 59.28 -9 1 30 904.40 60.81 -14 -2 3 155.19 31.49 -9 1 30 853.75 38.81 14 2 -3 83.12 38.67 -14 2 3 102.44 55.28 -14 2 3 0.29 25.59 9 1 -30 915.22 40.20 -9 1 30 773.60 33.61 14 2 -3 47.53 59.63 9 -1 -30 790.13 53.30 9 1 -30 889.72 70.62 -14 -2 3 61.78 55.78 14 2 -3 93.94 31.75 -14 2 3 125.17 57.55 -13 3 1913190.50 212.41 13 -3 -1912908.59 246.29 -13 -3 1912856.92 245.78 13 3 -1912656.45 241.23 -8 1 30 365.12 32.42 13 3 -1913220.33 213.02 -13 -3 1912506.71 226.81 -13 3 1912745.42 242.86 -8 1 30 412.63 51.34 8 1 -30 374.17 31.29 13 3 -1912964.65 205.40 13 -3 -1912599.02 196.41 8 -1 -30 291.56 26.72 8 1 -30 312.79 57.20 8 1 -30 398.88 48.71 -13 3 1912795.14 198.06 -1 5 -6 3850.17 96.19 -1 5 -6 3825.87 98.33 1 5 6 3875.18 92.09 1 5 6 3875.19 74.05 -1 5 -6 4012.86 109.50 -1 5 -6 3857.83 82.69 -7 4 -6 429.03 49.69 -7 -4 -6 390.30 31.03 -7 -4 -6 393.30 47.65 7 -4 6 425.45 31.79 7 -4 6 390.90 51.77 7 4 6 510.87 49.15 7 4 6 411.87 30.90 -7 4 -6 374.80 68.18 -7 4 -6 408.44 33.04 -16 0 23 3.96 30.44 -16 0 23 6.23 30.44 -3 3 -18 119.94 36.69 -3 3 -18 110.69 59.56 -3 3 -18 41.62 32.64 -3 -3 -18 127.51 35.21 3 -3 18 123.59 21.65 3 -3 18 93.71 36.62 -16 0 23 1.07 31.58 -3 3 -18 112.77 34.41 16 0 -23 -13.54 58.08 16 0 -23 54.58 19.49 -16 0 23 30.93 17.50 3 3 18 157.60 36.87 16 0 -23 45.12 20.59 16 0 -23 38.49 19.51 7 3 -25 720.07 49.48 -7 3 25 680.53 75.54 7 3 -25 747.28 76.76 -7 3 25 596.60 75.51 7 3 -25 749.39 49.56 1 5 -8 3411.11 100.87 1 5 -8 3423.90 98.01 -1 5 8 3394.21 72.41 -1 5 8 3260.63 70.60 1 5 -8 3386.44 72.24 1 5 -8 3743.04 102.70 -9 1 -13 979.50 41.45 -12 -3 1 239.40 41.45 -12 3 1 258.75 42.85 9 -1 13 1042.51 80.34 12 3 -1 237.32 41.11 -12 -3 1 301.00 41.77 12 3 -1 342.08 40.80 -9 -1 -13 1023.81 53.94 12 -3 -1 275.43 28.61 -12 3 1 291.93 29.09 -9 1 -13 1019.83 51.96 -9 -1 -13 1038.47 51.70 -12 3 1 263.64 40.58 -9 1 -13 958.48 56.19 -10 -2 -9 1987.17 92.37 10 -2 9 1972.05 66.33 10 2 9 2043.64 92.88 -10 2 -9 2011.67 94.58 -16 -1 9 73.38 36.14 16 1 -9 130.54 26.22 -16 1 9 52.26 49.65 -16 1 9 0.31 24.09 -16 -1 9 77.63 30.79 -15 0 26 712.82 42.78 -15 0 26 683.58 42.63 15 0 -26 645.78 43.37 15 0 -26 664.29 75.03 12 1 -29 100.97 37.74 -12 1 29 32.38 37.20 -12 1 29 36.19 34.93 15 0 -26 636.38 42.28 12 -1 -29 57.02 42.59 -4 5 0 -2.16 38.75 4 5 0 202.83 23.86 4 5 0 217.61 40.02 -4 5 0 208.00 24.01 -4 5 0 245.55 29.36 ; _shelx_hkl_checksum 37691 _shelx_res_file ; TITL 09040412 shelxl.res created by SHELXL-2016/6 at 17:18:47 on 12-Jul-2017 CELL 0.71075 11.94019 3.70050 21.79187 90.000 121.278 90.000 ZERR 2 0.00071 0.00021 0.00127 0.000 0.002 0.000 LATT 1 SYMM -X, +Y, .50-Z SFAC C H O N CL UNIT 32 24 12 4 4 SHEL 99999.000000 0.000000 L.S. 20 FMAP 2 PLAN -20 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -153.0 ACTA SIZE 0.390 0.360 0.210 LIST 4 WGHT 0.044300 0.355700 FVAR 4.54326 CL1 5 0.608688 0.786529 0.404027 11.00000 0.02123 0.01778 = 0.01883 0.00259 0.01512 0.00121 O1 3 0.339209 0.822906 0.375517 11.00000 0.01724 0.03037 = 0.01657 0.00798 0.00858 0.00463 O2 3 0.759994 0.405037 0.544527 11.00000 0.01243 0.02444 = 0.01724 0.00403 0.00790 0.00224 H2 2 0.803867 0.289490 0.587050 11.00000 -1.50000 O3 3 0.922191 0.119868 0.661640 11.00000 0.01491 0.03068 = 0.01845 0.00342 0.00950 0.00484 N1 4 1.131992 -0.073644 0.728582 11.00000 0.01582 0.01889 = 0.01448 0.00004 0.00862 0.00208 H1 2 1.128059 -0.015652 0.767157 11.00000 -1.50000 C1 1 0.415912 0.676534 0.432480 11.00000 0.01498 0.01380 = 0.01341 -0.00046 0.00834 0.00001 C2 1 0.553614 0.627449 0.458063 11.00000 0.01497 0.01386 = 0.01387 0.00024 0.00985 -0.00004 C3 1 0.636393 0.458732 0.521355 11.00000 0.01394 0.01366 = 0.01426 -0.00102 0.00845 -0.00054 C4 1 1.021744 -0.015273 0.663175 11.00000 0.01417 0.01700 = 0.01624 0.00116 0.00827 -0.00052 C5 1 1.028002 -0.111628 0.601683 11.00000 0.01781 0.02073 = 0.01459 0.00042 0.00823 -0.00109 AFIX 43 H5 2 0.953363 -0.080221 0.554948 11.00000 -1.20000 AFIX 0 C6 1 1.141713 -0.249714 0.609904 11.00000 0.02208 0.01888 = 0.01794 -0.00183 0.01306 -0.00150 AFIX 43 H6 2 1.145376 -0.312374 0.568705 11.00000 -1.20000 AFIX 0 C7 1 1.253297 -0.299510 0.679019 11.00000 0.01839 0.01903 = 0.02108 -0.00094 0.01194 0.00231 AFIX 43 H7 2 1.332337 -0.392760 0.684778 11.00000 -1.20000 AFIX 0 C8 1 1.245151 -0.210858 0.737317 11.00000 0.01568 0.01905 = 0.01742 0.00024 0.00782 0.00334 AFIX 43 H8 2 1.318846 -0.245048 0.784277 11.00000 -1.20000 AFIX 0 HKLF 4 REM 09040412 REM R1 = 0.0271 for 2316 Fo > 4sig(Fo) and 0.0278 for all 2401 data REM 124 parameters refined using 0 restraints END WGHT 0.0444 0.3544 REM Instructions for potential hydrogen bonds HTAB O2 O3 EQIV $2 x+1, -y+1, z+1/2 HTAB N1 O1_$2 EQIV $3 -x+2, y, -z+3/2 HTAB N1 O3_$3 EQIV $4 -x+2, -y, -z+1 HTAB C7 Cl1_$4 HTAB C8 O1_$2 REM Highest difference peak 0.489, deepest hole -0.244, 1-sigma level 0.059 Q1 1 0.4913 0.6561 0.4477 11.00000 0.05 0.49 Q2 1 0.3953 0.6041 0.4592 11.00000 0.05 0.47 Q3 1 0.5943 0.5461 0.4902 11.00000 0.05 0.47 Q4 1 1.0272 -0.0623 0.6317 11.00000 0.05 0.44 Q5 1 1.0901 -0.1883 0.6085 11.00000 0.05 0.43 Q6 1 1.2508 -0.2728 0.7075 11.00000 0.05 0.40 Q7 1 0.6905 0.4335 0.5305 11.00000 0.05 0.39 Q8 1 1.2031 -0.2711 0.6461 11.00000 0.05 0.38 Q9 1 1.0843 -0.0505 0.6963 11.00000 0.05 0.37 Q10 1 1.1898 -0.1391 0.7312 11.00000 0.05 0.35 Q11 1 0.9651 0.0592 0.6626 11.00000 0.05 0.32 Q12 1 0.8744 0.1717 0.6276 11.00000 0.05 0.28 Q13 1 0.3830 0.7786 0.4068 11.00000 0.05 0.25 Q14 1 0.6842 0.7852 0.4199 11.00000 0.05 0.20 Q15 1 0.7814 0.5213 0.5311 11.00000 0.05 0.16 Q16 1 0.5507 0.6938 0.3664 11.00000 0.05 0.15 Q17 1 0.9290 -0.1285 0.5694 11.00000 0.05 0.15 Q18 1 0.5779 0.6998 0.4380 11.00000 0.05 0.12 Q19 1 0.7719 -0.1054 0.6014 11.00000 0.05 0.12 Q20 1 0.4683 0.2580 0.3923 11.00000 0.05 0.12 ; _shelx_res_checksum 70922 data_II _audit_creation_method 'SHELXL-2016/6' _chemical_name_systematic 'Bis(3-hyroxypyridinium) 2,5-dichloro-3,6-dioxocyclohexa-1,4-diene-1,4-diolate' _chemical_name_common 'bis(3-hyroxypyridinium) chloranilate' _chemical_formula_moiety '2(C5 H6 N O 1+) , C6 Cl2 O4 2-' _chemical_formula_sum 'C16 H12 Cl2 N2 O6' _chemical_formula_iupac '2C5 H6 N O + , C6 Cl2 O4 2-' _chemical_formula_weight 399.19 _chemical_melting_point ? _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. ; _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3659(6) _cell_length_b 8.5492(6) _cell_length_c 11.7087(8) _cell_angle_alpha 90.0000 _cell_angle_beta 106.968(3) _cell_angle_gamma 90.0000 _cell_volume 800.98(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 13386 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 30.03 _cell_measurement_temperature 120.0(10) _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.210 _exptl_crystal_size_mid 0.200 _exptl_crystal_size_min 0.120 _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408.00 _exptl_absorpt_coefficient_mu 0.445 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; (NUMABS; Higashi, 1999) ; _shelx_estimated_absorpt_T_min 0.912 _shelx_estimated_absorpt_T_max 0.949 _exptl_absorpt_correction_T_min 0.903 _exptl_absorpt_correction_T_max 0.948 _diffrn_ambient_temperature 120(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPIDII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 15315 _diffrn_reflns_av_R_equivalents 0.0168 _diffrn_reflns_theta_min 2.998 _diffrn_reflns_theta_max 29.983 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? _reflns_number_total 2329 _reflns_number_gt 2166 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0294 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.0751 _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_restrained_S_all 1.072 _refine_ls_number_reflns 2329 _refine_ls_number_parameters 124 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.3570P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.517 _refine_diff_density_min -0.195 _refine_ls_extinction_method none _refine_ls_extinction_coef . 