data_Compound-15 _audit_creation_date 2017-04-25 _audit_creation_method ; Olex2 1.2-alpha (compiled 2016.12.12 svn.r3370 for OlexSys, GUI svn.r5282) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address 'BBRC,Syngene International Ltd, Biocon Park, Bangalore-99, Karnataka, India' _publ_contact_author_email 'Rajappa.Vaidyanathan@bms.com' _publ_contact_author_name 'Rajappa Vaidyanathan' _publ_contact_author_phone '91 80 66334401' loop_ _publ_author_name _publ_author_email _publ_author_address 'Prantik Maity' ; prantik.maity@syngeneintl.com ; ; BBRC,Syngene International Ltd, Biocon Park, Bangalore-99, Karnataka, India ; _publ_requested_journal 'Organic Letters' _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic '7-azainzole zinc acetate dimer' _chemical_formula_moiety 'C22 H24 N4 O8 Zn2' _chemical_formula_sum 'C22 H24 N4 O8 Zn2' _chemical_formula_weight 603.19 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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_IT_number 15 _space_group_name_H-M_alt 'C 1 2/c 1' _space_group_name_Hall '-C 2yc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.8444(9) _cell_length_b 8.1601(4) _cell_length_c 15.9017(8) _cell_angle_alpha 90 _cell_angle_beta 109.063(3) _cell_angle_gamma 90 _cell_volume 2433.8(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used 2478 _cell_measurement_temperature 296 _cell_measurement_theta_max 22.84 _cell_measurement_theta_min 2.71 _shelx_estimated_absorpt_T_max 0.905 _shelx_estimated_absorpt_T_min 0.631 _exptl_absorpt_coefficient_mu 2.026 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.4980 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1004 before and 0.0497 after correction. The Ratio of minimum to maximum transmission is 0.6679. The \l/2 correction factor is 0.00150.' _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear light colourless' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.646 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description plate _exptl_crystal_F_000 1232 _exptl_crystal_preparation 'In N2 filled glove box, 500 mg of 7-azainzole dissolved in 7 mL of toluene in 20 mL vial, followed by 0.5 equiv of Zn(OAc)2. The reaction mixture was heated at 90 C for 4h to get a clear solution which was cooled slowly to give crystalline 7-azainzole zinc acetate dimer (compound-15).' _exptl_crystal_recrystallization_method 'Crystallized directly from reaction mixture in toluene' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_unetI/netI 0.0379 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 8994 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 24.994 _diffrn_reflns_theta_max 24.994 _diffrn_reflns_theta_min 2.172 _diffrn_ambient_temperature 296.15 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'sealed tube' _diffrn_special_details ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1774 _reflns_number_total 2153 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v8.34A (Bruker, 2013)' _computing_data_collection ? _computing_data_reduction 'SAINT v8.34A (Bruker, 2013)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution ? _refine_diff_density_max 1.005 _refine_diff_density_min -0.254 _refine_diff_density_rms 0.071 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 169 _refine_ls_number_reflns 2153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0369 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0969 _refine_ls_wR_factor_ref 0.1018 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C1(H1), C2(H2), C6(H6), C3(H3), C5(H5) 2.b Idealised Me refined as rotating group: C9(H9A,H9B,H9C), C11(H11A,H11B,H11C) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.34491(2) 0.22328(5) 0.53157(2) 0.03733(18) Uani 1 1 d . . . . . O1 O 0.31675(12) 0.4454(3) 0.55189(15) 0.0433(6) Uani 1 1 d . . . . . O2 O 0.20689(12) 0.4380(3) 0.55678(16) 0.0506(6) Uani 1 1 d . . . . . O3 O 0.40745(13) 0.1178(3) 0.64095(16) 0.0563(7) Uani 1 1 d . . . . . N1 N 0.41728(15) 0.2827(3) 0.46913(19) 