# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2014 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rah203 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H20 N3 Ni O2 +,Cl -' _chemical_formula_sum 'C18 H20 Cl N3 Ni O2' _chemical_formula_weight 404.53 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' Ni Ni 0.3393 1.1124 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8103(12) _cell_length_b 14.5972(12) _cell_length_c 12.1913(14) _cell_angle_alpha 90 _cell_angle_beta 114.061(13) _cell_angle_gamma 90 _cell_volume 1756.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1632 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 26.68 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.530 _exptl_crystal_F_000 840 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_absorpt_coefficient_mu 1.273 _shelx_estimated_absorpt_T_min 0.883 _shelx_estimated_absorpt_T_max 0.939 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.890 _exptl_absorpt_correction_T_max 0.950 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 5795 _diffrn_reflns_av_unetI/netI 0.0940 _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.544 _diffrn_reflns_theta_max 25.025 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measured_fraction_theta_full 0.976 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_Laue_measured_fraction_full 0.976 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_point_group_measured_fraction_full 0.976 _reflns_number_total 3100 _reflns_number_gt 1890 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement SHELXL-2013 _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.1229P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 3100 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1282 _refine_ls_R_factor_gt 0.0856 _refine_ls_wR_factor_ref 0.2425 _refine_ls_wR_factor_gt 0.2020 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.22342(9) 0.25116(6) 0.09643(8) 0.0331(4) Uani 1 1 d . . . . . N1 N 0.3379(6) 0.2974(4) 0.2492(5) 0.0329(14) Uani 1 1 d . . . . . N2 N 0.2028(7) 0.3738(4) 0.0442(5) 0.0370(15) Uani 1 1 d . . . . . H2N H 0.133(7) 0.394(4) 0.045(5) 0.017(17) Uiso 1 1 d . . . . . N3 N 0.1210(7) 0.2210(4) -0.0611(5) 0.0388(15) Uani 1 1 d . . . . . O1 O 0.6361(7) 0.1521(4) 0.4673(5) 0.0464(15) Uani 1 1 d . . . . . H1O H 0.714(8) 0.140(6) 0.511(7) 0.05(3) Uiso 1 1 d . . . . . O2 O 0.2438(5) 0.1343(3) 0.1537(4) 0.0355(12) Uani 1 1 d . . . . . C1 C 0.6128(8) 0.2243(5) 0.5286(7) 0.0351(17) Uani 1 1 d . . . . . C2 C 0.6899(8) 0.2416(5) 0.6454(6) 0.0373(18) Uani 1 1 d . . . . . H2 H 0.7659 0.2040 0.6888 0.045 Uiso 1 1 calc R U . . . C3 C 0.6578(8) 0.3145(5) 0.7020(7) 0.0396(18) Uani 1 1 d . . . . . H3 H 0.7131 0.3276 0.7838 0.048 Uiso 1 1 calc R U . . . C4 C 0.5452(8) 0.3684(5) 0.6393(7) 0.0402(18) Uani 1 1 d . . . . . H4 H 0.5231 0.4183 0.6781 0.048 Uiso 1 1 calc R U . . . C5 C 0.4673(8) 0.3495(5) 0.5234(7) 0.0408(19) Uani 1 1 d . . . . . H5 H 0.3894 0.3860 0.4817 0.049 Uiso 1 1 calc R U . . . C6 C 0.4975(7) 0.2778(5) 0.4623(6) 0.0343(17) Uani 1 1 d . . . . . C7 C 0.4129(7) 0.2516(5) 0.3409(6) 0.0322(17) Uani 1 1 d . . . . . H7 H 0.4132 0.1877 0.3265 0.039 Uiso 1 1 calc R U . . . C8 C 0.3425(8) 0.3986(5) 0.2497(7) 0.0400(18) Uani 1 1 d . . . . . H8A H 0.4316 0.4206 0.3083 0.048 Uiso 1 1 calc R U . . . H8B H 0.2710 0.4241 0.2720 0.048 Uiso 1 1 calc R U . . . C9 C 0.3198(8) 0.4280(5) 0.1245(7) 0.0452(19) Uani 1 1 d . . . . . H9A H 0.2998 0.4944 0.1133 0.054 Uiso 1 1 calc R U . . . H9B H 0.4007 0.4150 0.1084 0.054 Uiso 1 1 calc R U . . . C10 C 0.1757(8) 0.3753(5) -0.0844(7) 0.0433(19) Uani 1 1 d . . . . . H10A H 0.2598 0.3632 -0.0958 0.052 Uiso 1 1 calc R U . . . H10B H 0.1392 0.4357 -0.1200 0.052 Uiso 1 1 calc R U . . . C11 C 0.0739(9) 0.3016(6) -0.1412(6) 0.048(2) Uani 1 1 d . . . . . H11A H -0.0169 0.3211 -0.1486 0.057 Uiso 1 1 calc R U . . . H11B H 0.0686 0.2869 -0.2223 0.057 Uiso 1 1 calc R U . . . C12 C 0.0912(7) 0.1399(5) -0.1041(7) 0.0384(18) Uani 1 1 d . . . . . H12 H 0.0359 0.1339 -0.1875 0.046 Uiso 1 1 calc R U . . . C13 C 0.1355(7) 0.0576(5) -0.0349(6) 0.0343(17) Uani 1 1 d . . . . . C14 C 0.1002(7) -0.0277(5) -0.0953(7) 0.0405(18) Uani 1 1 d . . . . . H14 H 0.0461 -0.0277 -0.1792 0.049 Uiso 1 1 calc R U . . . C15 C 0.1397(9) -0.1080(5) -0.0394(7) 0.045(2) Uani 1 1 d . . . . . H15 H 0.1147 -0.1643 -0.0818 0.054 Uiso 1 1 calc R U . . . C16 C 0.2205(8) -0.1057(6) 0.0858(7) 0.0418(19) Uani 1 1 d . . . . . H16 H 0.2528 -0.1616 0.1277 0.050 Uiso 1 1 calc R U . . . C17 C 0.2532(8) -0.0242(5) 0.1480(6) 0.0387(18) Uani 1 1 d . . . . . H17 H 0.3073 -0.0248 0.2320 0.046 Uiso 1 1 calc R U . . . C18 C 0.2078(7) 0.0594(5) 0.0891(6) 0.0353(17) Uani 1 1 d . . . . . Cl Cl -0.0720(2) 0.39384(14) 0.07592(17) 0.0449(5) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni 0.0354(6) 0.0321(6) 0.0317(6) 0.0008(4) 0.0136(5) 0.0019(4) N1 0.033(3) 0.028(3) 0.038(4) 0.006(3) 0.015(3) 0.001(3) N2 0.031(4) 0.039(4) 0.040(4) 0.002(3) 0.013(3) 0.010(3) N3 0.039(4) 0.033(3) 0.041(4) 0.004(3) 0.013(3) 0.009(3) O1 0.051(4) 0.046(3) 0.037(3) -0.002(2) 0.013(3) 0.012(3) O2 0.045(3) 0.025(3) 0.038(3) -0.003(2) 0.019(2) -0.004(2) C1 0.037(4) 0.030(4) 0.041(4) 0.002(3) 0.019(4) 0.005(3) C2 0.042(5) 0.040(5) 0.034(4) 0.006(3) 0.020(4) 0.008(4) C3 0.044(5) 0.041(4) 0.041(4) -0.007(3) 0.024(4) -0.008(4) C4 0.048(5) 0.033(4) 0.046(5) -0.016(3) 0.025(4) -0.006(4) C5 0.038(4) 0.035(4) 0.053(5) 0.003(3) 0.021(4) 0.005(4) C6 0.035(4) 0.029(4) 0.046(5) -0.003(3) 0.023(4) -0.006(3) C7 0.034(4) 0.036(4) 0.033(4) 0.000(3) 0.020(4) 0.000(3) C8 0.038(4) 0.034(4) 0.046(5) -0.001(3) 0.015(4) -0.001(4) C9 0.050(5) 0.034(4) 0.054(5) 0.007(4) 0.023(4) -0.001(4) C10 0.049(5) 0.040(5) 0.044(5) 0.006(4) 0.023(4) 0.008(4) C11 0.056(5) 0.048(5) 0.036(5) 0.004(4) 0.016(4) 0.019(4) C12 0.031(4) 0.045(5) 0.040(4) -0.003(3) 0.016(3) -0.001(4) C13 0.032(4) 0.035(4) 0.041(4) -0.003(3) 0.020(3) 0.001(3) C14 0.033(4) 0.050(5) 0.043(4) -0.009(4) 0.020(4) -0.002(4) C15 0.070(6) 0.028(4) 0.045(5) -0.015(3) 0.033(4) -0.008(4) C16 0.044(5) 0.044(5) 0.039(4) 0.005(3) 0.019(4) 0.007(4) C17 0.044(5) 0.040(5) 0.033(4) -0.002(3) 0.017(3) -0.009(4) C18 0.038(4) 0.035(4) 0.041(4) -0.004(3) 0.025(4) -0.006(3) Cl 0.0434(11) 0.0484(12) 0.0477(12) 0.0042(9) 0.0236(9) 0.0008(9) _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 Ni N1 1.891(6) . ? Ni N2 1.883(6) . ? Ni N3 1.837(6) . ? Ni O2 1.823(5) . ? N1 C7 1.271(9) . ? N1 C8 1.478(9) . ? N2 H2N 0.81(6) . ? N2 C9 1.474(10) . ? N2 C10 1.473(9) . ? N3 C11 1.480(10) . ? N3 C12 1.282(9) . ? O1 H1O 0.82(8) . ? O1 C1 1.374(9) . ? O2 C18 1.311(8) . ? C1 C2 1.348(10) . ? C1 C6 1.412(10) . ? C2 H2 0.950 . ? C2 C3 1.387(10) . ? C3 H3 0.950 . ? C3 C4 1.388(10) . ? C4 H4 0.950 . ? C4 C5 1.346(10) . ? C5 H5 0.950 . ? C5 C6 1.397(10) . ? C6 C7 1.439(10) . ? C7 H7 0.950 . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C8 C9 1.507(10) . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C10 C11 1.493(11) . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 H12 0.950 . ? C12 C13 1.433(10) . ? C13 C14 1.417(10) . ? C13 C18 1.390(10) . ? C14 H14 0.950 . ? C14 C15 1.336(10) . ? C15 H15 0.950 . ? C15 C16 1.416(11) . ? C16 H16 0.950 . ? C16 C17 1.377(10) . ? C17 H17 0.950 . ? C17 C18 1.399(10) . ? 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 N1 Ni N2 86.2(3) . . ? N1 Ni N3 171.4(3) . . ? N1 Ni O2 91.6(2) . . ? N2 Ni N3 86.4(3) . . ? N2 Ni O2 177.3(2) . . ? N3 Ni O2 96.0(2) . . ? Ni N1 C7 127.3(5) . . ? Ni N1 C8 111.6(4) . . ? C7 N1 C8 120.9(6) . . ? Ni N2 H2N 109(4) . . ? Ni N2 C9 109.6(5) . . ? Ni N2 C10 108.6(5) . . ? H2N N2 C9 110(5) . . ? H2N N2 C10 103(4) . . ? C9 N2 C10 116.3(6) . . ? Ni N3 C11 113.5(5) . . ? Ni N3 C12 126.3(5) . . ? C11 N3 C12 120.2(7) . . ? H1O O1 C1 101(6) . . ? Ni O2 C18 126.2(5) . . ? O1 C1 C2 123.1(7) . . ? O1 C1 C6 115.3(7) . . ? C2 C1 C6 121.5(7) . . ? C1 C2 H2 120.1 . . ? C1 C2 C3 119.8(7) . . ? H2 C2 C3 120.1 . . ? C2 C3 H3 119.9 . . ? C2 C3 C4 120.1(7) . . ? H3 C3 C4 119.9 . . ? C3 C4 H4 120.2 . . ? C3 C4 C5 119.6(7) . . ? H4 C4 C5 120.2 . . ? C4 C5 H5 119.0 . . ? C4 C5 C6 122.0(7) . . ? H5 C5 C6 119.0 . . ? C1 C6 C5 116.9(7) . . ? C1 C6 C7 118.9(6) . . ? C5 C6 C7 123.9(7) . . ? N1 C7 C6 132.5(7) . . ? N1 C7 H7 113.8 . . ? C6 C7 H7 113.8 . . ? N1 C8 H8A 110.4 . . ? N1 C8 H8B 110.4 . . ? N1 C8 C9 106.8(6) . . ? H8A C8 H8B 108.6 . . ? H8A C8 C9 110.4 . . ? H8B C8 C9 110.4 . . ? N2 C9 C8 105.1(6) . . ? N2 C9 H9A 110.7 . . ? N2 C9 H9B 110.7 . . ? C8 C9 H9A 110.7 . . ? C8 C9 H9B 110.7 . . ? H9A C9 H9B 108.8 . . ? N2 C10 H10A 110.6 . . ? N2 C10 H10B 110.6 . . ? N2 C10 C11 105.8(6) . . ? H10A C10 H10B 108.7 . . ? H10A C10 C11 110.6 . . ? H10B C10 C11 110.6 . . ? N3 C11 C10 106.0(6) . . ? N3 C11 H11A 110.5 . . ? N3 C11 H11B 110.5 . . ? C10 C11 H11A 110.5 . . ? C10 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? N3 C12 H12 117.8 . . ? N3 C12 C13 124.4(7) . . ? H12 C12 C13 117.8 . . ? C12 C13 C14 118.4(7) . . ? C12 C13 C18 122.0(7) . . ? C14 C13 C18 119.6(7) . . ? C13 C14 H14 118.5 . . ? C13 C14 C15 123.0(7) . . ? H14 C14 C15 118.5 . . ? C14 C15 H15 121.4 . . ? C14 C15 C16 117.2(7) . . ? H15 C15 C16 121.4 . . ? C15 C16 H16 119.3 . . ? C15 C16 C17 121.4(7) . . ? H16 C16 C17 119.3 . . ? C16 C17 H17 119.6 . . ? C16 C17 C18 120.8(7) . . ? H17 C17 C18 119.6 . . ? O2 C18 C13 124.5(7) . . ? O2 C18 C17 117.6(6) . . ? C13 C18 C17 117.8(7) . . ? 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 N2 Ni N1 C7 -170.4(6) . . . . ? N2 Ni N1 C8 4.0(5) . . . . ? O2 Ni N1 C7 11.1(6) . . . . ? O2 Ni N1 C8 -174.5(5) . . . . ? N1 Ni N2 C9 23.5(5) . . . . ? N1 Ni N2 C10 151.4(5) . . . . ? N3 Ni N2 C9 -152.2(5) . . . . ? N3 Ni N2 C10 -24.2(5) . . . . ? N2 Ni N3 C11 -2.1(5) . . . . ? N2 Ni N3 C12 176.8(7) . . . . ? O2 Ni N3 C11 176.5(5) . . . . ? O2 Ni N3 C12 -4.5(7) . . . . ? N1 Ni O2 C18 -167.6(6) . . . . ? N3 Ni O2 C18 8.2(6) . . . . ? O1 C1 C2 C3 -178.3(7) . . . . ? C6 C1 C2 C3 -1.3(11) . . . . ? C1 C2 C3 C4 1.3(11) . . . . ? C2 C3 C4 C5 0.0(11) . . . . ? C3 C4 C5 C6 -1.2(11) . . . . ? C4 C5 C6 C1 1.2(11) . . . . ? C4 C5 C6 C7 176.0(7) . . . . ? O1 C1 C6 C5 177.3(6) . . . . ? O1 C1 C6 C7 2.2(10) . . . . ? C2 C1 C6 C5 0.1(11) . . . . ? C2 C1 C6 C7 -175.0(7) . . . . ? Ni N1 C7 C6 -176.0(6) . . . . ? C8 N1 C7 C6 10.1(12) . . . . ? C1 C6 C7 N1 -151.1(8) . . . . ? C5 C6 C7 N1 34.2(12) . . . . ? Ni N1 C8 C9 -29.6(7) . . . . ? C7 N1 C8 C9 145.2(7) . . . . ? Ni N2 C9 C8 -44.5(7) . . . . ? C10 N2 C9 C8 -168.1(6) . . . . ? N1 C8 C9 N2 46.8(8) . . . . ? Ni N2 C10 C11 44.3(7) . . . . ? C9 N2 C10 C11 168.4(6) . . . . ? Ni N3 C11 C10 27.2(7) . . . . ? C12 N3 C11 C10 -151.8(7) . . . . ? N2 C10 C11 N3 -44.9(7) . . . . ? Ni N3 C12 C13 -1.0(11) . . . . ? C11 N3 C12 C13 177.9(7) . . . . ? N3 C12 C13 C14 -177.0(7) . . . . ? N3 C12 C13 C18 5.1(11) . . . . ? C12 C13 C14 C15 178.2(7) . . . . ? C18 C13 C14 C15 -3.9(11) . . . . ? C13 C14 C15 C16 -0.1(11) . . . . ? C14 C15 C16 C17 2.1(11) . . . . ? C15 C16 C17 C18 -0.2(11) . . . . ? Ni O2 C18 C13 -6.5(10) . . . . ? Ni O2 C18 C17 168.9(5) . . . . ? C12 C13 C18 O2 -1.1(11) . . . . ? C12 C13 C18 C17 -176.5(6) . . . . ? C14 C13 C18 O2 -179.0(6) . . . . ? C14 C13 C18 C17 5.6(10) . . . . ? C16 C17 C18 O2 -179.4(6) . . . . ? C16 C17 C18 C13 -3.7(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N Cl 0.81(6) 2.40(7) 3.162(7) 157(6) . O1 H1O Cl 0.82(8) 2.17(8) 2.958(7) 163(7) 4_666 _refine_diff_density_max 2.098 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.223 _shelxl_version_number 2013-2 _shelx_res_file ; TITL rah203 in P2(1)/c CELL 0.71073 10.8103 14.5972 12.1913 90.000 114.061 90.000 ZERR 4.00 0.0012 0.0012 0.0014 0.000 0.013 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H O Ni Cl N UNIT 72 80 8 4 4 12 SIZE 0.1 0.1 0.05 TEMP -123 L.S. 8 ACTA BOND $H CONF FMAP 2 PLAN 20 HTAB N2 Cl EQIV $1 x+1, -y+1/2, z+1/2 HTAB O1 Cl_$1 rem EXTI 0.000000 WGHT 0.122900 FVAR 0.14598 NI 4 0.223420 0.251161 0.096434 11.00000 0.03542 0.03214 = 0.03175 0.00077 0.01363 0.00185 N1 6 0.337858 0.297397 0.249210 11.00000 0.03334 0.02783 = 0.03826 0.00625 0.01542 0.00089 N2 6 0.202804 0.373848 0.044247 11.00000 0.03085 0.03870 = 0.03973 0.00224 0.01277 0.01029 H2N 2 0.133377 0.394240 0.044949 11.00000 0.01662 N3 6 0.121028 0.221033 -0.061136 11.00000 0.03936 0.03271 = 0.04102 0.00387 0.01298 0.00883 O1 3 0.636135 0.152055 0.467324 11.00000 0.05138 0.04633 = 0.03654 -0.00211 0.01301 0.01242 H1O 2 0.714430 0.139699 0.511140 11.00000 0.04541 O2 3 0.243797 0.134278 0.153711 11.00000 0.04513 0.02534 = 0.03811 -0.00298 0.01907 -0.00351 C1 1 0.612816 0.224331 0.528624 11.00000 0.03671 0.03032 = 0.04112 0.00247 0.01870 0.00520 C2 1 0.689875 0.241618 0.645377 11.00000 0.04229 0.04020 = 0.03426 0.00642 0.02043 0.00838 AFIX 43 H2 2 0.765902 0.203987 0.688763 11.00000 -1.20000 AFIX 0 C3 1 