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' 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; RAPID-AUTO (Rigaku, 2006) ; _computing_cell_refinement ; RAPID-AUTO (Rigaku, 2006) ; _computing_data_reduction ; RAPID-AUTO (Rigaku, 2006) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2016 (Sheldrick, 2015) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; CrystalStructure (Rigaku, 2010) and PLATON (Spek, 2009) ; loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl Cl1 0.93157(3) 0.73912(3) 0.68834(2) 0.01680(8) Uani d 1 . . O O1 1.24731(9) 0.58136(9) 0.69329(7) 0.01740(16) Uani d 1 . . O O2 0.68396(9) 0.61601(9) 0.46095(7) 0.01689(16) Uani d 1 . . O O3 0.41012(10) 0.51422(9) 0.30475(7) 0.01640(16) Uani d 1 . . H H3 0.509(2) 0.5340(19) 0.3482(15) 0.025 Uiso d 1 . . N N1 0.48820(11) 0.71217(11) 0.05541(8) 0.01529(17) Uani d 1 . . H H1 0.566(2) 0.7718(19) 0.0393(15) 0.023 Uiso d 1 . . C C1 1.13017(12) 0.54789(11) 0.60534(9) 0.01283(18) Uani d 1 . . C C2 0.96428(12) 0.60823(12) 0.58348(9) 0.01358(18) Uani d 1 . . C C3 0.83396(12) 0.56708(12) 0.48551(9) 0.01327(18) Uani d 1 . . C C4 0.51167(12) 0.66180(12) 0.16734(9) 0.01383(18) Uani d 1 . . H H4 0.609229 0.691448 0.228545 0.017 Uiso calc 1 . . C C5 0.39288(12) 0.56593(11) 0.19388(9) 0.01309(18) Uani d 1 . . C C6 0.25163(13) 0.52430(13) 0.10152(10) 0.0171(2) Uani d 1 . . H H6 0.169400 0.457667 0.116909 0.021 Uiso calc 1 . . C C7 0.23181(14) 0.58069(13) -0.01295(10) 0.0192(2) Uani d 1 . . H H7 0.135178 0.553857 -0.075971 0.023 Uiso calc 1 . . C C8 0.35290(14) 0.67593(13) -0.03506(9) 0.0180(2) Uani d 1 . . H H8 0.340534 0.715121 -0.113094 0.022 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl1 0.01596(13) 0.01889(13) 0.01530(13) 0.00248(8) 0.00420(9) -0.00478(8) O1 0.0143(3) 0.0210(4) 0.0144(3) 0.0017(3) 0.0004(3) -0.0030(3) O2 0.0118(3) 0.0224(4) 0.0151(3) 0.0047(3) 0.0018(3) -0.0023(3) O3 0.0141(3) 0.0203(4) 0.0142(3) -0.0010(3) 0.0032(3) 0.0034(3) N1 0.0148(4) 0.0160(4) 0.0155(4) -0.0020(3) 0.0050(3) 0.0005(3) C1 0.0129(4) 0.0133(4) 0.0121(4) 0.0010(3) 0.0034(3) 0.0006(3) C2 0.0134(4) 0.0151(4) 0.0122(4) 0.0021(3) 0.0036(3) -0.0021(3) C3 0.0132(4) 0.0144(4) 0.0120(4) 0.0016(3) 0.0034(3) 0.0006(3) C4 0.0122(4) 0.0142(4) 0.0142(4) -0.0007(3) 0.0025(3) 0.0001(3) C5 0.0121(4) 0.0127(4) 0.0144(4) 0.0010(3) 0.0037(3) 0.0001(3) C6 0.0129(4) 0.0180(5) 0.0194(5) -0.0033(3) 0.0031(4) 0.0000(4) C7 0.0167(5) 0.0209(5) 0.0169(5) -0.0031(4) -0.0001(4) -0.0019(4) C8 0.0198(5) 0.0199(5) 0.0132(4) -0.0014(4) 0.0031(4) -0.0005(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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 C2 . 1.7409(10) ? O1 C1 . 1.2302(12) ? O2 C3 . 1.2735(12) ? O3 C5 . 1.3387(12) ? O3 H3 . 0.850(18) ? N1 C4 . 1.3384(13) ? N1 C8 . 1.3414(14) ? N1 H1 . 0.891(17) ? C1 C2 . 1.4319(13) ? C1 C3 3_766 1.5409(14) ? C2 C3 . 1.3778(13) ? C4 C5 . 1.3915(13) ? C4 H4 . 0.9500 ? C5 C6 . 1.3952(14) ? C6 C7 . 1.3880(15) ? C6 H6 . 0.9500 ? C7 C8 . 1.3818(15) ? C7 H7 . 0.9500 ? C8 H8 . 0.9500 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C5 O3 H3 . . 109.0(11) ? C4 N1 C8 . . 123.22(9) ? C4 N1 H1 . . 119.0(11) ? C8 N1 H1 . . 117.8(11) ? O1 C1 C2 . . 124.03(9) ? O1 C1 C3 . 3_766 117.27(8) ? C2 C1 C3 . 3_766 118.70(8) ? C3 C2 C1 . . 123.17(9) ? C3 C2 Cl1 . . 120.15(7) ? C1 C2 Cl1 . . 116.69(7) ? O2 C3 C2 . . 126.33(9) ? O2 C3 C1 . 3_766 115.54(8) ? C2 C3 C1 . 3_766 118.13(8) ? N1 C4 C5 . . 119.86(9) ? N1 C4 H4 . . 120.1 ? C5 C4 H4 . . 120.1 ? O3 C5 C4 . . 121.95(9) ? O3 C5 C6 . . 119.64(9) ? C4 C5 C6 . . 118.41(9) ? C7 C6 C5 . . 119.69(9) ? C7 C6 H6 . . 120.2 ? C5 C6 H6 . . 120.2 ? C8 C7 C6 . . 119.88(9) ? C8 C7 H7 . . 120.1 ? C6 C7 H7 . . 120.1 ? N1 C8 C7 . . 118.94(9) ? N1 C8 H8 . . 120.5 ? C7 C8 H8 . . 120.5 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1 C1 C2 C3 . . . . -178.76(10) ? C3 C1 C2 C3 3_766 . . . 0.78(16) ? O1 C1 C2 Cl1 . . . . 1.08(14) ? C3 C1 C2 Cl1 3_766 . . . -179.38(7) ? C1 C2 C3 O2 . . . . 179.87(10) ? Cl1 C2 C3 O2 . . . . 0.03(15) ? C1 C2 C3 C1 . . . 3_766 -0.78(16) ? Cl1 C2 C3 C1 . . . 3_766 179.39(7) ? C8 N1 C4 C5 . . . . 0.55(16) ? N1 C4 C5 O3 . . . . -179.23(9) ? N1 C4 C5 C6 . . . . 0.30(15) ? O3 C5 C6 C7 . . . . 178.57(10) ? C4 C5 C6 C7 . . . . -0.97(15) ? C5 C6 C7 C8 . . . . 0.83(17) ? C4 N1 C8 C7 . . . . -0.70(16) ? C6 C7 C8 N1 . . . . -0.01(17) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O3 H3 O2 . 0.852(17) 1.803(17) 2.6277(12) 162.5(16) y O3 H3 O1 3_766 0.852(17) 2.438(17) 2.9738(12) 121.6(14) y N1 H1 O2 4_575 0.889(17) 1.807(17) 2.6684(12) 162.6(16) y C8 H8 O1 1_454 0.95 2.45 3.1481(13) 130 y _shelx_hkl_file ; 0 -1 1 4926.31 39.81 0 -1 1 4812.15 40.50 0 1 1 4818.37 40.97 0 -1 -1 4794.31 42.67 0 -1 -1 4706.88 40.21 0 1 -1 4802.48 40.78 0 1 1 4786.14 43.09 0 1 -1 4732.36 39.24 1 -1 0 30.90 6.84 1 1 0 26.12 6.27 -1 1 0 24.14 7.38 -1 -1 0 17.87 6.77 1 1 0 28.36 4.66 -1 0 -1 6.00 3.65 1 0 1 2.76 3.02 -1 0 -1 3.64 2.78 1 0 1 5.46 3.38 -1 -1 1 8724.13 79.21 -1 1 1 8746.19 75.30 1 -1 -1 8634.86 78.57 1 1 -1 8606.77 74.53 1 -1 -1 8536.29 75.70 -1 -1 1 8861.71 80.25 1 1 -1 8872.44 80.55 0 0 -2 951.91 9.17 0 0 2 944.62 11.21 0 0 2 973.76 9.12 0 0 -2 961.82 10.94 1 0 -2 1.45 3.67 -1 0 2 2965.38 28.36 -1 -1 -1 5975.12 61.42 1 -1 1 6015.84 56.37 1 -1 1 6193.20 50.48 1 1 1 5901.61 60.14 -1 -1 -1 5852.91 54.69 1 1 1 6004.39 56.76 -1 1 -1 5913.90 55.87 0 -1 244390.19 463.34 0 1 -245572.85 479.55 0 -1 -244845.40 474.77 0 1 244841.47 479.97 0 1 244468.54 469.47 0 -1 245267.76 476.10 0 -1 -244441.90 470.94 0 1 -245063.45 470.71 -1 -1 2 3119.60 31.22 1 1 -2 3314.39 38.50 -1 -1 2 3252.19 28.11 -1 1 2 3096.65 28.92 1 -1 -2 3170.02 27.24 -1 1 2 3124.55 28.69 1 -1 -2 3120.40 31.93 0 -2 0 2825.68 28.48 0 -2 0 2830.63 25.11 0 2 0 2853.44 33.41 2 0 -1 22.77 5.08 -2 0 1 2.21 3.98 2 0 -1 0.85 4.27 -2 0 1 -1.03 3.53 1 0 211807.16 116.09 -1 0 -211776.19 112.16 1 0 211746.58 112.27 -1 0 -211730.49 114.87 -2 0 0 1229.32 17.00 -2 0 0 1228.98 15.41 2 0 0 1260.59 16.33 2 0 0 1241.95 22.84 0 2 1 78.10 8.13 0 2 -1 68.64 8.77 0 -2 1 77.48 5.57 0 -2 -1 65.66 4.70 0 -2 1 68.86 5.98 0 2 1 74.83 9.64 0 -2 -1 83.52 6.10 0 2 -1 82.79 6.00 -1 0 3 9.39 7.24 -1 0 3 3.03 1.05 1 0 -3 1.94 0.94 1 0 -3 7.53 4.08 2 0 -229862.19 298.80 2 0 -229881.70 307.54 -2 0 229926.71 308.40 -2 0 229828.14 298.86 -1 -2 0 3350.77 34.40 1 2 0 3319.89 33.54 1 -2 0 3308.78 38.35 -1 -2 0 3310.41 33.82 -1 2 0 3330.70 33.21 1 2 0 3306.18 34.13 2 -1 -115622.60 145.55 2 1 -115343.14 151.98 -2 -1 114950.38 155.48 -2 -1 114857.65 142.42 -2 1 115396.61 146.69 -2 1 115342.16 148.43 2 -1 -115184.02 147.63 2 1 -115387.44 152.12 0 0 -3 5.64 2.84 0 0 3 2.58 7.24 0 0 -3 5.19 4.28 -1 -2 188306.22 1035.68 0 0 3 4.01 2.75 -1 2 189248.42 1022.66 1 2 -189489.26 1062.59 1 -2 -189114.80 1049.51 1 -2 -189895.37 1030.96 -1 -2 188018.16 1036.19 1 2 -188890.65 1045.71 -1 2 187731.76 1032.10 1 1 2 6230.58 60.73 1 -1 2 6171.14 59.92 1 1 2 6296.84 60.56 1 -1 2 6428.22 59.83 -1 -1 -2 6258.19 60.53 -1 1 -2 6095.92 64.30 -1 1 -2 6277.25 58.02 -1 -1 -2 6321.36 61.31 -2 1 020689.74 196.08 -2 -1 020843.23 214.35 2 -1 021042.22 218.29 -2 -1 020609.28 207.98 -2 1 020891.45 216.03 2 1 020862.39 218.20 2 1 021019.61 216.68 2 -1 021319.45 206.23 -1 1 3 1705.82 17.36 -1 -1 3 1689.31 21.11 -1 1 3 1669.58 23.73 -1 -1 3 1699.24 15.14 1 -1 -3 1654.56 18.83 1 -1 -3 1647.42 17.05 1 1 -3 1657.18 20.54 -2 -1 2 8730.82 86.37 -2 1 2 8784.84 86.55 2 -1 -2 8508.12 78.52 2 -1 -2 8686.43 85.16 -2 -1 2 8874.03 80.26 -2 1 2 8810.51 81.40 2 1 -2 8702.45 80.89 2 1 -2 8540.47 90.77 -2 0 -1 -2.05 4.97 2 0 1 2.95 5.49 2 0 1 8.14 4.67 -2 0 -1 4.35 4.00 1 -2 1 251.22 3.68 -1 -2 -1 235.00 8.66 1 -2 1 241.85 7.82 1 2 1 253.23 13.99 -1 -2 -1 244.87 8.29 1 -2 1 245.54 3.26 1 2 1 255.03 8.51 1 -2 1 265.06 9.04 0 1 -3 1803.92 21.26 0 1 3 1829.00 26.65 0 -1 3 1862.16 21.19 0 -1 -3 1846.49 18.87 0 -1 -3 1838.24 25.83 0 1 -3 1860.54 19.63 0 -1 3 1843.74 19.53 0 1 3 1858.43 22.30 0 -2 -2 1050.93 14.22 0 2 -2 1064.18 12.95 0 -2 2 1014.25 14.84 0 2 2 1096.67 18.84 0 -2 2 1078.05 13.16 0 2 2 1045.00 13.98 0 -2 -2 1030.39 17.96 0 2 -2 1004.87 14.90 -1 2 2 129677. 1610. -1 -2 2 125978. 1579. -1 2 2 128979. 1615. -1 -2 2 130001. 1619. 1 2 -2 126819. 1572. 1 2 -2 126170. 1576. 1 -2 -2 126731. 1577. 1 -2 -2 127859. 1578. -2 0 3 5.16 1.54 -2 0 3 1.73 5.22 2 0 -3 -2.22 0.92 2 0 -3 -2.60 4.76 2 -1 1 4357.61 42.55 2 -1 1 4319.55 44.84 2 1 1 4321.39 44.61 -2 1 -1 4233.49 50.32 2 1 1 4279.27 44.23 -2 1 -1 4343.44 41.17 -2 -1 -1 4197.83 49.51 -2 -1 -1 4278.79 49.75 -1 0 -3 8.48 4.43 -1 0 -3 -0.45 7.39 1 0 3 3.43 6.56 1 0 3 -2.75 3.91 -2 -1 3 410.82 11.00 -2 -1 3 420.52 7.35 -2 1 3 387.31 12.26 2 1 -3 391.54 16.67 -2 1 3 396.28 14.12 2 -1 -3 384.38 7.66 2 -1 -3 395.45 6.05 2 2 -112725.36 123.49 -2 2 112900.86 114.56 2 -2 -112515.75 129.62 2 2 -112421.75 124.49 -2 -2 112700.66 127.53 2 -2 -112734.58 123.43 -2 -2 112792.91 124.64 -1 2 -2 6093.63 52.75 1 2 2 5992.42 64.47 -1 2 -2 6088.07 65.64 1 2 2 5989.42 65.82 -1 -2 -2 5952.07 59.34 1 -2 2 5961.99 59.76 -1 -2 -2 6029.25 60.07 1 -2 2 6111.12 53.68 -1 0 4 10.03 1.65 1 0 -4 11.44 1.84 -1 0 4 3.27 8.14 1 0 -4 15.05 5.02 2 -2 047285.32 483.80 2 2 047070.11 516.28 -2 2 046522.05 513.80 -2 -2 046674.83 511.69 2 2 046725.83 524.01 2 -2 046222.22 511.58 -2 -2 047047.87 519.72 -2 0 -2 9056.10 87.59 2 0 2 9074.38 87.64 -2 0 -2 9048.10 90.09 2 0 2 8931.14 89.39 -1 -1 -3 1401.64 18.30 -1 1 -3 1407.71 17.52 1 -1 3 1377.52 15.72 1 -1 3 1430.91 22.72 1 1 3 1405.15 18.63 1 1 3 1398.17 22.48 -1 1 -3 1399.03 15.62 -1 -1 -3 1367.69 17.48 1 2 -344125.74 466.32 -1 -2 344297.09 489.36 -1 2 344850.17 483.89 1 -2 -345157.52 485.84 -1 2 345087.20 483.18 -1 -2 345519.67 481.52 1 2 -343836.09 477.04 1 -2 -344424.08 479.47 -2 -2 2 8110.25 76.40 -2 2 2 8062.53 75.86 2 -2 -2 8056.32 80.31 -2 2 2 8001.19 71.54 2 2 -2 8087.83 75.82 2 -2 -2 8074.55 78.64 -2 -2 2 8176.64 82.14 2 2 -2 8033.03 80.52 0 3 0 2.17 4.04 0 -3 0 -0.47 2.56 0 -3 0 3.75 6.76 0 -2 3 28.04 5.49 0 -2 3 29.85 3.70 0 -2 3 24.76 4.26 0 -2 -3 29.73 8.78 0 -2 3 32.02 4.16 0 -2 -3 25.39 7.99 0 2 3 32.56 4.75 0 2 3 28.22 9.13 0 0 4 2950.48 31.30 0 0 -4 2967.32 27.47 0 0 -4 2947.83 31.20 0 0 4 2932.77 26.98 3 0 -1 2.38 4.84 -3 0 1 -4.66 4.56 -3 0 1 2.08 7.62 3 0 -1 8.07 4.76 -1 1 4 4666.36 41.47 -1 -1 4 4657.90 38.44 1 -1 -4 4529.60 40.86 -1 -1 4 4660.21 37.98 1 -1 -4 4551.14 50.68 -1 -1 4 4540.20 45.30 -1 -1 4 4571.28 47.37 -1 1 4 4447.09 45.21 0 -3 -1 1871.01 27.73 0 3 1 1832.95 22.01 0 -3 1 1836.88 21.76 0 3 1 1848.96 19.54 0 3 -1 1845.01 21.46 0 -3 -1 1849.14 22.58 0 -3 1 1880.77 18.10 0 3 -1 1856.94 20.34 3 0 -246685.52 506.56 3 0 -246668.97 520.24 -3 0 246746.83 506.54 -3 0 246436.73 517.98 2 1 238129.62 420.32 -2 1 -238606.90 418.91 -2 -1 -238666.67 419.22 2 -1 239033.09 409.12 2 1 238878.58 420.39 -2 -1 -238682.90 418.37 -2 1 -239258.53 414.94 2 -1 238790.99 421.24 -2 0 4 41.39 9.60 2 0 -4 41.95 0.99 2 0 -4 45.21 1.04 -2 0 4 45.76 6.89 -2 2 -1 149.76 8.77 -2 -2 -1 161.24 13.57 -2 -2 -1 175.63 13.90 2 2 1 165.32 14.56 2 2 1 177.51 8.31 2 -2 1 173.76 8.69 2 -2 1 162.45 4.35 1 3 015997.83 164.60 1 -3 016242.07 143.31 -1 -3 016163.99 168.05 1 -3 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30.87 14.06 8 4 -11 -0.60 14.38 2 -10 4 2069.21 66.48 -1 3 14 1708.94 43.64 3 -10 -5 44.55 26.12 -3 -10 5 22.96 14.18 -1 -3 14 1743.19 38.24 2 10 4 2015.25 39.51 2 10 4 1950.44 45.79 3 -10 -5 34.51 18.64 -8 4 11 114.96 26.22 -2 -10 -4 2010.94 48.83 -3 -10 5 26.42 11.26 2 -10 4 2143.42 59.10 -8 -4 11 143.70 23.66 -1 -3 14 1632.26 40.76 -2 -10 -4 1995.16 65.05 -8 4 11 90.05 14.28 3 10 -5 55.79 17.97 1 -3 -14 1647.84 40.21 4 10 -3 311.08 28.36 4 10 -3 357.91 33.25 -4 -10 3 321.31 23.24 -4 -10 3 322.69 18.97 4 -10 -3 300.96 22.75 4 -10 -3 282.94 27.10 -7 -8 5 92.85 28.03 7 8 -5 229.23 16.65 7 -8 -5 202.76 28.63 7 8 -5 195.02 23.25 -7 -8 5 177.33 35.74 8 1 6 5.58 18.31 8 -1 6 24.21 12.15 8 1 6 1.24 23.70 -8 1 -6 2.90 17.02 -8 1 -6 25.88 17.14 -8 -1 -6 42.00 27.98 8 -1 6 17.08 18.17 -8 -1 -6 3.69 12.92 -6 -2 -9 311.12 35.08 6 2 9 351.06 24.48 -6 -2 -9 319.49 24.47 6 -2 9 376.05 28.96 -6 2 -9 289.07 23.21 6 -2 9 331.44 39.63 -6 2 -9 320.38 25.44 6 2 9 364.10 40.09 1 -10 5 964.61 34.43 1 -10 5 988.14 44.73 1 10 5 1037.96 32.52 -1 -10 -5 971.17 34.67 1 10 5 1004.91 37.17 -1 -10 -5 995.92 34.35 -10 2 0 -6.52 12.39 10 2 0 -3.44 14.90 -10 -2 0 -1.76 11.91 10 -2 0 15.47 16.27 10 -2 0 12.34 27.01 -10 2 0 -7.12 21.35 -10 -2 0 9.22 13.22 10 2 0 25.28 15.72 0 -2 14 286.73 21.45 0 2 14 320.08 25.03 0 -2 14 285.33 24.02 0 -2 -14 332.52 24.15 -3 -8 10 1478.23 28.45 -3 -8 10 1385.83 25.85 -8 5 10 233.40 16.69 -3 -8 10 1426.90 44.26 8 5 -10 188.54 25.87 -3 8 10 1401.20 40.91 -3 8 10 1391.65 29.68 3 -8 -10 1383.42 28.85 4 10 0 748.16 43.33 -4 -10 0 663.61 24.45 8 -5 -10 211.43 12.69 8 -5 -10 240.04 11.13 -3 -8 10 1426.62 36.53 4 -10 0 734.71 51.38 3 -8 -10 1364.51 40.11 -8 5 10 212.78 14.14 4 -10 0 696.07 29.79 -8 -5 10 242.00 41.09 -4 -10 0 647.77 46.24 4 10 0 597.90 36.55 0 -9 -8 102.76 18.01 5 -8 -9 159.10 14.14 0 -9 8 105.31 23.57 0 -9 -8 99.48 23.25 0 9 8 84.25 17.28 0 -9 8 96.09 26.68 5 8 -9 94.02 17.89 -5 8 9 128.75 12.62 -5 8 9 124.76 11.40 5 8 -9 110.45 18.04 0 9 8 99.20 15.81 -5 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19.96 8 -6 2 36.38 25.16 5 8 5 -15.07 24.25 -5 -8 -5 -6.11 14.14 -8 -6 -2 11.01 16.60 8 6 2 -9.19 16.92 -8 -6 -2 2.36 16.32 8 6 2 25.87 18.50 5 -8 5 -0.44 13.81 5 -8 5 -10.72 15.78 1 -10 -6 3.95 13.72 -1 -10 6 20.77 14.87 -1 -10 6 19.79 21.27 1 -10 -6 23.36 14.85 -1 10 6 9.00 14.48 -1 10 6 15.99 9.68 -6 2 14 1479.97 37.05 -6 -2 14 1462.88 38.40 3 7 9 1143.04 37.09 3 -7 9 1174.10 29.36 -6 2 14 1491.87 41.97 3 7 9 1186.65 32.86 3 -7 9 1172.65 46.45 -6 -2 14 1459.26 61.77 -3 -7 -9 1187.32 35.40 -3 -7 -9 1187.22 34.91 -9 4 -2 1642.05 63.77 -9 -4 -2 1678.97 42.23 9 4 2 1685.10 43.36 9 -4 2 1732.57 45.95 -9 -4 -2 1695.78 44.11 9 4 2 1718.63 44.70 -2 -2 -13 838.31 22.93 2 2 13 871.62 33.28 -2 2 -13 883.53 21.91 2 2 13 877.53 30.74 -2 2 -13 800.63 37.82 -2 -2 -13 908.91 31.81 2 -2 13 881.06 27.82 2 -2 13 909.85 31.21 10 0 1 -17.17 24.58 -10 0 -1 -13.10 26.48 10 0 1 -1.01 11.94 -10 0 -1 13.50 11.75 6 -8 -8 471.12 22.79 0 -7 11 890.96 22.91 0 7 11 884.45 24.71 0 -7 11 951.39 20.34 6 8 -8 521.88 24.79 -10 -1 9 112.64 21.57 -10 1 9 92.61 19.00 0 -7 -11 966.55 29.82 0 7 11 924.73 46.78 6 8 -8 501.55 25.89 -10 1 9 151.11 15.78 -6 -8 8 526.27 19.06 0 -7 11 947.45 23.36 -6 -8 8 566.69 27.71 0 -7 11 924.77 20.94 10 1 -9 114.56 34.32 6 -8 -8 491.00 29.65 0 -7 -11 893.13 26.15 -9 -3 -3 37.99 17.89 9 -3 3 42.63 30.17 -9 3 -3 20.54 12.99 9 3 3 21.70 28.50 -9 3 -3 11.48 18.77 -9 -3 -3 10.61 16.28 9 -3 3 13.36 8.79 9 3 3 20.15 27.67 5 3 10 129.96 35.61 5 -3 10 124.83 22.78 -5 -3 -10 135.73 33.14 5 3 10 127.18 19.14 5 -3 10 125.21 30.81 -5 3 -10 107.95 13.20 -5 3 -10 165.65 18.57 -5 -3 -10 133.63 19.01 -3 -10 -3 175.93 38.01 6 9 -1 98.14 19.44 -2 -10 6 87.67 16.52 -6 -9 1 101.27 20.51 4 -7 8 237.22 21.93 -3 -10 -3 151.80 26.94 6 -9 -1 74.57 22.33 3 10 3 185.79 18.23 3 10 3 142.44 22.23 -6 -9 1 103.72 19.48 6 -9 -1 72.32 30.46 -2 10 6 92.71 17.93 -2 -10 6 97.79 18.00 -6 7 10 1861.09 44.14 3 -10 3 231.68 24.33 -2 -10 6 82.70 11.47 6 9 -1 95.40 18.29 2 10 -6 -4.08 8.20 -4 -7 -8 209.30 35.87 -4 -7 -8 205.74 36.15 6 -7 -10 1872.57 44.67 4 -7 8 219.82 19.67 2 -10 -6 106.49 22.57 3 -10 3 206.07 21.55 -6 7 10 1897.66 32.40 4 7 8 220.34 21.54 6 -7 -10 1897.11 32.66 4 7 8 202.05 39.99 6 7 -10 1907.43 43.63 -9 -2 11 74.54 36.52 -9 2 11 102.42 18.06 -9 -2 11 73.36 18.76 -9 2 11 83.80 24.13 -5 6 12 590.30 23.12 -5 -6 12 607.18 37.19 -7 0 -8 24.59 15.81 7 0 8 22.14 18.09 -5 -6 12 592.07 29.21 -5 6 12 591.63 24.97 7 0 8 36.67 14.93 -7 0 -8 -0.09 12.04 -9 1 -4 1424.39 60.51 -9 1 -4 1323.09 29.38 0 6 12 17.09 10.30 9 -1 4 1390.10 31.18 -9 -1 -4 1461.42 41.55 0 -6 -12 17.03 17.92 0 -6 -12 22.47 15.47 0 -6 12 26.90 9.90 0 -6 12 14.71 17.82 7 -8 0 225.72 22.64 9 1 4 1406.77 36.23 7 8 0 224.89 25.14 9 1 4 1349.69 43.41 0 -6 12 23.49 14.38 9 -1 4 1372.21 43.74 7 8 0 234.28 35.16 -9 -1 -4 1329.77 46.28 0 6 12 28.87 26.62 -7 -8 0 61.69 38.08 0 -6 12 15.65 7.89 -7 -8 0 252.12 24.90 7 -8 0 251.99 40.96 6 -9 -4 6.26 15.00 4 -10 -4 1601.17 60.59 -3 0 15 -19.17 26.29 6 9 -4 -1.41 11.67 6 -9 -4 26.82 21.20 -6 -9 4 -8.69 21.87 -4 -10 4 1617.13 34.58 4 -10 -4 1620.38 54.64 -6 -9 4 -8.14 14.46 4 10 -4 1490.05 35.89 -3 0 15 -20.10 18.95 6 9 -4 8.91 13.99 -4 -10 4 1619.86 38.81 4 10 -4 1593.73 33.58 -7 3 13 151.47 18.21 -7 -3 13 137.52 24.66 -7 -3 13 132.40 20.68 -7 3 13 188.73 21.37 -7 -7 -3 2193.05 52.01 8 7 -6 54.08 18.68 8 -7 -6 0.33 23.19 -7 -7 -3 2255.72 51.18 7 -7 3 2166.95 46.83 8 7 -6 1.72 18.08 -8 -7 6 98.48 14.90 -8 -7 6 93.59 23.10 7 7 3 2220.10 52.26 7 7 3 2167.81 67.59 7 -7 3 2144.27 69.79 -8 3 12 9152.75 133.89 -8 -3 12 8990.46 125.73 -8 3 12 9011.06 125.27 -8 -3 12 9241.79 157.75 -3 -3 -12 635.07 23.21 3 -3 12 661.80 34.41 3 -3 12 712.67 33.79 -3 3 -12 625.97 21.40 -3 -3 -12 659.21 29.95 3 3 12 687.19 47.70 3 3 12 665.33 22.54 -3 3 -12 711.56 32.67 -10 -4 4 457.14 22.72 10 4 -4 460.84 32.68 10 -4 -4 428.46 36.96 -10 4 4 407.17 18.98 10 4 -4 386.00 28.98 10 -4 -4 404.22 20.77 -10 -4 4 472.96 29.46 9 -5 -8 788.30 29.00 -9 -5 8 773.60 20.22 9 5 -8 770.09 26.08 -9 5 8 772.47 26.03 9 -5 -8 733.59 23.05 -9 5 8 780.41 29.37 9 5 -8 768.25 35.37 -9 -5 8 806.22 36.68 -3 4 14 986.59 36.10 10 -1 1 37.19 20.73 -3 -4 14 1042.64 34.31 -3 -4 14 944.41 43.45 -3 4 14 1062.19 49.26 -10 1 -1 6.44 17.65 -10 -1 -1 -10.89 22.24 10 -1 1 30.13 19.56 10 1 1 21.59 15.50 -10 -1 -1 14.09 17.28 -10 1 -1 39.89 17.84 10 1 1 25.14 18.70 -4 -5 -10 738.09 31.77 4 5 10 807.54 40.37 4 -5 10 817.16 34.76 4 5 10 764.09 34.46 4 -5 10 765.51 19.92 4 -5 10 754.11 18.70 4 -5 10 782.08 41.54 -4 -5 -10 768.10 42.99 -9 -6 4 1309.60 47.95 9 6 -4 1196.38 61.13 9 6 -4 1208.74 30.80 9 -6 -4 1220.83 32.03 -9 -6 4 1251.51 41.67 9 -6 -4 1191.56 35.10 -4 -10 -1 1823.93 38.17 4 -10 1 1718.05 47.27 4 10 1 1728.76 42.54 -4 -10 -1 1812.01 45.76 4 -10 1 1709.98 58.74 4 10 1 1749.92 38.08 2 -9 7 -9.35 11.55 2 9 7 5.64 12.59 2 -9 7 -3.76 13.17 -2 -9 -7 14.45 15.57 -2 -9 -7 -2.57 19.97 2 9 7 -0.45 12.72 3 9 6 9.50 23.20 -4 0 15 16.62 27.91 -9 -6 3 1761.82 47.24 -9 -6 3 1724.00 55.70 9 -6 -3 1697.65 58.08 9 6 -3 1682.58 38.37 -4 0 15 4.17 14.74 9 6 -3 1811.49 67.33 3 9 6 8.41 23.44 -3 -9 -6 11.47 27.78 -3 -9 -6 21.26 14.48 3 -9 6 12.23 13.35 9 -6 -3 1674.03 37.81 3 -9 6 -5.41 24.54 5 6 8 968.43 56.49 -7 -1 -8 89.50 20.66 -7 1 -8 84.35 33.21 5 -6 8 1004.41 29.70 5 6 8 961.27 33.23 7 -1 8 111.39 26.40 -8 2 -6 861.30 31.16 -5 -6 -8 1023.34 50.57 7 1 8 97.32 35.15 7 -1 8 118.37 21.75 -8 -2 -6 863.30 52.28 8 -2 6 920.91 36.20 7 1 8 107.74 19.69 -5 -6 -8 971.22 35.29 5 -6 