0.0381(7) Uani 1 1 d . . . . . O4 O 0.30048(13) 0.0944(3) 0.64599(18) 0.0599(7) Uani 1 1 d . . . . . N2 N 0.34253(15) 0.4697(4) 0.36238(18) 0.0443(7) Uani 1 1 d . . . . . C8 C 0.26575(18) 0.5042(4) 0.5705(2) 0.0351(7) Uani 1 1 d . . . . . C7 C 0.40460(17) 0.3913(4) 0.4031(2) 0.0361(7) Uani 1 1 d . . . . . C10 C 0.3640(2) 0.0679(4) 0.6784(2) 0.0443(8) Uani 1 1 d . . . . . C4 C 0.45573(18) 0.4439(4) 0.3639(2) 0.0426(8) Uani 1 1 d . . . . . C1 C 0.48360(19) 0.2193(4) 0.4985(3) 0.0446(9) Uani 1 1 d . . . . . H1 H 0.4944 0.1438 0.5448 0.054 Uiso 1 1 calc R . . . . C2 C 0.5361(2) 0.2610(5) 0.4633(3) 0.0523(10) Uani 1 1 d . . . . . H2 H 0.5806 0.2110 0.4845 0.063 Uiso 1 1 calc R . . . . C6 C 0.3531(2) 0.5720(5) 0.2993(2) 0.0530(9) Uani 1 1 d . . . . . H6 H 0.3185 0.6399 0.2619 0.064 Uiso 1 1 calc R . . . . C3 C 0.52302(19) 0.3765(5) 0.3968(3) 0.0526(10) Uani 1 1 d . . . . . H3 H 0.5589 0.4084 0.3745 0.063 Uiso 1 1 calc R . . . . C5 C 0.4207(2) 0.5601(5) 0.2992(2) 0.0548(10) Uani 1 1 d . . . . . H5 H 0.4407 0.6182 0.2628 0.066 Uiso 1 1 calc R . . . . C9 C 0.2745(2) 0.6713(5) 0.6128(3) 0.0631(11) Uani 1 1 d . . . . . H9A H 0.2853 0.6600 0.6759 0.095 Uiso 1 1 calc GR . . . . H9B H 0.2311 0.7323 0.5886 0.095 Uiso 1 1 calc GR . . . . H9C H 0.3127 0.7282 0.6008 0.095 Uiso 1 1 calc GR . . . . C11 C 0.3958(2) -0.0210(5) 0.7654(3) 0.0710(13) Uani 1 1 d . . . . . H11A H 0.4011 -0.1351 0.7541 0.106 Uiso 1 1 calc GR . . . . H11B H 0.3650 -0.0096 0.8007 0.106 Uiso 1 1 calc GR . . . . H11C H 0.4417 0.0249 0.7970 0.106 Uiso 1 1 calc GR . . . . H2N H 0.294(3) 0.453(6) 0.378(3) 0.108(17) Uiso 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0382(3) 0.0343(3) 0.0412(3) -0.00336(16) 0.01533(19) -0.00283(16) O1 0.0438(14) 0.0338(13) 0.0558(14) -0.0078(11) 0.0209(12) -0.0033(11) O2 0.0470(15) 0.0518(15) 0.0585(15) -0.0213(13) 0.0247(12) -0.0124(12) O3 0.0532(15) 0.0654(18) 0.0525(15) 0.0106(13) 0.0204(13) 0.0038(14) N1 0.0368(16) 0.0348(15) 0.0449(16) -0.0087(13) 0.0164(13) -0.0033(12) O4 0.0406(15) 0.0651(18) 0.0689(18) 0.0040(14) 0.0108(13) -0.0016(13) N2 0.0418(17) 0.0500(18) 0.0452(16) 0.0023(14) 0.0196(14) 0.0053(14) C8 0.0396(19) 0.0288(17) 0.0346(17) -0.0018(13) 0.0090(15) -0.0042(15) C7 0.0399(19) 0.0325(17) 0.0395(17) -0.0109(14) 0.0178(15) -0.0062(15) C10 0.057(2) 0.0304(18) 0.0445(19) -0.0017(15) 0.0147(19) -0.0021(17) C4 0.047(2) 0.0390(19) 0.0477(19) -0.0114(16) 0.0241(17) -0.0084(16) C1 0.044(2) 0.0373(19) 0.053(2) -0.0077(16) 0.0160(18) 0.0005(16) C2 0.037(2) 0.058(2) 0.063(2) -0.0127(19) 0.0163(19) 0.0010(17) C6 0.061(2) 0.055(2) 0.049(2) 0.0082(18) 0.0260(19) 0.0084(19) C3 0.045(2) 0.058(2) 0.065(2) -0.014(2) 0.0310(19) -0.0113(18) C5 0.071(3) 0.053(2) 0.054(2) 0.0043(19) 0.039(2) -0.003(2) C9 0.070(3) 0.041(2) 0.077(3) -0.022(2) 0.022(2) 0.000(2) C11 0.086(3) 0.064(3) 0.052(2) 0.017(2) 0.007(2) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O1 1.955(2) . ? Zn1 O2 1.954(2) 7_556 ? Zn1 O3 1.974(2) . ? Zn1 N1 2.053(3) . ? Zn1 C10 2.574(3) . ? O1 C8 1.240(4) . ? O2 Zn1 1.954(2) 7_556 ? O2 C8 1.240(4) . ? O3 C10 1.264(4) . ? N1 C7 1.334(4) . ? N1 C1 1.348(4) . ? O4 C10 1.216(4) . ? N2 C7 1.350(4) . ? N2 C6 1.373(4) . ? N2 H2N 1.07(5) . ? C8 C9 1.504(5) . ? C7 C4 1.419(4) . ? C10 C11 1.507(5) . ? C4 C3 1.380(5) . ? C4 C5 1.405(5) . ? C1 H1 0.9300 . ? C1 C2 1.377(5) . ? C2 H2 0.9300 . ? C2 C3 1.376(5) . ? C6 H6 0.9300 . ? C6 C5 1.347(5) . ? C3 H3 0.9300 . ? C5 H5 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 O3 112.97(10) . . ? O1 Zn1 N1 98.28(10) . . ? O1 Zn1 C10 105.81(10) . . ? O2 Zn1 O1 129.17(10) 7_556 . ? O2 Zn1 O3 111.81(11) 7_556 . ? O2 Zn1 N1 95.63(10) 7_556 . ? O2 Zn1 C10 101.97(11) 7_556 . ? O3 Zn1 N1 101.03(11) . . ? O3 Zn1 C10 28.58(11) . . ? N1 Zn1 C10 129.49(12) . . ? C8 O1 Zn1 134.3(2) . . ? C8 O2 Zn1 131.6(2) . 