0.657821 0.314508 0.701958 11.00000 0.04360 0.04092 = 0.04071 -0.00729 0.02379 -0.00781 AFIX 43 H3 2 0.713093 0.327601 0.783776 11.00000 -1.20000 AFIX 0 C4 1 0.545175 0.368372 0.639321 11.00000 0.04774 0.03302 = 0.04577 -0.01631 0.02507 -0.00633 AFIX 43 H4 2 0.523128 0.418287 0.678058 11.00000 -1.20000 AFIX 0 C5 1 0.467304 0.349505 0.523358 11.00000 0.03763 0.03515 = 0.05252 0.00272 0.02143 0.00490 AFIX 43 H5 2 0.389412 0.386039 0.481736 11.00000 -1.20000 AFIX 0 C6 1 0.497530 0.277835 0.462334 11.00000 0.03463 0.02858 = 0.04575 -0.00330 0.02256 -0.00605 C7 1 0.412929 0.251603 0.340934 11.00000 0.03391 0.03629 = 0.03309 0.00042 0.02046 -0.00022 AFIX 43 H7 2 0.413224 0.187661 0.326525 11.00000 -1.20000 AFIX 0 C8 1 0.342479 0.398619 0.249701 11.00000 0.03789 0.03352 = 0.04627 -0.00079 0.01490 -0.00098 AFIX 23 H8A 2 0.431582 0.420581 0.308332 11.00000 -1.20000 H8B 2 0.271003 0.424109 0.271962 11.00000 -1.20000 AFIX 0 C9 1 0.319786 0.428023 0.124463 11.00000 0.04993 0.03367 = 0.05393 0.00722 0.02301 -0.00115 AFIX 23 H9A 2 0.299786 0.494403 0.113340 11.00000 -1.20000 H9B 2 0.400725 0.414970 0.108390 11.00000 -1.20000 AFIX 0 C10 1 0.175676 0.375339 -0.084389 11.00000 0.04871 0.04047 = 0.04433 0.00613 0.02281 0.00838 AFIX 23 H10A 2 0.259759 0.363233 -0.095816 11.00000 -1.20000 H10B 2 0.139218 0.435667 -0.120050 11.00000 -1.20000 AFIX 0 C11 1 0.073859 0.301591 -0.141239 11.00000 0.05586 0.04803 = 0.03622 0.00398 0.01630 0.01932 AFIX 23 H11A 2 -0.016917 0.321100 -0.148630 11.00000 -1.20000 H11B 2 0.068646 0.286908 -0.222291 11.00000 -1.20000 AFIX 0 C12 1 0.091152 0.139870 -0.104093 11.00000 0.03142 0.04517 = 0.04042 -0.00252 0.01638 -0.00112 AFIX 43 H12 2 0.035853 0.133857 -0.187454 11.00000 -1.20000 AFIX 0 C13 1 0.135533 0.057616 -0.034869 11.00000 0.03225 0.03472 = 0.04057 -0.00300 0.01966 0.00056 C14 1 0.100240 -0.027692 -0.095250 11.00000 0.03327 0.05023 = 0.04253 -0.00857 0.01996 -0.00246 AFIX 43 H14 2 0.046062 -0.027737 -0.179241 11.00000 -1.20000 AFIX 0 C15 1 0.139733 -0.108033 -0.039365 11.00000 0.07023 0.02785 = 0.04549 -0.01491 0.03276 -0.00766 AFIX 43 H15 2 0.114699 -0.164350 -0.081799 11.00000 -1.20000 AFIX 0 C16 1 0.220468 -0.105711 0.085770 11.00000 0.04353 0.04404 = 0.03940 0.00491 0.01863 0.00674 AFIX 43 H16 2 0.252758 -0.161566 0.127709 11.00000 -1.20000 AFIX 0 C17 1 0.253206 -0.024225 0.148012 11.00000 0.04407 0.03996 = 0.03284 -0.00219 0.01655 -0.00910 AFIX 43 H17 2 0.307320 -0.024770 0.232012 11.00000 -1.20000 AFIX 0 C18 1 0.207766 0.059366 0.089085 11.00000 0.03845 0.03490 = 0.04083 -0.00404 0.02476 -0.00591 CL 5 -0.072047 0.393840 0.075921 11.00000 0.04336 0.04838 = 0.04772 0.00418 0.02356 0.00078 HKLF 4 REM rah203 in P2(1)/c REM R1 = 0.0856 for 1890 Fo > 4sig(Fo) and 0.1282 for all 3100 data REM 234 parameters refined using 0 restraints END WGHT 0.1229 0.0000 REM Highest difference peak 2.098, deepest hole -0.844, 1-sigma level 0.223 Q1 1 0.2971 0.2530 0.1768 11.00000 0.05 2.10 Q2 1 0.1586 0.2449 0.0167 11.00000 0.05 1.88 Q3 1 0.2223 0.1770 0.0943 11.00000 0.05 1.47 Q4 1 0.2308 0.3224 0.1059 11.00000 0.05 1.40 Q5 1 0.3601 0.2319 0.2624 11.00000 0.05 1.16 Q6 1 0.1000 0.2598 -0.0774 11.00000 0.05 0.91 Q7 1 -0.1394 0.3793 -0.0008 11.00000 0.05 0.77 Q8 1 0.0593 0.2481 -0.1364 11.00000 0.05 0.73 Q9 1 0.1396 0.1249 -0.0233 11.00000 0.05 0.68 Q10 1 -0.0817 0.3222 0.0630 11.00000 0.05 0.64 Q11 1 -0.0669 0.4654 0.0890 11.00000 0.05 0.62 Q12 1 0.0018 0.3977 0.1550 11.00000 0.05 0.60 Q13 1 0.3246 0.1169 0.2315 11.00000 0.05 0.59 Q14 1 0.5620 0.2507 0.4997 11.00000 0.05 0.57 Q15 1 0.1412 0.3760 -0.0286 11.00000 0.05 0.56 Q16 1 0.1948 -0.0038 0.0812 11.00000 0.05 0.54 Q17 1 0.2476 0.4443 0.0901 11.00000 0.05 0.51 Q18 1 -0.0072 0.2674 -0.2228 11.00000 0.05 0.47 Q19 1 0.5983 0.3895 0.6875 11.00000 0.05 0.46 Q20 1 0.4214 0.3203 0.3352 11.00000 0.05 0.46 ; _shelx_res_checksum 79089 _shelx_hkl_file ; 0 0 -2 657.21 8.21 0 0 -3 -0.01 0.38 0 0 -4 239.07 7.29 0 0 -5 -0.28 0.65 0 0 -6 155.46 7.24 0 0 -7 0.23 0.57 0 0 -8 1.14 0.93 0 0 -9 -0.39 0.71 0 0 -10 0.01 0.70 0 0 -11 0.62 0.89 0 0 -12 12.44 2.99 0 0 -13 -0.71 1.06 0 1 -2 273.52 5.23 0 -1 -2 327.42 6.06 0 -1 3 28.39 1.22 0 1 -3 35.34 2.31 0 -1 -3 31.15 2.49 0 -1 -4 36.31 2.85 0 1 -4 37.13 2.79 0 -1 -5 6.76 1.53 0 1 -5 5.53 1.28 0 1 -6 14.21 2.23 0 -1 -6 13.55 2.35 0 -1 -7 8.42 1.82 0 1 -7 6.63 1.37 0 1 -8 41.33 4.22 0 -1 -8 41.91 4.34 0 1 -9 -0.73 0.74 0 -1 -9 -0.21 0.73 0 1 -10 2.25 1.27 0 -1 -10 1.60 0.79 0 1 -11 -1.09 0.86 0 -1 -11 0.40 1.30 0 -1 -12 9.96 2.78 0 1 -12 10.62 2.74 0 -1 -13 -1.32 1.03 0 1 -13 -1.65 1.37 0 2 0 903.88 8.69 0 2 1 8.70 1.15 0 -2 -1 13.08 1.14 0 2 -1 6.99 0.87 0 -2 2 11.03 0.85 0 2 -2 10.11 0.87 0 -2 -2 9.81 1.23 0 -2 -3 10.81 1.50 0 -2 3 14.22 1.01 0 2 -3 11.03 1.21 0 -2 -4 8.83 1.43 0 2 -4 10.90 1.55 0 -2 4 9.54 0.88 0 2 -5 84.38 4.69 0 -2 -5 78.80 4.83 0 -2 5 70.72 2.40 0 2 -6 11.38 1.84 0 -2 -6 10.70 2.01 0 2 -7 14.89 2.33 0 -2 -7 17.81 2.67 0 -2 -8 1.26 0.88 0 2 -8 1.72 1.12 0 2 -9 3.08 1.25 0 -2 -9 4.06 1.77 0 -2 -10 3.97 1.51 0 2 -10 7.46 1.95 0 2 -11 2.59 1.35 0 -2 -11 4.25 1.60 0 2 -12 2.49 1.48 0 -2 -12 6.32 2.77 0 -2 -13 -0.06 0.63 0 2 -13 -0.21 0.47 0 3 0 0.07 0.30 0 -3 0 0.37 0.18 0 -3 -1 49.62 2.22 0 3 1 43.42 2.80 0 3 -2 0.44 0.17 0 -3 -2 0.44 0.37 0 3 2 0.26 0.27 0 -3 2 -0.39 0.41 0 -3 -3 10.29 1.50 0 -3 3 12.48 1.11 0 3 -3 10.38 1.10 0 -3 4 1.20 0.40 0 -3 -4 1.39 0.62 0 3 -4 0.82 0.32 0 -3 5 4.64 0.68 0 3 -5 3.86 0.94 0 -3 -5 4.99 1.30 0 3 -6 23.90 2.67 0 -3 6 18.90 1.33 0 -3 -6 26.06 3.18 0 -3 -7 3.87 1.32 0 3 -7 2.44 0.73 0 -3 -8 50.96 4.97 0 3 -8 48.21 4.41 0 3 8 49.09 4.17 0 -3 -9 -0.74 0.83 0 3 -9 0.33 0.89 0 -3 -10 1.08 0.76 0 3 -10 3.03 1.28 0 -3 -11 -1.94 1.45 0 3 -11 0.83 0.82 0 3 -12 23.72 4.21 0 -3 -12 20.88 3.70 0 -3 -13 0.39 0.82 0 -4 0 14.04 0.96 0 4 0 18.70 1.76 0 4 1 55.40 3.10 0 -4 -1 46.35 2.46 0 4 -2 24.99 2.01 0 4 2 27.97 2.49 0 -4 -2 29.08 2.29 0 4 3 0.64 0.38 0 -4 3 0.56 0.50 0 -4 -3 1.08 0.59 0 4 -3 1.53 0.41 0 4 4 57.50 3.78 0 -4 -4 55.17 3.86 0 4 -4 55.78 2.93 0 -4 4 54.43 2.71 0 4 -5 6.63 1.18 0 -4 5 7.15 0.97 0 -4 -5 6.75 1.55 0 4 5 7.20 1.45 0 4 -6 6.32 1.25 0 4 6 6.98 1.46 0 -4 -6 5.35 1.56 0 -4 -7 3.52 0.92 0 4 -7 3.92 1.07 0 4 7 4.43 1.23 0 4 -8 7.40 1.84 0 -4 -8 6.61 1.97 0 4 8 6.88 1.69 0 -4 -9 1.24 0.77 0 4 -9 1.69 1.14 0 4 -10 17.74 3.12 0 -4 -10 18.44 3.42 0 -4 -11 -1.62 1.33 0 4 -11 -0.60 0.97 0 -4 -12 2.93 1.49 0 -5 0 0.22 0.26 0 5 0 -0.47 0.55 0 -5 -1 30.62 2.02 0 5 1 35.09 2.82 0 5 -1 22.37 2.33 0 -5 -2 127.66 4.74 0 5 2 133.74 5.68 0 -5 -3 7.67 1.40 0 5 3 6.98 1.50 0 -5 3 8.36 1.39 0 5 -3 7.01 0.80 0 -5 -4 77.24 4.82 0 5 -4 77.65 3.37 0 5 4 78.33 4.88 0 -5 4 81.70 3.87 0 -5 -5 10.18 1.97 0 -5 5 12.32 1.41 0 5 5 13.40 2.14 0 5 -5 13.20 1.65 0 5 6 47.70 4.22 0 -5 -6 59.34 5.05 0 5 -6 54.50 3.88 0 5 -7 34.05 3.36 0 -5 -7 34.47 3.98 0 5 7 29.25 3.42 0 -5 -8 111.93 7.65 0 5 -8 129.10 7.27 0 5 8 114.27 6.89 0 5 -9 1.76 1.14 0 -5 -9 1.28 1.14 0 -5 -10 0.56 0.49 0 -5 -11 -0.19 0.49 0 -5 -12 22.89 4.03 0 -6 0 367.89 5.95 0 6 0 411.78 9.91 0 6 -1 3.83 1.04 0 6 1 4.08 1.07 0 -6 -1 3.20 0.74 0 6 2 58.86 4.31 0 6 -2 51.21 3.64 0 -6 -2 59.83 3.48 0 6 -3 0.22 0.16 0 6 3 0.83 0.79 0 -6 -3 1.33 0.59 0 -6 3 1.18 0.64 0 6 -4 68.71 3.03 0 -6 -4 69.18 4.60 0 -6 4 77.24 4.42 0 6 4 63.73 4.54 0 -6 -5 0.26 0.48 0 -6 5 1.34 0.59 0 6 -5 1.07 0.60 0 6 5 0.32 0.52 0 6 -6 109.10 5.35 0 -6 -6 116.15 7.05 0 6 6 100.50 6.23 0 6 -7 17.63 2.46 0 6 7 15.03 2.55 0 -6 -7 14.92 2.73 0 6 8 0.51 0.66 0 -6 -8 0.40 0.92 0 -6 -9 33.54 4.44 0 -6 -10 8.17 2.15 0 -6 -11 -0.90 1.02 0 -6 -12 9.07 2.65 0 7 0 -0.76 0.71 0 -7 0 0.63 0.30 0 -7 -1 -0.17 0.28 0 7 -1 0.27 0.46 0 7 1 -0.51 0.42 0 -7 1 0.29 0.15 0 -7 -2 221.83 7.09 0 7 -2 197.02 8.15 0 -7 -3 88.81 4.99 0 7 3 98.00 5.90 0 -7 3 96.42 6.10 0 7 4 70.62 5.17 0 -7 -4 67.81 4.74 0 -7 4 84.36 5.21 0 -7 -5 2.21 1.11 0 7 5 1.41 0.80 0 7 -5 2.11 0.58 0 -7 5 2.70 0.93 0 -7 -6 7.62 1.84 0 7 6 7.61 2.00 0 7 7 32.97 3.79 0 -7 -7 26.83 3.78 0 -7 -8 3.20 1.48 0 7 8 3.73 1.42 0 -7 -9 3.48 1.68 0 7 9 3.23 1.29 0 -7 -10 -0.18 1.02 0 -7 -11 -0.04 0.51 0 -7 -12 2.58 1.40 0 8 0 397.68 11.40 0 -8 0 403.91 7.57 0 -8 -1 72.88 3.76 0 8 -1 59.90 4.57 0 8 1 71.57 4.81 0 8 -2 80.18 5.53 0 -8 -2 86.02 4.62 0 8 2 93.03 5.58 0 8 3 53.49 4.46 0 -8 -3 50.55 3.86 0 -8 3 57.81 5.19 0 8 4 105.70 6.45 0 -8 4 105.20 6.64 0 -8 5 48.57 4.24 0 -8 -5 46.29 4.43 0 8 5 40.80 4.28 0 -8 -6 24.90 3.45 0 8 6 21.08 3.13 0 8 7 0.00 0.51 0 -8 -7 0.07 0.76 0 -8 -8 -0.05 0.45 0 8 8 -0.22 0.80 0 8 9 0.78 1.00 0 -8 -9 0.07 0.67 0 -8 -10 5.13 1.86 0 -8 -11 1.03 0.90 0 9 0 -0.41 0.67 0 -9 0 0.32 0.29 0 9 -1 9.71 1.98 0 9 1 12.43 2.08 0 -9 -1 13.13 1.74 0 9 -2 61.69 5.17 0 9 2 76.43 5.32 0 -9 -2 72.71 4.43 0 -9 -3 -0.37 0.77 0 -9 3 -0.03 0.80 0 9 3 0.41 0.71 0 9 4 14.55 2.40 0 -9 -4 14.25 2.31 0 -9 4 14.63 2.97 0 9 5 1.89 1.07 0 -9 -5 1.88 0.98 0 9 6 12.92 2.46 0 -9 -6 13.10 2.36 0 -9 -7 4.80 1.43 0 9 7 5.46 1.67 0 9 8 4.75 1.84 0 -9 -8 5.71 1.71 0 -9 -9 -0.23 0.44 0 9 9 -0.21 0.78 0 -9 -10 -1.95 1.35 0 -9 -11 2.99 1.23 0 10 0 44.53 4.25 0 10 -1 2.03 1.15 0 10 1 2.37 1.05 0 10 2 21.69 2.95 0 10 -2 23.49 3.41 0 -10 -2 23.63 2.67 0 10 3 6.77 1.71 0 -10 -3 5.84 1.36 0 -10 3 6.05 2.15 0 -10 4 59.03 5.97 0 -10 -4 45.65 4.27 0 10 4 45.71 4.55 0 10 5 14.72 2.96 0 -10 -5 19.11 3.05 0 10 6 0.40 0.48 0 -10 -6 0.96 0.44 0 10 7 3.74 1.43 0 -10 -7 2.06 1.21 0 10 8 1.31 1.18 0 -10 -8 3.99 1.58 0 10 9 1.19 1.12 0 -10 -9 -1.20 1.30 0 -10 -10 11.11 2.71 0 11 0 -2.47 1.43 0 11 1 5.60 1.50 0 11 -1 6.99 1.72 0 11 -2 34.05 4.35 0 11 2 30.60 3.71 0 11 3 2.81 1.22 0 -11 3 3.82 1.81 0 11 4 1.35 1.12 0 -11 -4 1.45 0.53 0 -11 4 0.36 1.10 0 11 5 4.26 1.66 0 -11 -5 3.61 1.57 0 -11 -6 22.50 3.51 0 11 6 21.67 3.35 0 -11 -7 1.95 1.21 0 11 7 -0.32 0.55 0 11 8 13.39 2.80 0 -11 -8 14.25 2.90 0 -11 -9 0.15 0.54 0 11 9 2.83 1.53 0 -11 -10 -0.49 0.78 0 12 0 2.45 1.22 0 12 1 1.42 0.76 0 12 -1 0.86 0.57 0 12 -2 -0.49 1.06 0 12 2 -2.27 1.30 0 12 3 0.56 0.56 0 -12 3 -0.49 1.28 0 12 4 14.63 2.79 0 -12 4 22.17 4.17 0 12 5 0.14 0.41 0 12 6 2.98 1.47 0 -12 -6 7.67 2.18 0 -12 -7 1.64 1.09 0 12 7 2.52 1.49 0 -12 -8 1.88 1.09 0 12 8 1.71 1.16 0 -12 -9 -0.09 0.91 0 12 9 0.33 0.82 0 13 0 -0.20 0.55 0 13 1 -1.88 1.00 0 13 -1 -1.36 0.96 0 13 -2 28.75 4.52 0 13 2 21.74 3.59 0 -13 3 1.31 1.03 0 13 3 0.67 0.82 0 13 4 34.86 4.54 0 13 5 0.32 0.68 0 13 6 -0.51 0.65 0 13 7 2.24 1.31 0 -13 -8 20.16 3.54 0 13 8 22.54 4.01 0 14 0 27.97 4.54 0 14 -1 9.76 2.78 0 14 1 4.70 1.75 0 14 -2 0.07 0.79 0 14 2 -0.41 0.76 0 -14 2 0.69 0.81 0 -14 3 5.18 2.13 0 14 3 3.15 1.58 0 14 4 11.53 2.75 0 14 5 2.22 1.35 0 14 6 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2.04 10 5 -9 6.09 2.16 10 -5 -8 0.73 0.92 10 -5 -8 2.77 1.67 10 -5 -7 -1.30 1.13 10 -5 -7 -0.96 0.68 10 5 -6 3.78 1.58 10 -5 -6 5.10 1.81 10 -5 -6 2.27 1.80 10 -5 -5 1.15 0.96 10 5 -5 0.54 0.47 10 -5 -4 9.16 2.68 10 -5 -3 4.36 1.69 10 -5 -2 -0.47 0.46 10 -5 -1 0.61 0.84 10 -5 0 20.75 3.69 10 -5 1 2.29 1.29 10 -5 2 12.29 2.81 10 -6 -11 -0.79 1.03 10 6 -11 -0.04 0.76 10 -6 -10 0.18 0.58 10 -6 -10 1.16 1.16 10 6 -10 1.90 1.32 10 -6 -9 1.01 0.75 10 -6 -9 2.56 1.58 10 -6 -8 22.82 4.41 10 -6 -8 23.46 4.18 10 -6 -7 2.43 1.51 10 -6 -7 -1.23 1.23 10 -6 -6 -0.56 1.08 10 -6 -6 0.31 0.77 10 -6 -5 -1.24 1.04 10 -6 -4 11.94 2.90 10 -6 -3 0.10 0.52 10 -6 -2 18.49 3.58 10 -6 -1 1.33 0.99 10 -6 0 1.82 0.86 10 -6 1 9.84 2.63 10 -6 2 8.82 2.45 10 -7 -11 0.79 0.92 10 7 -11 -1.20 1.03 10 -7 -10 4.05 1.77 10 -7 -10 3.65 2.12 10 -7 -9 4.50 2.17 10 -7 -9 4.94 2.21 10 -7 -8 -0.92 1.13 10 -7 -8 2.41 1.79 10 -7 -7 -0.54 0.74 10 -7 -7 -0.18 1.01 10 -7 -6 13.83 3.53 10 -7 -6 14.52 3.24 10 -7 -5 -0.18 1.19 10 -7 -4 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0.42 11 -8 -4 13.51 3.67 11 -8 -3 -0.80 1.00 11 -8 -2 0.62 1.01 11 -9 -5 1.08 1.19 12 0 -10 2.52 1.58 12 0 -9 -0.09 0.96 12 0 -8 23.89 4.12 12 0 -7 -1.07 0.98 12 0 -6 13.66 3.27 12 0 -5 -0.90 0.97 12 0 -4 -0.22 0.58 12 0 -3 -0.65 0.69 12 0 -2 15.78 3.65 12 0 -1 1.91 1.63 12 -1 -10 3.59 1.57 12 1 -10 2.88 1.59 12 -1 -9 0.54 0.79 12 -1 -9 1.44 1.19 12 -1 -8 -0.84 1.11 12 1 -8 1.46 1.25 12 -1 -7 2.67 1.53 12 1 -7 2.45 1.63 12 -1 -6 -0.72 0.88 12 1 -6 0.54 1.03 12 -1 -5 1.01 1.34 12 1 -5 -0.16 0.59 12 -1 -4 6.44 2.19 12 1 -4 5.70 2.01 12 1 -3 4.43 1.96 12 -1 -3 2.22 1.75 12 1 -2 2.83 1.69 12 -1 -2 1.92 1.52 12 1 -1 2.59 1.48 12 -1 -1 3.91 1.86 12 -2 -10 1.85 1.19 12 2 -10 -2.58 1.41 12 -2 -9 1.92 1.22 12 -2 -9 0.24 0.64 12 2 -8 9.32 2.86 12 -2 -8 6.61 2.29 12 2 -7 -0.19 0.98 12 -2 -7 -0.49 0.40 12 -2 -6 3.27 1.41 12 2 -6 3.52 1.84 12 -2 -5 2.81 1.52 12 2 -5 0.13 0.83 12 -2 -4 -0.25 0.55 12 2 -4 1.31 1.13 12 -2 -3 1.65 1.01 12 2 -3 0.65 1.35 12 -2 -2 6.66 2.25 12 2 -2 10.20 3.13 12 2 -1 -0.05 1.27 12 -2 -1 -0.92 0.79 12 -3 -9 -0.52 0.69 12 -3 -9 0.03 0.63 12 -3 -8 0.31 0.64 12 -3 -8 0.95 1.08 12 3 -7 2.01 1.53 12 -3 -7 2.41 1.49 12 3 -6 14.70 3.66 12 -3 -6 14.24 3.20 12 -3 -5 0.00 1.16 12 3 -5 1.32 1.32 12 -3 -4 9.08 2.61 12 3 -4 9.95 2.96 12 -3 -3 -0.12 0.39 12 3 -3 1.30 1.20 12 -3 -2 2.09 1.58 12 3 -2 1.35 1.30 12 -4 -9 1.70 1.17 12 -4 -9 1.74 0.82 12 -4 -8 17.01 4.23 12 -4 -8 18.00 3.70 12 -4 -7 0.31 0.92 12 4 -7 -1.03 1.00 12 4 -6 8.67 2.75 12 -4 -6 10.99 2.92 12 4 -5 -0.21 0.60 12 -4 -5 -0.08 0.87 12 4 -4 5.31 2.22 12 -4 -4 2.00 1.13 12 4 -3 -1.25 1.76 12 -4 -3 0.40 0.87 12 -4 -2 7.23 2.46 12 4 -2 8.41 2.89 12 -5 -8 -0.14 0.73 12 -5 -8 1.14 1.19 12 -5 -7 3.99 1.81 12 -5 -6 4.99 1.87 12 -5 -5 1.32 1.07 12 -5 -4 5.11 2.09 12 -5 -3 -1.31 1.36 12 -6 -6 4.60 2.03 12 -6 -5 -0.95 1.21 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 54031 _database_code_depnum_ccdc_archive 'CCDC 959697' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rah36 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H23 Cl N5 Ni +,Cl -,C H4 O' _chemical_formula_sum 'C17 H27 Cl2 N5 Ni O' _chemical_formula_weight 447.04 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_H-M_alt 'P 21/c' _space_group_name_Hall '-P 2ybc' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.9076(7) _cell_length_b 11.3295(5) _cell_length_c 14.1620(7) _cell_angle_alpha 90 _cell_angle_beta 117.8704(8) _cell_angle_gamma 90 _cell_volume 1972.62(16) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7691 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 26.92 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.505 _exptl_crystal_F_000 936 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_absorpt_coefficient_mu 1.271 _shelx_estimated_absorpt_T_min 0.702 _shelx_estimated_absorpt_T_max 0.