8 928.78 49.34 8 2 6 924.95 53.11 -8 -2 -6 969.96 43.99 -8 2 -6 870.30 34.77 8 2 6 888.49 48.22 8 -2 6 841.57 34.04 7 8 -6 -0.31 8.62 -10 -4 5 322.55 27.35 10 4 -5 253.80 26.14 -10 -4 5 242.77 18.42 10 -4 -5 256.56 26.96 -10 4 5 236.19 11.57 -10 4 5 253.73 13.71 7 -8 -6 2.79 11.55 -7 -8 6 2.83 18.07 -7 -8 6 8.17 25.27 7 -8 -6 8.96 15.45 7 8 -6 -5.26 13.27 10 4 -5 268.42 17.63 10 -4 -5 227.40 32.14 0 -10 6 997.81 30.58 0 -10 6 1114.42 48.73 0 -10 -6 1034.08 33.39 0 -10 -6 1040.75 48.81 -3 -1 15 7.31 15.01 0 10 6 1076.48 32.47 0 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284.20 35.32 2 3 14 262.76 47.06 -1 -4 15 16.42 23.65 2 3 14 309.89 25.58 -1 -4 15 -2.52 27.59 -1 4 15 30.45 19.31 6 -10 0 152.91 37.39 10 -6 -3 453.02 29.24 -2 -3 -14 321.84 27.13 6 10 0 165.54 35.21 10 6 -3 432.45 25.05 -2 -3 -14 311.42 42.42 -6 -10 0 202.21 22.53 10 6 -3 453.30 33.07 -6 -10 0 165.75 42.51 4 -9 7 367.37 24.66 4 -9 7 358.59 28.39 -4 -9 -7 290.77 30.69 4 9 7 313.40 44.87 4 9 7 255.69 41.92 -4 -9 -7 352.13 25.87 5 -4 11 24.13 27.27 -5 -4 -11 38.92 28.21 -5 -4 -11 34.98 20.63 5 4 11 24.03 16.77 -5 4 -11 47.16 11.18 5 -4 11 39.76 12.07 5 4 11 40.31 22.25 -5 4 -11 51.55 17.02 -10 3 11 63.20 23.03 10 3 -11 26.88 21.73 -10 -3 11 69.15 38.25 -10 3 11 28.04 27.41 2 -9 9 154.94 34.50 2 9 9 171.43 23.83 -2 -9 -9 188.41 21.58 -2 -9 -9 217.18 23.53 2 9 9 171.68 34.35 2 -9 9 207.48 18.61 6 -10 -5 379.21 38.41 -6 -10 5 420.43 25.79 -6 -10 5 444.65 26.77 6 -10 -5 486.24 45.63 6 10 -5 374.17 23.03 6 10 -5 396.79 24.72 9 -7 0 122.81 35.12 9 7 0 94.09 36.11 8 -8 1 -3.15 15.92 -2 -6 14 419.14 21.63 9 -7 0 146.43 26.11 8 8 1 -9.74 13.90 8 -8 1 20.46 22.06 -8 -8 -1 8.85 31.36 8 8 1 8.98 25.20 -2 -6 14 393.40 24.71 2 -6 -14 422.14 26.05 -9 -7 0 110.76 40.97 9 7 0 147.76 26.39 -2 6 14 433.46 43.11 -9 -7 0 127.91 24.60 -8 -8 -1 21.73 31.54 -4 0 -13 1.44 10.68 -4 0 -13 -0.37 19.90 4 0 13 -1.66 15.00 4 0 13 -6.00 11.61 4 11 1 28.37 14.99 4 -11 1 26.26 19.64 -4 -11 -1 23.45 14.72 4 11 1 44.12 19.48 4 -11 1 24.35 22.58 -4 -11 -1 37.75 20.84 8 1 8 48.26 21.90 -8 -1 -8 -1.55 31.33 -4 6 14 1140.81 56.01 -1 -6 -13 215.80 18.34 8 -1 8 61.92 15.98 -4 -6 14 1142.38 33.34 -8 1 -8 31.84 12.75 1 6 13 225.63 16.72 -8 1 -8 11.53 19.18 -1 -6 -13 183.21 39.86 1 -6 13 244.53 17.74 -4 6 14 1116.21 34.98 -4 -6 14 1149.67 37.69 8 -1 8 18.44 35.60 8 1 8 49.19 30.92 1 6 13 172.18 43.11 -8 -1 -8 -1.96 14.90 1 -6 13 190.71 15.64 -8 -5 -6 800.39 55.65 -8 5 -6 756.30 37.70 8 5 6 728.01 52.47 8 5 6 671.62 37.23 -8 -5 -6 747.05 35.94 8 -5 6 711.89 37.26 -10 -1 12 854.14 46.57 -10 -1 12 817.73 38.14 -10 1 12 807.41 34.33 -10 1 12 827.78 29.72 0 -11 6 851.93 31.59 0 -11 -6 752.97 32.14 0 -11 -6 860.62 51.52 0 -11 6 892.28 34.63 0 11 6 856.67 25.19 0 11 6 904.22 34.11 -5 -1 -12 312.38 37.99 -5 -1 -12 251.83 21.84 -5 1 -12 261.74 22.02 10 4 2 157.20 25.13 5 -1 12 290.05 23.14 -10 -4 -2 130.14 25.07 -5 1 -12 330.08 20.97 10 4 2 122.18 25.54 5 1 12 231.16 35.30 5 -1 12 311.91 22.99 -10 -4 -2 120.44 24.17 10 -4 2 127.70 26.61 -10 4 -2 140.35 26.62 5 1 12 233.30 41.48 -11 -2 0 372.16 26.33 -11 2 0 381.69 28.08 7 -3 9 1967.89 50.89 7 3 9 1951.47 72.40 -7 -3 -9 1949.00 47.33 -11 -2 0 370.13 29.51 11 2 0 292.50 45.16 7 -3 9 1971.94 37.15 -7 3 -9 1959.47 49.13 -7 3 -9 1861.33 33.96 11 -2 0 460.00 48.47 11 2 0 327.95 43.54 -11 2 0 386.37 30.27 -7 -3 -9 1941.63 48.92 7 3 9 2100.80 68.59 11 -2 0 364.28 28.96 7 9 -7 87.46 13.95 7 -9 -7 1.03 18.86 7 -9 -7 66.04 25.12 -7 -9 7 67.47 16.07 7 9 -7 51.38 32.57 -7 -9 7 71.16 21.62 -11 2 9 0.30 13.70 11 2 -9 12.61 19.12 -11 -2 9 9.60 18.38 -11 2 9 11.54 17.36 1 -10 8 82.22 19.34 -1 -10 -8 58.31 25.54 8 7 -10 1787.58 49.10 1 10 8 88.07 30.88 -1 -10 -8 89.36 33.30 1 -10 8 61.91 27.12 -8 -7 10 1700.99 50.05 8 -7 -10 1677.86 34.65 1 10 8 71.33 18.10 8 -7 -10 1678.92 41.67 4 -10 5 1369.30 56.24 -4 -10 -5 1333.54 37.70 4 -10 5 1321.03 43.77 4 10 5 1302.66 40.82 -4 -10 -5 1326.99 44.70 4 10 5 1310.75 39.40 11 3 -1 46.47 19.09 -1 -7 13 275.57 19.80 -1 7 13 300.18 40.67 -11 -3 1 14.67 19.05 1 -7 -13 305.57 18.05 -11 3 1 32.47 31.53 -1 7 13 311.00 24.91 -11 -3 1 37.42 31.19 11 3 -1 32.14 20.52 1 -7 -13 261.36 36.51 -1 -7 13 254.44 16.70 11 -3 -1 13.95 20.78 4 -1 13 113.43 32.72 -2 -2 16 394.51 31.56 -2 2 16 422.16 48.56 4 1 13 147.71 23.35 -4 -1 -13 134.81 34.40 10 0 4 1391.70 49.97 11 4 -4 1202.52 48.07 11 -4 -4 1220.54 33.04 11 -4 -5 412.66 25.06 -4 1 -13 123.59 29.80 -11 -4 4 1265.89 44.04 -10 0 -4 1269.45 44.47 -2 2 16 443.17 33.73 -11 -4 4 1290.21 36.06 4 1 13 163.95 27.25 11 -4 -4 1200.32 36.73 11 4 -5 373.31 21.94 11 4 -5 396.85 33.34 11 -4 -5 469.47 32.69 -10 0 -4 1297.74 34.18 11 4 -4 1226.48 65.11 -2 -2 16 447.16 42.82 10 0 4 1346.78 46.30 -4 1 -13 168.35 28.11 4 -1 13 107.21 17.75 -11 -4 5 396.63 33.95 -11 -4 5 499.80 36.59 11 3 -8 588.30 51.66 11 -3 -8 549.10 22.07 -11 3 8 554.97 23.90 11 -3 -8 484.53 18.47 -11 -3 8 538.61 34.59 -11 3 8 523.43 20.28 10 -6 -6 81.11 28.60 7 -8 4 589.58 36.57 -7 -8 -4 591.20 37.26 10 -6 -6 55.38 15.43 -10 -6 6 64.44 23.62 -10 -6 6 0.99 23.12 7 -8 4 693.59 32.85 7 8 4 695.69 36.80 7 8 4 631.78 33.37 10 6 -6 76.96 14.39 10 6 -6 31.73 24.94 -7 -8 -4 673.72 53.08 10 -3 3 903.16 60.72 -10 -3 -3 894.15 52.45 10 3 3 907.54 54.96 -8 -6 -5 401.87 30.16 10 3 3 900.17 38.76 -10 3 -3 933.86 60.66 8 6 5 357.99 32.92 -10 -3 -3 891.44 39.16 -8 -6 -5 380.87 32.71 8 -6 5 354.92 28.65 8 6 5 393.05 30.06 8 -6 5 409.54 32.66 -1 0 16 25.32 33.44 -1 0 16 17.68 29.74 -6 -9 -4 80.77 21.18 6 9 4 53.66 22.85 6 -9 4 80.95 21.13 6 -9 4 56.34 23.80 -6 -9 -4 -4.41 39.01 6 9 4 60.80 35.62 -8 -3 14 556.76 31.71 -10 -6 2 1064.76 42.65 -8 -3 14 680.34 37.15 -8 3 14 598.77 46.91 -10 -6 2 1089.97 36.76 10 6 -2 1067.72 51.06 10 6 -2 1034.52 43.73 10 -6 -2 1000.43 38.47 10 -6 -2 1009.59 49.99 -8 3 14 625.33 27.75 -6 0 -11 -2.60 12.70 6 0 11 14.54 15.55 6 0 11 1.99 15.34 -6 0 -11 9.19 13.82 9 -2 6 713.22 23.86 -9 -2 -6 762.49 37.08 9 2 6 632.80 36.29 -9 2 -6 694.51 36.01 9 -2 6 791.87 39.31 -9 -2 -6 727.42 44.65 9 2 6 732.05 33.10 -9 2 -6 709.11 22.00 6 -8 6 23.65 28.93 -6 -8 -6 29.50 28.75 6 8 6 32.92 21.70 -2 10 9 796.18 25.06 -2 10 9 814.35 41.06 6 -8 6 15.35 20.70 6 8 6 30.85 19.55 2 -10 -9 758.93 32.76 -2 -10 9 765.85 25.84 2 -10 -9 827.05 44.12 -6 -8 -6 0.01 18.99 -3 -4 -13 26.44 26.07 -3 -4 -13 -0.57 11.52 -4 -8 12 101.77 30.89 -1 -8 12 370.53 16.72 3 -4 13 3.42 18.09 -4 8 12 93.44 25.71 1 -8 -12 317.20 31.33 4 -8 -12 113.51 23.90 -1 8 12 375.42 19.38 -4 8 12 156.43 29.18 -1 -8 12 344.89 29.11 3 -4 13 17.28 10.78 3 4 13 -37.63 17.88 3 4 13 6.61 28.04 4 -8 -12 109.67 14.10 -1 8 12 366.96 25.54 1 -8 -12 379.37 23.91 1 2 15 21.74 18.77 1 -2 15 16.26 16.00 1 -2 15 -1.84 27.81 -1 -2 -15 17.15 18.31 -10 1 -4 246.44 27.66 10 -5 -9 13.91 18.22 10 5 -9 -0.11 20.94 -10 -5 9 18.73 22.65 10 -1 4 280.66 30.16 -10 5 9 35.88 18.59 -10 1 -4 259.82 30.03 10 -5 -9 15.41 15.43 10 1 4 284.92 31.19 -10 -1 -4 233.72 21.56 -10 -1 -4 221.04 29.44 10 -1 4 259.78 19.74 -10 5 9 10.45 15.86 10 1 4 231.84 23.65 6 -9 -9 39.83 22.99 -6 -9 9 48.25 12.58 6 -9 -9 49.78 16.43 -6 -9 9 7.25 18.61 6 9 -9 38.81 29.34 -5 -2 16 1243.88 39.58 -5 2 16 1183.73 65.72 -5 -2 16 1172.05 44.58 -5 2 16 1295.88 58.50 -11 -4 3 3324.49 67.82 11 -4 -6 897.09 38.37 -11 -4 3 3124.29 60.49 11 -4 -3 2957.26 60.10 11 -4 -6 901.99 30.77 11 4 -3 3015.14 57.01 -11 -4 6 919.31 28.93 3 11 -6 3428.82 63.18 -3 -11 6 3678.61 64.35 11 4 -6 922.20 27.45 11 4 -3 3244.35 91.33 -11 -4 6 955.01 41.39 3 -11 -6 3546.69 66.48 3 -11 -6 3550.86 69.83 11 4 -6 895.78 39.60 3 11 -6 3582.38 61.73 -1 -1 16 531.67 51.22 -1 1 16 443.09 33.82 -1 1 16 491.63 30.01 -1 -1 16 461.63 29.66 -7 -6 -7 823.19 36.81 7 6 7 854.87 37.11 7 6 7 837.34 40.93 -7 -6 -7 831.77 38.65 7 -6 7 899.32 49.79 7 -6 7 807.35 38.54 -8 -8 8 1886.79 36.52 8 -8 -8 1735.66 40.43 -9 -6 10 1442.40 48.66 -8 -8 8 2013.52 73.08 8 8 -8 1708.61 49.10 8 8 -8 1812.97 44.23 8 -8 -8 1731.47 36.13 9 6 -10 1407.18 47.73 -11 0 -1 19.14 18.99 -6 -4 -10 1620.63 43.51 -9 -5 -4 131.14 24.85 11 0 1 8.45 17.39 -6 -4 -10 1614.22 45.45 -9 5 -4 104.03 26.53 11 0 1 -10.19 13.31 9 5 4 112.65 26.42 9 -5 4 96.49 27.35 -6 4 -10 1479.26 59.40 6 -4 10 1737.39 44.69 6 4 10 1711.57 50.18 -9 -5 -4 122.27 26.30 -11 0 -1 -1.34 21.94 6 4 10 1684.76 61.28 9 5 4 127.40 24.95 0 -12 0 977.64 56.21 0 12 0 919.62 36.42 -6 -1 -11 -1.68 16.14 6 -1 11 0.05 28.68 6 1 11 5.23 17.72 -5 -9 10 1770.44 59.00 6 -1 11 34.85 16.21 6 1 11 46.16 18.66 5 -9 -10 1587.90 38.05 -6 1 -11 2.53 13.71 -6 -1 -11 43.76 16.09 5 -9 -10 1622.83 35.39 -11 0 10 706.12 27.77 -11 0 10 758.42 33.67 -6 1 -11 33.98 25.98 -1 -10 9 435.74 36.44 -1 -10 9 441.82 22.51 -1 10 9 427.55 25.02 1 -10 -9 493.60 20.92 1 -10 -9 486.92 26.11 -1 10 9 506.48 34.17 6 -8 -11 294.90 27.94 -6 8 11 293.34 28.09 6 -8 -11 256.54 16.32 -6 -8 11 289.64 27.14 -6 8 11 318.55 16.88 -9 3 13 566.94 37.38 -9 -3 13 670.27 55.82 -9 3 13 