7_556 ? C10 O3 Zn1 103.1(2) . . ? C7 N1 Zn1 123.8(2) . . ? C7 N1 C1 116.1(3) . . ? C1 N1 Zn1 120.0(2) . . ? C7 N2 C6 107.8(3) . . ? C7 N2 H2N 125(3) . . ? C6 N2 H2N 127(3) . . ? O1 C8 C9 118.2(3) . . ? O2 C8 O1 125.8(3) . . ? O2 C8 C9 116.0(3) . . ? N1 C7 N2 126.9(3) . . ? N1 C7 C4 124.6(3) . . ? N2 C7 C4 108.5(3) . . ? O3 C10 Zn1 48.33(16) . . ? O3 C10 C11 116.2(3) . . ? O4 C10 Zn1 72.7(2) . . ? O4 C10 O3 121.0(3) . . ? O4 C10 C11 122.7(4) . . ? C11 C10 Zn1 164.6(3) . . ? C3 C4 C7 117.1(3) . . ? C3 C4 C5 137.1(3) . . ? C5 C4 C7 105.8(3) . . ? N1 C1 H1 118.4 . . ? N1 C1 C2 123.2(4) . . ? C2 C1 H1 118.4 . . ? C1 C2 H2 119.9 . . ? C3 C2 C1 120.2(4) . . ? C3 C2 H2 119.9 . . ? N2 C6 H6 124.9 . . ? C5 C6 N2 110.3(3) . . ? C5 C6 H6 124.9 . . ? C4 C3 H3 120.6 . . ? C2 C3 C4 118.7(3) . . ? C2 C3 H3 120.6 . . ? C4 C5 H5 126.2 . . ? C6 C5 C4 107.6(3) . . ? C6 C5 H5 126.2 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11B 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Zn1 O1 C8 O2 -22.3(5) . . . . ? Zn1 O1 C8 C9 158.3(3) . . . . ? Zn1 O2 C8 O1 -26.7(5) 7_556 . . . ? Zn1 O2 C8 C9 152.7(3) 7_556 . . . ? Zn1 O3 C10 O4 -1.9(4) . . . . ? Zn1 O3 C10 C11 179.7(3) . . . . ? Zn1 N1 C7 N2 -5.2(4) . . . . ? Zn1 N1 C7 C4 174.6(2) . . . . ? Zn1 N1 C1 C2 -176.1(3) . . . . ? N1 C7 C4 C3 0.3(5) . . . . ? N1 C7 C4 C5 -178.7(3) . . . . ? N1 C1 C2 C3 2.2(6) . . . . ? N2 C7 C4 C3 -179.8(3) . . . . ? N2 C7 C4 C5 1.2(4) . . . . ? N2 C6 C5 C4 0.8(4) . . . . ? C7 N1 C1 C2 -0.5(5) . . . . ? C7 N2 C6 C5 0.0(4) . . . . ? C7 C4 C3 C2 1.4(5) . . . . ? C7 C4 C5 C6 -1.2(4) . . . . ? C1 N1 C7 N2 179.4(3) . . . . ? C1 N1 C7 C4 -0.8(4) . . . . ? C1 C2 C3 C4 -2.7(5) . . . . ? C6 N2 C7 N1 179.1(3) . . . . ? C6 N2 C7 C4 -0.7(4) . . . . ? C3 C4 C5 C6 -179.9(4) . . . . ? C5 C4 C3 C2 -180.0(4) . . . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma -2 0 0 857.71 34.4 2 0 0 832.72 34.4 -2 0 0 849.22 34.4 -4 0 0 2762.82 113.29 -4 0 0 2929.31 113.39 -6 0 0 1789.92 74.19 -6 0 0 1831.52 74.29 -8 0 0 269.87 15.1 -8 0 0 276.07 15.1 -10 0 0 412.36 21.2 -10 0 0 386.36 20.9 12 0 0 669.23 31.6 -12 0 0 612.74 31.3 -14 0 0 190.28 14.1 -16 0 0 1375.26 63.59 -16 0 0 1400.36 62.59 18 0 0 35.2 7.2 -18 0 0 37.3 8.3 -18 0 0 22.9 7.8 -20 0 0 176.98 17.4 -20 0 0 173.48 18.1 -22 0 0 48.3 11.5 -24 0 0 5.2 8.5 1 -1 0 455.35 18.2 -1 -1 0 425.86 18.3 1 -1 0 445.76 18 -1 -1 0 398.26 18.8 -1 1 0 432.66 18.2 -1 1 0 442.36 18 1 1 0 459.45 18.6 3 -1 0 236.28 10.3 -3 -1 0 239.68 12.2 -3 -1 0 226.48 10.2 3 -1 0 236.98 10.6 -3 1 0 236.28 10.7 3 1 0 224.58 10.1 3 1 0 231.98 12.1 -3 1 0 251.57 10.4 5 -1 0 114.79 6.6 -5 -1 0 119.59 6.1 -5 -1 0 113.99 8.3 5 1 0 139.89 6.2 -5 1 0 118.99 7.3 -5 1 0 117.99 6.5 5 1 0 122.99 8.5 -7 -1 0 -0.9 1.6 7 -1 0 -0.6 1.4 -7 -1 0 3.2 2.7 -7 1 0 0.4 1.9 7 1 0 2 1.3 -7 1 0 2.3 1.5 7 1 0 -0.2 2.3 -9 -1 0 482.25 25.2 9 -1 0 500.85 23 -9 1 0 467.85 24.3 -9 1 0 450.15 22.4 9 1 0 481.95 21.8 -9 1 0 510.05 23.1 -11 -1 0 5.6 3.9 -11 1 0 5.9 4.1 11 1 0 6.8 2.8 -11 1 0 12.9 3.5 -11 1 0 6.2 3 -13 -1 0 59.69 9.4 -13 1 0 58.69 8.4 -13 1 0 58.99 9.5 -13 1 0 45.3 6.8 13 1 0 50.99 6.6 -15 -1 0 141.29 14.7 -15 1 0 139.19 14.9 -15 1 0 144.29 11.7 -17 -1 0 62.49 10.9 -17 1 0 92.59 13.2 -17 1 0 75.99 10.3 19 -1 0 51.99 9.7 -19 -1 0 38.3 9.4 -19 -1 0 60.29 10.9 -19 1 0 70.09 12.1 -19 1 0 36.6 7.8 -21 -1 0 -0.4 5.7 -21 -1 0 -1.3 6.4 -21 1 0 15.5 9.5 -23 -1 0 2 7.2 -23 1 0 -4.6 7.6 0 -2 0 13.1 2.7 0 -2 0 14.6 2.4 0 -2 0 17.2 3.4 0 2 0 11.8 2.8 0 2 0 17.4 2.4 -2 -2 0 476.65 22.9 2 -2 0 517.55 21.4 -2 -2 0 466.25 21.7 2 -2 0 481.15 21 -2 2 0 506.25 21.2 -2 2 0 510.05 21.6 4 -2 0 146.19 7.1 4 -2 0 132.29 7.1 -4 -2 0 124.69 7 -4 -2 0 116.69 8.9 -4 2 0 139.19 7.1 4 2 0 133.59 9.5 -4 2 0 145.79 7.7 4 2 0 133.29 7.4 6 -2 0 1329.17 53.49 -6 -2 0 1349.96 57.49 6 -2 0 1316.17 52.79 -6 -2 0 1249.88 52.59 6 2 0 1272.37 56.89 6 2 0 1331.77 52.79 -6 2 0 1300.77 52.89 -6 2 0 1302.17 54.09 8 -2 0 105.89 6.8 -8 -2 0 109.49 6.2 -8 2 0 116.19 7 -8 2 0 114.79 8.4 8 2 0 119.89 10.2 8 2 0 110.69 6.2 10 -2 0 1224.38 51.09 -10 -2 0 1195.98 56.19 -10 2 0 1197.28 53.49 -10 2 0 1196.58 51.09 10 2 0 1193.98 49.4 10 2 0 1288.57 56.39 -12 -2 0 588.04 31.4 -12 2 0 556.04 26.3 -12 2 0 