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.700 _exptl_absorpt_correction_T_max 0.800 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'sealed tube' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11514 _diffrn_reflns_av_unetI/netI 0.0465 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 1.656 _diffrn_reflns_theta_max 28.950 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.919 _diffrn_measured_fraction_theta_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.919 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.919 _diffrn_reflns_point_group_measured_fraction_full 0.999 _reflns_number_total 4799 _reflns_number_gt 3783 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement SHELXL-2013 _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+0.8912P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4799 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0713 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.22626(2) 0.40783(2) 0.25735(2) 0.01368(8) Uani 1 1 d . . . . . Cl1 Cl 0.03288(4) 0.36786(5) 0.20099(4) 0.02228(13) Uani 1 1 d . . . . . N1 N 0.24817(14) 0.48300(15) 0.40120(14) 0.0164(4) Uani 1 1 d . . . . . N2 N 0.19288(15) 0.58339(16) 0.21324(15) 0.0175(4) Uani 1 1 d . . . . . H2N H 0.254(2) 0.619(2) 0.227(2) 0.032(7) Uiso 1 1 d . . . . . N3 N 0.21136(15) 0.39404(16) 0.10191(15) 0.0182(4) Uani 1 1 d . . . . . H3N H 0.1659(19) 0.346(2) 0.0650(19) 0.016(6) Uiso 1 1 d . . . . . N4 N 0.39552(15) 0.41488(17) 0.30422(15) 0.0174(4) Uani 1 1 d . . . . . H4N H 0.420(2) 0.477(2) 0.340(2) 0.032(8) Uiso 1 1 d . . . . . N5 N 0.26875(15) 0.23189(15) 0.30377(14) 0.0180(4) Uani 1 1 d . . . . . C1 C 0.30373(18) 0.4395(2) 0.49989(18) 0.0208(5) Uani 1 1 d . . . . . H1 H 0.3344 0.3628 0.5085 0.025 Uiso 1 1 calc R U . . . C2 C 0.31867(19) 0.5010(2) 0.59013(19) 0.0260(5) Uani 1 1 d . . . . . H2 H 0.3587 0.4671 0.6591 0.031 Uiso 1 1 calc R U . . . C3 C 0.2742(2) 0.6130(2) 0.5782(2) 0.0282(5) Uani 1 1 d . . . . . H3 H 0.2826 0.6571 0.6387 0.034 Uiso 1 1 calc R U . . . C4 C 0.21732(19) 0.6591(2) 0.47641(19) 0.0252(5) Uani 1 1 d . . . . . H4 H 0.1862 0.7357 0.4661 0.030 Uiso 1 1 calc R U . . . C5 C 0.20587(17) 0.59300(19) 0.38927(18) 0.0189(4) Uani 1 1 d . . . . . C6 C 0.14581(19) 0.6372(2) 0.27662(18) 0.0221(5) Uani 1 1 d . . . . . H6A H 0.0678 0.6162 0.2458 0.027 Uiso 1 1 calc R U . . . H6B H 0.1517 0.7242 0.2755 0.027 Uiso 1 1 calc R U . . . C7 C 0.12588(18) 0.58668(19) 0.09755(17) 0.0199(5) Uani 1 1 d . . . . . H7A H 0.1186 0.6689 0.0715 0.024 Uiso 1 1 calc R U . . . H7B H 0.0523 0.5556 0.0776 0.024 Uiso 1 1 calc R U . . . C8 C 0.18069(18) 0.51122(19) 0.04804(18) 0.0207(5) Uani 1 1 d . . . . . H8A H 0.1306 0.5000 -0.0289 0.025 Uiso 1 1 calc R U . . . H8B H 0.2466 0.5519 0.0549 0.025 Uiso 1 1 calc R U . . . C9 C 0.31823(18) 0.35300(19) 0.11605(18) 0.0203(5) Uani 1 1 d . . . . . H9A H 0.3228 0.3649 0.0490 0.024 Uiso 1 1 calc R U . . . H9B H 0.3267 0.2677 0.1331 0.024 Uiso 1 1 calc R U . . . C10 C 0.40794(18) 0.4215(2) 0.20583(18) 0.0207(5) Uani 1 1 d . . . . . H10A H 0.4795 0.3886 0.2202 0.025 Uiso 1 1 calc R U . . . H10B H 0.4054 0.5050 0.1843 0.025 Uiso 1 1 calc R U . . . C11 C 0.45137(18) 0.31294(19) 0.37285(19) 0.0229(5) Uani 1 1 d . . . . . H11A H 0.4810 0.3363 0.4487 0.027 Uiso 1 1 calc R U . . . H11B H 0.5131 0.2893 0.3606 0.027 Uiso 1 1 calc R U . . . C12 C 0.37611(18) 0.20920(19) 0.35098(17) 0.0194(5) Uani 1 1 d . . . . . C13 C 0.4165(2) 0.0952(2) 0.38048(19) 0.0267(5) Uani 1 1 d . . . . . H13 H 0.4927 0.0813 0.4137 0.032 Uiso 1 1 calc R U . . . C14 C 0.3449(2) 0.0020(2) 0.3611(2) 0.0305(6) Uani 1 1 d . . . . . H14 H 0.3711 -0.0764 0.3804 0.037 Uiso 1 1 calc R U . . . C15 C 0.2352(2) 0.0257(2) 0.31334(19) 0.0281(5) Uani 1 1 d . . . . . H15 H 0.1843 -0.0362 0.2996 0.034 Uiso 1 1 calc R U . . . C16 C 0.19990(19) 0.14079(19) 0.28553(18) 0.0226(5) Uani 1 1 d . . . . . H16 H 0.1240 0.1562 0.2522 0.027 Uiso 1 1 calc R U . . . Cl2 Cl 0.43188(5) 0.70144(5) 0.33477(5) 0.02603(14) Uani 1 1 d . . . . . C17 C 0.0324(2) 0.1288(2) -0.0366(2) 0.0355(6) Uani 1 1 d . . . . . H17A H 0.0775 0.0580 -0.0233 0.053 Uiso 1 1 calc R U . . . H17B H -0.0416 0.1120 -0.0925 0.053 Uiso 1 1 calc R U . . . H17C H 0.0304 0.1516 0.0292 0.053 Uiso 1 1 calc R U . . . O1 O 0.07714(15) 0.22224(15) -0.07018(15) 0.0298(4) Uani 1 1 d . . . . . H1O H 0.074(3) 0.198(3) -0.127(3) 0.051(10) 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 Ni 0.01426(13) 0.01290(13) 0.01336(13) 0.00060(11) 0.00602(11) 0.00097(10) Cl1 0.0159(3) 0.0258(3) 0.0225(3) 0.0050(2) 0.0068(2) -0.0014(2) N1 0.0154(9) 0.0172(9) 0.0157(9) 0.0000(7) 0.0065(8) 0.0001(7) N2 0.0183(9) 0.0153(9) 0.0184(9) 0.0017(7) 0.0081(8) 0.0004(7) N3 0.0178(9) 0.0177(10) 0.0169(9) -0.0027(8) 0.0064(8) -0.0022(8) N4 0.0188(9) 0.0155(9) 0.0182(9) -0.0016(8) 0.0088(8) 0.0000(8) N5 0.0213(10) 0.0161(9) 0.0166(9) 0.0005(7) 0.0090(8) 0.0014(7) C1 0.0207(11) 0.0225(12) 0.0193(11) 0.0012(9) 0.0093(10) -0.0005(9) C2 0.0258(12) 0.0345(14) 0.0158(11) 0.0010(10) 0.0081(10) -0.0043(10) C3 0.0330(14) 0.0316(14) 0.0246(12) -0.0102(11) 0.0174(11) -0.0063(11) C4 0.0284(13) 0.0227(12) 0.0292(13) -0.0046(10) 0.0174(11) 0.0019(10) C5 0.0171(10) 0.0200(11) 0.0197(11) -0.0017(9) 0.0088(9) -0.0002(9) C6 0.0242(12) 0.0192(11) 0.0242(12) 0.0011(9) 0.0123(10) 0.0060(9) C7 0.0207(11) 0.0189(11) 0.0195(11) 0.0051(9) 0.0090(10) 0.0036(9) C8 0.0203(11) 0.0244(12) 0.0173(11) 0.0021(9) 0.0088(10) 0.0009(9) C9 0.0256(12) 0.0202(11) 0.0199(11) -0.0005(9) 0.0146(10) 0.0044(9) C10 0.0205(11) 0.0222(12) 0.0238(12) 0.0025(9) 0.0141(10) 0.0036(9) C11 0.0171(11) 0.0268(12) 0.0209(11) 0.0036(10) 0.0058(10) 0.0046(9) C12 0.0257(12) 0.0202(11) 0.0144(10) 0.0007(9) 0.0111(10) 0.0044(9) C13 0.0314(13) 0.0275(13) 0.0224(12) 0.0055(10) 0.0137(11) 0.0128(10) C14 0.0522(17) 0.0183(12) 0.0245(13) 0.0039(10) 0.0210(13) 0.0106(11) C15 0.0452(16) 0.0153(11) 0.0267(13) -0.0005(10) 0.0194(12) -0.0033(10) C16 0.0279(12) 0.0194(11) 0.0212(11) -0.0008(9) 0.0120(10) -0.0020(9) Cl2 0.0230(3) 0.0190(3) 0.0298(3) 0.0008(2) 0.0071(3) -0.0033(2) C17 0.0374(15) 0.0335(14) 0.0397(16) 0.0028(12) 0.0213(14) -0.0010(12) O1 0.0382(10) 0.0257(9) 0.0277(10) -0.0064(8) 0.0172(9) -0.0059(8) _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 Ni Cl1 2.4634(6) . ? Ni N1 2.0948(17) . ? Ni N2 2.0714(18) . ? Ni N3 2.1181(19) . ? Ni N4 2.1277(18) . ? Ni N5 2.0956(17) . ? N1 C1 1.336(3) . ? N1 C5 1.355(3) . ? N2 H2N 0.87(3) . ? N2 C6 1.468(3) . ? N2 C7 1.458(3) . ? N3 H3N 0.81(2) . ? N3 C8 1.491(3) . ? N3 C9 1.479(3) . ? N4 H4N 0.84(3) . ? N4 C10 1.484(3) . ? N4 C11 1.475(3) . ? N5 C12 1.345(3) . ? N5 C16 1.348(3) . ? C1 H1 0.950 . ? C1 C2 1.383(3) . ? C2 H2 0.950 . ? C2 C3 1.388(3) . ? C3 H3 0.950 . ? C3 C4 1.382(3) . ? C4 H4 0.950 . ? C4 C5 1.387(3) . ? C5 C6 1.499(3) . ? C6 H6A 0.990 . ? C6 H6B 0.990 . ? C7 H7A 0.990 . ? C7 H7B 0.990 . ? C7 C8 1.518(3) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C9 C10 1.514(3) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C11 C12 1.507(3) . ? C12 C13 1.392(3) . ? C13 H13 0.950 . ? C13 C14 1.388(4) . ? C14 H14 0.950 . ? C14 C15 1.376(4) . ? C15 H15 0.950 . ? C15 C16 1.384(3) . ? C16 H16 0.950 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C17 O1 1.418(3) . ? O1 H1O 0.83(3) . ? 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 Cl1 Ni N1 91.73(5) . . ? Cl1 Ni N2 91.26(5) . . ? Cl1 Ni N3 95.06(5) . . ? Cl1 Ni N4 171.51(5) . . ? Cl1 Ni N5 91.82(5) . . ? N1 Ni N2 79.23(7) . . ? N1 Ni N3 160.01(7) . . ? N1 Ni N4 92.56(7) . . ? N1 Ni N5 100.96(7) . . ? N2 Ni N3 81.85(7) . . ? N2 Ni N4 96.74(7) . . ? N2 Ni N5 176.91(7) . . ? N3 Ni N4 83.31(7) . . ? N3 Ni N5 97.60(7) . . ? N4 Ni N5 80.17(7) . . ? Ni N1 C1 128.14(14) . . ? Ni N1 C5 113.30(14) . . ? C1 N1 C5 118.37(18) . . ? Ni N2 H2N 108.4(17) . . ? Ni N2 C6 108.39(13) . . ? Ni N2 C7 107.38(13) . . ? H2N N2 C6 109.6(17) . . ? H2N N2 C7 106.5(18) . . ? C6 N2 C7 116.29(17) . . ? Ni N3 H3N 112.8(16) . . ? Ni N3 C8 109.38(13) . . ? Ni N3 C9 106.18(13) . . ? H3N N3 C8 108.4(17) . . ? H3N N3 C9 107.9(16) . . ? C8 N3 C9 112.23(17) . . ? Ni N4 H4N 106.8(18) . . ? Ni N4 C10 107.84(13) . . ? Ni N4 C11 109.95(13) . . ? H4N N4 C10 109.9(18) . . ? H4N N4 C11 108.5(18) . . ? C10 N4 C11 113.67(17) . . ? Ni N5 C12 114.99(14) . . ? Ni N5 C16 126.67(15) . . ? C12 N5 C16 118.22(19) . . ? N1 C1 H1 118.5 . . ? N1 C1 C2 123.0(2) . . ? H1 C1 C2 118.5 . . ? C1 C2 H2 120.6 . . ? C1 C2 C3 118.8(2) . . ? H2 C2 C3 120.6 . . ? C2 C3 H3 120.7 . . ? C2 C3 C4 118.5(2) . . ? H3 C3 C4 120.7 . . ? C3 C4 H4 120.1 . . ? C3 C4 C5 119.7(2) . . ? H4 C4 C5 120.1 . . ? N1 C5 C4 121.5(2) . . ? N1 C5 C6 115.68(19) . . ? C4 C5 C6 122.8(2) . . ? N2 C6 C5 109.03(17) . . ? N2 C6 H6A 109.9 . . ? N2 C6 H6B 109.9 . . ? C5 C6 H6A 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? N2 C7 H7A 110.1 . . ? N2 C7 H7B 110.1 . . ? N2 C7 C8 108.03(17) . . ? H7A C7 H7B 108.4 . . ? H7A C7 C8 110.1 . . ? H7B C7 C8 110.1 . . ? N3 C8 C7 110.52(17) . . ? N3 C8 H8A 109.5 . . ? N3 C8 H8B 109.5 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? N3 C9 H9A 109.8 . . ? N3 C9 H9B 109.8 . . ? N3 C9 C10 109.51(17) . . ? H9A C9 H9B 108.2 . . ? H9A C9 C10 109.8 . . ? H9B C9 C10 109.8 . . ? N4 C10 C9 110.54(17) . . ? N4 C10 H10A 109.5 . . ? N4 C10 H10B 109.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? N4 C11 H11A 109.2 . . ? N4 C11 H11B 109.2 . . ? N4 C11 C12 111.97(18) . . ? H11A C11 H11B 107.9 . . ? H11A C11 C12 109.2 . . ? H11B C11 C12 109.2 . . ? N5 C12 C11 117.14(18) . . ? N5 C12 C13 121.7(2) . . ? C11 C12 C13 121.2(2) . . ? C12 C13 H13 120.2 . . ? C12 C13 C14 119.6(2) . . ? H13 C13 C14 120.2 . . ? C13 C14 H14 120.8 . . ? C13 C14 C15 118.5(2) . . ? H14 C14 C15 120.8 . . ? C14 C15 H15 120.4 . . ? C14 C15 C16 119.2(2) . . ? H15 C15 C16 120.4 . . ? N5 C16 C15 122.7(2) . . ? N5 C16 H16 118.6 . . ? C15 C16 H16 118.6 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17A C17 O1 109.5 . . ? H17B C17 H17C 109.5 . . ? H17B C17 O1 109.5 . . ? H17C C17 O1 109.5 . . ? C17 O1 H1O 104(2) . . ? 