460.68 44.29 -9 -3 13 584.33 48.28 4 11 -5 188.01 17.36 -8 4 -7 1098.35 41.37 -4 -11 5 263.09 29.58 4 -11 -5 220.32 23.59 4 -11 -5 189.46 41.93 4 11 -5 167.41 20.20 -4 -11 5 216.19 23.14 -8 -4 -7 1127.83 39.02 -8 -4 -7 1122.09 41.71 8 4 7 1044.50 62.55 8 -4 7 1136.60 62.85 8 4 7 1061.80 59.93 -9 -4 -5 55.83 20.94 9 7 -8 1558.39 40.79 9 -7 -8 1542.71 33.49 9 -4 5 28.83 36.00 9 4 5 29.09 34.50 -9 -7 8 1648.81 73.78 -9 -4 -5 50.38 23.64 -9 4 -5 55.69 37.96 9 -7 -8 1562.92 36.82 9 7 -8 1554.30 48.59 9 4 5 34.15 21.94 -9 -7 8 1709.08 45.41 -3 0 -14 2404.00 43.07 10 5 1 43.96 22.98 10 -5 1 41.69 23.55 -10 -5 -1 17.28 20.63 -10 -5 -1 31.15 32.91 -10 5 -1 23.80 21.26 -3 0 -14 2538.04 67.49 10 5 1 31.87 32.91 3 0 14 2620.53 74.84 3 0 14 2540.08 56.02 6 10 1 118.53 36.64 6 -10 1 109.21 26.66 -6 -10 -1 125.95 34.32 -6 -10 -1 104.40 25.21 6 -10 1 105.89 22.47 6 10 1 116.22 22.12 ; _shelx_hkl_checksum 52700 _shelx_res_file ; TITL 10032318 shelxl.res created by SHELXL-2016/6 at 17:51:52 on 14-Sep-2017 CELL 0.71075 8.36590 8.54923 11.70870 90.000 106.968 90.000 ZERR 2 0.00055 0.00053 0.00073 0.000 0.002 0.000 LATT 1 SYMM -X, .50+Y, .50-Z SFAC C H O N CL UNIT 32 24 12 4 4 SHEL 99999.000000 0.000000 L.S. 20 FMAP 2 PLAN -20 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -153.0 ACTA SIZE 0.210 0.200 0.120 LIST 4 WGHT 0.041100 0.357000 FVAR 2.57294 CL1 5 0.931568 0.739120 0.688345 11.00000 0.01596 0.01889 = 0.01530 -0.00478 0.00420 0.00248 O1 3 1.247310 0.581358 0.693289 11.00000 0.01431 0.02100 = 0.01445 -0.00296 0.00035 0.00171 O2 3 0.683956 0.616007 0.460945 11.00000 0.01181 0.02240 = 0.01511 -0.00235 0.00180 0.00466 O3 3 0.410123 0.514224 0.304745 11.00000 0.01410 0.02032 = 0.01418 0.00338 0.00317 -0.00102 H3 2 0.508684 0.534005 0.348151 11.00000 -1.50000 N1 4 0.488197 0.712165 0.055407 11.00000 0.01477 0.01597 = 0.01553 0.00052 0.00505 -0.00204 H1 2 0.566239 0.771775 0.039275 11.00000 -1.50000 C1 1 1.130172 0.547893 0.605345 11.00000 0.01286 0.01334 = 0.01213 0.00060 0.00343 0.00103 C2 1 0.964281 0.608229 0.583480 11.00000 0.01338 0.01505 = 0.01222 -0.00211 0.00358 0.00208 C3 1 0.833956 0.567080 0.485513 11.00000 0.01321 0.01440 = 0.01203 0.00064 0.00340 0.00159 C4 1 0.511671 0.661803 0.167343 11.00000 0.01221 0.01418 = 0.01425 0.00007 0.00253 -0.00067 AFIX 43 H4 2 0.609229 0.691448 0.228545 11.00000 -1.20000 AFIX 0 C5 1 0.392879 0.565933 0.193880 11.00000 0.01209 0.01271 = 0.01437 0.00008 0.00371 0.00103 C6 1 0.251627 0.524297 0.101521 11.00000 0.01286 0.01798 = 0.01938 0.00003 0.00308 -0.00332 AFIX 43 H6 2 0.169400 0.457667 0.116909 11.00000 -1.20000 AFIX 0 C7 1 0.231810 0.580690 -0.012948 11.00000 0.01668 0.02088 = 0.01686 -0.00187 -0.00009 -0.00306 AFIX 43 H7 2 0.135178 0.553857 -0.075971 11.00000 -1.20000 AFIX 0 C8 1 0.352902 0.675931 -0.035065 11.00000 0.01975 0.01988 = 0.01318 -0.00048 0.00311 -0.00139 AFIX 43 H8 2 0.340534 0.715121 -0.113094 11.00000 -1.20000 AFIX 0 HKLF 4 REM 10032318 REM R1 = 0.0275 for 2166 Fo > 4sig(Fo) and 0.0294 for all 2329 data REM 124 parameters refined using 0 restraints END WGHT 0.0410 0.3586 REM Instructions for potential hydrogen bonds EQIV $1 -x+2, -y+1, -z+1 HTAB O3 O1_$1 HTAB O3 O2 EQIV $2 x, -y+3/2, z-1/2 HTAB N1 O2_$2 HTAB C4 Cl1_$2 EQIV $3 -x+1, y-1/2, -z+1/2 HTAB C7 Cl1_$3 EQIV $4 x-1, y, z-1 HTAB C8 O1_$4 HTAB C8 O3_$2 REM Highest difference peak 0.517, deepest hole -0.195, 1-sigma level 0.060 Q1 1 0.4510 0.6081 0.1801 11.00000 0.05 0.52 Q2 1 1.0454 0.5752 0.5944 11.00000 0.05 0.49 Q3 1 0.8945 0.5864 0.5363 11.00000 0.05 0.47 Q4 1 1.1462 0.4873 0.5586 11.00000 0.05 0.47 Q5 1 0.3208 0.5426 0.1474 11.00000 0.05 0.46 Q6 1 0.3025 0.6226 -0.0244 11.00000 0.05 0.44 Q7 1 0.2481 0.5541 0.0433 11.00000 0.05 0.40 Q8 1 0.4973 0.6726 0.1075 11.00000 0.05 0.35 Q9 1 0.4207 0.6869 0.0114 11.00000 0.05 0.34 Q10 1 0.7537 0.5915 0.4827 11.00000 0.05 0.29 Q11 1 0.3980 0.5433 0.2442 11.00000 0.05 0.28 Q12 1 0.9444 0.6590 0.6270 11.00000 0.05 0.26 Q13 1 1.1840 0.5591 0.6507 11.00000 0.05 0.25 Q14 1 0.8221 0.7570 0.6666 11.00000 0.05 0.25 Q15 1 1.0232 0.7741 0.7026 11.00000 0.05 0.21 Q16 1 1.3155 0.5548 0.6911 11.00000 0.05 0.18 Q17 1 0.9553 0.6980 0.7632 11.00000 0.05 0.18 Q18 1 0.9042 0.8153 0.6379 11.00000 0.05 0.18 Q19 1 0.6714 0.6702 0.5012 11.00000 0.05 0.17 Q20 1 1.2347 0.6409 0.7147 11.00000 0.05 0.17 ; _shelx_res_checksum 60720 data_III _audit_creation_method 'SHELXL-2016/6' _chemical_name_systematic 'Bis(4-hyroxypyridinium) 2,5-dichloro-3,6-dioxocyclohexa-1,4-diene-1,4-diolate' _chemical_name_common 'bis(4-hyroxypyridinium) chloranilate' _chemical_formula_moiety '2(C5 H6 N O 1+), C6 Cl2 O4 2-' _chemical_formula_sum 'C16 H12 Cl2 N2 O6' _chemical_formula_iupac '2C5 H6 N O +, C6 Cl2 O4 2-' _chemical_formula_weight 399.19 _chemical_melting_point ? _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. ; _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.49136(13) _cell_length_b 8.2195(4) _cell_length_c 18.1382(9) _cell_angle_alpha 102.177(3) _cell_angle_beta 93.952(3) _cell_angle_gamma 95.316(4) _cell_volume 793.52(6) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11077 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 30.09 _cell_measurement_temperature 120.0(10) _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.350 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.120 _exptl_crystal_density_diffrn 1.671 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 408.00 _exptl_absorpt_coefficient_mu 0.448 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; (NUMABS; Higashi, 1999) ; _exptl_absorpt_correction_T_min 0.890 _exptl_absorpt_correction_T_max 0.948 _diffrn_ambient_temperature 120(2) _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPIDII' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_reflns_number 12373 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_theta_min 3.021 _diffrn_reflns_theta_max 29.983 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_decay_% ? _reflns_number_total 4597 _reflns_number_gt 4124 _reflns_threshold_expression I>2\s(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0399 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_gt 0.0770 _refine_ls_wR_factor_ref 0.0798 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_number_reflns 4597 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_hydrogen_treatment mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0406P)^2^+0.3136P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.752 _refine_diff_density_min -0.341 _refine_ls_extinction_method none _refine_ls_extinction_coef . 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' 'O' 'O' 0.0106 0.0060 '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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ; RAPID-AUTO (Rigaku, 2006) ; _computing_cell_refinement ; RAPID-AUTO (Rigaku, 2006) ; _computing_data_reduction ; RAPID-AUTO (Rigaku, 2006) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _computing_structure_refinement ; SHELXL2016 (Sheldrick, 2015) ; _computing_molecular_graphics ; ORTEP-3 for Windows (Farrugia, 2012) ; _computing_publication_material ; CrystalStructure (Rigaku, 2010) and PLATON (Spek, 2009) ; loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cl Cl1 0.42856(5) 0.16233(3) -0.07860(2) 0.01668(7) Uani d 1 . . Cl Cl2 1.13911(5) 0.28348(3) 0.52483(2) 0.01730(7) Uani d 1 . . O O1 0.03685(16) -0.10701(11) -0.14946(5) 0.02014(18) Uani d 1 . . O O2 0.33010(15) 0.24516(10) 0.08473(5) 0.01729(17) Uani d 1 . . O O3 1.55337(16) 0.23416(11) 0.62981(5) 0.01865(17) Uani d 1 . . O O4 1.14201(15) 0.00027(10) 0.38854(5) 0.01586(16) Uani d 1 . . O O5 0.18017(16) 0.33437(10) 0.25526(5) 0.01818(17) Uani d 1 . . H H5 0.118(3) 0.263(2) 0.2115(10) 0.027 Uiso d 1 . . O O6 0.74923(17) 0.40347(11) 0.05992(5) 0.02044(18) Uani d 1 . . H H6 0.617(3) 0.350(2) 0.0681(11) 0.031 Uiso d 1 . . N N1 0.76255(18) 0.16991(12) 0.35832(6) 0.01695(19) Uani d 1 . . H H1 0.896(3) 0.128(2) 0.3779(10) 0.025 Uiso d 1 . . N N2 1.04584(18) 0.71260(12) 0.25721(6) 0.01696(19) Uani d 1 . . H H2 1.114(3) 0.777(2) 0.2998(10) 0.025 Uiso d 1 . . C C1 0.02618(19) -0.05358(13) -0.08002(6) 0.01355(19) Uani d 1 . . C C2 0.19204(19) 0.07509(13) -0.03554(6) 0.01332(19) Uani d 1 . . C C3 0.18242(19) 0.13365(13) 0.04220(6) 0.01289(19) Uani d 1 . . C C4 1.52060(19) 0.12916(13) 0.56903(6) 0.01293(19) Uani d 1 . . C C5 1.33437(19) 0.12624(13) 0.51055(6) 0.01346(19) Uani d 1 . . C C6 1.30221(19) 0.00728(13) 0.44252(6) 0.01271(19) Uani d 1 . . C C7 0.6571(2) 0.30150(14) 0.39505(7) 0.0178(2) Uani d 1 . . H H7 0.719110 0.355184 0.445342 0.021 Uiso calc 1 . . C C8 0.4617(2) 0.35945(14) 0.36116(7) 0.0169(2) Uani d 1 . . H H8 0.390102 0.453256 0.387366 0.020 Uiso calc 1 . . C C9 0.3693(2) 0.27801(13) 0.28719(6) 0.0141(2) Uani d 1 . . C C10 0.4863(2) 0.14337(14) 0.24949(6) 0.0169(2) Uani d 1 . . H H10 0.430463 0.088006 0.198898 0.020 