555.44 26 12 2 0 536.65 24 -12 2 0 516.05 28.9 -14 -2 0 128.49 14.9 -14 2 0 136.29 14.7 -14 2 0 129.69 9.6 -14 2 0 109.49 9.5 14 2 0 101.49 7.1 -16 -2 0 617.34 34.3 -16 2 0 612.84 34 -16 2 0 534.45 29 18 -2 0 22.8 7.4 -18 -2 0 7.9 6.2 -18 2 0 -2.2 6.7 20 -2 0 13.6 6.8 -20 -2 0 31.6 9.6 -20 2 0 23.7 10 -22 -2 0 54.59 12.1 -22 -2 0 76.19 13.7 -22 2 0 61.29 13.9 1 -3 0 287.67 16.4 1 -3 0 311.67 15.1 -1 -3 0 274.47 14.2 -1 -3 0 294.87 15.6 -1 -3 0 303.67 15.7 1 -3 0 282.97 14.1 -1 3 0 276.57 15.2 -1 3 0 287.17 14 1 3 0 302.37 16.1 -3 -3 0 1008.9 43.9 -3 -3 0 988.3 41.8 3 -3 0 943.21 40.5 3 -3 0 981.2 41.1 -3 3 0 995.7 41.6 3 3 0 939.61 43.9 -3 3 0 977 41 5 -3 0 143.99 8.3 -5 -3 0 144.89 8.7 5 -3 0 149.29 8.4 -5 3 0 146.59 8.6 5 3 0 157.98 11.7 -5 3 0 165.58 9.4 7 -3 0 725.73 29.8 7 -3 0 680.53 30.2 -7 -3 0 717.73 30.1 7 3 0 663.23 34.7 -7 3 0 714.13 30 -7 3 0 695.33 31.3 7 3 0 656.13 30.5 9 -3 0 663.53 28.7 -9 -3 0 671.03 28.3 9 3 0 695.03 35.4 9 3 0 599.34 28.5 -9 3 0 677.43 31.3 -9 3 0 699.03 29 -11 -3 0 7.8 5.5 11 -3 0 12.6 3.3 -11 3 0 15.9 3.4 -11 3 0 13.4 4.9 11 3 0 14.7 6.4 13 -3 0 338.07 17.4 -13 -3 0 350.46 24.7 13 3 0 330.97 23.3 -13 3 0 341.37 17.3 -13 3 0 335.07 17.4 -13 3 0 314.57 21 -15 -3 0 43.4 10.7 -15 3 0 27.5 8.1 -15 3 0 36.2 6.1 -17 -3 0 1.5 6.5 17 -3 0 8.3 6.5 -17 3 0 3.9 7.1 19 -3 0 62.09 12.5 -19 -3 0 53.29 12.4 -19 3 0 34.7 10.9 21 -3 0 3.2 7.1 -21 -3 0 17 9.6 -21 3 0 8.7 9.4 -23 -3 0 18.7 10.2 -23 3 0 16 11.1 0 -4 0 1608.84 66.59 0 -4 0 1631.54 69.19 0 4 0 1583.04 68.89 -2 -4 0 207.18 12.8 2 -4 0 193.18 10.9 2 -4 0 165.68 11.2 -2 -4 0 185.68 11.4 2 -4 0 204.78 14.3 -2 4 0 177.78 10.6 -2 4 0 173.38 12.1 2 4 0 213.58 14 4 -4 0 462.55 21.6 4 -4 0 422.46 25.3 4 -4 0 460.45 20.8 -4 -4 0 423.26 22.2 -4 -4 0 456.95 22.5 -4 4 0 449.06 21.4 4 4 0 493.05 25.8 -4 4 0 441.76 22.2 6 -4 0 1170.58 49.9 6 -4 0 1152.08 49.6 -6 -4 0 1196.38 50.89 -6 4 0 1194.78 50.89 -6 4 0 1225.78 50.89 6 4 0 1221.08 55.99 -8 -4 0 4.9 3.1 8 -4 0 8.1 3 8 -4 0 8.9 3.1 8 4 0 3 4.2 -8 4 0 8.9 2.9 -8 4 0 8.5 3.6 -10 -4 0 1290.87 53.49 10 -4 0 1243.08 53.19 10 4 0 1253.07 61.59 -10 4 0 1335.27 54.19 -10 4 0 1309.37 56.69 12 -4 0 257.77 13.5 12 -4 0 296.87 21.8 12 4 0 245.08 20.6 -12 4 0 241.48 13.6 -12 4 0 267.67 17.5 14 -4 0 40.9 10.4 -14 -4 0 53.19 12.9 -14 4 0 35.4 7.1 14 4 0 21.3 9.2 -14 4 0 51.89 9.8 16 -4 0 166.18 20.7 -16 -4 0 160.48 21.3 -16 4 0 145.29 17.4 18 -4 0 31 10.1 -18 -4 0 36.7 12.9 -18 4 0 33.9 10.2 20 -4 0 41.2 11.6 -20 -4 0 23.3 11.3 -20 4 0 32.5 12 22 -4 0 45.5 12.9 -22 -4 0 39.6 13.8 -22 4 0 41.5 14 1 -5 0 307.37 19.7 -1 -5 0 313.17 17.3 -1 -5 0 322.97 19.4 1 -5 0 297.77 16.7 1 5 0 346.47 20.5 -1 5 0 313.37 19.4 3 -5 0 147.19 9.8 -3 -5 0 147.39 11.7 3 -5 0 158.88 16.4 -3 5 0 158.88 10 3 5 0 119.79 13.9 -3 5 0 132.79 11.2 5 -5 0 -2 4.4 5 -5 0 2.7 3.3 5 -5 0 1.4 2.4 -5 -5 0 5 3.7 -5 5 0 -1.2 2.7 -5 5 0 5.7 3.1 5 5 0 4 4.5 7 -5 0 1160.88 50.39 7 -5 0 1197.58 51.09 7 -5 0 1238.68 59.39 -7 -5 0 1237.48 52.59 -7 5 0 1216.58 52.59 -7 5 0 1153.88 52.09 7 5 0 1184.78 57.99 9 -5 0 396.96 21.3 -9 -5 0 350.76 19.1 9 -5 0 361.86 18.1 9 -5 0 371.26 25.8 -9 5 0 351.86 20 -9 5 0 319.57 18.6 9 5 0 359.76 24.9 -11 -5 0 3.9 3.4 11 -5 0 7.2 6.5 11 5 0 -2 5.3 -11 5 0 3.9 3.9 -11 5 0 0 2.4 -13 -5 0 134.39 19.1 13 -5 0 139.99 19 -13 5 0 145.19 14.9 13 5 0 147.19 19.4 -15 -5 0 13.1 7.3 15 -5 0 55.69 13.5 15 5 0 47.9 12.9 -15 5 0 47.4 9.6 17 -5 0 53.69 12.9 -17 -5 0 40.6 13.4 -17 5 0 40.7 10.1 -19 -5 0 109.29 20 19 -5 0 71.09 15.7 -19 5 0 59.89 14 -21 -5 0 8.9 10.7 21 -5 0 -5.1 7.5 0 -6 0 1111.49 50.49 0 -6 0 1141.09 53.89 0 6 0 1152.48 54.69 -2 -6 0 -1.2 3.5 2 -6 0 0.5 4.1 2 -6 0 1.8 3.1 2 6 0 1.7 4.4 -2 6 0 -0.1 3.5 -4 -6 0 342.47 20.7 4 -6 0 307.47 17.1 4 -6 0 304.77 22.5 4 6 0 308.67 22.4 -4 6 0 356.16 21.1 -4 6 0 305.67 17.4 -6 -6 0 379.46 22.3 6 -6 0 402.46 27.1 6 -6 0 373.26 19.2 -6 6 0 357.06 20.2 6 6 0 389.16 26.6 -6 6 0 402.36 22.8 8 -6 0 54.19 12.5 -8 -6 0 60.59 8.9 -8 6 0 54.89 8.4 8 6 0 55.09 11.5 -8 6 0 56.29 7.8 -10 -6 0 