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 Ni N1 C1 C2 175.57(16) . . . . ? C5 N1 C1 C2 0.9(3) . . . . ? N1 C1 C2 C3 0.0(3) . . . . ? C1 C2 C3 C4 -0.5(3) . . . . ? C2 C3 C4 C5 0.1(4) . . . . ? Ni N1 C5 C4 -176.72(17) . . . . ? Ni N1 C5 C6 3.8(2) . . . . ? C1 N1 C5 C4 -1.3(3) . . . . ? C1 N1 C5 C6 179.18(19) . . . . ? C3 C4 C5 N1 0.8(3) . . . . ? C3 C4 C5 C6 -179.7(2) . . . . ? Ni N2 C6 C5 40.8(2) . . . . ? C7 N2 C6 C5 161.80(18) . . . . ? N1 C5 C6 N2 -29.8(3) . . . . ? C4 C5 C6 N2 150.6(2) . . . . ? Ni N2 C7 C8 -49.93(19) . . . . ? C6 N2 C7 C8 -171.49(18) . . . . ? Ni N3 C8 C7 -23.2(2) . . . . ? C9 N3 C8 C7 -140.82(19) . . . . ? N2 C7 C8 N3 48.9(2) . . . . ? Ni N3 C9 C10 -44.51(19) . . . . ? C8 N3 C9 C10 74.9(2) . . . . ? Ni N4 C10 C9 -33.2(2) . . . . ? C11 N4 C10 C9 89.0(2) . . . . ? N3 C9 C10 N4 53.5(2) . . . . ? Ni N4 C11 C12 26.2(2) . . . . ? C10 N4 C11 C12 -94.8(2) . . . . ? Ni N5 C12 C11 5.1(2) . . . . ? Ni N5 C12 C13 -176.12(16) . . . . ? C16 N5 C12 C11 -178.57(19) . . . . ? C16 N5 C12 C13 0.2(3) . . . . ? N4 C11 C12 N5 -21.5(3) . . . . ? N4 C11 C12 C13 159.8(2) . . . . ? N5 C12 C13 C14 0.0(3) . . . . ? C11 C12 C13 C14 178.7(2) . . . . ? C12 C13 C14 C15 -0.3(3) . . . . ? C13 C14 C15 C16 0.5(4) . . . . ? Ni N5 C16 C15 175.84(17) . . . . ? C12 N5 C16 C15 0.0(3) . . . . ? C14 C15 C16 N5 -0.4(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2N Cl2 0.87(3) 2.41(3) 3.233(2) 157(2) . N3 H3N O1 0.81(2) 2.22(2) 2.993(3) 158(2) . N4 H4N Cl2 0.84(3) 2.55(3) 3.283(2) 146(2) . O1 H1O Cl1 0.83(3) 2.35(3) 3.1715(19) 170(3) 4_565 _refine_diff_density_max 0.377 _refine_diff_density_min -0.369 _refine_diff_density_rms 0.073 _shelxl_version_number 2013-2 _shelx_res_file ; TITL rah36 in P2(1)/c CELL 0.71073 13.9076 11.3295 14.1620 90.000 117.8704 90.000 ZERR 4.00 0.0007 0.0005 0.0007 0.000 0.0008 0.000 LATT 1 SYMM -X, 0.5+Y, 0.5-Z SFAC C H N CL NI O UNIT 68 108 20 8 4 4 TEMP -123 SIZE 0.3 0.2 0.2 REM purple block L.S. 8 ACTA BOND $H CONF FMAP 2 PLAN 10 HTAB N2 CL2 HTAB N3 O1 HTAB N4 CL2 HTAB O1 CL1_$1 EQIV $1 x, -y+1/2, z-1/2 REM EXTI 0.000000 WGHT 0.026400 0.891200 FVAR 0.42427 NI 5 0.226264 0.407829 0.257345 11.00000 0.01426 0.01290 = 0.01336 0.00060 0.00602 0.00097 CL1 4 0.032880 0.367857 0.200987 11.00000 0.01591 0.02578 = 0.02250 0.00500 0.00676 -0.00145 N1 3 0.248171 0.482998 0.401199 11.00000 0.01537 0.01716 = 0.01572 0.00003 0.00650 0.00005 N2 3 0.192885 0.583386 0.213244 11.00000 0.01828 0.01526 = 0.01836 0.00171 0.00813 0.00036 H2N 2 0.253745 0.618732 0.227085 11.00000 0.03225 N3 3 0.211365 0.394045 0.101912 11.00000 0.01785 0.01767 = 0.01694 -0.00275 0.00639 -0.00216 H3N 2 0.165877 0.346139 0.064975 11.00000 0.01625 N4 3 0.395521 0.414884 0.304218 11.00000 0.01879 0.01554 = 0.01816 -0.00156 0.00884 0.00002 H4N 2 0.419638 0.477107 0.340369 11.00000 0.03221 N5 3 0.268751 0.231893 0.303775 11.00000 0.02134 0.01606 = 0.01665 0.00048 0.00903 0.00137 C1 1 0.303730 0.439482 0.499891 11.00000 0.02070 0.02251 = 0.01927 0.00123 0.00931 -0.00054 AFIX 43 H1 2 0.334382 0.362812 0.508505 11.00000 -1.20000 AFIX 0 C2 1 0.318669 0.500961 0.590127 11.00000 0.02578 0.03448 = 0.01580 0.00104 0.00807 -0.00433 AFIX 43 H2 2 0.358682 0.467059 0.659069 11.00000 -1.20000 AFIX 0 C3 1 0.274189 0.613023 0.578188 11.00000 0.03301 0.03157 = 0.02458 -0.01023 0.01740 -0.00626 AFIX 43 H3 2 0.282644 0.657115 0.638654 11.00000 -1.20000 AFIX 0 C4 1 0.217320 0.659077 0.476406 11.00000 0.02842 0.02266 = 0.02919 -0.00461 0.01744 0.00189 AFIX 43 H4 2 0.186198 0.735662 0.466143 11.00000 -1.20000 AFIX 0 C5 1 0.205867 0.592998 0.389270 11.00000 0.01710 0.02005 = 0.01968 -0.00169 0.00881 -0.00024 C6 1 0.145815 0.637189 0.276620 11.00000 0.02418 0.01923 = 0.02423 0.00106 0.01235 0.00597 AFIX 23 H6A 2 0.067848 0.616230 0.245763 11.00000 -1.20000 H6B 2 0.151736 0.724206 0.275542 11.00000 -1.20000 AFIX 0 C7 1 0.125882 0.586676 0.097553 11.00000 0.02065 0.01889 = 0.01953 0.00508 0.00899 0.00357 AFIX 23 H7A 2 0.118593 0.668922 0.071458 11.00000 -1.20000 H7B 2 0.052317 0.555639 0.077629 11.00000 -1.20000 AFIX 0 C8 1 0.180688 0.511222 0.048038 11.00000 0.02034 0.02435 = 0.01731 0.00207 0.00876 0.00094 AFIX 23 H8A 2 0.130597 0.499961 -0.028945 11.00000 -1.20000 H8B 2 0.246625 0.551947 0.054882 11.00000 -1.20000 AFIX 0 C9 1 0.318225 0.352999 0.116047 11.00000 0.02558 0.02022 = 0.01988 -0.00048 0.01464 0.00440 AFIX 23 H9A 2 0.322797 0.364936 0.049010 11.00000 -1.20000 H9B 2 0.326731 0.267664 0.133059 11.00000 -1.20000 AFIX 0 C10 1 0.407938 0.421478 0.205833 11.00000 0.02054 0.02223 = 0.02382 0.00251 0.01414 0.00355 AFIX 23 H10A 2 0.479465 0.388615 0.220231 11.00000 -1.20000 H10B 2 0.405406 0.505020 0.184293 11.00000 -1.20000 AFIX 0 C11 1 0.451372 0.312938 0.372846 11.00000 0.01714 0.02684 = 0.02089 0.00358 0.00576 0.00456 AFIX 23 H11A 2 0.481047 0.336347 0.448698 11.00000 -1.20000 H11B 2 0.513144 0.289269 0.360553 11.00000 -1.20000 AFIX 0 C12 1 0.376108 0.209199 0.350979 11.00000 0.02572 0.02024 = 0.01437 0.00075 0.01112 0.00442 C13 1 0.416527 0.095204 0.380483 11.00000 0.03143 0.02753 = 0.02237 0.00546 0.01366 0.01278 AFIX 43 H13 2 0.492700 0.081296 0.413690 11.00000 -1.20000 AFIX 0 C14 1 0.344926 0.002014 0.361116 11.00000 0.05218 0.01834 = 0.02451 0.00391 0.02098 0.01061 AFIX 43 H14 2 0.371074 -0.076363 0.380410 11.00000 -1.20000 AFIX 0 C15 1 0.235238 0.025725 0.313345 11.00000 0.04520 0.01532 = 0.02670 -0.00052 0.01937 -0.00332 AFIX 43 H15 2 0.184317 -0.036184 0.299604 11.00000 -1.20000 AFIX 0 C16 1 0.199904 0.140795 0.285528 11.00000 0.02793 0.01935 = 0.02115 -0.00075 0.01197 -0.00203 AFIX 43 H16 2 0.123974 0.156232 0.252187 11.00000 -1.20000 AFIX 0 CL2 4 0.431884 0.701443 0.334772 11.00000 0.02298 0.01903 = 0.02980 0.00085 0.00710 -0.00328 C17 1 0.032401 0.128754 -0.036589 11.00000 0.03740 0.03350 = 0.03966 0.00275 0.02133 -0.00104 AFIX 137 H17A 2 0.077488 0.058026 -0.023301 11.00000 -1.50000 H17B 2 -0.041623 0.112037 -0.092483 11.00000 -1.50000 H17C 2 0.030425 0.151611 0.029221 11.00000 -1.50000 AFIX 0 O1 6 0.077144 0.222244 -0.070176 11.00000 0.03820 0.02566 = 0.02770 -0.00637 0.01720 -0.00585 H1O 2 0.074497 0.197939 -0.126995 11.00000 0.05100 HKLF 4 REM rah36 in P2(1)/c REM R1 = 0.0348 for 3783 Fo > 4sig(Fo) and 0.0520 for all 4799 data REM 252 parameters refined using 0 restraints END WGHT 0.0258 0.9198 REM Highest difference peak 0.377, deepest hole -0.369, 1-sigma level 0.073 Q1 1 0.1558 0.5381 0.0781 11.00000 0.05 0.38 Q2 1 0.0002 0.3603 0.2405 11.00000 0.05 0.35 Q3 1 0.1901 0.4213 0.3007 11.00000 0.05 0.35 Q4 1 0.2942 0.0262 0.3231 11.00000 0.05 0.35 Q5 1 0.4060 0.2657 0.3701 11.00000 0.05 0.35 Q6 1 0.1677 0.3672 0.2109 11.00000 0.05 0.34 Q7 1 0.2157 0.5201 0.2471 11.00000 0.05 0.34 Q8 1 0.2552 0.3420 0.2417 11.00000 0.05 0.32 Q9 1 0.2544 0.4560 0.2241 11.00000 0.05 0.32 Q10 1 0.3203 0.2207 0.3420 11.00000 0.05 0.32 ; _shelx_res_checksum 96600 _shelx_hkl_file ; 1 0 0 6.82 0.84 1 1 0 0 11.11 0.90 2 2 0 0 5310.75 146.18 2 3 0 0 148.69 6.37 2 3 0 0 157.06 6.45 1 4 0 0 2481.39 69.23 1 4 0 0 2415.61 69.31 2 5 0 0 4725.96 131.84 2 5 0 0 4741.59 131.44 1 6 0 0 1543.26 47.11 2 6 0 0 1599.07 47.23 1 7 0 0 292.05 12.81 1 8 0 0 183.81 10.17 1 -8 0 0 186.09 7.27 3 9 0 0 900.26 31.55 1 10 0 0 3.82 4.19 1 11 0 0 1049.61 37.51 1 12 0 0 160.69 11.88 1 13 0 0 4.86 5.34 1 14 0 0 15.31 6.47 1 0 -1 0 1.68 0.39 1 0 1 0 -0.02 0.37 2 1 1 0 2135.50 58.62 2 1 1 0 2049.20 57.54 3 1 -1 0 2104.18 58.69 1 2 1 0 18.58 2.07 2 2 -1 0 16.55 1.88 1 2 1 0 15.28 1.88 1 3 -1 0 22.97 2.66 1 3 1 0 21.97 2.79 1 3 1 0 27.18 3.09 2 4 1 0 1282.84 36.85 1 4 -1 0 1166.56 36.45 1 4 1 0 1271.69 37.11 2 5 1 0 980.66 29.45 2 5 1 0 911.19 28.96 1 5 -1 0 882.63 28.74 1 6 -1 0 1609.30 48.11 1 6 1 0 1618.50 48.27 1 6 1 0 1592.84 48.42 2 7 -1 0 0.18 2.34 1 7 1 0 1.87 2.79 1 7 1 0 -0.37 2.76 2 8 1 0 46.08 5.90 1 -8 1 0 55.46 4.43 3 8 -1 0 60.65 6.19 1 8 1 0 50.80 5.98 2 9 -1 0 173.22 10.51 1 9 1 0 186.00 10.88 1 9 1 0 185.26 10.85 2 10 1 0 49.00 6.62 1 10 -1 0 56.31 6.73 1 11 -1 0 251.12 14.31 1 11 1 0 230.30 13.87 1 12 -1 0 176.77 12.33 1 12 1 0 162.88 12.12 1 13 -1 0 52.26 9.54 1 13 1 0 69.72 9.05 1 14 -1 0 74.36 10.28 1 15 -1 0 -7.45 6.25 1 -15 -1 0 -0.81 8.13 1 0 2 0 940.24 27.22 2 0 2 0 948.57 26.20 3 0 -2 0 948.32 27.07 1 1 -2 0 67.00 2.89 1 -1 -2 0 67.68 3.16 1 1 2 0 70.23 3.19 3 -1 2 0 73.39 3.24 2 1 2 0 65.83 3.54 2 2 2 0 4265.29 113.89 3 2 -2 0 4313.75 118.39 1 2 2 0 4396.65 119.39 2 -2 -2 0 4285.44 118.61 1 3 2 0 11.21 2.41 2 3 2 0 7.83 2.03 1 3 -2 0 9.16 2.03 1 4 2 0 172.51 8.02 2 4 2 0 184.95 8.03 1 4 -2 0 156.38 7.26 1 5 -2 0 348.67 13.06 1 5 2 0 364.17 13.81 2 5 2 0 326.74 13.25 1 6 -2 0 84.28 6.09 1 6 2 0 94.62 6.45 1 6 2 0 91.38 6.77 2 7 2 0 458.99 18.17 2 7 2 0 457.90 17.85 1 7 -2 0 441.22 17.32 1 8 -2 0 150.71 9.48 1 -8 2 0 158.55 7.96 3 8 2 0 165.58 10.06 2 8 2 0 168.48 9.85 1 9 2 0 50.03 6.90 2 -9 2 0 57.08 5.22 3 9 2 0 57.52 6.51 1 9 -2 0 54.85 6.09 1 10 2 0 65.67 7.66 2 10 -2 0 79.07 7.78 1 10 2 0 72.06 7.99 1 11 2 0 263.65 15.24 2 11 2 0 283.90 15.38 1 11 -2 0 248.10 14.50 1 12 -2 0 -5.66 4.50 1 12 2 0 2.65 4.68 1 -13 -2 0 64.11 9.71 1 13 -2 0 68.10 9.23 1 14 -2 0 57.30 10.64 1 -14 -2 0 58.70 10.22 1 15 -2 0 -4.60 7.69 1 -15 -2 0 -10.23 7.71 1 0 3 0 1.13 1.45 2 0 3 0 2.36 1.79 3 0 -3 0 0.64 0.95 1 -1 3 0 1550.79 43.46 2 -1 3 0 1477.39 42.11 3 1 -3 0 1492.49 42.72 1 1 3 0 1572.69 43.97 2 -1 -3 0 1530.64 42.98 1 1 3 0 1530.69 41.74 3 2 -3 0 980.86 28.24 1 -2 -3 0 956.09 28.64 1 2 3 0 969.01 27.35 3 -2 3 0 962.23 28.60 2 2 3 0 1024.50 29.73 2 3 -3 0 36.33 3.23 1 3 3 0 41.68 3.92 2 -3 3 0 37.98 3.08 2 3 3 0 33.77 2.75 3 -3 -3 0 37.97 3.72 1 -4 -3 0 1082.32 32.39 1 4 3 0 1008.67 32.74 2 4 -3 0 1081.57 31.80 1 5 3 0 1971.91 57.28 2 5 -3 0 1876.69 55.74 1 6 3 0 1405.48 41.67 1 6 3 0 1290.44 42.05 2 6 -3 0 1332.06 40.98 1 -7 3 0 38.21 4.52 3 7 -3 0 44.89 5.12 1 7 3 0 43.60 6.01 2 7 3 0 37.25 5.01 1 8 3 0 60.33 6.17 1 8 -3 0 78.37 6.89 1 8 3 0 67.74 7.17 2 -8 3 0 82.02 6.11 3 -9 3 0 4.96 3.25 3 9 3 0 -2.09 3.30 1 9 -3 0 2.61 3.78 1 9 3 0 1.39 4.07 2 10 -3 0 1880.23 59.01 1 10 3 0 1872.31 60.18 2 -11 -3 0 8.71 5.75 1 11 -3 0 6.36 4.74 1 11 3 0 4.62 5.48 2 12 3 0 298.96 17.32 2 12 -3 0 302.73 16.78 1 -12 -3 0 302.48 17.52 1 -13 -3 0 11.71 8.56 1 13 -3 0 6.07 5.33 1 14 -3 0 273.52 17.31 1 -14 -3 0 219.31 17.77 1 -15 -3 0 94.40 14.80 1 15 -3 0 91.18 13.59 1 0 4 0 3188.50 83.40 3 0 4 0 3086.53 86.71 2 0 -4 0 3019.58 85.42 1 1 -4 0 1349.85 38.77 1 1 4 0 1379.79 38.65 3 -1 -4 0 1350.32 39.00 1 -1 4 0 1446.93 40.10 2 -1 4 0 1330.02 39.05 3 1 4 0 1394.57 40.52 2 -2 4 0 39.52 3.20 2 -2 -4 0 41.93 3.34 1 -2 4 0 41.12 3.96 3 2 4 0 47.01 3.60 3 2 4 0 39.73 4.11 2 2 -4 0 35.27 2.84 1 -3 4 0 160.45 6.93 2 3 4 0 147.30 6.50 3 3 -4 0 161.48 6.75 1 -3 -4 0 167.82 7.33 1 -4 -4 0 996.81 30.09 1 4 4 0 965.01 27.26 3 4 4 0 975.79 31.00 2 -4 4 0 922.51 29.20 2 4 -4 0 953.97 29.26 1 -5 4 0 1551.52 43.28 3 5 -4 0 1435.48 43.75 1 5 4 0 1479.62 45.68 2 -5 -4 0 1439.30 44.58 1 6 -4 0 2.29 2.56 1 -6 -4 0 8.52 3.93 1 -6 4 0 5.43 3.19 3 6 4 0 9.02 3.31 2 -7 4 0 229.49 11.13 3 -7 -4 0 258.39 12.88 1 7 -4 0 245.77 11.60 1 7 4 0 226.75 12.32 2 8 4 0 9.78 4.76 2 -8 -4 0 14.97 5.55 1 -8 4 0 11.70 3.91 3 8 -4 0 16.62 4.45 1 9 4 0 170.59 11.31 2 -9 4 0 159.88 9.39 3 9 -4 0 161.38 10.08 1 -9 -4 0 144.85 11.37 1 10 -4 0 51.71 7.26 1 -10 -4 0 43.33 7.73 1 10 4 0 57.95 8.51 2 -10 4 0 45.45 5.93 3 -11 -4 0 647.40 27.90 1 11 -4 0 695.43 26.88 1 11 4 0 639.16 27.51 2 -12 -4 0 480.62 23.17 1 12 4 0 471.27 23.08 2 12 -4 0 453.90 21.66 1 13 -4 0 4.08 5.63 1 13 4 0 -0.33 5.10 2 -13 -4 0 2.36 7.43 1 -14 -4 0 5.07 6.95 1 14 -4 0 -7.36 6.39 1 15 -4 0 45.56 10.36 1 -15 -4 0 35.59 10.34 1 0 -5 0 1.46 1.29 1 0 5 0 0.47 1.95 2 0 5 0 4.56 2.45 3 -1 5 0 345.83 13.48 3 1 -5 0 364.50 11.75 1 -1 5 0 384.50 13.28 2 1 5 0 366.76 13.31 3 -1 -5 0 372.33 12.12 1 1 5 0 372.56 13.79 2 -2 5 0 171.76 8.56 3 2 -5 0 162.08 6.46 1 2 5 0 156.54 8.10 2 -2 5 0 159.02 7.34 2 -2 -5 0 161.90 7.06 1 2 5 0 160.55 7.47 3 -3 -5 0 359.22 12.97 1 3 5 0 355.34 12.50 3 -3 5 0 368.49 14.06 3 3 -5 0 342.45 12.11 1 3 5 0 337.36 14.04 2 -3 5 0 346.26 12.58 2 4 5 0 28.92 4.80 2 -4 5 0 44.73 5.07 3 4 5 0 31.30 3.69 3 -4 5 0 33.69 3.66 2 4 -5 0 27.40 3.59 1 -4 -5 0 32.07 4.09 1 5 -5 0 31.40 4.08 1 -5 5 0 32.33 4.14 2 5 5 0 27.37 3.58 3 -5 -5 0 32.51 4.73 1 -5 5 0 34.61 4.70 3 5 5 0 27.00 5.08 2 -6 5 0 93.52 7.29 3 6 5 0 100.59 8.15 2 -6 5 0 100.81 6.44 2 6 -5 0 96.05 6.49 1 -6 -5 0 92.44 7.17 1 -7 5 0 1025.85 33.84 2 -7 5 0 1049.22 34.01 3 7 5 0 1054.18 36.47 2 7 -5 0 1088.61 34.64 1 -7 -5 0 1119.82 35.77 1 8 5 0 58.53 7.44 2 -8 5 0 65.70 6.77 3 8 -5 0 68.91 6.70 1 -8 -5 0 67.91 7.43 1 9 5 0 17.48 5.40 2 -9 5 0 15.98 4.85 3 9 -5 0 8.82 4.47 1 -9 -5 0 14.07 5.39 1 -10 -5 0 54.32 8.34 1 10 -5 0 39.81 6.98 1 10 5 0 44.55 7.86 2 -10 5 0 50.36 6.98 3 -11 -5 0 97.99 10.31 1 11 -5 0 95.96 9.16 1 11 5 0 106.45 10.30 2 12 5 0 204.62 15.11 2 12 -5 0 214.20 14.02 1 -12 -5 0 236.78 15.55 1 13 5 0 10.31 6.75 2 -13 -5 0 5.48 7.19 1 13 -5 0 6.21 6.84 1 14 -5 0 6.22 7.49 1 14 5 0 20.46 8.68 2 -14 -5 0 -3.49 7.25 1 15 -5 0 49.64 11.07 1 -15 -5 0 39.07 10.63 1 0 6 0 910.62 28.71 2 0 6 0 906.02 28.30 3 0 -6 0 885.45 26.40 1 -1 -6 0 15.72 2.39 1 1 6 0 18.36 3.62 2 -1 6 0 11.82 3.72 3 1 -6 0 17.44 2.36 1 -1 6 0 18.42 3.54 2 1 6 0 26.12 3.92 3 -2 6 0 812.91 25.26 2 2 -6 0 767.75 23.41 1 2 6 0 785.58 26.22 2 -2 -6 0 738.99 23.92 1 -2 6 0 802.57 25.85 3 2 6 0 779.68 24.64 3 3 6 0 290.22 11.60 3 3 6 0 283.10 12.82 2 -3 6 0 287.34 12.88 3 3 -6 0 298.15 10.84 1 -3 6 0 310.58 11.88 2 -3 -6 0 298.49 11.58 1 4 6 0 196.02 8.74 3 -4 -6 0 155.25 8.66 1 4 -6 0 188.51 8.27 1 -4 6 0 178.07 9.80 3 -4 6 0 194.68 8.73 2 4 6 0 188.91 10.28 2 5 6 0 522.51 16.92 3 -5 6 0 500.78 17.86 2 -5 6 0 500.86 19.35 3 -5 -6 0 527.57 19.08 1 5 6 0 493.32 20.11 2 5 -6 0 491.08 17.72 1 6 6 0 751.86 27.48 2 6 -6 0 745.86 24.90 1 -6 6 0 717.41 24.59 2 -6 6 0 734.38 25.85 3 -6 -6 0 745.44 25.97 1 -7 6 0 301.90 14.66 3 