Uiso calc 1 . . C C11 0.6819(2) 0.09297(15) 0.28659(7) 0.0180(2) Uani d 1 . . H H11 0.761693 0.002289 0.261273 0.022 Uiso calc 1 . . C C12 0.8247(2) 0.62477(14) 0.25631(6) 0.0169(2) Uani d 1 . . H H12 0.743357 0.635815 0.301370 0.020 Uiso calc 1 . . C C13 0.7170(2) 0.51997(14) 0.19096(6) 0.0152(2) Uani d 1 . . H H13 0.560916 0.459117 0.190415 0.018 Uiso calc 1 . . C C14 0.8392(2) 0.50334(13) 0.12492(6) 0.0145(2) Uani d 1 . . C C15 1.0695(2) 0.59750(15) 0.12741(7) 0.0178(2) Uani d 1 . . H H15 1.155223 0.590054 0.083294 0.021 Uiso calc 1 . . C C16 1.1663(2) 0.69955(15) 0.19462(7) 0.0181(2) Uani d 1 . . H H16 1.321913 0.762460 0.197088 0.022 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cl1 0.01602(12) 0.01837(13) 0.01388(12) -0.00454(9) 0.00310(9) 0.00181(9) Cl2 0.01776(13) 0.01555(12) 0.01668(13) 0.00527(9) -0.00194(9) -0.00109(9) O1 0.0204(4) 0.0252(4) 0.0108(4) -0.0062(3) 0.0022(3) -0.0016(3) O2 0.0165(4) 0.0179(4) 0.0136(4) -0.0054(3) -0.0007(3) -0.0014(3) O3 0.0202(4) 0.0181(4) 0.0140(4) 0.0038(3) -0.0031(3) -0.0038(3) O4 0.0164(4) 0.0164(4) 0.0129(4) 0.0021(3) -0.0034(3) 0.0005(3) O5 0.0183(4) 0.0175(4) 0.0162(4) 0.0037(3) -0.0050(3) -0.0004(3) O6 0.0196(4) 0.0230(4) 0.0135(4) -0.0083(3) 0.0008(3) -0.0029(3) N1 0.0157(4) 0.0177(4) 0.0181(5) 0.0022(3) -0.0003(4) 0.0057(4) N2 0.0177(4) 0.0173(4) 0.0128(4) -0.0016(3) -0.0028(4) -0.0006(3) C1 0.0126(4) 0.0151(5) 0.0117(5) -0.0008(4) 0.0003(4) 0.0014(4) C2 0.0118(4) 0.0151(4) 0.0121(5) -0.0025(4) 0.0018(4) 0.0023(4) C3 0.0120(4) 0.0131(4) 0.0126(5) -0.0004(3) 0.0000(4) 0.0019(4) C4 0.0134(4) 0.0129(4) 0.0116(5) 0.0001(4) 0.0011(4) 0.0012(4) C5 0.0135(4) 0.0128(4) 0.0133(5) 0.0028(4) -0.0001(4) 0.0007(4) C6 0.0122(4) 0.0124(4) 0.0126(5) -0.0005(3) -0.0001(4) 0.0020(4) C7 0.0200(5) 0.0153(5) 0.0162(5) 0.0000(4) -0.0032(4) 0.0016(4) C8 0.0196(5) 0.0141(5) 0.0154(5) 0.0020(4) -0.0011(4) 0.0003(4) C9 0.0144(4) 0.0131(4) 0.0146(5) 0.0000(4) 0.0006(4) 0.0032(4) C10 0.0201(5) 0.0171(5) 0.0125(5) 0.0027(4) 0.0010(4) 0.0012(4) C11 0.0197(5) 0.0180(5) 0.0170(5) 0.0045(4) 0.0043(4) 0.0034(4) C12 0.0170(5) 0.0198(5) 0.0129(5) 0.0010(4) 0.0016(4) 0.0015(4) C13 0.0132(4) 0.0164(5) 0.0147(5) -0.0011(4) 0.0008(4) 0.0019(4) C14 0.0149(5) 0.0137(4) 0.0129(5) -0.0006(4) -0.0006(4) 0.0002(4) C15 0.0156(5) 0.0205(5) 0.0148(5) -0.0039(4) 0.0023(4) 0.0001(4) C16 0.0146(5) 0.0191(5) 0.0181(5) -0.0032(4) -0.0001(4) 0.0010(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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cl1 C2 . 1.7363(11) ? Cl2 C5 . 1.7438(11) ? O1 C1 . 1.2508(13) ? O2 C3 . 1.2532(12) ? O3 C4 . 1.2390(13) ? O4 C6 . 1.2586(13) ? O5 C9 . 1.3223(13) ? O5 H5 . 0.907(18) ? O6 C14 . 1.3208(13) ? O6 H6 . 0.852(19) ? N1 C11 . 1.3456(15) ? N1 C7 . 1.3469(15) ? N1 H1 . 0.918(18) ? N2 C16 . 1.3430(16) ? N2 C12 . 1.3511(15) ? N2 H2 . 0.877(18) ? C1 C2 . 1.3997(14) ? C1 C3 2 1.5410(15) ? C2 C3 . 1.3970(15) ? C4 C5 . 1.4165(14) ? C4 C6 2_856 1.5426(15) ? C5 C6 . 1.3924(15) ? C7 C8 . 1.3722(16) ? C7 H7 . 0.9500 ? C8 C9 . 1.4035(15) ? C8 H8 . 0.9500 ? C9 C10 . 1.4065(16) ? C10 C11 . 1.3703(16) ? C10 H10 . 0.9500 ? C11 H11 . 0.9500 ? C12 C13 . 1.3693(15) ? C12 H12 . 0.9500 ? C13 C14 . 1.4009(16) ? C13 H13 . 0.9500 ? C14 C15 . 1.4126(15) ? C15 C16 . 1.3671(15) ? C15 H15 . 0.9500 ? C16 H16 . 0.9500 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag C9 O5 H5 . . 111.3(11) ? C14 O6 H6 . . 107.1(13) ? C11 N1 C7 . . 120.85(10) ? C11 N1 H1 . . 114.5(11) ? C7 N1 H1 . . 124.6(11) ? C16 N2 C12 . . 121.30(10) ? C16 N2 H2 . . 119.3(12) ? C12 N2 H2 . . 119.4(12) ? O1 C1 C2 . . 123.43(10) ? O1 C1 C3 . 2 117.79(9) ? C2 C1 C3 . 2 118.79(9) ? C3 C2 C1 . . 123.56(10) ? C3 C2 Cl1 . . 118.10(8) ? C1 C2 Cl1 . . 118.31(8) ? O2 C3 C2 . . 125.93(10) ? O2 C3 C1 . 2 116.43(9) ? C2 C3 C1 . 2 117.64(9) ? O3 C4 C5 . . 124.83(10) ? O3 C4 C6 . 2_856 116.58(9) ? C5 C4 C6 . 2_856 118.59(9) ? C6 C5 C4 . . 123.72(10) ? C6 C5 Cl2 . . 118.75(8) ? C4 C5 Cl2 . . 117.52(8) ? O4 C6 C5 . . 126.22(10) ? O4 C6 C4 . 2_856 116.09(9) ? C5 C6 C4 . 2_856 117.69(9) ? N1 C7 C8 . . 121.23(11) ? N1 C7 H7 . . 119.4 ? C8 C7 H7 . . 119.4 ? C7 C8 C9 . . 118.99(11) ? C7 C8 H8 . . 120.5 ? C9 C8 H8 . . 120.5 ? O5 C9 C8 . . 118.46(10) ? O5 C9 C10 . . 122.89(10) ? C8 C9 C10 . . 118.62(10) ? C11 C10 C9 . . 119.23(10) ? C11 C10 H10 . . 120.4 ? C9 C10 H10 . . 120.4 ? N1 C11 C10 . . 121.03(11) ? N1 C11 H11 . . 119.5 ? C10 C11 H11 . . 119.5 ? N2 C12 C13 . . 120.52(11) ? N2 C12 H12 . . 119.7 ? C13 C12 H12 . . 119.7 ? C12 C13 C14 . . 119.37(10) ? C12 C13 H13 . . 120.3 ? C14 C13 H13 . . 120.3 ? O6 C14 C13 . . 123.08(10) ? O6 C14 C15 . . 118.05(10) ? C13 C14 C15 . . 118.87(10) ? C16 C15 C14 . . 118.63(11) ? C16 C15 H15 . . 120.7 ? C14 C15 H15 . . 120.7 ? N2 C16 C15 . . 121.29(10) ? N2 C16 H16 . . 119.4 ? C15 C16 H16 . . 119.4 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag O1 C1 C2 C3 . . . . -179.19(11) ? C3 C1 C2 C3 2 . . . 1.29(18) ? O1 C1 C2 Cl1 . . . . -1.30(16) ? C3 C1 C2 Cl1 2 . . . 179.17(7) ? C1 C2 C3 O2 . . . . 178.00(11) ? Cl1 C2 C3 O2 . . . . 0.11(16) ? C1 C2 C3 C1 . . . 2 -1.27(17) ? Cl1 C2 C3 C1 . . . 2 -179.16(7) ? O3 C4 C5 C6 . . . . 179.64(11) ? C6 C4 C5 C6 2_856 . . . -0.41(17) ? O3 C4 C5 Cl2 . . . . 0.75(16) ? C6 C4 C5 Cl2 2_856 . . . -179.29(7) ? C4 C5 C6 O4 . . . . -179.11(10) ? Cl2 C5 C6 O4 . . . . -0.23(16) ? C4 C5 C6 C4 . . . 2_856 0.40(17) ? Cl2 C5 C6 C4 . . . 2_856 179.28(7) ? C11 N1 C7 C8 . . . . 1.17(18) ? N1 C7 C8 C9 . . . . 0.81(18) ? C7 C8 C9 O5 . . . . 179.64(10) ? C7 C8 C9 C10 . . . . -2.23(17) ? O5 C9 C10 C11 . . . . 179.80(10) ? C8 C9 C10 C11 . . . . 1.75(17) ? C7 N1 C11 C10 . . . . -1.68(17) ? C9 C10 C11 N1 . . . . 0.18(17) ? C16 N2 C12 C13 . . . . -0.23(17) ? N2 C12 C13 C14 . . . . 0.54(17) ? C12 C13 C14 O6 . . . . 179.17(11) ? C12 C13 C14 C15 . . . . -0.92(17) ? O6 C14 C15 C16 . . . . -179.08(11) ? C13 C14 C15 C16 . . . . 1.01(17) ? C12 N2 C16 C15 . . . . 0.33(18) ? C14 C15 C16 N2 . . . . -0.72(18) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag O5 H5 O1 2_555 0.905(17) 1.640(17) 2.5208(13) 163.2(17) y O6 H6 O2 . 0.852(17) 1.800(17) 2.6510(13) 177.3(18) y N1 H1 O4 . 0.919(17) 1.810(17) 2.7000(13) 162.3(16) y N2 H2 O4 1_565 0.876(18) 2.156(17) 2.9603(14) 152.3(15) y N2 H2 O3 2_866 0.876(18) 2.176(17) 2.8384(14) 132.1(14) y C7 H7 Cl2 . 0.95 2.81 3.4540(12) 126 y C12 H12 O3 2_766 0.95 2.32 3.1541(14) 146 y C13 H13 O2 . 0.95 2.49 3.1685(14) 128 y C16 H16 Cl1 2_765 0.95 2.77 3.4427(12) 128 y _shelx_hkl_file ; 0 1 1 6032.64 65.01 0 -1 -1 5968.59 61.13 0 -1 -1 6029.64 62.08 0 1 1 5956.75 61.33 0 1 -216034.38 172.54 0 1 -216050.27 171.24 0 -1 215861.63 168.71 0 -1 215883.32 168.26 0 0 -3 713.98 13.46 0 0 3 734.41 14.86 -1 0 0 148.14 4.94 1 0 0 150.08 5.09 1 0 0 146.71 6.87 -1 0 0 154.75 5.14 0 -1 -226552.87 315.57 0 1 227293.78 326.10 -1 0 1 868.66 9.76 1 0 -1 858.47 11.60 -1 0 1 847.76 11.78 -1 0 1 830.87 9.27 0 1 -3 489.74 10.83 0 -1 3 508.51 7.49 0 1 -3 497.51 8.07 0 1 -3 520.01 7.65 1 0 1 6102.83 62.10 -1 0 -1 5952.62 63.28 -1 0 -1 6155.64 63.62 1 0 1 6085.85 65.09 1 0 -2 -1.00 1.00 -1 0 2 4938.69 46.20 -1 1 0 3935.10 42.90 1 -1 0 3975.65 43.02 1 -1 1 2241.57 32.54 -1 1 -1 2256.54 27.19 1 -1 -1 9024.70 97.60 -1 1 1 9131.22 99.03 1 0 2 246.62 7.70 -1 0 -2 235.53 9.37 1 0 2 229.03 15.37 -1 0 -2 231.22 5.75 0 0 -4 360.00 9.49 0 0 4 369.97 10.06 1 1 -1 1004.11 14.88 -1 -1 1 1018.75 14.44 1 1 -1 997.04 15.80 -1 -1 1 1045.03 16.61 0 -1 -316599.16 201.16 0 1 316266.42 188.41 -1 -1 028630.50 347.25 1 1 027923.44 337.99 -1 -1 028432.99 338.59 1 1 028544.52 344.92 0 1 -4 9485.29 107.62 0 -1 4 9821.00 112.49 0 -1 4 9905.34 105.40 -1 1 -230801.16 383.58 -1 1 -230749.40 379.01 -1 1 -232172.84 358.86 1 -1 229826.70 364.75 1 0 -3 -0.63 0.71 -1 0 354928.71 707.55 -1 -1 2 1260.56 12.91 -1 -1 2 1228.63 19.04 1 1 -2 1225.11 12.84 1 1 -2 1196.32 25.34 1 -1 -2 1505.56 26.49 -1 1 2 1498.49 20.39 0 2 -133189.90 410.30 0 -2 133573.53 418.28 0 -2 133554.33 416.90 0 2 -132774.72 406.61 0 -2 025256.37 306.62 0 2 025857.78 314.85 0 2 026060.99 318.02 1 1 1 615.26 13.32 1 1 1 623.64 12.92 -1 -1 -1 600.57 14.04 -1 -1 -1 630.56 12.77 0 -2 025746.73 312.36 0 -2 2 3116.33 36.04 0 2 -2 3190.42 37.35 0 -2 2 3065.51 35.56 0 2 -2 3078.98 35.55 1 0 3 3375.20 35.42 1 0 3 3391.45 42.69 1 1 -3 123641. 1896. -1 -1 3 126569. 1962. -1 0 -3 3480.16 42.59 -1 0 -3 3380.12 42.80 -1 1 -3 1777.74 35.78 1 -1 3 1843.17 27.83 -1 1 -3 1752.17 25.54 1 -1 3 1868.73 14.12 0 2 1 926.51 19.62 0 -2 -1 981.65 29.07 0 -2 -1 895.74 20.17 0 2 -334318.52 424.03 0 2 -334787.09 431.92 0 -2 334653.94 429.32 0 -2 334777.39 440.32 1 -1 -3 2789.56 40.64 -1 1 3 2957.74 36.42 -1 -1 -217549.88 208.17 1 1 217501.40 205.54 1 1 217562.53 208.15 -1 -1 -217666.67 207.66 1 0 -4 11.56 2.31 -1 0 4 1038.41 16.90 0 -1 -421673.13 273.02 0 1 421991.40 278.54 0 0 515940.72 186.78 0 0 -515704.10 183.49 0 -1 5 5081.26 57.80 0 1 -5 4723.46 53.73 -1 2 -1 213299. 