52.69 8.2 10 -6 0 56.79 13.8 -10 6 0 48.1 7.9 -10 6 0 44.1 7.1 10 6 0 52.89 12.6 -12 -6 0 22 10.8 12 -6 0 3.5 6.1 -12 6 0 14.8 6.4 12 6 0 8.3 8.4 14 -6 0 9.1 8.9 -14 -6 0 15.9 11 14 6 0 33.2 12.1 -14 6 0 11.4 6.1 16 -6 0 48.2 13.6 -16 -6 0 72.49 18.6 18 -6 0 7.1 9.5 -18 -6 0 4.8 11.1 20 -6 0 -2.3 9 -20 -6 0 13.2 12.8 -1 -7 0 98.19 13.5 1 -7 0 130.19 15.9 -1 7 0 95.59 14.3 1 7 0 90.69 14.5 -3 -7 0 505.45 29.3 3 -7 0 484.95 31 3 7 0 524.65 32.5 -3 7 0 486.25 29.9 5 -7 0 180.78 21.1 -5 -7 0 165.88 16.9 5 7 0 145.89 19.6 -5 7 0 173.08 12.3 -5 7 0 188.68 18.2 -7 -7 0 402.86 24.4 7 -7 0 341.77 27.6 -7 7 0 379.46 24.2 -7 7 0 403.66 21.6 7 7 0 393.86 28.6 9 -7 0 30 10.7 -9 -7 0 40.8 8.6 9 7 0 54.59 12.8 -9 7 0 22 6.1 -9 7 0 22.6 7.3 11 -7 0 118.89 19.5 11 7 0 141.79 20.7 13 -7 0 204.98 26.7 -13 -7 0 293.07 32.7 13 7 0 248.98 29.1 -15 -7 0 15.2 11.3 15 -7 0 12.3 11.1 15 7 0 12.9 10.2 -17 -7 0 39.1 16.5 17 -7 0 16.6 11 0 -8 0 3.1 5.8 0 8 0 -6 5.1 2 -8 0 2.3 6.4 -2 -8 0 12.7 7.4 2 8 0 1.8 6.5 -2 8 0 0.9 6.1 -4 -8 0 -2.4 5.3 4 -8 0 -12.7 5.6 -4 8 0 -3.4 5.2 4 8 0 -7.6 6 6 -8 0 -3.5 7.2 -6 -8 0 5.9 6.6 6 8 0 11.4 8.2 -6 8 0 3.7 6.2 -8 -8 0 7.1 7 8 -8 0 23.3 10.6 8 8 0 11 8.8 10 -8 0 4.4 8.7 10 8 0 4.7 9.3 12 -8 0 15.1 11.3 -12 -8 0 10.3 10.6 12 8 0 3.5 8.7 -14 -8 0 3.3 10.8 14 -8 0 2.2 9.7 14 8 0 16.6 11.1 16 -8 0 3.9 5.9 -16 -8 0 3.6 11.2 -1 -9 0 70.69 13.8 1 -9 0 74.79 14.3 -1 9 0 89.89 16.1 1 9 0 95.39 17.4 3 -9 0 202.28 23.4 -3 -9 0 180.58 20.8 -3 9 0 200.68 23.4 3 9 0 169.58 23.7 5 -9 0 43.7 13.8 -5 -9 0 35.3 10.5 5 9 0 32.5 12.2 -5 9 0 15.8 8.5 -7 -9 0 152.78 19.4 7 -9 0 131.89 22 7 9 0 175.08 24.7 9 -9 0 133.49 22.2 9 9 0 100.29 19.5 -11 -9 0 18.2 12.1 11 -9 0 -0.5 9.6 11 9 0 4.3 9.9 13 9 0 65.99 18 0 -10 0 -5 7.6 0 10 0 0.6 8.5 2 -10 0 -5 8 -2 -10 0 1.8 8.9 2 10 0 -13 6.9 -2 10 0 -4.8 7.6 4 -10 0 -4.8 8.3 -4 -10 0 -10.2 7 4 10 0 -7.2 8.5 6 -10 0 11.6 10.9 6 10 0 7.5 11.7 8 -10 0 18 11.7 -8 -10 0 12.1 12.8 8 10 0 10.6 12.2 -24 0 1 3.7 7.9 -22 0 1 3.3 6.7 -20 0 1 3.8 6.2 -20 0 1 3 5.4 18 0 -1 -0.2 3.5 -18 0 1 0.5 4.5 -16 0 1 7.9 4.8 16 0 -1 -0.3 3.4 14 0 -1 1 2.5 -14 0 1 2.8 3.4 -12 0 1 3 3.1 -10 0 1 -2.1 1.9 -10 0 1 -2.4 2.1 8 0 -1 1 2.3 -8 0 1 0.8 1.9 -8 0 1 -0.8 1.9 -6 0 1 -0.7 1.7 6 0 -1 0.4 1.6 4 0 -1 0 1.2 4 0 -1 -1.4 0.7 -4 0 1 -0.3 1.1 -2 0 1 -2.2 0.6 -2 0 1 -4.3 0.3 2 0 -1 -3.5 0.7 2 0 -1 -2.5 0.6 0 0 1 -9.9 0.8 0 0 -1 -10.2 0.6 0 0 -1 -9.9 0.7 -2 0 -1 0.2 0.8 -2 0 -1 -0.1 0.6 2 0 1 -0.6 0.7 2 0 1 0.6 0.7 -2 0 -1 0 0.9 2 0 1 -0.5 0.7 -4 0 -1 2.2 1.5 4 0 1 1.3 1.2 4 0 1 0.3 1.1 -4 0 -1 -0.1 1 6 0 1 -0.9 1.6 6 0 1 1.3 1.7 -6 0 -1 -1 1.3 -6 0 -1 2 1.6 8 0 1 3.5 2.5 -8 0 -1 -1.4 1.7 -8 0 -1 -0.8 1.8 -10 0 -1 10.1 3.6 -10 0 -1 0 2.1 10 0 1 1.6 2.6 -12 0 -1 2.9 3 -12 0 -1 -0.6 3.8 -14 0 -1 2.2 3.5 -14 0 -1 1 4.3 -16 0 -1 7 5 -16 0 -1 5.8 6.3 -18 0 -1 -3.9 4.1 -18 0 -1 2.9 6 -20 0 -1 2.4 7.9 -20 0 -1 4.5 6.7 -22 0 -1 3.2 8.3 -23 -1 1 27 10.1 -23 -1 1 34.9 11 -23 1 1 7.8 8 -21 -1 1 280.77 21 -21 1 1 227.48 22 -19 -1 1 15.7 6.9 19 -1 -1 15.3 6.4 -19 1 1 12.8 6.1 -19 1 1 32.3 8.8 17 -1 -1 255.57 17.4 -17 -1 1 250.77 19.1 -17 1 1 270.47 19.4 -17 1 1 222.08 16.6 15 -1 -1 1073.09 49.9 -15 -1 1 1139.09 51.89 -15 1 1 1060.69 49.3 -15 1 1 1141.59 51.19 15 1 -1 1029 45.3 15 1 -1 1040.1 45.9 -13 -1 1 253.67 17.3 13 -1 -1 223.28 15.5 -13 1 1 292.17 17.1 13 1 -1 248.88 12.9 -13 1 1 235.68 15.2 13 1 -1 219.28 12.4 -11 -1 1 933.41 45.3 11 -1 -1 963.2 43.3 -11 1 1 968.5 43.2 11 1 -1 973.1 40.5 -11 1 1 984.9 43.3 -9 -1 1 52.79 7.6 9 -1 -1 44.1 5.9 9 1 -1 43.3 3.4 -9 1 1 45.6 5.8 -7 -1 1 1125.99 46.7 7 -1 -1 1006.7 43.9 -7 -1 1 966 46.1 -7 1 1 1080.79 44.2 5 -1 -1 5679.13 219.78 -5 -1 1 5503.25 222.08 5 -1 -1 5552.64 221.48 -5 1 1 5613.64 219.98 3 -1 -1 23.6 3.4 -3 -1 1 20.9 3.6 3 -1 -1 22.7 2.7 -3 -1 1 24.2 3.7 -3 1 1 24.6 2 -3 1 1 20 2.5 3 1 -1 20.2 3.5 1 -1 -1 7284.17 286.27 1 -1 -1 7585.94 284.77 -1 -1 1 7155.78 285.07 -1 -1 1 7260.97 285.27 -1 -1 1 7341.17 284.67 -1 1 1 7486.75 285.67 -1 1 1 7044.4 284.97 1 1 -1 7066.09 285.17 1 1 -1 7258.37 284.57 -1 -1 -1 5061.19 200.08 -1 -1 -1 4962.3 200.48 1 -1 1 5044 199.38 1 -1 1 5131.99 199.98 1 1 1 5256.67 200.68 -1 1 -1 5159.18 200.08 -1 1 -1 4989.9 199.48 1 1 1 5156.58 200.08 3 -1 1 4109.59 152.58 -3 -1 -1 3756.42 152.38 -3 -1 -1 3872.91 153.78 3 1 1 3712.63 153.58 -3 1 -1 3881.91 152.68 3 1 1 3876.01 152.48 5 -1 1 3296.77 132.29 -5 -1 -1 3190.58 131.99 -5 -1 -1 3356.36 134.09 5 1 1 3422.46 133.99 -5 1 -1 3223.68 131.19 -5 1 -1 3409.96 131.09 5 1 1 3374.76 132.19 -5 1 -1 3380.86 132.89 -7 -1 -1 100.09 8.1 -7 1 -1 95.39 6.1 7 1 1 90.59 7.7 -7 1 -1 101.49 8.9 -7 1 -1 87.29 5.9 7 1 1 90.19 6.5 -9 -1 -1 169.08 12.4 -9 1 -1 172.08 12.2 9 1 1 197.08 12.9 9 1 1 196.78 11 -9 1 -1 167.38 10.4 -9 1 -1 168.78 10.2 -11 -1 -1 1226.98 56.19 -11 1 -1 1236.98 56.29 -11 1 -1 1297.07 53.69 11 1 1 1214.58 53.39 -11 1 -1 1239.68 53.19 -13 -1 -1 8.7 5 -13 1 -1 7.6 3.6 -13 1 -1 5.1 5.2 -13 1 -1 1.1 3 13 1 1 6.2 3.7 -15 -1 -1 563.24 31.2 -15 1 -1 557.64 28.4 -15 1 -1 575.54 32.6 -17 -1 -1 45 9.5 -17 -1 -1 61.29 10.4 -17 1 -1 69.29 11.9 -17 1 -1 45.3 7.6 -19 -1 -1 72.99 12 -19 -1 -1 82.69 13.2 -19 1 -1 58.99 12.5 -21 -1 -1 111.29 14.8 -21 -1 -1 138.19 17.6 -21 1 -1 147.69 18.9 -23 -1 -1 -6.3 7.5 -23 1 -1 3.9 9.2 -24 -2 1 7.5 8.2 -24 -2 1 3.6 10.2 -24 2 1 5.3 9.3 -22 -2 1 6.8 7.4 -22 2 1 0.3 7.2 -20 -2 1 58.19 11.9 20 -2 -1 35.2 9.2 -20 2 1 61.09 12.4 -18 -2 1 62.29 12 18 -2 -1 92.19 12.7 -18 2 1 81.39 10.7 -18 2 1 84.79 13.6 -16 -2 1 22.8 7.9 16 -2 -1 11.2 6.4 -16 2 1 12.1 4.9 -16 2 1 2.8 5.9 14 -2 -1 45.7 8.8 -14 -2 1 38.2 8.8 -14 2 1 48.3 8.9 -14 2 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3 18 19.3 10.9 7 3 -18 -7.2 9.7 5 -3 -18 16.2 11.5 -5 -3 18 12.8 9 -5 3 18 19.4 11.3 5 3 -18 28.1 13.5 3 -3 -18 32 13 3 3 -18 15 12.6 -3 3 18 24.6 11.8 1 -3 -18 2.6 11.3 -1 3 18 -7.2 7.8 1 3 -18 -7.6 11.1 -1 -3 -18 6.8 12.7 -1 -3 -18 13.4 12.2 1 3 18 1.5 9.2 -1 3 -18 29 15.3 -14 -4 18 3.5 10.1 14 -4 -18 -5.2 9.9 -14 4 18 -1.5 7.8 -12 -4 18 18.8 12 12 -4 -18 12.9 10.1 12 4 -18 31.9 13.8 -12 4 18 19.6 10.6 10 -4 -18 45.2 16.5 -10 -4 18 72.19 14.9 -10 4 18 53.89 14.7 10 4 -18 50.89 15.9 8 -4 -18 5.5 9.7 -8 -4 18 4.3 8.7 -8 4 18 6.5 10.2 8 4 -18 18.9 12.9 6 -4 -18 93.19 19.3 -6 -4 18 106.99 17 -6 4 18 97.99 19.6 6 4 -18 115.79 21.5 4 -4 -18 12.9 12.7 4 4 -18 8.4 12.4 -4 4 18 13.5 10.2 2 -4 -18 41.8 15.9 2 4 -18 22.8 14.9 -2 4 18 28.1 12.4 0 -4 -18 29.1 14.7 0 4 18 30.3 12.9 -11 -5 18 4.2 9.4 -11 5 18 3.6 9 -9 -5 18 104.59 17.6 9 -5 -18 57.59 17.8 -9 5 18 94.49 18.6 7 -5 -18 -4.9 9 -7 5 18 21.1 11.8 5 -5 -18 14.4 14.3 -5 5 18 19.4 12.4 -16 0 19 -5.2 10.7 16 0 -19 2.8 13.1 -14 0 19 1.8 8.7 14 0 -19 -4.6 10.2 -12 0 19 -1.5 9.7 12 0 -19 -1.5 8.9 12 0 -19 10.6 13.7 10 0 -19 4.3 10.9 10 0 -19 0.4 8.5 -10 0 19 9 9.8 8 0 -19 12 11.7 -8 0 19 -1.7 8.4 8 0 -19 6.6 9 -6 0 19 1.4 8.3 6 0 -19 -8.1 8.4 6 0 -19 -7.7 9.3 -4 0 19 -2.2 7.7 4 0 -19 1.8 10.4 4 0 -19 3 9.4 -2 0 19 0.6 8.3 2 0 -19 -2 8.7 2 0 -19 -0.8 10.3 0 0 -19 8.8 11.7 0 0 -19 6.2 11.2 0 0 19 0.7 8.1 17 -1 -19 54.09 19 -17 -1 19 81.19 19.8 -17 1 19 67.79 17.5 15 -1 -19 66.49 20.9 -15 -1 19 44.9 15 -15 1 19 79.39 17.9 15 1 -19 35.8 16.1 -13 -1 19 38.8 13.1 13 -1 -19 47.3 17.5 13 1 -19 32.7 11.8 -13 1 19 33.8 14.4 13 1 -19 73.49 19.1 -11 -1 19 105.89 18.5 11 -1 -19 103.49 22.6 11 1 -19 117.29 18.4 11 1 -19 113.29 24.2 -11 1 19 119.99 20.6 9 -1 -19 -13.3 8.8 9 -1 -19 -1.7 8 -9 -1 19 -8.3 7.9 9 1 -19 -1.9 10.5 9 1 -19 3.7 9.4 -9 1 19 6 8.6 7 -1 -19 81.79 15.2 7 -1 -19 56.29 17.8 -7 -1 19 68.29 14.9 7 1 -19 57.09 14.5 -7 1 19 49.99 13.9 7 1 -19 51.79 17.4 5 -1 -19 23.7 13.2 5 -1 -19 30.1 11.6 -5 -1 19 45.5 12.4 5 1 -19 30 13.6 -5 1 19 30.4 12.3 5 1 -19 45.5 14.1 3 -1 -19 5 11.4 -3 -1 19 4.4 8.9 3 -1 -19 13.5 11.2 3 1 -19 4 11.4 -3 1 19 19.3 10.8 3 1 -19 20.5 12.7 1 -1 -19 76.69 17.2 1 -1 -19 41.3 14.7 1 1 -19 62.79 18.4 1 1 -19 71.39 17.9 -1 1 19 86.39 15.6 -1 -1 -19 22.7 13.7 -1 -1 -19 12.2 12.5 -1 1 -19 -3.3 12.8 1 1 19 13.6 10.5 -16 -2 19 29.9 14.2 16 -2 -19 17.8 14.6 -16 2 19 27 