7 -6 0 324.37 14.13 1 -7 6 0 356.25 14.34 2 7 6 0 343.57 16.36 2 -7 -6 0 328.69 15.21 1 8 6 0 129.35 10.43 2 -8 6 0 128.01 8.62 2 -8 -6 0 123.36 9.44 1 8 -6 0 134.27 8.91 1 -8 6 0 131.14 9.18 3 -9 6 0 60.32 7.23 3 9 6 0 51.99 7.27 2 9 -6 0 59.12 6.80 1 -9 -6 0 53.72 7.92 1 -10 6 0 220.27 13.24 3 10 6 0 211.05 14.23 2 -10 -6 0 233.53 14.19 1 10 -6 0 232.07 13.20 1 11 -6 0 242.78 14.20 1 -11 -6 0 253.09 15.51 1 11 6 0 219.88 15.61 2 12 -6 0 35.88 7.76 1 -12 -6 0 43.27 8.92 1 12 6 0 33.59 8.97 2 13 6 0 84.92 11.26 2 -13 -6 0 75.51 10.62 1 13 -6 0 77.06 10.74 1 14 6 0 82.47 12.96 2 -14 -6 0 94.93 13.14 1 14 -6 0 100.21 11.58 1 -15 -6 0 -3.43 7.86 1 0 7 0 -2.75 2.34 2 0 7 0 -3.42 2.51 3 0 -7 0 -1.38 1.62 1 1 7 0 480.73 18.20 3 -1 -7 0 504.41 16.24 1 1 -7 0 487.17 15.87 1 -1 7 0 530.89 18.35 2 1 7 0 508.87 18.81 2 -1 7 0 491.66 18.80 3 2 7 0 3.75 2.86 3 2 -7 0 2.61 2.04 1 -2 -7 0 5.37 2.47 1 -2 7 0 0.13 2.93 3 2 7 0 -3.30 2.05 2 -2 7 0 0.29 2.46 2 3 7 0 6.93 3.34 2 -3 7 0 10.99 3.74 3 3 -7 0 11.58 2.89 1 -3 7 0 9.20 3.19 2 3 7 0 11.04 3.56 3 -3 -7 0 5.10 2.67 1 -4 7 0 256.59 11.30 2 -4 7 0 255.02 12.84 3 4 -7 0 243.81 10.33 1 -4 -7 0 261.05 11.41 1 4 7 0 260.22 11.30 3 4 7 0 249.23 12.64 2 -5 -7 0 624.04 22.57 1 5 7 0 632.82 20.97 3 -5 7 0 662.77 23.90 3 -5 7 0 650.47 21.90 2 5 -7 0 624.19 21.32 1 5 7 0 598.62 23.98 2 -6 -7 0 556.24 21.02 1 6 -7 0 516.55 19.44 1 -6 7 0 536.64 19.63 2 -6 7 0 565.74 21.73 3 6 7 0 561.45 22.77 2 7 7 0 21.59 6.23 2 -7 7 0 13.44 5.28 3 -7 -7 0 14.52 4.97 1 7 -7 0 11.85 4.26 1 -8 -7 0 45.35 7.13 1 8 -7 0 42.00 6.41 1 -8 7 0 35.82 6.81 3 8 7 0 30.36 7.09 2 -9 7 0 3.77 4.70 3 9 7 0 2.45 4.65 2 -9 -7 0 -2.28 4.58 1 9 -7 0 7.78 4.84 1 -10 7 0 407.06 19.48 3 10 7 0 432.20 21.90 2 -10 -7 0 434.14 20.40 1 -11 -7 0 -4.11 5.03 1 -11 7 0 -4.76 5.37 3 11 7 0 -2.11 5.56 2 12 7 0 34.03 8.93 2 -12 -7 0 35.22 8.72 1 13 7 0 3.87 6.82 2 -13 -7 0 6.41 7.29 1 -14 -7 0 53.51 11.43 1 14 7 0 64.49 12.63 2 0 8 0 192.36 10.38 2 0 8 0 212.10 11.01 3 1 8 0 763.88 25.78 3 -1 8 0 763.30 25.68 2 -1 8 0 721.89 25.95 3 1 8 0 723.52 26.10 2 2 8 0 70.61 6.75 2 2 8 0 60.95 6.42 3 -2 8 0 74.45 6.21 2 -2 8 0 88.65 7.82 3 -3 8 0 224.72 10.53 2 3 8 0 213.38 11.00 3 3 8 0 206.22 11.65 2 -3 8 0 208.72 12.02 3 -4 8 0 175.24 9.43 2 -4 8 0 178.86 11.04 3 4 8 0 163.79 9.61 3 4 8 0 189.88 11.25 2 -5 8 0 -4.44 2.95 2 -5 8 0 2.06 4.19 3 -5 -8 0 -0.68 3.02 1 5 8 0 5.03 4.51 2 -6 8 0 239.70 13.65 3 -6 -8 0 236.39 12.37 1 6 8 0 226.32 13.76 2 7 8 0 55.83 8.63 2 -7 -8 0 50.91 6.93 1 -7 8 0 55.37 8.27 3 8 8 0 32.53 7.09 2 -8 -8 0 37.25 6.80 1 -8 8 0 43.86 7.99 3 -9 8 0 59.50 8.96 3 9 8 0 60.28 9.55 2 -9 -8 0 60.38 8.47 1 -10 8 0 43.13 8.29 3 10 8 0 21.79 7.36 2 -10 -8 0 43.55 8.39 1 -11 8 0 26.83 7.93 3 11 8 0 21.78 7.57 2 -11 -8 0 32.21 8.38 1 -12 -8 0 0.42 6.62 1 12 8 0 14.99 7.55 2 13 8 0 54.39 11.09 2 -13 -8 0 63.83 11.35 1 0 9 0 3.63 4.08 3 0 9 0 -4.68 2.72 2 1 9 0 58.39 6.75 3 1 9 0 44.73 6.29 2 -1 9 0 41.87 5.95 2 -1 9 0 55.33 6.50 3 2 9 0 0.68 3.62 2 2 9 0 -2.86 3.49 3 -2 9 0 2.00 3.41 2 -2 9 0 1.70 4.33 3 -3 9 0 270.75 14.21 3 -3 9 0 268.53 12.59 2 3 9 0 269.07 13.15 3 3 9 0 243.75 13.57 2 4 9 0 179.37 10.56 3 -4 9 0 172.50 11.37 3 4 9 0 163.01 11.18 2 5 9 0 27.93 6.55 2 -5 9 0 43.75 7.07 3 -6 9 0 65.14 8.27 3 6 9 0 50.23 8.55 2 -7 9 0 421.71 20.25 3 7 9 0 455.33 21.33 2 8 9 0 246.13 15.76 2 -8 9 0 246.06 15.32 3 9 9 0 -1.90 5.22 2 -9 9 0 -1.17 4.70 3 10 9 0 9.71 7.43 2 -10 9 0 12.77 7.28 3 -11 9 0 8.02 6.85 3 11 9 0 -3.85 7.17 2 12 9 0 519.73 27.67 2 0 10 0 1332.72 43.21 2 0 10 0 1294.30 42.77 3 1 10 0 246.87 13.53 2 -1 10 0 257.51 14.04 3 -1 10 0 251.60 12.95 2 1 10 0 241.30 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14 0 34.77 9.43 3 -3 14 0 50.35 10.92 3 -4 14 0 88.95 13.26 3 5 14 0 -7.82 7.85 2 6 14 0 36.62 10.82 2 0 15 0 -5.02 7.81 3 1 15 0 69.46 12.66 3 -1 15 0 85.70 13.54 3 16 0 -1 7.30 7.78 1 15 0 -1 -0.98 6.12 1 14 0 -1 2.46 5.16 1 13 0 -1 -4.98 4.11 1 12 0 -1 -6.92 4.01 1 11 0 -1 2.57 3.60 1 10 0 -1 5.00 3.77 1 9 0 -1 -0.35 3.23 2 9 0 -1 -6.49 2.86 1 -8 0 1 -1.05 1.65 3 8 0 -1 1.68 2.69 2 8 0 -1 -2.75 2.55 1 -7 0 1 -1.91 1.35 3 7 0 -1 -1.17 1.93 2 7 0 -1 2.42 2.37 1 6 0 -1 -2.51 1.74 1 6 0 -1 1.57 2.29 2 -6 0 1 -0.82 1.22 3 5 0 -1 -1.87 1.73 2 5 0 -1 -0.37 1.64 1 -5 0 1 0.61 1.13 3 4 0 -1 -0.67 1.67 1 -4 0 1 2.04 1.09 3 4 0 -1 -0.32 1.55 2 3 0 -1 -0.90 1.10 2 -3 0 1 1.96 0.88 3 3 0 -1 1.12 1.44 1 2 0 -1 1.24 0.75 2 2 0 -1 -1.04 0.70 1 0 0 -1 -0.05 0.34 1 -1 0 -1 0.01 0.93 1 2 0 1 2.14 1.42 1 3 0 1 -0.72 1.66 1 4 0 1 -0.04 1.98 1 5 0 1 -2.02 1.74 1 6 0 1 -0.16 2.16 1 7 0 1 -0.89 2.85 1 8 0 1 1.64 3.24 1 9 0 1 -2.69 3.49 1 10 0 1 -5.17 3.65 1 11 0 1 -3.93 4.52 1 -13 0 -1 -5.53 5.26 1 -14 0 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1465.64 40.85 2 2 -1 -1 1392.15 40.43 1 -2 1 1 1424.44 38.82 3 2 1 -1 1471.77 40.45 1 1 1 -1 5324.58 150.72 1 1 -1 -1 4914.22 145.68 1 1 1 -1 5667.52 146.86 2 -1 1 1 5339.26 139.82 3 0 1 1 40.45 1.99 2 0 1 -1 44.30 2.23 2 1 1 1 2998.41 82.83 2 -1 -1 -1 3003.86 82.50 1 1 -1 1 2946.62 82.47 1 -2 -1 -1 430.57 13.93 1 2 -1 1 414.96 13.35 1 3 1 1 148.31 6.92 2 3 -1 1 160.87 6.82 1 4 1 1 227.05 9.79 2 4 1 1 240.10 9.73 1 4 -1 1 211.18 9.11 1 5 1 1 656.18 22.60 2 5 -1 1 660.57 22.23 1 5 1 1 683.96 22.68 1 6 -1 1 553.04 19.67 1 6 1 1 537.65 19.84 1 6 1 1 544.31 19.99 2 7 1 1 4.15 3.23 1 7 -1 1 -4.01 2.14 1 7 1 1 -0.15 2.94 2 8 -1 1 78.84 7.15 1 8 1 1 77.30 7.28 1 9 1 1 58.34 6.99 1 9 -1 1 61.51 6.68 1 10 -1 1 644.86 25.50 1 10 1 1 623.69 25.36 1 11 -1 1 51.27 8.34 1 -12 -1 -1 87.00 9.58 1 12 -1 1 103.50 10.25 1 -13 -1 -1 15.53 8.27 1 13 -1 1 11.86 6.04 1 -14 1 -1 101.27 11.24 1 -14 -1 -1 96.48 12.97 1 -15 1 -1 4.53 9.64 1 -15 -1 -1 1.30 9.40 1 16 -2 -1 417.88 23.59 1 -16 -2 1 409.49 24.19 1 15 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65.89 11.36 1 -14 -7 -1 1.62 9.06 1 13 8 -1 440.43 25.19 2 12 8 -1 60.36 10.80 2 11 8 -1 193.97 15.05 2 -11 8 1 184.57 13.67 3 -10 8 1 15.19 6.61 3 10 8 -1 18.62 6.81 2 9 8 -1 248.89 15.80 2 -9 8 1 256.83 15.03 3 -8 8 1 71.30 8.41 3 8 8 -1 56.31 9.04 2 -7 8 1 627.96 25.07 3 7 8 -1 640.92 26.11 2 -6 8 1 155.49 10.86 3 6 8 -1 151.40 10.99 2 5 8 -1 83.02 8.19 2 5 8 -1 102.98 7.26 3 -5 8 1 88.91 8.52 3 4 8 -1 659.03 23.08 3 -4 8 1 687.35 25.26 3 4 8 -1 660.46 25.39 2 -4 8 1 698.70 23.02 2 3 8 -1 133.62 9.09 2 3 8 -1 133.79 8.44 3 -3 8 1 112.29 8.72 3 -3 8 1 143.35 7.93 2 2 8 -1 327.67 14.12 3 2 8 -1 325.29 14.73 2 -2 8 1 311.52 14.56 3 -2 8 1 306.03 13.05 2 -1 8 1 22.44 4.41 2 1 8 -1 20.58 4.73 3 1 8 -1 17.08 4.37 2 -1 8 1 13.78 4.68 3 0 8 1 230.97 11.51 2 0 8 -1 220.85 11.67 3 0 8 1 246.15 12.33 3 0 8 -1 244.69 11.79 2 1 8 1 96.74 7.24 2 -1 8 -1 92.64 7.10 2 -1 -8 -1 95.47 5.96 1 -1 8 -1 83.97 7.38 3 1 8 1 88.84 7.40 3 -2 -8 -1 1228.04 39.58 1 2 8 1 1295.02 40.27 3 -2 8 -1 1322.29 41.56 3 -2 8 -1 1364.17 41.53 2 2 8 1 1343.48 42.28 2 3 8 1 204.70 10.79 3 3 8 1 217.69 11.70 2 -3 8 -1 197.28 10.45 2 -3 8 -1 214.88 12.22 3 -3 -8 -1 190.58 9.87 1 4 8 1 31.76 5.77 2 -4 -8 -1 40.59 5.57 1 -4 8 -1 26.43 5.18 2 4 8 1 26.37 5.17 3 -4 8 -1 24.24 5.58 3 -5 8 -1 317.96 13.85 2 -5 8 -1 307.70 15.49 3 -5 -8 -1 297.35 14.23 1 5 8 1 316.87 16.06 2 6 8 1 141.12 10.66 2 -6 8 -1 157.97 9.51 2 -6 -8 -1 149.48 9.91 1 -6 8 -1 143.35 10.58 3 -7 -8 -1 578.52 23.56 1 -7 8 -1 584.85 24.22 3 7 8 1 585.14 25.21 2 8 8 1 250.60 15.90 2 -8 -8 -1 258.50 14.95 1 -8 8 -1 291.30 15.98 3 -9 8 -1 109.64 10.62 3 9 8 1 113.38 11.47 2 -9 -8 -1 110.38 10.34 1 -10 -8 -1 3.06 5.62 1 -10 8 -1 7.95 6.55 3 10 8 1 0.22 6.21 2 -11 -8 -1 309.06 18.08 1 -11 8 -1 298.66 17.62 3 11 8 1 286.70 18.84 2 12 8 1 12.05 8.32 2 -12 -8 -1 38.51 9.23 1 -13 -8 -1 293.48 19.47 1 13 9 -1 1.34 8.73 2 -12 9 1 87.85 12.37 3 12 9 -1 94.89 13.68 2 11 9 -1 11.33 6.74 2 -11 9 1 6.89 6.46 3 10 9 -1 196.75 14.83 2 -10 9 1 186.57 14.20 3 9 9 -1 -4.64 4.86 2 -9 9 1 -5.60 5.07 3 8 9 -1 37.50 8.09 2 -8 9 1 35.91 7.98 3 -7 9 1 -0.46 4.95 3 7 9 -1 4.53 5.50 2 -6 9 1 378.51 17.94 3 6 9 -1 330.84 17.52 2 -5 9 1 325.65 16.34 3 5 9 -1 316.61 16.39 2 4 9 -1 116.12 9.63 2 -4 9 1 136.02 10.40 3 4 9 -1 127.95 8.85 3 3 9 -1 40.00 6.10 3 -3 9 1 38.43 6.65 3 3 9 -1 47.32 6.15 2 -3 9 1 47.94 5.63 2 -2 9 1 65.90 6.54 2 2 9 -1 67.66 7.51 2 2 9 -1 68.63 7.06 3 -2 9 1 73.93 7.58 3 1 9 -1 60.00 6.96 2 -1 9 1 70.76 7.74 3 1 9 -1 61.49 6.91 3 -1 9 1 80.42 7.23 2 0 9 1 -3.57 3.65 3 0 9 -1 1.46 3.57 2 0 9 -1 -1.50 3.29 3 0 9 1 -5.47 3.13 2 1 9 1 157.60 9.92 2 -1 9 -1 165.19 9.89 2 -1 9 -1 169.98 10.92 3 1 9 1 156.53 10.24 3 2 9 1 263.41 13.34 3 2 9 1 295.16 14.11 2 -2 9 -1 258.33 12.97 2 -2 9 -1 262.19 14.25 3 -3 9 -1 0.39 3.40 2 3 9 1 5.14 4.45 2 3 9 1 -4.50 3.54 3 -3 9 -1 -0.37 4.32 3 4 9 1 98.49 8.93 2 4 9 1 110.63 8.65 3 -4 9 -1 108.27 8.00 2 -4 9 -1 107.73 9.31 3 5 9 1 58.26 7.95 2 -5 9 -1 71.15 8.46 3 6 9 1 66.09 9.27 2 -6 9 -1 62.11 8.54 3 7 9 1 -3.67 4.18 2 -7 9 -1 -9.85 4.41 3 8 9 1 54.80 9.10 2 -8 9 -1 38.13 8.49 3 9 9 1 -7.27 4.65 2 -9 9 -1 -2.29 6.07 3 10 9 1 87.37 11.47 2 -10 9 -1 112.12 11.82 3 11 9 1 -2.11 7.57 2 -11 9 -1 0.37 7.10 3 12 9 1 -6.80 6.68 2 12 10 -1 10.96 8.72 2 -12 10 1 4.44 8.82 3 11 10 -1 -7.16 7.28 2 -11 10 1 6.08 7.91 3 -10 10 1 -1.28 6.88 3 10 10 -1 12.63 7.44 2 -9 10 1 81.75 10.97 3 9 10 -1 82.85 11.75 2 -8 10 1 93.10 10.70 3 8 10 -1 77.44 10.07 2 -7 10 1 1.71 6.00 3 7 10 -1 -1.36 4.78 2 6 10 -1 215.43 14.40 2 -6 10 1 214.36 14.35 3 -5 10 1 25.07 6.42 3 5 10 -1 41.08 7.25 2 4 10 -1 -1.75 4.23 2 -4 10 1 -0.39 4.71 3 4 10 -1 0.98 3.99 3 3 10 -1 81.80 8.53 2 -3 10 1 107.13 9.34 3 3 10 -1 79.38 8.09 3 2 10 -1 405.30 17.90 3 2 10 -1 401.38 18.28 2 -2 10 1 392.04 18.64 3 1 10 -1 107.52 9.13 2 -1 10 1 110.19 8.86 2 1 10 -1 109.50 9.25 3 -1 10 1 133.11 10.24 3 0 10 1 60.72 7.68 3 0 10 -1 68.78 7.85 3 0 10 -1 65.86 7.27 2 0 10 1 59.68 6.84 2 1 10 1 237.48 13.72 3 -1 10 -1 265.00 13.52 2 1 10 1 264.99 13.78 2 -1 10 -1 273.07 14.53 3 -2 10 -1 127.01 10.22 3 2 10 1 139.90 10.17 3 -2 10 -1 145.17 9.62 2 2 10 1 131.35 9.86 2 3 10 1 58.66 7.32 3 -3 10 -1 62.81 6.94 2 3 10 1 55.21 7.14 2 -3 10 -1 60.93 7.72 3 -4 10 -1 3.43 5.05 3 4 10 1 1.90 4.81 2 5 10 1 54.72 8.69 2 -5 10 -1 58.75 8.95 3 6 10 1 72.81 10.04 2 -6 10 -1 64.46 8.50 3 7 10 1 9.91 6.27 2 -7 10 -1 5.72 6.05 3 8 10 1 22.45 7.93 2 -8 10 -1 25.03 8.07 3 9 10 1 2.04 7.26 2 -9 10 -1 11.01 7.53 3 10 10 1 -3.67 7.43 2 -10 10 -1 0.83 7.48 3 -11 10 -1 60.80 11.79 3 11 10 1 54.66 11.46 2 11 11 -1 14.49 9.66 2 -11 11 1 9.87 8.20 3 -10 11 1 56.77 11.79 3 10 11 -1 48.68 11.25 2 9 11 -1 81.31 11.33 2 -9 11 1 57.81 11.01 3 8 11 -1 338.89 20.14 2 -8 11 1 348.23 19.99 3 7 11 -1 247.84 16.25 2 -7 11 1 272.54 16.84 3 -6 11 1 108.82 11.18 3 6 11 -1 126.63 11.67 2 5 11 -1 109.69 10.48 2 -5 11 1 102.39 10.13 3 4 11 -1 1069.39 39.02 2 -4 11 1 1070.44 38.87 3 3 11 -1 573.80 23.66 3 3 11 -1 599.12 25.03 2 -3 11 1 589.57 25.24 3 2 11 -1 18.03 6.07 3 -2 11 1 30.57 7.38 3 2 11 -1 11.09 5.57 2 1 11 -1 788.46 29.41 2 1 11 -1 780.09 29.13 3 -1 11 1 716.51 29.10 3 0 11 1 1.86 4.27 2 0 11 -1 3.61 4.74 2 0 11 1 -1.73 4.95 3 0 11 -1 -2.12 4.16 3 1 11 1 357.09 17.80 3 -1 11 -1 322.49 17.56 3 1 11 1 360.34 17.29 2 -1 11 -1 398.02 17.53 2 -2 11 -1 -0.35 5.35 3 2 11 1 4.11 5.27 3 2 11 1 -3.95 4.46 2 3 11 1 389.16 18.72 2 -3 11 -1 330.02 18.37 3 3 11 1 361.76 17.53 3 -4 11 -1 342.30 18.65 3 4 11 1 342.54 18.19 2 -5 11 -1 173.40 13.60 3 5 11 1 191.84 14.00 2 -6 11 -1 85.70 11.68 3 6 11 1 90.89 10.86 2 -7 11 -1 266.09 17.11 3 7 11 1 230.13 16.56 2 -8 11 -1 331.01 19.35 3 8 11 1 294.28 19.27 2 9 11 1 6.68 7.11 2 -9 11 -1 4.00 8.49 3 -10 11 -1 18.96 9.65 3 10 11 1 -0.21 7.80 2 -10 12 1 -6.82 8.26 3 9 12 -1 83.83 13.40 2 -9 12 1 91.84 11.80 3 8 12 -1 68.12 11.93 2 -8 12 1 75.67 11.68 3 7 12 -1 56.83 10.72 2 -7 12 1 58.80 10.40 3 6 12 -1 21.42 7.11 2 -6 12 1 8.98 7.04 3 5 12 -1 3.49 6.40 2 -5 12 1 -1.53 6.17 3 4 12 -1 80.74 9.83 2 -4 12 1 53.73 9.93 3 -3 12 1 139.38 12.08 3 3 12 -1 149.74 12.06 3 3 12 -1 119.18 11.13 2 2 12 -1 266.03 15.90 3 -2 12 1 298.78 17.27 3 2 12 -1 280.82 16.17 2 -1 12 1 -3.71 5.49 3 1 12 -1 3.82 5.72 2 1 12 -1 11.37 6.32 3 0 12 -1 38.29 7.83 2 0 12 -1 28.80 7.85 3 0 12 1 35.73 7.71 3 1 12 1 -1.47 5.59 3 -1 12 -1 0.30 5.09 3 -2 12 -1 356.94 19.03 3 2 12 1 356.42 18.52 2 2 12 1 358.27 18.47 3 3 12 1 37.78 8.19 2 -3 12 -1 33.94 7.89 3 -4 12 -1 75.24 9.62 3 4 12 1 81.55 9.93 2 -5 12 -1 21.43 8.03 3 5 12 1 28.78 8.33 2 -6 12 -1 21.53 8.68 3 6 12 1 7.40 7.55 2 -7 12 -1 83.31 12.01 3 7 12 1 74.71 12.17 2 8 12 1 57.67 11.53 2 -8 12 -1 51.48 10.54 3 9 12 1 -3.76 8.86 2 -9 12 -1 4.20 7.92 3 8 13 -1 22.88 9.99 2 -7 13 1 7.76 8.20 3 7 13 -1 -9.72 6.98 2 -6 13 1 35.64 9.67 3 6 13 -1 61.30 10.71 2 5 13 -1 29.33 8.99 2 -5 13 1 4.16 7.73 3 -4 13 1 14.51 7.53 3 4 13 -1 7.10 6.72 2 -3 13 1 28.98 9.28 3 3 13 -1 47.37 9.43 2 2 13 -1 68.48 10.06 2 2 13 -1 66.56 10.12 3 -2 13 1 61.19 10.18 3 -1 13 1 -12.77 5.93 