3638. -1 2 -1 213763. 3604. 1 -2 1 209615. 3563. -1 -1 491013.97 1329.49 1 1 -495110.57 1308.64 1 1 -492881.21 1366.39 1 1 -492734.61 1276.01 -1 2 012326.34 156.48 1 -2 012177.81 143.36 0 2 2 759.53 19.45 0 -2 -2 717.52 18.01 0 2 2 751.54 18.79 0 2 -436307.50 460.56 0 2 -436262.97 454.48 0 -2 436092.42 449.67 0 -2 436238.25 453.01 -1 2 -2 198570. 3268. -1 2 -2 196703. 3309. 1 -2 2 193730. 3245. 1 -1 440185.51 525.67 -1 1 -440656.11 533.94 -1 0 -411336.67 135.45 1 0 411513.74 126.04 1 0 411539.85 138.05 -1 2 1 134.05 11.38 1 -2 -1 144.77 18.49 -1 -1 -3 5563.81 66.98 1 1 3 5491.77 77.36 -1 -1 -3 5489.45 67.58 1 1 3 5455.12 65.09 -1 1 4 1841.62 25.90 1 -1 -4 1831.83 33.79 -1 -2 1 232.14 13.69 -1 -2 1 393.94 12.12 1 2 -1 213.80 8.69 1 2 -1 248.20 20.25 -1 2 -332601.89 381.88 1 -2 330999.47 404.17 -1 2 -331964.78 407.25 1 -2 331334.61 366.92 1 2 -256831.78 760.41 -1 -2 259099.61 825.73 1 2 -257366.69 784.25 -1 -2 258570.12 780.97 1 0 -5 1828.01 25.34 -1 0 5 1946.30 22.68 1 2 0 4810.17 64.04 -1 -2 0 4893.50 57.40 1 2 0 4797.43 70.54 -1 -2 0 4897.39 62.01 1 -2 -2 551.65 24.95 -1 2 2 546.75 16.86 -1 -1 552216.98 719.50 -1 -1 553328.02 677.92 0 2 314977.90 182.36 0 -2 -315046.71 183.90 0 2 314946.22 183.68 1 2 -3 173825. 2850. -1 -2 3 177452. 2951. 1 2 -3 167983. 2701. -1 -2 3 177402. 2870. 0 -1 -5 5171.00 64.23 0 1 5 5296.65 76.25 0 -2 5 93.68 7.38 0 2 -5 103.90 8.17 0 2 -5 98.75 12.34 0 -2 5 103.70 11.75 0 2 -5 112.37 12.07 0 1 -6 274.56 16.88 0 -1 6 317.33 11.98 0 0 -639607.07 525.42 0 0 640869.39 545.01 1 2 1 8395.28 107.82 -1 -2 -1 8451.12 99.31 -1 -2 -1 8359.80 102.09 1 2 1 8284.90 110.44 -1 1 -521943.12 272.59 1 -1 522340.61 279.14 1 -2 410935.01 141.07 -1 2 -412058.91 120.37 1 -2 411530.31 116.00 -1 2 -411078.79 135.33 -1 2 -411065.45 132.60 -1 0 -5 177.59 12.58 1 0 5 180.62 14.01 1 0 5 179.02 12.98 1 2 -456067.38 767.85 -1 -2 458487.30 765.19 -1 -2 457416.99 789.71 1 2 -456504.74 738.56 -1 -1 -435238.11 460.33 1 1 435652.85 469.20 -1 -1 -436397.50 468.20 1 1 435942.75 469.45 -1 2 3 12.52 8.70 1 -2 -3 13.45 8.30 -1 1 5 401.22 12.38 1 -1 -5 389.25 19.37 -2 0 1 2329.07 33.92 2 0 -1 2364.11 37.94 -2 0 1 2352.41 30.56 -2 0 1 2317.60 32.52 2 0 0 1912.48 26.07 -2 0 0 1972.51 26.15 -2 0 0 1941.79 24.92 -2 0 0 1979.55 31.12 2 0 0 1965.86 25.10 0 -3 1 7513.42 101.84 0 3 -1 7602.65 100.88 0 3 -1 7637.07 92.38 0 -3 1 7643.34 102.01 0 3 -2 6386.10 76.71 0 -3 2 6459.76 78.03 0 -3 2 6636.00 88.01 0 3 -2 6478.51 77.17 1 2 2 1597.59 27.36 1 2 2 1598.13 26.69 -1 -2 -2 1648.95 27.24 -1 -2 -2 1603.58 28.16 -1 0 615382.69 174.32 1 0 -615076.47 170.41 0 2 4 -5.74 6.96 0 -2 -4 2.89 7.86 0 2 4 5.23 6.57 -1 -1 653385.36 693.08 -1 -1 652722.56 719.71 1 1 -6 -3.58 1.51 -2 0 2 144.91 6.06 -2 0 2 141.22 10.18 -2 0 2 132.91 9.15 -2 1 0 5284.82 69.05 2 -1 0 5135.07 60.17 -2 1 0 5283.06 62.01 0 2 -6 4653.07 61.76 0 2 -6 4446.22 51.29 0 -2 6 4310.59 54.56 0 3 0 531.40 16.69 0 -3 0 526.41 25.58 0 -3 0 482.93 26.42 0 3 0 504.16 25.15 -2 0 -1 149.56 7.12 2 0 1 143.74 11.06 -2 0 -1 147.20 9.40 2 0 1 151.34 15.07 0 3 -3 221.69 10.40 0 3 -3 234.92 10.95 0 -3 3 211.47 10.57 0 -3 3 223.16 10.66 -2 1 1 427.68 11.12 2 -1 -1 428.10 11.10 -2 1 -120452.67 251.91 -2 1 -120833.37 242.54 -2 1 -120411.88 256.40 -1 2 -5 5.76 12.63 1 -2 5 7.01 2.72 -1 2 -5 2.48 6.99 1 2 -5 912.65 12.85 1 2 -5 944.53 19.09 -1 -2 5 887.08 19.08 -1 -2 5 873.99 11.88 0 -1 -6 9842.38 118.76 0 1 610231.44 133.78 0 1 -7 5902.48 69.84 0 -1 7 5996.42 70.87 2 -1 -2 1018.25 16.38 -2 1 2 1112.10 22.86 -2 0 3 2957.71 30.70 -2 0 3 2762.05 37.01 2 0 -3 2717.12 27.92 1 -1 6 5015.17 64.61 -1 1 -6 4947.55 63.37 0 -3 -150694.66 694.03 0 -3 -150175.58 686.92 0 3 149675.20 676.84 0 3 149260.37 672.97 -2 1 -2 7173.85 97.29 -2 1 -2 7158.52 85.52 -2 1 -2 7483.10 79.29 1 -2 -491907.04 1367.40 -1 2 493441.48 1394.86 0 3 -4 5865.90 73.88 -2 0 -2 5979.93 69.96 2 0 2 5752.23 78.43 0 -3 4 5931.36 76.02 -2 0 -2 5933.29 80.95 2 0 2 5763.40 66.82 0 -3 4 5710.72 66.15 0 3 -4 5699.87 66.99 -1 3 -1 9112.31 111.33 1 -3 1 8925.17 108.88 -1 3 -1 8969.79 110.00 -2 -1 135517.87 466.58 -2 -1 135217.22 439.45 2 1 -134629.06 445.99 2 1 -135164.22 444.18 0 0 -725113.53 313.74 0 0 726257.86 329.83 -1 3 -2 202.57 12.70 -1 3 -2 208.32 8.07 1 -3 2 187.97 12.11 1 2 331640.55 408.72 1 2 331739.08 421.45 2 1 -2 6917.54 71.97 1 -3 015119.80 185.59 1 1 566343.49 941.09 -1 -2 -332273.64 417.58 -1 -2 -331711.65 410.42 -1 3 015587.40 185.21 1 1 564902.26 909.42 -1 -1 -564881.75 919.33 -2 -1 2 7236.18 78.53 -1 3 014822.78 182.40 -2 -1 2 6877.64 91.34 2 1 -2 6745.14 80.50 -1 0 -6 3867.21 61.54 1 0 6 4000.54 53.28 1 0 6 3927.09 45.92 2 1 0 7103.34 80.42 -2 -1 0 7571.05 97.31 2 1 0 7141.58 90.77 -2 -1 0 7378.55 83.51 -1 3 -3 1107.08 18.87 1 -3 3 1077.00 29.69 -1 3 -3 1122.02 21.85 1 -3 3 1098.97 15.25 1 -1 -6 238.56 16.25 -1 1 6 265.90 10.32 -2 1 3 3966.10 51.01 2 -1 -3 4408.73 49.65 2 1 -313020.36 164.95 -2 -1 313162.81 159.74 -2 -1 314291.63 151.82 -2 -1 314076.12 151.08 -1 3 1 7121.81 99.73 1 -3 -1 6907.69 85.53 -1 3 1 7233.07 96.90 -2 -1 -186593.45 1265.76 -2 -1 -187150.65 1283.79 2 1 185156.31 1250.89 2 1 185889.15 1262.04 -2 0 4 4418.51 63.65 2 0 -4 2705.31 26.54 -2 0 4 4460.27 47.98 -2 1 -343797.84 585.67 -2 1 -344152.44 596.55 -2 1 -344911.46 560.71 2 -1 3 -0.61 1.22 0 -3 -2 80.22 11.20 0 3 2 71.79 11.16 0 -3 -2 101.76 12.03 0 3 2 63.29 18.99 1 2 -6 8566.18 111.74 -1 -2 6 8387.56 100.10 1 2 -6 8611.71 89.33 0 2 530783.21 399.43 0 -2 -531006.30 402.61 0 3 -5 3166.80 39.09 0 3 -5 3205.37 38.33 0 -3 5 3142.61 38.31 0 -3 5 3242.65 39.31 2 0 3 172.80 17.54 -2 0 -3 121.30 10.74 -2 0 -3 148.09 10.05 2 0 3 141.34 5.90 -1 2 -6 6501.12 81.30 1 -2 6 6694.72 67.24 -1 2 -6 6465.82 86.81 0 2 -720108.38 249.97 0 2 -719909.86 244.76 0 -2 719967.36 237.65 1 1 -7 385.29 6.58 -1 -1 7 448.70 10.81 2 -2 017722.32 223.72 -2 2 018505.36 226.25 1 0 -7 1.90 4.03 -1 0 7 6.00 7.48 -2 2 -1 744.53 25.33 2 -2 1 648.14 15.93 1 3 -214095.24 171.96 -1 -3 214171.83 174.03 1 3 -214113.83 164.82 -1 -3 214585.18 176.22 -1 3 -4 4038.59 44.61 1 -3 4 3857.12 58.33 1 -3 4 3756.40 43.03 -1 3 -4 3877.57 50.58 -1 -3 124776.69 316.01 1 3 -124441.54 309.94 1 3 -124280.39 300.04 -1 -3 125631.25 326.05 -2 2 1 2359.95 33.65 2 -2 -1 2185.76 30.96 -2 -1 421808.79 237.23 -2 -1 422147.11 241.16 -2 -1 420634.90 268.24 2 1 -420453.34 254.89 -1 -3 3 370.08 14.88 1 3 -3 385.35 9.94 -2 2 -220902.06 260.27 1 3 -3 443.31 21.42 2 -2 220381.70 262.05 -1 -3 3 526.87 10.94 -2 -1 -2 2224.72 39.88 2 1 2 2191.96 31.17 -2 -1 -2 2294.09 31.40 2 1 2 2205.61 29.66 1 -3 -2 3901.01 52.40 -1 3 2 2258.05 34.88 -1 2 5 128.65 11.17 1 -2 -5 126.26 10.94 -2 1 452595.72 711.87 2 -1 -451960.21 693.40 -1 -3 041401.84 556.40 1 3 040297.87 537.27 -1 -3 041235.24 546.18 1 3 039917.56 536.83 -1 -2 -4 5834.98 73.80 1 2 4 5701.81 72.63 -1 -2 -4 5717.13 84.31 1 2 4 5683.74 72.15 -1 1 -7 4925.51 63.78 1 -1 7 5184.49 76.93 -2 1 -4 4205.74 42.60 2 -1 4 4143.84 55.34 -2 1 -4 4127.94 53.11 -2 1 -4 4076.05 54.79 0 1 7 4890.81 71.97 0 -1 -7 4706.80 69.00 -2 2 242542.08 566.74 2 -2 -240406.68 532.81 -2 0 5 131.03 10.71 0 -1 8 6005.87 72.16 2 0 -5 42.47 3.80 -2 0 5 119.21 7.02 0 1 -8 5797.19 69.67 1 3 -4 189.29 11.27 1 3 -4 174.45 11.09 -1 -3 4 183.79 6.84 -1 -3 4 184.12 18.84 0 -3 -3 68.40 11.38 0 3 3 55.13 10.91 0 3 3 55.38 11.40 -2 2 -3 1650.23 36.86 -2 2 -3 1708.02 29.70 2 -2 3 1705.65 27.55 -1 -1 -6 120.68 11.79 1 1 6 86.05 11.59 1 1 6 98.51 9.96 0 3 -6 57.13 10.75 0 -3 6 45.17 6.89 0 3 -6 67.47 7.25 0 -3 6 59.89 6.45 -2 0 -419523.12 228.07 2 0 419338.64 229.23 -2 0 -418998.32 239.14 2 0 418896.13 238.23 -1 3 -542519.95 571.48 1 -3 542862.83 544.63 -1 3 -543624.96 548.14 1 -3 542408.48 568.48 -1 0 -739804.85 534.73 1 0 7 202.25 10.61 1 3 110873.02 134.22 -1 -3 -110954.84 149.22 -1 -3 -111250.14 137.32 1 3 110677.15 138.58 0 0 -8 3819.08 49.72 0 0 8 3858.64 58.74 -2 -1 517190.40 222.47 1 2 -7 1636.30 19.53 -1 -2 7 1647.19 26.07 1 -1 -7 515.66 21.40 -1 1 7 569.17 21.07 -2 -1 -3 26.92 7.37 -2 -1 -3 21.46 8.53 2 1 3 14.94 13.37 2 1 3 21.54 6.56 -2 -2 2 2927.57 41.93 1 -3 -3 1000.18 21.99 -1 3 3 1008.48 22.90 2 2 -2 2804.51 31.00 2 2 -2 2816.25 39.32 -2 -2 2 2935.06 36.67 2 2 -1 36.45 14.48 -2 -2 1 35.91 15.36 2 2 -1 32.88 8.92 -2 -2 1 37.98 9.33 -1 2 -715429.85 202.66 -1 2 -715388.62 188.60 1 -2 715797.92 174.76 -2 2 312748.49 154.15 2 -2 -312677.90 160.24 1 3 -522777.72 287.42 -1 -3 522849.30 289.00 -1 -3 523701.45 283.05 1 3 -522995.62 271.87 0 -2 -611701.60 157.37 0 2 611873.45 148.03 2 2 -3 8650.02 116.02 -2 -2 3 8855.61 119.15 -2 -2 3 9327.83 97.48 2 2 -3 8916.05 92.99 2 -1 -5 9388.08 106.28 -2 1 5 9684.53 111.41 -2 -2 0 529.73 18.17 2 2 0 531.94 15.06 -2 -2 0 492.34 16.02 2 2 0 510.45 17.49 0 -2 8 405.55 12.25 0 2 -8 360.74 10.68 0 2 -8 361.72 17.11 0 -2 8 384.59 10.25 -2 2 -4 1418.34 36.76 -2 2 -4 1422.81 34.98 1 1 -8 261.46 10.45 -1 -1 8 276.14 7.27 -1 0 821407.97 265.62 1 0 -820903.82 