13.9 -14 -2 19 -11.3 9.2 14 -2 -19 1.2 12 14 2 -19 1.8 11.8 -14 2 19 -1 10.2 -12 -2 19 3.7 10.1 12 -2 -19 5.3 12.6 12 2 -19 0.6 11.6 12 2 -19 8.7 10 -12 2 19 -1.2 8 10 -2 -19 -8 10.1 -10 -2 19 -9.3 7.7 10 2 -19 8.4 12.6 -10 2 19 -5.3 7.9 10 2 -19 5.3 10.4 8 -2 -19 -7.4 9.2 -8 -2 19 6.6 9.2 -8 2 19 3.7 9.5 8 2 -19 0.5 9.9 8 2 -19 -3.5 10.6 6 -2 -19 5.4 10 -6 -2 19 13.5 9.2 -6 2 19 21.6 10.9 6 2 -19 -5.5 11.5 6 2 -19 5.9 11.4 -4 -2 19 20.7 9.4 4 -2 -19 31.2 14.4 4 -2 -19 0.1 11.2 -4 2 19 16.1 11.2 4 2 -19 13.5 12.7 2 -2 -19 -9.1 9.3 2 -2 -19 6.8 10.7 -2 2 19 3.6 8.8 2 2 -19 8.4 13.4 0 -2 -19 8.4 12 0 -2 -19 6 11.8 0 2 -19 5.7 13.2 0 2 19 13 10.3 13 -3 -19 20.1 12.9 -13 -3 19 24.2 12.2 -13 3 19 12.6 10.1 13 3 -19 -3.2 10.8 11 -3 -19 67.49 18.2 -11 -3 19 66.19 16.3 11 3 -19 82.99 17.9 -11 3 19 81.59 18.3 -9 -3 19 23.7 11.2 9 -3 -19 13.7 12.4 -9 3 19 14.6 10.9 9 3 -19 5.8 11.4 7 -3 -19 48.8 16.3 -7 -3 19 57.49 13.6 -7 3 19 77.29 16.5 7 3 -19 62.59 17.5 -5 -3 19 43.2 12.1 5 -3 -19 30.2 14.2 5 3 -19 24.9 14.4 -5 3 19 32.7 13 3 -3 -19 4.8 10.5 3 3 -19 17.8 13.6 -3 3 19 18.2 11.9 1 -3 -19 29.2 15 -1 3 19 35.9 12.8 10 -4 -19 22.3 14.5 -10 -4 19 28.4 12.8 -10 4 19 31.3 13.1 10 4 -19 -8.9 13.2 8 -4 -19 47.2 16.7 -8 -4 19 35.2 12.3 -8 4 19 32.7 13.9 8 4 -19 57.59 24.8 6 -4 -19 13.3 12.1 -6 4 19 4.4 8.9 -14 0 20 -0.2 10.5 14 0 -20 11.8 12.7 -12 0 20 62.89 16 12 0 -20 62.29 20.6 12 0 -20 60.19 15.1 10 0 -20 57.39 19.2 10 0 -20 61.19 14.5 -10 0 20 63.59 16.7 -8 0 20 11.1 9.9 8 0 -20 17.7 11.5 8 0 -20 7.8 12.8 6 0 -20 50.29 16.5 -6 0 20 29.5 11.1 6 0 -20 27.4 12.9 4 0 -20 1.6 10.7 4 0 -20 -9.2 9.6 -4 0 20 -8.3 7.8 -2 0 20 51.69 13.9 2 0 -20 44.7 15.7 2 0 -20 25.5 15 13 -1 -20 26.5 15 -13 -1 20 1.9 10.4 13 1 -20 -0.2 9.8 13 1 -20 -7 10.7 -13 1 20 12.2 10.5 11 -1 -20 -8.9 11.5 -11 -1 20 -4.4 9 -11 1 20 20.1 12.1 11 1 -20 12.7 13.4 11 1 -20 16.2 11.8 9 -1 -20 -1.5 11.2 -9 -1 20 13.4 10.8 -9 1 20 11.9 10.9 9 1 -20 7.6 13.3 9 1 -20 11.3 10.8 -7 -1 20 -1.2 8.5 7 -1 -20 13.4 12.6 7 -1 -20 14.8 11.2 7 1 -20 -4.8 10.4 -7 1 20 -3.1 9.6 7 1 -20 17 11.4 -5 -1 20 -3 8 5 -1 -20 7.8 10.6 5 -1 -20 0.3 11.2 5 1 -20 4.4 11.2 5 1 -20 0.9 10.8 -5 1 20 7.4 10 -3 -1 20 -5.4 8.5 3 -1 -20 -2.1 10.9 3 -1 -20 2.1 12 -3 1 20 -0.7 8.9 3 1 -20 15.6 13.5 3 1 -20 -14.5 8 -12 -2 20 89.79 18.4 12 -2 -20 106.09 24.1 12 2 -20 102.39 24.6 12 2 -20 57.19 15.7 -12 2 20 76.09 17.1 -10 -2 20 2.6 9.4 10 -2 -20 34.7 16.6 10 2 -20 15.7 14.2 10 2 -20 -11.7 9.5 -10 2 20 9.2 10.1 -8 -2 20 118.89 18.7 8 -2 -20 128.59 25.5 8 2 -20 98.19 18.9 -8 2 20 101.69 18.3 8 2 -20 122.79 25 6 -2 -20 42.6 17 -6 -2 20 42.7 13 6 2 -20 29.7 14.7 -6 2 20 27.8 12.2 4 -2 -20 0 11.7 -4 2 20 -2.3 8.3 4 2 -20 5.1 13.2 _iucr_refine_instructions_details ; a0446-072-02_a.res created by SHELXL-2014/7 TITL A0446-072-02_a.res in C2/c REM Old TITL A0446-072-02 in C2/c REM SHELXT solution in C2/c REM R1 0.091, Rweak 0.003, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C11 N3 O3 Zn CELL 0.71073 19.8444 8.1601 15.9017 90 109.063 90 ZERR 4 0.0009 0.0004 0.0008 0 0.003 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O Zn UNIT 88 96 16 32 8 L.S. 10 PLAN 20 SIZE 0.05 0.2 0.25 TEMP 23 BOND $H LIST 6 CONF HTAB ACTA WPDB -1 fmap 2 OMIT 0 50 REM REM REM WGHT 0.055700 FVAR 0.31003 ZN1 5 0.344910 0.223281 0.531573 11.00000 0.03823 0.03433 = 0.04117 -0.00336 0.01533 -0.00283 O1 4 0.316754 0.445428 0.551893 11.00000 0.04378 0.03382 = 0.05582 -0.00780 0.02094 -0.00334 O2 4 0.206892 0.437983 0.556785 11.00000 0.04699 0.05180 = 0.05852 -0.02131 0.02470 -0.01245 O3 4 0.407446 0.117766 0.640954 11.00000 0.05319 0.06542 = 0.05251 0.01059 0.02037 0.00375 N1 3 0.417279 0.282669 0.469126 11.00000 0.03676 0.03483 = 0.04487 -0.00873 0.01636 -0.00327 O4 4 0.300480 0.094420 0.645991 11.00000 0.04056 0.06506 = 0.06895 0.00397 0.01078 -0.00156 N2 3 0.342533 0.469701 0.362383 11.00000 0.04177 0.05000 = 0.04521 0.00231 0.01963 0.00532 C8 1 0.265753 0.504231 0.570549 11.00000 0.03963 0.02880 = 0.03459 -0.00180 0.00903 -0.00424 