3 1 13 -1 12.57 7.22 3 0 13 1 9.06 6.49 3 0 13 -1 19.30 7.92 3 1 13 1 77.45 10.10 3 -1 13 -1 81.85 11.61 3 2 13 1 1.01 6.89 3 -2 13 -1 6.84 6.18 3 -3 13 -1 30.47 8.43 3 -4 13 -1 -11.19 5.46 3 4 13 1 -2.94 6.30 2 -5 13 -1 -0.39 6.80 3 5 13 1 10.57 7.69 2 -6 13 -1 51.87 10.50 3 6 13 1 37.54 9.87 2 7 13 1 141.31 15.22 2 6 14 -1 198.02 16.78 2 -5 14 1 52.03 11.99 3 5 14 -1 90.52 11.77 2 4 14 -1 8.32 8.01 2 -4 14 1 -18.04 6.90 3 -3 14 1 7.01 7.33 3 -2 14 1 59.92 11.38 3 2 14 -1 69.46 10.90 3 1 14 -1 48.67 10.70 3 -1 14 1 58.20 11.12 3 0 14 -1 89.52 11.75 3 0 14 1 93.01 12.73 3 1 14 1 93.83 11.81 3 -1 14 -1 78.49 12.54 3 -2 14 -1 105.74 12.95 3 -3 14 -1 111.72 13.20 3 -4 14 -1 8.91 7.87 3 6 14 1 147.05 15.29 2 1 15 -1 5.93 8.75 3 -1 15 1 3.71 8.90 3 0 15 1 12.19 8.93 3 0 15 -1 1.14 9.17 3 -1 15 -1 105.98 14.82 3 16 0 -2 195.62 15.35 1 15 0 -2 98.98 11.31 1 14 0 -2 71.29 8.74 1 13 0 -2 26.32 6.26 1 12 0 -2 17.03 5.17 1 11 0 -2 2008.09 61.84 1 11 0 -2 1928.72 61.01 2 10 0 -2 115.78 8.29 2 10 0 -2 92.92 7.96 1 9 0 -2 231.82 11.89 1 9 0 -2 221.52 11.26 2 -8 0 2 12.92 2.23 3 8 0 -2 12.87 3.39 1 8 0 -2 12.16 3.36 2 -7 0 2 1711.11 45.95 3 7 0 -2 1692.73 50.48 2 6 0 -2 884.99 28.22 2 -6 0 2 900.98 25.31 3 6 0 -2 950.31 28.97 1 5 0 -2 9506.29 263.67 1 5 0 -2 9835.65 264.58 2 4 0 -2 533.00 16.56 2 3 0 -2 57.91 3.11 2 3 0 -2 58.14 3.38 1 2 0 -2 3020.41 84.60 2 2 0 -2 3058.72 83.89 1 1 0 -2 350.63 10.82 1 0 0 -2 5804.70 158.88 1 -1 0 -2 1131.37 32.69 1 -2 0 -2 292.68 10.64 1 -3 0 -2 2240.66 63.99 1 -4 0 -2 3894.22 109.15 1 -9 0 -2 386.01 18.09 1 -10 0 -2 41.59 7.55 1 -11 0 -2 29.74 7.28 1 -12 0 -2 72.69 10.20 1 -13 0 -2 91.66 12.25 1 -14 0 -2 0.02 7.44 1 16 1 -2 9.23 7.39 1 16 -1 -2 21.47 8.18 1 15 -1 -2 19.25 6.92 1 15 1 -2 28.50 7.82 1 14 1 -2 52.67 9.33 1 14 -1 -2 45.97 8.21 1 13 -1 -2 57.07 8.90 1 13 1 -2 50.80 8.45 1 12 1 -2 47.67 7.58 2 12 -1 -2 48.36 6.80 1 12 1 -2 54.75 8.03 1 11 1 -2 6.88 4.11 2 11 -1 -2 16.40 5.07 1 11 1 -2 8.24 5.05 1 10 1 -2 156.13 9.89 2 10 -1 -2 137.79 9.49 1 10 1 -2 138.25 9.48 1 -9 1 2 906.72 26.49 3 9 1 -2 899.63 30.84 2 9 1 -2 867.88 30.70 1 9 -1 -2 937.34 31.22 1 8 -1 -2 650.20 22.15 2 8 1 -2 618.23 22.61 2 -8 1 2 647.31 19.52 3 8 1 -2 646.20 22.97 1 7 1 -2 26.88 4.37 1 7 -1 -2 26.00 3.58 2 -7 1 2 24.49 3.20 3 7 1 -2 29.12 4.29 2 7 -1 -2 30.08 4.25 1 6 1 -2 2056.07 57.95 1 6 -1 -2 1986.65 58.02 1 -6 1 2 1948.18 53.85 3 6 -1 -2 2085.25 57.27 2 6 1 -2 1879.20 57.72 2 5 1 -2 1752.06 53.47 2 5 1 -2 1863.96 53.51 1 5 -1 -2 1807.73 53.53 1 -5 1 2 1938.26 50.45 3 5 -1 -2 1933.23 52.91 2 4 -1 -2 16.11 2.18 2 -4 1 2 22.60 2.49 3 4 -1 -2 22.10 2.92 1 4 1 -2 24.94 2.99 2 4 1 -2 22.89 2.65 1 3 -1 -2 1646.15 47.55 1 3 -1 -2 1614.29 47.41 2 3 1 -2 1751.55 47.83 2 -3 1 2 1712.20 45.45 3 3 1 -2 1673.37 47.33 1 2 -1 -2 111.12 4.65 1 2 1 -2 106.36 4.26 1 2 1 -2 111.56 4.68 2 1 1 -2 854.17 25.34 1 1 1 -2 898.74 25.95 2 1 -1 -2 923.86 25.88 1 0 1 -2 41.67 2.25 1 0 1 -2 42.60 2.83 2 0 -1 -2 50.02 2.89 1 -1 -1 -2 1295.42 37.77 1 -1 1 -2 1322.21 37.26 1 2 1 2 4.70 2.04 2 -2 1 -2 1.63 1.90 1 -2 -1 -2 0.25 1.86 1 -3 -1 -2 1206.69 37.02 1 3 1 2 1264.70 37.34 2 -4 -1 -2 75.31 5.78 1 4 -1 2 77.81 5.29 1 -5 -1 -2 39.37 5.19 1 5 -1 2 35.42 4.76 1 -6 -1 -2 377.51 15.80 1 6 -1 2 357.25 15.01 1 7 -1 2 358.29 15.73 1 -7 -1 -2 362.35 16.30 1 8 -1 2 65.31 6.75 1 -8 -1 -2 95.29 8.33 1 -9 -1 -2 -3.33 4.69 1 9 -1 2 -1.33 3.49 1 -10 -1 -2 160.38 12.23 1 -11 1 -2 423.87 20.79 1 -11 -1 -2 428.88 21.75 1 -12 1 -2 60.38 9.68 1 -12 -1 -2 59.54 10.28 1 -13 1 -2 65.80 12.36 1 -13 -1 -2 78.59 11.52 1 -14 1 -2 -5.29 8.48 1 -14 -1 -2 -8.82 5.22 1 -15 1 -2 98.28 13.78 1 16 -2 -2 106.73 12.38 1 16 2 -2 95.21 12.15 1 15 -2 -2 -6.68 6.34 1 15 2 -2 -8.07 4.79 1 14 -2 -2 -1.77 4.83 1 14 2 -2 -4.00 5.93 1 14 2 -2 -1.18 5.33 2 13 2 -2 318.37 17.68 2 13 -2 -2 344.54 18.11 1 13 2 -2 343.33 17.91 1 12 -2 -2 82.28 8.38 1 12 2 -2 78.73 8.53 2 12 2 -2 73.34 8.39 1 11 2 -2 57.14 6.76 1 11 -2 -2 53.34 7.12 1 11 2 -2 53.52 7.30 2 10 2 -2 48.15 6.79 2 10 -2 -2 44.65 5.93 1 10 2 -2 50.33 6.02 1 9 2 -2 544.63 20.84 1 9 -2 -2 558.71 21.12 1 -9 2 2 551.19 18.12 3 9 2 -2 513.73 20.92 2 8 -2 -2 8.98 3.63 1 -8 2 2 10.96 2.95 3 8 2 -2 9.90 3.54 2 8 2 -2 10.47 3.58 1 7 2 -2 1362.33 41.44 2 7 -2 -2 1297.55 40.95 1 -7 2 2 1303.20 37.86 3 7 2 -2 1354.22 40.97 1 6 -2 -2 -1.84 1.85 1 6 2 -2 -0.74 1.85 1 6 2 -2 -1.43 2.28 2 -6 2 2 2.12 2.00 3 5 2 -2 119.24 6.46 2 -5 2 2 118.55 5.84 3 5 -2 -2 113.50 6.35 1 5 2 -2 115.73 6.15 1 4 2 -2 376.53 13.35 2 4 2 -2 370.87 12.52 1 4 -2 -2 365.29 12.88 1 -4 2 2 361.20 12.27 3 -3 2 2 1981.73 52.62 3 3 -2 -2 1981.27 54.70 1 3 2 -2 1898.51 55.13 2 3 2 -2 1868.63 54.03 1 2 2 -2 9.09 1.34 1 -2 2 2 6.94 2.00 3 2 2 -2 12.87 2.19 2 2 -2 -2 5.04 1.53 1 -1 2 2 14.71 2.16 3 1 -2 -2 13.69 2.14 1 -1 2 2 11.93 1.42 2 1 2 -2 13.12 1.14 1 1 2 -2 11.79 2.04 2 0 -2 -2 4.29 1.56 1 0 2 -2 1.35 1.55 2 0 2 2 2.69 1.31 2 0 2 -2 3.18 0.95 1 1 2 2 509.90 16.51 2 -1 2 -2 520.69 15.58 1 -1 2 -2 496.89 16.61 2 -1 -2 -2 533.64 16.72 1 -2 -2 -2 101.47 5.61 1 2 -2 2 102.50 4.89 1 2 2 2 103.68 5.59 2 -3 -2 -2 431.15 15.03 1 3 -2 2 387.05 13.95 1 -4 -2 -2 20.82 3.87 1 4 -2 2 22.34 3.58 1 4 2 2 25.71 3.83 2 5 -2 2 528.37 18.67 1 5 2 2 515.20 19.36 2 -5 -2 -2 515.71 19.32 1 6 2 2 400.42 16.43 2 -6 -2 -2 379.46 16.37 1 6 -2 2 397.66 15.78 1 7 2 2 263.88 13.26 2 7 -2 2 264.33 12.87 1 -7 -2 -2 263.26 13.78 1 -8 -2 -2 128.72 9.83 1 8 -2 2 125.23 9.22 1 -9 -2 -2 7.90 5.68 1 9 -2 2 6.66 4.99 1 10 -2 2 7.93 5.31 1 -10 -2 -2 9.96 5.73 1 -11 -2 -2 138.30 11.66 1 -12 -2 -2 43.86 8.81 1 -12 2 -2 45.79 8.71 1 -13 -2 -2 12.83 7.25 1 -13 2 -2 26.10 9.27 1 -14 -2 -2 6.37 6.98 1 -14 2 -2 20.32 9.91 1 -15 2 -2 3.58 10.93 1 16 -3 -2 217.86 16.72 1 -16 -3 2 206.46 16.99 1 15 3 -2 177.32 14.55 2 15 -3 -2 170.06 13.52 1 15 3 -2 134.66 12.81 1 14 3 -2 99.59 10.82 2 14 3 -2 81.35 10.00 1 14 -3 -2 99.70 10.40 1 13 3 -2 2.10 5.42 1 13 3 -2 -1.20 5.06 2 13 -3 -2 1.93 5.14 1 12 3 -2 539.79 23.49 1 12 -3 -2 528.28 23.36 1 12 3 -2 549.46 24.05 2 11 3 -2 32.01 6.90 2 11 3 -2 31.28 6.15 1 11 -3 -2 37.01 6.92 1 10 3 -2 990.49 35.58 2 -10 3 2 981.80 31.39 3 10 3 -2 1079.35 35.36 1 10 -3 -2 1015.02 35.03 1 9 3 -2 7.00 3.87 2 9 -3 -2 4.29 3.32 1 -9 3 2 3.96 3.09 3 9 3 -2 4.24 3.48 1 8 -3 -2 363.45 15.80 1 8 3 -2 390.27 16.49 2 8 3 -2 377.96 15.65 1 -8 3 2 414.11 14.74 3 7 3 -2 1477.05 46.95 2 7 -3 -2 1544.20 46.53 1 7 3 -2 1528.35 46.13 1 -7 3 2 1542.93 43.83 3 -6 3 2 2222.87 59.98 3 6 3 -2 2200.14 62.45 1 6 -3 -2 2149.14 62.68 1 6 3 -2 2059.72 63.42 2 -5 3 2 1237.55 35.61 3 5 3 -2 1229.88 37.79 2 5 -3 -2 1217.15 36.91 1 5 3 -2 1229.22 36.58 1 4 -3 -2 415.02 14.37 1 -4 3 2 422.57 14.23 3 4 3 -2 388.54 14.94 2 4 3 -2 412.43 13.82 1 -4 3 2 430.55 12.71 2 3 -3 -2 94.17 5.08 1 3 3 -2 89.52 5.64 2 -3 3 2 106.16 5.74 3 3 3 -2 98.36 4.55 1 -3 3 2 91.87 3.66 2 2 3 -2 14.97 2.59 2 -2 3 2 12.17 1.72 2 -2 3 2 20.41 2.98 3 2 3 -2 12.83 1.63 1 2 -3 -2 19.60 2.53 1 -1 3 2 3077.34 86.66 2 -1 3 2 3217.26 83.88 3 1 3 -2 3221.93 87.81 2 1 -3 -2 2997.51 86.66 1 0 3 -2 33.03 3.34 2 0 -3 -2 40.60 3.30 1 0 3 2 32.01 3.41 3 0 3 2 30.51 2.89 2 -1 -3 -2 377.18 12.94 1 -1 3 -2 353.10 12.94 2 1 3 2 371.96 12.92 2 -2 -3 -2 32.27 3.47 1 2 3 2 38.19 3.70 2 -2 3 -2 32.51 3.68 2 2 -3 2 35.70 2.95 1 -3 -3 -2 158.29 8.01 1 3 -3 2 164.82 7.15 1 3 3 2 156.01 8.20 2 4 -3 2 808.26 25.55 1 4 3 2 834.68 27.11 2 -4 -3 -2 778.37 26.58 1 5 3 2 1355.13 42.97 2 -5 -3 -2 1386.92 42.87 1 5 -3 2 1366.98 41.55 1 6 -3 2 386.58 15.67 1 6 3 2 385.03 16.75 2 -6 -3 -2 407.67 16.93 1 -7 -3 -2 4.07 3.52 1 7 3 2 -1.87 3.25 2 7 -3 2 -2.72 2.84 1 8 3 2 231.20 12.92 2 8 -3 2 184.95 11.34 1 -8 -3 -2 221.64 12.83 1 -9 -3 -2 98.69 9.13 1 9 3 2 98.69 9.07 2 9 -3 2 99.96 8.83 1 10 -3 2 556.18 23.62 1 -10 -3 -2 546.64 24.14 1 -11 -3 -2 -3.22 5.22 1 11 -3 2 -0.61 5.05 1 -12 -3 -2 62.76 10.57 1 -13 -3 -2 8.20 7.48 1 -13 3 -2 19.68 8.31 1 -14 -3 -2 148.89 14.03 1 -14 3 -2 152.44 16.04 1 -16 -4 2 82.64 15.02 1 16 -4 -2 92.79 11.29 1 16 4 -2 75.12 12.99 2 15 4 -2 69.01 11.41 2 15 -4 -2 76.43 11.34 1 -15 -4 2 68.16 12.05 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3 2 6 -2 1537.26 48.49 2 -2 6 2 1677.20 46.73 2 -1 6 2 27.35 3.73 2 1 -6 -2 24.89 3.41 1 1 6 -2 26.82 4.32 2 -1 6 2 21.40 4.26 3 0 6 2 1363.64 40.02 3 0 6 -2 1341.24 41.42 2 0 -6 -2 1340.79 39.99 1 0 6 2 1337.31 40.53 2 -1 -6 -2 0.30 2.15 1 1 6 2 1.26 2.63 2 -1 6 -2 1.08 2.64 2 1 6 2 1.44 2.76 3 2 6 2 971.87 30.84 2 -2 -6 -2 974.61 30.01 1 2 6 2 947.38 29.08 3 2 -6 2 900.72 27.17 1 -2 6 -2 896.81 30.11 2 3 -6 2 232.66 9.02 1 -3 -6 -2 253.38 11.32 1 3 6 2 225.67 11.38 2 -3 6 -2 240.87 11.02 2 4 -6 2 117.38 6.30 1 4 6 2 110.20 8.26 2 -4 -6 -2 103.01 7.50 1 -4 6 -2 111.36 7.33 2 5 -6 2 712.95 22.85 1 5 6 2 649.49 25.35 2 -5 6 -2 687.39 24.27 2 -5 -6 -2 661.98 24.83 1 -6 -6 -2 401.81 18.15 1 -6 6 -2 439.36 17.84 2 6 -6 2 415.21 16.37 1 6 6 2 440.09 19.19 2 7 6 2 453.97 20.59 2 7 -6 2 446.35 17.98 1 -7 6 -2 451.69 18.96 2 -7 -6 -2 447.72 19.72 1 8 6 2 1.26 4.50 2 8 -6 2 6.80 4.35 1 -8 6 -2 4.33 4.80 2 -8 -6 -2 5.50 5.10 1 9 6 2 346.36 18.66 2 9 -6 2 366.06 16.98 1 -9 6 -2 353.52 17.20 3 -9 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24.57 2 5 -7 -2 626.03 21.99 1 -5 7 2 632.32 23.72 3 5 7 -2 660.24 21.40 3 -5 -7 2 662.35 21.66 1 4 7 -2 1.81 3.35 2 4 7 -2 0.83 2.70 3 -4 7 2 -0.10 3.07 3 4 -7 -2 4.67 2.72 1 -4 -7 2 1.47 2.38 1 -4 7 2 2.72 2.47 2 3 7 -2 267.29 12.74 2 -3 7 2 274.28 10.64 2 -3 7 2 248.37 12.42 3 3 7 -2 252.15 11.48 3 3 -7 -2 257.81 10.78 1 -2 7 2 101.53 7.52 3 2 -7 -2 105.85 6.14 1 -2 7 2 108.90 6.56 2 2 7 -2 106.78 7.32 3 2 7 -2 106.76 7.71 2 1 -7 -2 940.63 29.15 1 -1 7 2 931.89 30.47 3 1 7 -2 921.56 31.15 2 -1 7 2 961.62 29.94 2 0 7 2 1.07 2.70 2 0 -7 -2 1.88 2.33 1 0 7 -2 -3.49 2.70 2 0 7 2 -4.30 2.20 3 1 7 2 258.81 11.63 2 1 7 2 249.66 11.54 3 -1 7 -2 234.91 11.38 2 -1 -7 -2 217.76 10.34 1 2 7 2 0.64 2.94 3 2 7 2 0.73 3.20 2 -2 -7 -2 -0.86 2.78 1 -2 7 -2 1.11 2.82 2 -3 7 -2 112.43 7.85 2 3 7 2 101.87 7.27 3 -3 -7 -2 124.10 7.85 1 3 7 2 107.88 8.20 2 4 7 2 175.06 10.97 2 -4 7 -2 195.75 10.23 2 -4 -7 -2 191.11 10.45 1 5 7 2 242.32 13.41 2 -5 -7 -2 228.27 12.28 1 -5 7 -2 224.47 11.68 2 6 7 2 4.43 4.67 2 -6 7 -2 0.96 3.72 2 -6 -7 -2 4.68 4.04 1 -7 7 -2 8.07 4.25 2 -7 -7 -2 12.53 5.16 1 7 7 2 11.00 5.87 2 -8 7 -2 60.10 8.71 3 -8 7 -2 56.71 7.42 2 8 7 2 61.40 8.89 2 -8 -7 -2 55.28 7.37 1 -9 -7 -2 5.43 5.59 1 -9 7 -2 8.92 6.37 3 9 7 2 13.00 6.16 2 -10 7 -2 216.86 14.27 3 -10 -7 -2 204.09 14.36 1 10 7 2 189.45 14.48 2 -11 -7 -2 -5.80 5.52 1 11 7 2 -2.85 6.32 2 -12 -7 -2 8.85 7.87 1 12 7 2 13.71 8.32 2 -13 -7 -2 17.12 8.17 1 14 8 -2 51.77 12.14 2 13 8 -2 -2.26 6.77 2 -12 8 2 160.88 13.08 3 12 8 -2 151.95 14.02 2 11 8 -2 18.75 7.50 2 -11 8 2 18.29 7.16 3 -10 8 2 80.71 8.90 3 10 8 -2 79.97 9.87 2 -9 8 2 -3.27 4.40 3 9 8 -2 -0.58 4.47 2 8 8 -2 -0.71 4.14 2 -8 8 2 -1.38 4.08 3 7 8 -2 96.80 9.16 2 -7 8 2 93.16 9.09 3 6 -8 -2 66.78 6.39 1 -6 8 2 69.25 8.03 3 6 8 -2 64.97 7.43 2 -5 8 2 304.59 15.05 3 5 -8 -2 296.32 12.55 1 5 8 -2 273.72 14.66 2 5 8 -2 271.53 12.32 3 -4 8 2 126.33 9.11 3 4 -8 -2 100.80 6.88 1 4 8 -2 102.45 7.52 3 4 8 -2 116.77 9.23 2 -3 8 2 20.97 4.02 2 3 -8 -2 20.57 3.66 1 3 8 -2 25.37 4.96 3 3 8 -2 16.61 5.13 2 -3 8 2 17.07 4.68 3 -2 8 2 164.29 8.60 2 2 -8 -2 132.66 7.52 1 -2 8 2 145.37 9.81 3 2 8 -2 153.96 9.34 3 2 8 -2 138.87 9.37 2 -1 8 2 69.12 5.96 2 1 8 -2 52.74 6.11 2 1 -8 -2 49.62 4.89 1 1 8 -2 61.49 6.61 3 -1 8 2 58.83 6.70 3 0 8 2 2.85 3.32 2 0 8 -2 -3.10 3.22 3 0 8 2 -0.11 3.28 3 0 -8 -2 -1.78 2.49 1 0 8 -2 0.12 3.14 2 1 8 2 287.58 13.76 2 -1 -8 -2 321.70 13.03 1 -1 8 -2 330.62 14.47 2 1 8 2 320.40 14.35 3 2 8 2 37.85 5.68 3 -2 8 -2 41.51 5.71 2 2 8 2 24.78 5.31 2 -2 -8 -2 34.36 4.98 1 3 8 2 318.72 15.19 2 -3 8 -2 306.20 14.15 2 3 8 2 318.72 14.02 3 -3 -8 -2 309.65 13.75 1 4 8 2 4.68 4.23 2 -4 8 -2 -0.25 3.09 2 -4 -8 -2 2.14 3.35 1 -5 8 -2 16.42 4.66 2 -5 -8 -2 13.99 4.96 1 5 8 2 14.39 5.58 2 -6 -8 -2 39.67 6.84 1 6 8 2 49.14 8.36 2 -6 8 -2 42.57 7.65 3 -6 8 -2 55.93 7.15 2 7 8 2 107.88 9.88 2 -7 8 -2 94.84 9.81 3 -7 -8 -2 115.48 9.80 1 8 8 2 56.54 9.34 2 -8 -8 -2 47.41 8.58 1 -8 8 -2 56.74 9.14 3 -9 8 -2 29.54 7.49 3 9 8 2 39.06 8.76 2 -9 -8 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142.73 14.88 1 -14 -3 -3 117.41 13.72 1 17 4 -3 112.92 15.57 2 16 -4 -3 85.94 12.27 1 16 4 -3 51.65 10.87 2 15 4 -3 29.44 8.71 1 15 -4 -3 29.71 7.86 1 15 4 -3 21.98 8.61 2 14 -4 -3 44.63 8.69 1 14 4 -3 41.84 8.78 1 14 4 -3 45.37 9.43 2 13 4 -3 103.71 10.17 1 13 -4 -3 97.64 9.91 1 13 4 -3 102.99 10.26 2 12 4 -3 79.00 9.01 2 12 -4 -3 72.15 8.30 1 12 4 -3 68.91 8.09 1 11 4 -3 532.96 21.92 1 11 4 -3 536.26 22.94 2 -11 4 3 504.33 19.49 3 10 4 -3 44.02 6.51 1 10 -4 -3 32.68 6.19 1 10 4 -3 24.33 5.56 2 -10 4 3 24.54 4.83 3 9 4 -3 299.32 14.67 2 9 4 -3 269.62 13.07 1 9 -4 -3 271.58 13.62 1 -9 4 3 