258.07 2 -1 5 324.90 15.40 -2 1 -5 325.12 15.16 1 3 2 119.03 12.64 -1 -3 -2 124.22 12.98 -1 -3 -2 104.77 11.82 1 3 2 141.39 18.49 -1 -2 -5 9.31 14.79 1 2 5 4.48 8.21 1 2 5 3.65 7.93 2 0 -6 2479.92 26.92 -2 0 6 4126.05 46.19 1 -2 -611156.55 137.80 -1 2 610991.15 144.91 -2 -2 4 225.46 13.07 2 2 -4 211.23 5.18 -2 -2 4 227.53 5.58 2 2 -4 249.41 12.58 0 3 412627.40 160.61 0 3 412484.50 158.23 0 -3 -412409.66 156.67 -1 3 -633746.79 455.65 1 -3 633211.56 434.45 1 -3 633548.98 410.82 -1 3 -634666.60 423.83 -1 3 -633557.01 446.20 -2 -2 -1 787.15 16.66 2 2 1 739.23 25.17 2 2 1 692.88 22.13 -2 -2 -1 776.85 19.24 0 3 -716896.76 199.69 0 3 -715953.00 193.82 0 -3 715859.10 194.25 0 3 -715869.31 197.59 0 -3 716251.42 193.12 -2 0 -5 600.61 18.37 2 0 5 600.48 27.46 2 0 5 592.80 14.82 -2 0 -5 637.29 17.71 -2 -1 625563.91 338.24 1 3 -642473.72 548.73 -1 -3 642772.38 576.92 1 3 -643062.47 590.00 -1 -3 643941.70 565.49 2 -2 -4 1150.98 20.31 -2 2 4 1136.58 29.40 0 -4 2 2635.53 38.01 0 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10 -17 705.49 44.08 0 10 -17 817.08 30.35 -1 -9 -10 836.51 49.32 1 9 10 915.68 53.48 1 9 10 938.24 52.69 -5 -3 20 1878.27 90.59 -3 -7 -12 23.01 27.58 3 7 12 2.51 21.87 3 7 12 16.93 25.02 -7 5 -6 141.50 28.28 -7 3 10 57.78 32.69 -7 -1 12 1071.40 69.69 -7 5 -6 127.68 30.04 -5 9 3 81.92 35.42 -5 9 3 129.66 19.50 5 -4 -17 217.66 17.86 5 -9 -3 63.07 25.98 -4 9 -14 -7.27 23.08 -6 6 -12 296.95 62.77 -6 6 -12 274.67 58.26 -3 -1 24 255.11 31.19 -4 9 -14 -24.41 38.45 3 -11 4 391.35 36.60 -3 11 -4 502.30 43.67 -3 11 -5 555.07 45.37 3 -11 5 456.75 61.61 -2 1 24 463.90 38.50 2 -1 -24 403.81 37.50 -6 8 -4 294.93 38.42 -6 -5 -5 3568.40 107.89 -6 8 -4 427.23 59.26 -5 7 -15 36.88 28.21 6 5 5 2963.96 66.42 -5 7 -15 65.07 30.02 -6 -5 -5 3578.59 75.92 6 5 5 3123.14 63.61 -4 -7 -9 1657.99 57.94 -5 8 8 511.96 54.90 -2 -2 25 148.03 39.41 4 7 9 1400.30 76.31 5 -8 -8 480.98 33.70 4 7 9 1547.98 74.79 -5 8 8 528.13 42.42 6 3 10 72.71 16.14 -6 -3 -10 80.12 43.71 6 3 10 77.09 24.81 4 0 20 830.43 77.51 -4 0 -20 960.02 83.91 -5 -8 3 53.58 53.95 5 8 -3 24.42 41.30 2 -11 11 89.06 26.37 -2 11 -11 126.61 28.71 3 -8 -13 41.25 24.65 -3 8 13 56.71 50.74 -3 8 13 45.95 30.50 3 10 -10 688.13 42.75 -3 -6 22 41.90 22.95 -3 -10 10 665.35 48.25 3 -11 3 248.77 56.30 -3 11 -3 244.63 32.98 -3 11 -3 332.13 42.92 ; _shelx_hkl_checksum 6799 _shelx_res_file ; TITL 10031710 shelxl.res created by SHELXL-2016/6 at 17:26:39 on 11-Jul-2017 CELL 0.71075 5.49136 8.21945 18.13818 102.177 93.952 95.316 ZERR 2 0.00013 0.00039 0.00091 0.003 0.003 0.003 LATT 1 SFAC C H O N CL UNIT 32 24 12 4 4 SHEL 99999.000000 0.000000 L.S. 20 FMAP 2 PLAN -20 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -153.0 ACTA SIZE 0.350 0.250 0.120 LIST 4 WGHT 0.040600 0.313600 FVAR 3.18813 CL1 5 0.428557 0.162328 -0.078602 11.00000 0.01602 0.01837 = 0.01388 0.00181 0.00310 -0.00454 CL2 5 1.139111 0.283479 0.524830 11.00000 0.01776 0.01555 = 0.01668 -0.00109 -0.00194 0.00527 O1 3 0.036849 -0.107014 -0.149462 11.00000 0.02037 0.02520 = 0.01082 -0.00157 0.00221 -0.00623 O2 3 0.330104 0.245162 0.084728 11.00000 0.01650 0.01795 = 0.01358 -0.00139 -0.00066 -0.00539 O3 3 1.553370 0.234157 0.629812 11.00000 0.02020 0.01814 = 0.01402 -0.00380 -0.00306 0.00382 O4 3 1.142007 0.000270 0.388542 11.00000 0.01643 0.01637 = 0.01294 0.00051 -0.00340 0.00207 O5 3 0.180174 0.334373 0.255256 11.00000 0.01833 0.01754 = 0.01624 -0.00038 -0.00502 0.00370 H5 2 0.117898 0.262635 0.211466 11.00000 -1.50000 O6 3 0.749226 0.403474 0.059916 11.00000 0.01959 0.02305 = 0.01346 -0.00293 0.00077 -0.00830 H6 2 0.616546 0.350434 0.068057 11.00000 -1.50000 N1 4 0.762553 0.169915 0.358325 11.00000 0.01566 0.01772 = 0.01806 0.00569 -0.00034 0.00219 H1 2 0.896214 0.128349 0.377917 11.00000 -1.50000 N2 4 1.045837 0.712600 0.257211 11.00000 0.01771 0.01731 = 0.01283 -0.00064 -0.00278 -0.00162 H2 2 1.114240 0.776950 0.299836 11.00000 -1.50000 C1 1 0.026177 -0.053577 -0.080018 11.00000 0.01263 0.01512 = 0.01167 0.00142 0.00031 -0.00082 C2 1 0.192044 0.075087 -0.035541 11.00000 0.01184 0.01505 = 0.01211 0.00233 0.00179 -0.00253 C3 1 0.182420 0.133650 0.042204 11.00000 0.01203 0.01312 = 0.01263 0.00194 -0.00001 -0.00041 C4 1 1.520598 0.129160 0.569026 11.00000 0.01339 0.01290 = 0.01160 0.00122 0.00112 0.00013 C5 1 1.334368 0.126237 0.510553 11.00000 0.01348 0.01278 = 0.01327 0.00074 -0.00010 0.00281 C6 1 1.302207 0.007277 0.442523 11.00000 0.01225 0.01240 = 0.01258 0.00195 -0.00007 -0.00055 C7 1 0.657087 0.301496 0.395045 11.00000 0.02003 0.01534 = 0.01623 0.00165 -0.00320 0.00002 AFIX 43 H7 2 0.719110 0.355184 0.445342 11.00000 -1.20000 AFIX 0 C8 1 0.461722 0.359447 0.361160 11.00000 0.01959 0.01408 = 0.01536 0.00032 -0.00115 0.00200 AFIX 43 H8 2 0.390102 0.453256 0.387366 11.00000 -1.20000 AFIX 0 C9 1 0.369320 0.278012 0.287190 11.00000 0.01441 0.01315 = 0.01456 0.00318 0.00062 -0.00001 C10 1 0.486337 0.143365 0.249493 11.00000 0.02006 0.01713 = 0.01252 0.00120 0.00105 0.00272 AFIX 43 H10 2 0.430463 0.088006 0.198898 11.00000 -1.20000 AFIX 0 C11 1 0.681860 0.092968 0.286591 11.00000 0.01973 0.01798 = 0.01697 0.00339 0.00434 0.00453 AFIX 43 H11 2 0.761693 0.002289 0.261273 11.00000 -1.20000 AFIX 0 C12 1 0.824738 0.624774 0.256310 11.00000 0.01696 0.01975 = 0.01288 0.00154 0.00158 0.00102 AFIX 43 H12 2 0.743357 0.635815 0.301370 11.00000 -1.20000 AFIX 0 C13 1 0.717031 0.519973 0.190963 11.00000 0.01319 0.01645 = 0.01473 0.00189 0.00080 -0.00107 AFIX 43 H13 2 0.560916 0.459117 0.190415 11.00000 -1.20000 AFIX 0 C14 1 0.839230 0.503342 0.124921 11.00000 0.01488 0.01371 = 0.01292 0.00021 -0.00064 -0.00063 C15 1 1.069462 0.597495 0.127411 11.00000 0.01559 0.02049 = 0.01476 0.00012 0.00229 -0.00393 AFIX 43 H15 2 1.155223 0.590054 0.083294 11.00000 -1.20000 AFIX 0 C16 1 1.166322 0.699546 0.194617 11.00000 0.01456 0.01909 = 0.01813 0.00098 -0.00009 -0.00323 AFIX 43 H16 2 1.321913 0.762460 0.197088 11.00000 -1.20000 AFIX 0 HKLF 4 REM 10031710 REM R1 = 0.0304 for 4124 Fo > 4sig(Fo) and 0.0399 for all 4597 data REM 247 parameters refined using 0 restraints END WGHT 0.0406 0.3144 REM Instructions for potential hydrogen bonds EQIV $1 -x, -y, -z HTAB O5 O1_$1 HTAB O5 O2 HTAB O6 O2 HTAB N1 Cl2 HTAB N1 O4 EQIV $3 -x+3, -y+1, -z+1 HTAB N2 O3_$3 EQIV $4 x, y+1, z HTAB N2 O4_$4 HTAB C7 Cl2 EQIV $5 -x+2, -y+1, -z+1 HTAB C7 Cl2_$5 HTAB C8 O3_$5 EQIV $6 -x+1, -y, -z HTAB C10 Cl1_$6 HTAB C12 O3_$5 HTAB C13 O2 EQIV $7 -x+2, -y+1, -z HTAB C15 Cl1_$7 HTAB C16 Cl1_$7 REM Highest difference peak 0.752, deepest hole -0.341, 1-sigma level 0.114 Q1 1 1.3160 0.0593 0.4780 11.00000 0.05 0.75 Q2 1 1.6115 0.0616 0.5587 11.00000 0.05 0.69 Q3 1 -0.0651 -0.0935 -0.0629 11.00000 0.05 0.66 Q4 1 0.0979 0.0122 -0.0606 11.00000 0.05 0.65 Q5 1 1.1162 0.6462 0.1631 11.00000 0.05 0.55 Q6 1 0.1841 0.1158 0.0067 11.00000 0.05 0.50 Q7 1 1.4333 0.1312 0.5385 11.00000 0.05 0.49 Q8 1 0.7723 0.5835 0.2232 11.00000 0.05 0.46 Q9 1 0.5864 0.1137 0.2747 11.00000 0.05 0.46 Q10 1 0.5651 0.3263 0.3820 11.00000 0.05 0.44 Q11 1 0.9621 0.5499 0.1301 11.00000 0.05 0.43 Q12 1 0.7043 0.1296 0.3244 11.00000 0.05 0.42 Q13 1 0.4150 0.3161 0.3267 11.00000 0.05 0.41 Q14 1 1.0790 0.2678 0.4818 11.00000 0.05 0.41 Q15 1 0.7711 0.5166 0.1592 11.00000 0.05 0.40 Q16 1 1.1222 0.6565 0.0683 11.00000 0.05 0.39 Q17 1 1.2006 0.0108 0.4303 11.00000 0.05 0.38 Q18 1 0.7837 0.4599 0.0929 11.00000 0.05 0.37 Q19 1 0.3540 0.2591 0.1324 11.00000 0.05 0.37 Q20 1 0.9396 0.6651 0.2558 11.00000 0.05 0.37 ; _shelx_res_checksum 80037 data_global _journal_date_recd_electronic 2017-09-17 _journal_date_accepted 2017-09-21 _journal_name_full 'Acta Crystallographica, Section E' _journal_year 2017 _journal_volume 73 _journal_issue 10 _journal_page_first 1546 _journal_page_last 1550 _journal_paper_category GO _journal_paper_doi 10.1107/S2056989017013536 _journal_coeditor_code LH5855 _publ_contact_author_name 'Professor Hiroyuki Ishida' _publ_contact_author_address ; Department of Chemistry Faculty of Science Okayama University Okayama 700-8530 Japan ; _publ_contact_author_email ishidah@cc.okayama-u.ac.jp _publ_contact_author_fax ' 81-86-251-7832' _publ_contact_author_phone ' 81-86-251-7832' _publ_section_title ; Crystal structures of three hydrogen-bonded 1:2 compounds of chloranilic acid with 2-pyridone, 3-hydroxypyridine and 4-hyroxypyridine ; loop_ _publ_author_name _publ_author_address 'Gotoh, Kazuma' ; Department of Chemistry Faculty of Science Okayama University Okayama 700-8530 Japan ; 'Ishida, Hiroyuki' ; Department of Chemistry Faculty of Science Okayama University Okayama 700-8530 Japan ; _publ_section_synopsis ; Crystal structures of hydrogen-bonded 1:2 compounds of chloranilic acid with 2-pyridone, 3-hydroxypyridine and 4-hyroxypyridine have been determined at 120 K. In each crystal structure, the acid and base molecules are linked by short O---H...O and N---H...O hydrogen bonds. ;