C7 1 0.404596 0.391341 0.403063 11.00000 0.03990 0.03250 = 0.03952 -0.01093 0.01778 -0.00625 C10 1 0.364021 0.067854 0.678393 11.00000 0.05657 0.03039 = 0.04450 -0.00173 0.01472 -0.00211 C4 1 0.455734 0.443930 0.363921 11.00000 0.04735 0.03900 = 0.04774 -0.01143 0.02407 -0.00838 C1 1 0.483600 0.219332 0.498495 11.00000 0.04354 0.03725 = 0.05328 -0.00766 0.01603 0.00046 AFIX 43 H1 2 0.494433 0.143780 0.544791 11.00000 -1.20000 AFIX 0 C2 1 0.536095 0.261027 0.463301 11.00000 0.03670 0.05760 = 0.06253 -0.01269 0.01627 0.00101 AFIX 43 H2 2 0.580564 0.210979 0.484542 11.00000 -1.20000 AFIX 0 C6 1 0.353082 0.572044 0.299263 11.00000 0.06096 0.05543 = 0.04852 0.00825 0.02604 0.00841 AFIX 43 H6 2 0.318452 0.639898 0.261919 11.00000 -1.20000 AFIX 0 C3 1 0.523021 0.376484 0.396808 11.00000 0.04492 0.05802 = 0.06452 -0.01405 0.03098 -0.01134 AFIX 43 H3 2 0.558858 0.408431 0.374470 11.00000 -1.20000 AFIX 0 C5 1 0.420744 0.560100 0.299173 11.00000 0.07120 0.05277 = 0.05429 0.00432 0.03930 -0.00259 AFIX 43 H5 2 0.440692 0.618218 0.262837 11.00000 -1.20000 AFIX 0 C9 1 0.274514 0.671297 0.612779 11.00000 0.06986 0.04075 = 0.07735 -0.02235 0.02229 0.00017 AFIX 137 H9A 2 0.285305 0.659978 0.675905 11.00000 -1.50000 H9B 2 0.231098 0.732306 0.588591 11.00000 -1.50000 H9C 2 0.312729 0.728210 0.600788 11.00000 -1.50000 AFIX 0 C11 1 0.395836 -0.021027 0.765443 11.00000 0.08567 0.06420 = 0.05157 0.01671 0.00673 -0.00543 AFIX 137 H11A 2 0.401146 -0.135059 0.754144 11.00000 -1.50000 H11B 2 0.364965 -0.009591 0.800654 11.00000 -1.50000 H11C 2 0.441671 0.024935 0.796997 11.00000 -1.50000 AFIX 0 H2N 2 0.294018 0.453357 0.377603 11.00000 0.10806 HKLF 4 REM A0446-072-02_a.res in C2/c REM R1 = 0.0369 for 1774 Fo > 4sig(Fo) and 0.0472 for all 2153 data REM 169 parameters refined using 0 restraints END WGHT 0.0557 0.0000 REM Instructions for potential hydrogen bonds HTAB N2 O1 EQIV $1 -x+1/2, -y+1/2, -z+1 HTAB N2 O4_$1 REM Highest difference peak 1.005, deepest hole -0.254, 1-sigma level 0.071 Q1 1 0.2744 0.3604 0.4120 11.00000 0.05 1.01 Q2 1 0.3096 0.2840 0.4868 11.00000 0.05 0.45 Q3 1 0.3229 0.6776 0.6632 11.00000 0.05 0.36 Q4 1 0.3633 0.4090 0.3760 11.00000 0.05 0.31 Q5 1 0.2798 0.0429 0.6844 11.00000 0.05 0.29 Q6 1 0.3730 0.1886 0.6125 11.00000 0.05 0.29 Q7 1 0.2301 0.3791 0.5910 11.00000 0.05 0.29 Q8 1 0.4617 0.1676 0.4762 11.00000 0.05 0.26 Q9 1 0.4432 0.4777 0.3215 11.00000 0.05 0.25 Q10 1 0.3824 0.2359 0.4831 11.00000 0.05 0.25 Q11 1 0.3032 0.4513 0.3477 11.00000 0.05 0.24 Q12 1 0.5155 0.3156 0.4177 11.00000 0.05 0.24 Q13 1 0.3817 0.0818 0.8194 11.00000 0.05 0.24 Q14 1 0.5303 0.3527 0.3783 11.00000 0.05 0.24 Q15 1 0.1983 0.3795 0.4997 11.00000 0.05 0.23 Q16 1 0.3209 0.1314 0.6956 11.00000 0.05 0.23 Q17 1 0.4951 0.4650 0.4037 11.00000 0.05 0.22 Q18 1 0.3916 0.3346 0.4438 11.00000 0.05 0.22 Q19 1 0.4768 0.3968 0.3530 11.00000 0.05 0.22 Q20 1 0.4282 0.5856 0.2786 11.00000 0.05 0.22 REM The information below was added by Olex2. REM REM R1 = 0.0369 for 1774 Fo > 4sig(Fo) and 0.0472 for all 11355 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.01, deepest hole -0.25 REM Mean Shift 0, Max Shift 0.000. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0472 REM R1_gt = 0.0369 REM wR_ref = 0.1018 REM GOOF = 1.112 REM Shift_max = 0.000 REM Shift_mean = 0 REM Reflections_all = 11355 REM Reflections_gt = 1774 REM Parameters = n/a REM Hole = -0.25 REM Peak = 1.01 REM Flack = n/a ; _olex2_exptl_crystal_mounting_method 'Thick plate shaped (Rhombus-like) colourless crystal mounted on a nylon cryoloop with paratone oil.' _olex2_submission_original_sample_id '7-azainzole zinc acetate dimer' _olex2_submission_special_instructions 'No special instructions were received' # start Validation Reply Form _vrf_PLAT353_Compound-15 ; PROBLEM: Long N-H (N0.87,N1.01A) N2 - H2N .. 1.08 Ang. RESPONSE: The N-H hydrogen atom was located and refined isotropically owing to good data quality and participation of this hydrogen in H-bonding. ; # end Validation Reply Form