276.94 12.47 3 8 4 -3 114.72 7.40 1 8 4 -3 107.04 8.26 2 -8 4 3 99.46 7.17 3 8 -4 -3 108.45 7.47 1 7 -4 -3 168.04 9.41 1 7 4 -3 167.80 9.86 2 -7 4 3 185.48 9.32 3 7 4 -3 178.59 8.89 1 6 4 -3 238.37 11.62 2 -6 4 3 265.69 11.24 3 6 -4 -3 251.70 11.13 1 6 4 -3 239.54 10.24 1 -6 4 3 254.84 8.58 2 5 -4 -3 215.56 9.74 1 5 4 -3 219.69 8.90 1 -5 4 3 206.12 9.82 3 5 4 -3 220.69 10.62 2 -5 4 3 219.61 7.08 2 4 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1 8 4 3 1.10 3.89 2 9 4 3 178.55 12.40 2 -9 4 -3 162.80 11.32 1 -9 -4 -3 152.04 11.63 1 -10 -4 -3 16.05 6.85 1 -10 4 -3 7.46 5.74 1 -11 4 -3 68.13 10.42 1 -11 -4 -3 47.85 8.93 1 -12 4 -3 64.99 11.96 1 -12 -4 -3 63.09 10.41 1 -13 -4 -3 148.49 13.70 1 -13 4 -3 116.98 14.15 1 -14 4 -3 1.19 8.66 1 16 -5 -3 26.41 9.26 1 16 5 -3 21.90 9.50 2 -16 -5 3 34.44 10.66 1 -15 -5 3 -3.79 7.43 1 15 -5 -3 -6.14 5.43 1 15 5 -3 -5.84 6.59 2 14 5 -3 151.07 13.24 2 14 -5 -3 184.28 13.48 1 13 5 -3 136.32 11.24 1 13 -5 -3 133.95 11.47 1 13 5 -3 133.70 11.83 2 12 5 -3 82.34 8.50 1 12 -5 -3 127.67 10.02 1 12 5 -3 104.20 10.51 2 -11 5 3 33.94 5.95 3 11 5 -3 28.76 7.11 2 11 5 -3 37.03 6.86 1 11 -5 -3 38.74 7.02 1 10 -5 -3 65.02 7.27 1 10 5 -3 75.55 7.50 1 -10 5 3 51.91 6.92 3 10 5 -3 66.15 8.03 2 -9 5 3 178.29 10.22 3 9 5 -3 183.78 11.70 2 9 -5 -3 163.66 10.37 1 9 5 -3 157.60 9.83 1 8 -5 -3 1011.55 32.48 1 8 5 -3 983.80 31.62 1 -8 5 3 925.42 30.95 3 8 5 -3 910.16 33.18 2 7 -5 -3 36.29 5.19 1 7 5 -3 37.92 4.95 1 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17.32 2 -4 5 -3 413.98 17.06 2 4 -5 3 434.94 15.33 1 -4 -5 -3 431.43 17.55 1 5 5 3 708.68 26.38 2 5 -5 3 680.39 23.79 1 -5 5 -3 716.59 25.64 2 -5 -5 -3 724.95 26.22 1 6 -5 3 475.07 18.58 1 -6 -5 -3 507.96 20.80 1 6 5 3 481.50 20.67 2 -6 5 -3 482.97 19.89 2 7 -5 3 965.54 32.91 1 -7 -5 -3 933.30 34.77 1 7 5 3 1034.16 35.76 2 -8 -5 -3 163.23 11.80 1 8 -5 3 140.39 9.71 1 8 5 3 136.50 10.87 2 -9 -5 -3 -3.57 4.68 1 9 5 3 -3.25 4.25 2 -10 5 -3 174.24 12.40 1 10 5 3 185.76 14.10 2 -10 -5 -3 178.75 13.32 1 -11 5 -3 0.76 7.08 1 -11 -5 -3 7.56 6.65 1 -12 -5 -3 97.17 11.89 1 -12 5 -3 98.98 12.90 1 -13 -5 -3 174.17 15.66 1 -13 5 -3 171.40 16.37 1 -14 5 -3 104.45 14.90 1 -16 -6 3 87.90 15.55 1 16 -6 -3 85.71 12.69 1 16 6 -3 102.40 13.42 2 15 -6 -3 60.88 11.04 1 -15 -6 3 68.25 13.11 1 15 6 -3 49.96 10.99 2 14 -6 -3 1.75 5.71 1 -14 -6 3 2.74 8.64 1 14 6 -3 -6.02 6.31 2 13 6 -3 13.36 6.78 2 13 -6 -3 8.15 6.55 1 -13 -6 3 23.46 7.70 1 12 6 -3 10.68 6.53 2 12 -6 -3 1.57 5.06 1 -12 -6 3 -2.64 4.67 1 11 -6 -3 375.77 17.87 1 11 6 -3 328.71 18.21 2 -11 6 3 368.11 16.98 3 -10 6 3 75.87 7.75 3 10 6 -3 80.37 8.50 2 10 -6 -3 70.58 7.71 1 10 6 -3 64.62 6.92 1 9 6 -3 31.22 6.48 2 9 -6 -3 44.14 6.13 1 9 6 -3 46.58 5.71 1 -9 6 3 43.30 6.65 3 8 -6 -3 4.78 3.48 1 8 6 -3 8.53 4.69 2 8 6 -3 3.22 3.31 1 -8 6 3 0.86 3.86 3 7 -6 -3 659.92 23.06 1 -7 6 3 614.14 22.89 3 7 6 -3 617.44 24.37 2 6 -6 -3 865.76 28.02 1 6 6 -3 845.84 25.39 3 -6 6 3 820.18 28.11 3 -6 -6 3 826.26 26.78 1 6 6 -3 816.22 29.60 2 5 6 -3 41.53 5.50 2 -5 -6 3 45.03 5.07 1 -5 6 3 42.65 5.74 3 -5 6 3 46.17 3.52 2 5 -6 -3 52.32 5.00 1 -4 -6 3 -2.00 1.65 1 4 6 -3 0.97 3.16 2 -4 6 3 -4.44 2.09 3 -4 6 3 2.47 1.85 2 4 -6 -3 -0.88 2.17 1 -3 6 3 9.50 2.32 2 3 -6 -3 3.41 2.44 1 -3 6 3 7.31 3.32 3 -3 -6 3 9.50 1.73 1 3 6 -3 5.97 3.05 2 2 6 -3 200.30 10.32 2 -2 6 3 201.89 8.48 2 2 -6 -3 202.36 9.20 1 -2 6 3 201.83 10.15 3 1 -6 -3 322.20 12.49 1 -1 6 3 320.49 13.34 3 -1 6 3 313.19 12.06 2 1 6 -3 303.78 13.46 2 0 6 3 156.06 8.43 3 0 -6 -3 171.14 8.20 1 0 6 -3 143.93 8.62 2 0 6 3 140.27 7.73 2 1 6 3 6.97 3.20 3 1 6 3 9.73 3.19 2 -1 -6 -3 5.56 2.84 1 -1 6 -3 9.35 3.35 2 -2 6 -3 561.11 20.84 2 2 6 3 555.20 20.97 2 -2 6 -3 581.22 17.76 1 -2 -6 -3 608.70 20.96 1 -3 6 -3 -1.30 2.02 1 -3 -6 -3 3.43 3.10 1 -3 6 -3 -0.05 2.57 2 3 6 3 -1.18 2.53 2 4 -6 3 701.13 22.56 1 -4 6 -3 710.00 25.01 2 4 6 3 690.29 25.70 2 -4 -6 -3 667.77 25.07 1 -5 -6 -3 2.47 3.79 1 5 -6 3 6.29 3.17 1 5 6 3 6.66 4.31 2 -5 6 -3 -0.22 3.26 2 6 -6 3 -0.98 3.33 1 -6 -6 -3 -2.69 3.44 1 -6 6 -3 -3.71 3.48 2 6 6 3 5.21 4.51 2 -7 -6 -3 60.72 8.28 1 -7 6 -3 53.88 6.98 2 7 6 3 39.66 7.14 2 7 -6 3 46.90 6.17 1 -8 6 -3 59.63 7.80 2 -8 -6 -3 51.45 8.35 1 8 6 3 58.93 8.88 2 -9 6 -3 281.03 15.72 2 9 6 3 277.22 16.87 2 -9 -6 -3 287.11 16.69 1 10 6 3 7.32 5.50 2 -10 -6 -3 1.21 5.50 1 -10 6 -3 9.37 5.82 2 11 6 3 11.29 7.12 2 -11 -6 -3 14.16 7.68 1 -12 -6 -3 1.87 6.61 1 -13 -6 -3 80.39 12.52 1 15 7 -3 97.12 14.73 2 15 -7 -3 95.93 13.27 1 14 -7 -3 13.88 8.00 1 -14 -7 3 30.43 9.01 1 14 7 -3 8.80 7.72 2 13 7 -3 67.96 11.43 2 13 -7 -3 91.73 10.18 1 -13 -7 3 85.03 11.57 1 12 7 -3 57.20 10.20 2 12 -7 -3 64.77 8.66 1 -12 7 3 46.92 8.34 3 -12 -7 3 48.83 9.75 1 -11 7 3 116.62 10.28 3 -11 -7 3 129.30 11.97 1 11 7 -3 101.72 10.49 2 11 -7 -3 118.25 10.12 1 10 -7 -3 219.67 12.94 1 10 7 -3 202.65 14.01 2 -10 7 3 215.06 13.12 3 -10 -7 3 221.40 13.60 1 -9 -7 3 337.73 16.23 1 9 -7 -3 343.45 16.17 1 9 7 -3 362.65 18.06 2 -9 7 3 343.39 16.69 3 8 7 -3 46.53 6.90 2 -8 7 3 30.29 6.24 3 8 -7 -3 35.39 5.69 1 -8 -7 3 32.53 6.34 1 7 7 -3 155.19 10.66 2 -7 7 3 165.21 10.39 3 -7 -7 3 156.44 9.03 1 7 -7 -3 144.52 9.22 1 6 7 -3 499.87 17.52 3 6 -7 -3 520.58 19.25 1 -6 7 3 499.86 20.16 3 6 7 -3 502.86 21.07 2 5 -7 -3 56.31 5.47 1 5 7 -3 69.90 7.33 2 -5 7 3 58.53 6.47 3 5 7 -3 61.67 5.79 3 -4 7 3 1492.73 45.98 3 -4 7 3 1512.33 43.69 2 4 7 -3 1524.50 47.77 2 4 -7 -3 1471.88 45.34 1 3 7 -3 812.42 29.55 2 -3 7 3 883.58 26.88 2 3 -7 -3 894.79 28.04 1 -3 7 3 870.64 29.23 3 2 -7 -3 429.88 15.83 1 2 7 -3 414.21 17.34 2 -2 7 3 441.62 15.47 2 -1 7 3 368.23 15.88 3 1 -7 -3 415.46 15.14 1 -1 7 3 400.05 14.89 2 1 7 -3 378.54 16.02 2 0 7 -3 345.91 15.05 2 0 7 3 381.53 14.58 2 0 -7 -3 342.19 14.11 1 0 7 3 355.77 15.01 3 -1 7 -3 278.44 13.01 2 -1 -7 -3 299.19 12.54 1 1 7 3 255.85 12.23 3 1 7 3 264.85 12.31 2 2 7 3 112.26 8.04 2 -2 -7 -3 111.31 7.66 1 -2 7 -3 123.77 8.18 2 -3 -7 -3 274.44 12.90 1 3 7 3 275.99 13.56 2 -3 7 -3 259.21 12.81 2 -4 7 -3 185.45 10.51 2 -4 -7 -3 171.99 10.55 1 4 7 3 189.65 11.35 2 5 7 3 390.15 18.09 2 -5 7 -3 379.87 16.77 2 -5 -7 -3 365.60 17.12 1 6 7 3 95.89 9.46 2 -6 7 -3 105.28 8.41 2 -6 -7 -3 101.67 8.97 1 -7 -7 -3 88.76 8.93 1 -7 7 -3 70.78 7.85 2 7 7 3 80.89 8.76 2 -8 7 -3 312.40 16.68 2 -8 -7 -3 334.57 17.96 1 8 7 3 346.14 18.45 2 9 7 3 31.07 7.63 2 -9 -7 -3 37.63 8.11 1 -10 7 -3 -1.78 5.84 3 -10 -7 -3 -8.76 5.41 1 10 7 3 3.01 5.71 2 -11 -7 -3 34.69 9.37 1 11 7 3 38.09 9.08 2 -12 -7 -3 136.34 13.31 1 14 8 -3 44.04 11.31 2 13 8 -3 348.43 20.98 2 12 8 -3 64.00 11.02 2 -12 8 3 70.10 9.99 3 11 8 -3 259.80 16.74 2 -11 8 3 251.65 15.47 3 10 8 -3 0.60 5.63 2 -10 8 3 -0.66 5.63 3 10 -8 -3 -3.28 4.68 1 9 8 -3 736.72 29.85 2 9 -8 -3 707.66 27.14 1 -9 8 3 715.97 27.99 3 -8 8 3 158.73 11.45 3 8 -8 -3 127.55 9.21 1 8 8 -3 162.72 11.88 2 7 -8 -3 26.20 5.55 1 -7 8 3 40.41 7.24 3 7 8 -3 37.98 6.84 2 6 8 -3 49.83 6.65 2 6 -8 -3 47.47 5.48 1 -6 8 3 54.50 6.87 3 5 -8 -3 147.11 8.76 1 5 8 -3 152.03 10.56 2 5 8 -3 161.05 9.04 3 -5 8 3 157.27 10.70 3 4 8 -3 402.97 18.10 2 4 8 -3 435.23 16.82 3 -4 8 3 413.21 18.23 3 4 -8 -3 416.64 16.20 1 -3 8 3 487.36 19.47 3 3 8 -3 447.91 19.22 2 3 -8 -3 441.63 17.02 1 -2 8 3 169.23 10.37 3 2 -8 -3 156.80 8.53 1 2 8 -3 160.16 10.24 2 -2 8 3 176.22 8.76 2 -1 8 3 42.83 5.72 3 1 8 -3 41.33 5.80 2 -1 8 3 38.57 5.27 2 1 -8 -3 43.84 4.99 1 0 -8 -3 756.91 25.33 1 0 8 3 757.89 25.76 2 0 8 -3 744.09 26.94 2 0 8 3 725.14 25.95 3 1 8 3 43.35 5.89 2 -1 -8 -3 35.47 4.77 1 -1 8 -3 46.19 6.34 2 1 8 3 35.50 5.98 3 2 8 3 1123.45 37.83 2 -2 -8 -3 1163.11 37.15 1 2 8 3 1126.66 36.39 3 -2 8 -3 1172.66 38.12 2 -3 8 -3 11.54 4.24 2 3 8 3 11.23 4.35 2 -3 -8 -3 20.14 4.67 1 4 8 3 22.91 5.85 2 -4 -8 -3 22.34 5.26 1 -4 8 -3 18.82 4.83 2 -5 8 -3 386.05 17.46 2 5 8 3 405.73 19.08 2 -5 -8 -3 394.94 18.08 1 6 8 3 339.80 17.76 2 -6 -8 -3 317.35 16.46 1 -6 8 -3 321.74 15.86 2 -7 -8 -3 198.07 13.15 1 7 8 3 193.83 13.60 2 -7 8 -3 209.14 12.65 2 8 8 3 96.11 10.78 2 -8 -8 -3 130.77 10.86 1 -8 8 -3 133.23 11.78 3 9 8 3 112.91 12.00 2 -9 -8 -3 126.95 11.81 1 -9 8 -3 134.01 12.07 3 10 8 3 -4.09 6.37 2 -10 8 -3 1.25 7.05 3 -10 -8 -3 1.93 6.13 1 11 8 3 575.82 28.63 2 -11 -8 -3 556.54 27.50 1 -12 -8 -3 11.21 8.85 1 13 9 -3 19.45 9.07 2 12 9 -3 84.84 11.18 2 -12 9 3 68.63 10.76 3 11 9 -3 49.21 9.37 2 -11 9 3 48.21 9.44 3 10 9 -3 49.99 9.22 2 -10 9 3 57.76 9.06 3 -9 9 3 6.05 5.15 3 9 9 -3 -8.07 5.37 2 8 9 -3 6.50 5.71 2 -8 9 3 -2.05 4.94 3 -7 9 3 -2.92 4.69 3 7 9 -3 9.06 5.15 2 6 9 -3 34.15 6.87 2 -6 9 3 46.77 7.82 3 5 9 -3 0.08 4.02 3 5 9 -3 1.54 4.26 2 -5 9 3 2.15 4.70 3 4 9 -3 3.36 3.82 3 4 9 -3 -2.81 3.91 2 -3 9 3 -1.31 3.75 3 3 9 -3 1.11 3.45 2 3 9 -3 1.29 3.73 3 2 9 -3 -3.37 3.73 3 2 9 -3 1.62 3.60 2 -2 9 3 0.03 3.82 3 -1 9 3 179.48 11.53 3 1 9 -3 177.55 11.37 3 1 9 -3 201.02 11.74 2 -1 9 3 211.59 10.77 2 0 9 3 0.76 3.43 2 0 9 -3 0.31 3.63 2 1 9 3 30.74 5.77 2 1 9 3 35.32 6.34 3 -1 9 -3 35.60 6.08 2 2 9 3 80.64 7.91 2 -2 9 -3 82.54 7.95 2 -2 -9 -3 82.52 7.34 1 2 9 3 78.28 7.83 3 -3 9 -3 182.52 11.18 2 -3 -9 -3 167.02 10.54 1 3 9 3 170.25 11.45 2 -4 -9 -3 1.04 4.27 1 4 9 3 3.53 4.87 2 -4 9 -3 2.43 3.96 2 -5 9 -3 27.10 5.95 2 5 9 3 36.75 7.62 2 -5 -9 -3 35.48 6.63 1 -6 9 -3 -1.75 5.52 3 -6 -9 -3 -1.53 4.44 1 6 9 3 9.36 5.49 2 -6 9 -3 1.36 4.32 2 7 9 3 21.57 7.45 2 -7 9 -3 2.04 6.11 3 -7 -9 -3 16.68 6.06 1 -8 9 -3 96.24 10.54 3 -8 -9 -3 84.70 9.84 1 8 9 3 88.59 10.49 2 -9 -9 -3 50.40 9.83 1 -9 9 -3 53.47 10.41 3 9 9 3 72.77 11.26 2 -10 -9 -3 141.28 13.34 1 -10 9 -3 201.31 15.93 3 10 9 3 174.18 15.02 2 11 9 3 6.58 7.78 2 -11 -9 -3 19.26 8.26 1 12 10 -3 32.17 9.35 2 -12 10 3 49.69 10.86 3 -11 10 3 29.34 9.15 3 11 10 -3 30.03 8.75 2 -10 10 3 47.75 9.59 3 10 10 -3 25.95 8.85 2 9 10 -3 219.28 15.46 2 -9 10 3 203.96 14.50 3 8 10 -3 146.90 12.16 2 -8 10 3 140.54 11.92 3 -7 10 3 2.45 5.66 3 7 10 -3 3.94 6.01 2 -6 10 3 28.34 7.18 3 6 10 -3 21.48 6.82 2 5 10 -3 114.08 9.92 2 -5 10 3 99.53 9.95 3 4 10 -3 34.86 6.72 2 -4 10 3 26.51 7.00 3 4 10 -3 35.83 6.45 3 3 10 -3 21.56 6.11 2 3 10 -3 24.72 5.86 3 -3 10 3 17.51 6.16 3 2 10 -3 154.61 11.13 2 -2 10 3 172.65 11.63 3 2 10 -3 176.27 11.37 3 -1 10 3 140.04 10.52 3 1 10 -3 156.18 10.89 2 1 10 -3 154.70 10.73 3 0 10 3 363.10 16.13 2 0 10 3 349.16 16.94 3 0 10 -3 340.99 17.12 3 0 10 -3 329.93 16.35 2 1 10 3 128.13 9.59 2 1 10 3 118.01 9.97 3 -1 10 -3 125.74 10.13 3 -1 10 -3 123.02 9.64 2 -2 10 -3 426.39 19.26 2 2 10 3 442.16 19.28 3 2 10 3 437.15 19.45 2 -2 10 -3 418.67 19.71 3 -3 10 -3 61.24 7.96 3 -3 10 -3 73.95 8.01 2 3 10 3 67.58 8.20 2 4 10 3 48.69 8.02 2 -4 10 -3 36.03 7.41 2 -4 10 -3 28.34 7.48 3 -5 10 -3 27.50 7.98 3 5 10 3 34.74 7.64 2 -6 10 -3 544.62 24.77 3 6 10 3 524.03 24.98 2 -7 10 -3 86.40 11.00 3 7 10 3 75.15 10.45 2 8 10 3 7.71 7.71 2 -8 10 -3 25.33 9.35 3 -9 10 -3 -4.11 7.63 3 10 10 3 6.82 8.66 2 -10 10 -3 20.64 9.60 3 -11 10 -3 155.88 16.13 3 -12 11 3 52.61 11.73 3 -11 11 3 -9.94 7.80 3 11 11 -3 -10.38 7.33 2 -10 11 3 112.33 12.89 3 10 11 -3 126.61 13.22 2 9 11 -3 68.98 11.18 2 -9 11 3 65.71 11.14 3 8 11 -3 176.53 14.27 2 -8 11 3 196.50 14.90 3 7 11 -3 91.85 10.07 2 -7 11 3 91.40 10.81 3 -6 11 3 210.12 14.90 3 6 11 -3 215.17 14.88 2 5 11 -3 52.10 8.65 2 -5 11 3 37.44 8.03 3 4 11 -3 289.51 16.56 2 -4 11 3 283.02 16.49 3 4 11 -3 268.94 14.75 3 -3 11 3 407.49 20.14 3 3 11 -3 421.89 19.30 3 3 11 -3 425.19 20.23 2 2 11 -3 27.83 7.13 2 2 11 -3 45.51 7.39 3 -2 11 3 40.21 7.65 3 1 11 -3 218.01 13.45 3 1 11 -3 213.38 13.34 2 -1 11 3 223.78 14.15 3 0 11 -3 248.69 14.37 2 0 11 -3 262.23 15.25 3 0 11 3 245.69 14.76 3 -1 11 -3 541.91 23.47 3 -1 11 -3 514.10 22.51 2 1 11 3 526.08 22.79 3 -2 11 -3 5.75 6.16 3 -2 11 -3 5.76 4.90 2 2 11 3 1.64 5.25 3 2 11 3 -0.11 4.77 2 -3 11 -3 78.90 9.42 3 -3 11 -3 102.92 9.59 2 3 11 3 107.96 10.16 2 -4 11 -3 4.68 6.59 3 4 11 3 30.26 7.85 2 -5 11 -3 194.03 14.25 3 5 11 3 175.16 13.74 2 -6 11 -3 62.08 10.85 3 6 11 3 65.10 10.88 2 7 11 3 83.95 12.24 2 -7 11 -3 79.64 11.61 3 8 11 3 237.41 17.90 2 -8 11 -3 225.40 17.41 3 9 11 3 50.49 12.09 2 -9 11 -3 50.89 11.31 3 10 12 -3 -8.40 7.96 2 -10 12 3 3.03 7.36 3 9 12 -3 97.75 11.86 2 -9 12 3 97.82 12.66 3 -8 12 3 0.97 7.82 3 8 12 -3 3.95 7.20 2 -7 12 3 0.04 7.28 3 7 12 -3 10.48 6.31 2 -6 12 3 -0.49 6.47 3 6 12 -3 11.27 7.19 2 -5 12 3 10.80 7.60 3 5 12 -3 20.31 6.73 2 -4 12 3 117.52 11.28 3 4 12 -3 105.84 11.09 2 3 12 -3 70.59 10.19 2 3 12 -3 57.17 9.07 3 -3 12 3 75.00 10.22 3 -2 12 3 48.80 9.52 3 2 12 -3 70.26 9.56 3 2 12 -3 60.81 9.22 2 1 12 -3 30.70 7.30 2 -1 12 3 32.61 8.12 3 1 12 -3 24.64 7.98 3 0 12 3 122.04 10.95 3 0 12 -3 134.01 11.70 3 0 12 -3 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28.26 5.58 2 -5 -5 -4 26.51 5.52 1 -5 5 -4 19.26 4.61 1 -6 -5 -4 18.23 5.73 1 6 5 4 12.89 4.82 2 -6 5 -4 17.76 5.16 1 -6 5 -4 21.30 5.05 2 -7 5 -4 3.88 4.77 1 -7 -5 -4 5.99 4.62 1 7 5 4 3.35 4.76 2 -8 5 -4 6.55 5.62 1 -8 -5 -4 5.11 5.49 1 8 5 4 1.61 4.59 2 -9 5 -4 80.57 9.61 1 -9 -5 -4 78.97 9.61 1 -10 -5 -4 3.96 5.89 1 -10 5 -4 0.94 5.91 1 -11 -5 -4 21.22 7.46 1 -11 5 -4 17.54 7.43 1 -12 5 -4 212.93 15.72 1 -12 -5 -4 214.11 16.80 1 16 6 -4 6.69 8.97 2 -16 -6 4 7.28 9.81 1 16 -6 -4 9.84 8.74 1 15 -6 -4 97.18 11.59 1 -15 -6 4 96.24 11.77 1 15 6 -4 88.76 11.89 2 14 6 -4 -6.57 5.24 2 14 -6 -4 1.52 6.11 1 13 6 -4 220.43 15.62 2 13 -6 -4 224.49 14.56 1 13 6 -4 207.12 13.63 1 12 -6 -4 -5.34 4.38 1 12 6 -4 4.42 5.06 1 12 6 -4 1.46 5.63 2 -12 6 4 3.14 4.98 3 11 -6 -4 55.61 8.25 1 -11 6 4 55.47 7.52 3 11 6 -4 50.49 7.76 1 11 6 -4 58.24 9.05 2 10 6 -4 11.33 5.11 1 10 -6 -4 6.67 4.35 1 -10 6 4 5.92 4.74 3 10 6 -4 2.49 4.14 2 -9 6 4 1220.67 39.20 3 9 6 -4 1220.53 41.90 2 9 -6 -4 1228.70 40.41 1 9 6 -4 1182.68 38.91 1 8 6 -4 53.74 5.78 1 -8 6 4 57.65 6.36 3 8 6 -4 58.14 6.83 2 8 -6 -4 50.48 5.73 1 7 -6 -4 889.72 29.65 1 7 6 -4 862.81 27.95 1 -7 6 4 892.75 29.65 3 7 6 -4 823.03 30.74 2 -6 6 4 134.18 8.66 3 6 6 -4 126.82 8.91 2 6 -6 -4 96.01 7.36 1 6 6 -4 111.39 6.61 1 -5 6 4 310.00 14.26 3 5 6 -4 333.65 11.83 1 5 -6 -4 357.70 14.13 1 5 6 -4 310.83 14.63 2 -4 -6 4 834.43 25.07 1 -4 6 4 868.67 28.33 3 4 -6 -4 875.06 28.01 1 4 6 -4 812.86 29.07 2 -4 6 4 861.33 25.02 2 3 -6 -4 28.77 4.31 1 3 6 -4 28.13 4.93 2 -3 6 4 32.61 5.10 3 -3 6 4 28.85 3.27 2 2 6 -4 744.05 26.35 2 -2 6 4 800.88 23.81 2 2 -6 -4 737.01 25.02 1 -2 6 4 746.23 25.44 3 -1 6 4 98.32 6.11 2 1 6 -4 103.97 7.52 2 1 -6 -4 84.97 6.29 1 -1 6 4 110.20 7.55 3 0 6 4 849.74 26.93 2 0 6 -4 801.19 28.05 2 0 -6 -4 823.09 27.43 1 -1 6 -4 94.92 6.95 2 -1 -6 -4 101.70 6.93 1 1 6 4 94.65 6.96 2 -2 6 -4 559.78 21.52 2 -2 -6 -4 586.46 21.51 1 2 6 4 586.04 21.51 2 -3 6 -4 82.42 6.88 2 3 6 4 87.63 7.37 2 -3 -6 -4 77.43 6.85 1 -4 6 -4 160.18 10.22 2 4 6 4 157.68 10.25 2 -4 -6 -4 195.57 11.18 1 -5 -6 -4 8.16 4.73 1 5 6 4 4.17 4.03 2 -5 6 -4 6.50 4.52 2 -6 6 -4 166.63 11.30 2 -6 -6 -4 168.65 11.42 1 6 6 4 171.75 11.55 2 -7 -6 -4 1.99 4.72 1 7 6 4 2.36 4.12 2 -7 6 -4 -1.51 4.59 2 -8 -6 -4 1.58 4.25 1 8 6 4 0.78 4.50 2 -8 6 -4 -7.10 4.61 2 -9 6 -4 15.07 6.01 2 -9 -6 -4 15.96 6.33 1 9 6 4 24.47 7.15 2 -10 -6 -4 68.58 10.29 1 -10 6 -4 71.86 10.40 2 -11 -6 -4 204.97 16.06 1 -12 -6 -4 28.53 9.77 1 16 -7 -4 72.34 13.04 1 15 7 -4 -3.31 7.85 2 15 -7 -4 9.03 7.94 1 14 -7 -4 36.35 8.84 1 14 7 -4 19.75 9.18 2 13 7 -4 22.78 7.98 2 13 -7 -4 7.74 5.96 1 -12 7 4 211.19 13.49 3 12 7 -4 207.94 15.06 2 12 -7 -4 203.47 13.59 1 11 -7 -4 0.09 4.93 1 -11 7 4 7.23 5.46 3 11 7 -4 7.83 6.02 2 10 7 -4 84.42 9.45 2 10 -7 -4 92.76 8.60 1 -10 7 4 93.29 8.96 3 9 7 -4 54.50 7.71 2 9 -7 -4 64.79 7.11 1 -9 7 4 70.31 7.95 3 -8 7 4 109.65 8.87 3 8 -7 -4 101.89 8.29 1 8 7 -4 118.90 9.61 2 7 7 -4 64.29 7.19 2 7 -7 -4 59.84 6.45 1 -7 7 4 58.61 7.16 3 6 -7 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8 4 82.47 6.57 2 -1 8 4 70.60 7.49 3 1 8 -4 73.69 6.97 2 1 -8 -4 71.45 6.45 1 0 -8 -4 5.71 3.51 1 0 8 4 3.10 3.58 3 0 8 -4 5.60 4.02 2 0 8 4 4.08 3.78 2 -1 -8 -4 3.89 3.65 1 -1 8 -4 4.91 3.87 2 1 8 4 2.69 3.57 2 -2 8 -4 222.62 12.13 2 -2 -8 -4 205.10 11.45 1 2 8 4 201.32 11.60 2 -3 8 -4 149.36 10.14 2 -3 -8 -4 148.50 10.02 1 3 8 4 145.13 10.07 2 -4 8 -4 -2.62 3.74 2 4 8 4 0.73 4.38 2 -4 -8 -4 0.87 3.54 1 -5 -8 -4 351.63 17.60 1 5 8 4 367.34 18.48 2 -5 8 -4 388.52 17.75 2 -6 -8 -4 27.01 6.70 1 -6 8 -4 10.88 5.24 2 6 8 4 24.92 6.82 2 7 8 4 124.34 11.15 2 -7 -8 -4 116.40 10.42 1 -7 8 -4 102.75 9.76 2 -8 -8 -4 45.91 9.28 1 8 8 4 40.81 9.23 2 9 8 4 42.20 8.94 2 -9 -8 -4 58.27 10.05 1 10 8 4 19.54 8.08 2 -10 -8 -4 13.66 8.15 1 -10 8 -4 32.47 9.62 3 -11 -8 -4 13.83 9.04 1 14 9 -4 327.06 22.04 2 13 9 -4 42.08 10.35 2 12 9 -4 61.96 10.53 2 -12 9 4 66.46 10.46 3 11 9 -4 9.20 6.09 2 -11 9 4 -5.41 5.62 3 10 9 -4 346.09 19.46 2 -10 9 4 350.19 18.75 3 -9 9 4 94.83 10.06 3 9 9 -4 80.58 9.33 2 -8 9 4 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76.79 10.47 2 -8 -7 -7 2.86 6.58 1 -8 7 -7 -2.90 6.89 2 -9 7 -7 34.57 9.38 2 -9 -7 -7 15.68 8.49 1 -10 7 -7 44.21 11.33 2 16 -8 -7 95.77 13.08 1 15 -8 -7 150.10 14.36 1 15 8 -7 132.72 14.95 2 14 8 -7 204.83 16.84 2 14 -8 -7 247.26 16.66 1 13 -8 -7 8.88 6.66 1 13 8 -7 2.92 6.18 2 12 8 -7 69.93 9.84 2 12 -8 -7 58.41 9.45 1 11 -8 -7 67.40 9.66 1 -11 8 7 59.20 9.57 3 11 8 -7 65.45 9.00 2 10 -8 -7 0.76 4.25 1 -10 8 7 3.26 4.79 3 10 8 -7 -5.21 4.88 2 9 -8 -7 144.10 10.85 1 9 8 -7 133.76 11.22 2 -9 8 7 117.81 10.67 3 8 -8 -7 1.06 4.26 1 8 8 -7 3.11 4.91 2 7 -8 -7 120.12 9.36 1 7 8 -7 116.72 10.24 2 6 8 -7 -4.28 4.14 2 6 -8 -7 -0.13 3.43 1 5 -8 -7 303.90 15.19 1 5 8 -7 336.97 17.01 2 4 -8 -7 83.62 7.70 1 4 8 -7 95.01 8.62 2 3 -8 -7 -2.00 3.42 1 3 8 -7 5.70 4.44 2 2 8 -7 44.84 7.07 2 2 -8 -7 36.51 6.24 1 1 -8 -7 220.95 12.62 1 1 8 -7 203.73 13.23 2 0 8 7 267.90 13.14 2 0 -8 -7 236.97 13.32 1 0 8 -7 215.81 13.39 2 1 8 7 82.96 8.02 2 -1 -8 -7 89.99 8.68 1 -1 8 -7 84.37 8.87 2 2 8 7 137.33 10.39 2 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51.27 6.57 1 4 5 -11 51.76 6.91 2 4 -5 -11 54.53 7.56 1 3 -5 -11 376.50 18.60 1 3 5 -11 395.96 18.97 2 2 5 -11 112.34 10.25 2 2 -5 -11 135.92 10.61 1 1 5 -11 3.25 4.66 2 1 -5 -11 10.33 5.36 1 0 5 -11 229.51 14.59 2 0 -5 -11 223.51 14.18 1 -1 5 -11 49.43 8.47 2 -1 -5 -11 65.73 9.77 1 -2 -5 -11 27.80 7.11 1 -2 5 -11 15.22 7.47 2 -3 5 -11 362.67 20.86 2 -3 -5 -11 376.59 20.79 1 -4 5 -11 5.50 6.96 2 -4 -5 -11 -5.64 6.11 1 -5 5 -11 32.67 9.56 2 -5 -5 -11 19.34 8.50 1 -6 -5 -11 18.96 7.95 1 -6 5 -11 23.08 8.57 2 16 -6 -11 38.14 9.36 1 15 6 -11 0.59 7.46 2 15 -6 -11 -8.93 6.59 1 14 -6 -11 264.06 17.31 1 14 6 -11 252.59 17.23 2 13 6 -11 31.60 8.62 2 13 -6 -11 36.86 7.93 1 12 -6 -11 -4.77 5.27 1 12 6 -11 -2.83 5.95 2 11 6 -11 85.80 9.62 2 11 -6 -11 86.98 9.47 1 10 -6 -11 -0.27 4.56 1 10 6 -11 3.52 4.82 2 9 -6 -11 191.19 13.05 1 9 6 -11 207.41 13.78 2 8 6 -11 -0.90 4.94 2 8 -6 -11 0.10 5.04 1 7 -6 -11 7.05 5.03 1 7 6 -11 -0.30 4.26 2 6 -6 -11 7.91 4.58 1 6 6 -11 -0.63 4.62 2 5 6 -11 150.90 11.67 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73.73 10.99 2 2 -6 -15 69.77 11.18 1 1 6 -15 49.88 9.98 2 1 -6 -15 48.43 10.67 1 13 7 -15 63.35 12.51 2 12 7 -15 203.01 16.49 2 12 -7 -15 181.34 15.78 1 11 -7 -15 10.17 6.94 1 11 7 -15 -3.55 6.19 2 10 -7 -15 -6.71 6.05 1 10 7 -15 3.56 7.35 2 9 -7 -15 13.49 6.56 1 9 7 -15 15.68 7.05 2 8 -7 -15 17.49 8.23 1 8 7 -15 22.98 8.84 2 7 -7 -15 75.84 10.57 1 7 7 -15 102.70 11.33 2 6 -7 -15 203.62 15.40 1 6 7 -15 224.27 16.96 2 5 7 -15 -4.05 6.12 2 5 -7 -15 -4.89 5.61 1 4 -7 -15 35.71 9.64 1 4 7 -15 49.22 10.48 2 3 -7 -15 29.21 8.74 1 3 7 -15 24.26 8.12 2 2 -7 -15 52.12 10.32 1 2 7 -15 60.07 11.41 2 12 8 -15 123.86 14.46 2 11 8 -15 18.18 9.04 2 10 8 -15 -1.35 7.92 2 10 -8 -15 2.10 6.07 1 9 8 -15 125.59 14.05 2 9 -8 -15 133.44 13.77 1 8 -8 -15 0.62 5.85 1 7 -8 -15 256.17 17.62 1 7 8 -15 234.86 17.57 2 6 -8 -15 29.10 8.85 1 6 8 -15 35.42 9.78 2 5 -8 -15 49.18 10.55 1 5 8 -15 52.69 11.52 2 4 8 -15 0.70 7.99 2 4 -8 -15 7.89 7.62 1 15 0 -16 3.20 7.12 1 14 0 -16 48.59 9.66 1 13 0 -16 131.08 12.67 1 12 0 -16 -9.73 5.56 1 11 0 -16 63.10 9.54 1 10 0 -16 421.96 21.47 1 9 0 -16 118.60 10.77 1 8 0 -16 49.76 8.35 1 7 0 -16 50.98 8.69 1 6 0 -16 -4.02 4.76 1 5 0 -16 404.22 20.38 1 4 0 -16 12.25 6.28 2 4 0 -16 16.41 6.85 1 3 0 -16 -0.36 5.90 2 3 0 -16 -3.66 5.10 1 2 0 -16 10.03 6.96 2 2 0 -16 7.35 6.15 1 1 0 -16 75.25 11.13 1 1 0 -16 82.27 11.56 2 0 0 -16 19.40 9.19 2 0 0 -16 15.58 8.22 1 -1 0 -16 44.75 10.60 2 -1 0 -16 71.06 11.69 1 16 1 -16 65.47 12.69 1 15 1 -16 136.29 13.02 1 15 -1 -16 135.75 13.06 1 14 1 -16 92.02 11.14 1 14 -1 -16 121.94 12.34 1 13 -1 -16 15.06 8.08 1 13 1 -16 19.70 7.70 1 12 1 -16 -2.95 5.88 1 12 -1 -16 -4.88 6.37 1 11 -1 -16 63.45 10.11 1 11 1 -16 66.99 9.22 1 10 -1 -16 155.65 12.65 1 10 1 -16 153.61 12.30 1 9 1 -16 34.24 7.50 1 9 -1 -16 30.70 8.39 1 8 1 -16 70.85 8.65 1 8 -1 -16 65.90 8.76 1 7 1 -16 14.25 6.03 1 7 -1 -16 14.43 6.72 1 6 -1 -16 20.43 7.01 1 6 1 -16 35.64 7.68 1 5 1 -16 13.30 6.32 1 5 1 -16 12.65 5.94 2 5 -1 -16 16.18 6.70 1 4 1 -16 144.50 12.07 1 4 -1 -16 145.35 12.38 1 4 1 -16 144.03 12.19 2 3 1 -16 2.05 5.68 1 3 -1 -16 1.45 5.88 1 3 1 -16 -1.51 5.54 2 2 1 -16 -6.15 5.44 1 2 -1 -16 7.69 7.32 2 2 -1 -16 -6.67 5.02 1 2 1 -16 9.55 6.92 2 1 -1 -16 0.62 6.85 2 1 1 -16 1.12 6.13 1 1 -1 -16 2.67 6.56 1 1 1 -16 2.39 7.71 2 0 1 -16 6.43 8.48 2 0 -1 -16 0.03 7.40 2 0 1 -16 -5.39 6.22 1 0 -1 -16 4.93 7.24 1 -1 -1 -16 275.54 18.17 1 -1 -1 -16 260.99 19.17 2 -1 1 -16 268.48 19.10 2 16 2 -16 -13.13 7.40 1 15 -2 -16 49.82 10.55 1 15 2 -16 49.59 11.31 1 14 2 -16 66.45 11.08 1 14 -2 -16 66.63 11.90 1 13 -2 -16 21.27 8.89 1 13 2 -16 19.95 7.22 1 12 -2 -16 99.30 11.23 1 12 2 -16 100.71 10.97 1 11 2 -16 4.15 6.25 1 11 -2 -16 8.62 5.90 1 10 -2 -16 5.39 5.99 1 10 2 -16 6.98 5.89 1 9 -2 -16 48.49 9.35 1 9 2 -16 28.64 7.60 1 8 2 -16 19.79 7.05 1 8 -2 -16 -0.49 5.13 1 7 -2 -16 88.92 10.28 1 6 2 -16 -4.43 5.32 2 6 -2 -16 2.04 6.05 1 5 2 -16 196.35 14.26 2 5 -2 -16 169.18 13.71 1 4 2 -16 -0.02 5.48 2 4 -2 -16 -0.64 5.90 1 3 -2 -16 97.51 10.26 1 3 2 -16 87.08 10.73 2 2 2 -16 7.79 6.68 2 2 -2 -16 -1.67 5.77 1 1 -2 -16 6.31 5.79 1 1 2 -16 3.00 7.26 2 0 2 -16 7.38 8.25 2 0 -2 -16 -2.07 7.32 2 0 -2 -16 12.21 8.05 1 14 -3 -16 32.68 9.66 1 13 -3 -16 12.55 8.37 1 12 -3 -16 199.57 15.60 1 11 -3 -16 290.27 18.46 1 10 -3 -16 340.13 19.75 1 9 -3 -16 10.78 7.03 1 8 -3 -16 102.74 10.65 1 8 3 -16 91.97 10.44 2 7 3 -16 11.82 6.40 2 7 -3 -16 18.26 6.64 1 6 -3 -16 289.54 17.34 1 6 3 -16 271.28 17.04 2 5 -3 -16 28.18 8.54 1 5 3 -16 50.73 9.18 2 4 3 -16 119.77 11.97 2 4 -3 -16 108.91 11.51 1 3 3 -16 76.60 9.89 2 3 -3 -16 79.30 10.20 1 2 -3 -16 11.48 7.00 1 2 3 -16 -1.95 5.36 2 1 3 -16 85.78 12.79 2 1 -3 -16 125.89 12.18 1 0 3 -16 145.20 14.58 2 0 -3 -16 148.13 14.26 1 13 -4 -16 74.36 12.66 1 12 -4 -16 48.24 9.98 1 11 -4 -16 30.38 8.28 1 10 -4 -16 -2.35 5.18 1 9 -4 -16 242.43 16.30 1 9 4 -16 188.44 14.82 2 8 -4 -16 28.08 7.41 1 8 4 -16 27.28 7.95 2 7 -4 -16 -0.42 5.06 1 7 4 -16 -2.60 5.56 2 6 4 -16 30.38 8.42 2 6 -4 -16 46.43 9.22 1 5 4 -16 116.53 12.26 2 5 -4 -16 127.36 12.07 1 4 4 -16 54.23 9.78 2 4 -4 -16 40.74 9.39 1 3 -4 -16 6.68 6.88 1 3 4 -16 3.58 6.89 2 2 -4 -16 11.31 7.45 1 2 4 -16 -10.66 5.55 2 1 4 -16 20.25 7.83 2 1 -4 -16 26.43 8.99 1 12 -5 -16 18.60 7.76 1 11 -5 -16 20.43 8.11 1 10 5 -16 -4.83 7.10 2 10 -5 -16 11.33 6.75 1 9 -5 -16 97.09 11.16 1 9 5 -16 77.37 10.87 2 8 -5 -16 23.01 7.56 1 8 5 -16 5.09 6.67 2 7 5 -16 -0.73 6.33 2 7 -5 -16 3.75 6.24 1 6 -5 -16 7.53 6.30 1 6 5 -16 6.82 7.38 2 5 5 -16 31.21 8.28 2 5 -5 -16 6.25 6.98 1 4 -5 -16 -3.58 6.51 1 4 5 -16 5.55 6.62 2 3 -5 -16 7.32 6.22 1 3 5 -16 5.17 6.73 2 2 5 -16 64.84 11.44 2 2 -5 -16 70.65 11.67 1 11 -6 -16 72.39 11.80 1 11 6 -16 72.63 11.87 2 10 -6 -16 82.23 10.92 1 10 6 -16 77.65 12.48 2 9 -6 -16 10.15 7.41 1 9 6 -16 -2.39 7.50 2 8 -6 -16 58.05 9.64 1 8 6 -16 52.12 10.88 2 7 6 -16 50.16 10.68 2 7 -6 -16 62.34 10.51 1 6 6 -16 0.51 6.80 2 6 -6 -16 -1.76 6.29 1 5 6 -16 44.51 9.99 2 5 -6 -16 47.56 9.64 1 4 -6 -16 -0.09 6.18 1 4 6 -16 -13.17 6.45 2 3 6 -16 108.15 12.78 2 3 -6 -16 105.65 11.66 1 12 7 -16 37.36 11.12 2 11 7 -16 88.94 13.33 2 10 7 -16 79.84 13.00 2 9 -7 -16 12.56 8.54 1 9 7 -16 23.72 8.08 2 8 -7 -16 9.66 7.35 1 8 7 -16 8.26 8.05 2 7 7 -16 62.70 11.95 2 7 -7 -16 52.82 10.15 1 6 -7 -16 57.06 11.35 1 6 7 -16 72.71 12.06 2 5 7 -16 5.64 7.40 2 14 0 -17 1.60 6.98 1 13 0 -17 -7.09 7.48 1 12 0 -17 3.99 7.02 1 11 0 -17 -2.70 5.98 1 10 0 -17 -4.36 5.62 1 9 0 -17 -0.90 5.26 1 8 0 -17 -2.65 5.77 1 7 0 -17 5.63 6.30 1 6 0 -17 0.71 5.68 1 5 0 -17 -1.18 4.95 1 4 0 -17 4.34 5.55 1 3 0 -17 2.32 6.06 1 2 0 -17 -4.43 7.39 2 2 0 -17 -2.55 6.93 1 1 0 -17 -3.07 5.89 1 1 0 -17 -4.40 8.08 2 15 1 -17 100.41 13.66 1 14 1 -17 18.64 8.50 1 14 -1 -17 21.07 9.41 1 13 1 -17 17.37 7.94 1 13 -1 -17 4.22 6.63 1 12 1 -17 6.81 6.74 1 12 -1 -17 2.59 7.37 1 11 1 -17 134.30 12.47 1 11 -1 -17 160.75 13.40 1 10 1 -17 46.19 8.84 1 10 -1 -17 43.55 9.72 1 9 -1 -17 35.09 8.78 1 9 1 -17 46.47 8.70 1 8 -1 -17 40.96 8.29 1 8 1 -17 44.03 8.76 1 7 1 -17 23.80 7.14 1 7 -1 -17 15.81 6.55 1 6 1 -17 113.02 10.91 1 6 -1 -17 96.40 10.71 1 5 1 -17 19.28 6.83 1 5 -1 -17 -1.66 6.27 1 4 -1 -17 30.42 7.86 1 4 1 -17 27.38 8.42 2 4 1 -17 22.46 8.00 1 3 1 -17 4.20 6.31 2 3 -1 -17 12.11 6.97 1 2 -1 -17 4.74 6.92 1 2 1 -17 5.74 6.90 2 1 1 -17 39.64 10.77 2 1 -1 -17 29.78 9.30 1 0 -1 -17 78.28 13.76 2 13 -2 -17 3.52 6.67 1 12 -2 -17 104.91 12.06 1 11 -2 -17 -0.96 5.62 1 10 -2 -17 46.51 9.39 1 9 -2 -17 138.37 12.56 1 8 -2 -17 12.48 6.93 1 7 -2 -17 7.63 6.56 1 6 -2 -17 44.26 9.37 1 5 -2 -17 353.09 20.49 1 5 2 -17 374.40 20.78 2 4 -2 -17 9.80 6.97 1 4 2 -17 14.46 7.02 2 3 -2 -17 140.09 12.73 1 3 2 -17 118.45 12.92 2 2 2 -17 8.43 7.49 2 2 -2 -17 -6.76 6.36 1 1 2 -17 89.29 13.50 2 13 -3 -17 34.51 9.68 1 12 -3 -17 -3.71 6.63 1 11 -3 -17 7.35 6.55 1 10 -3 -17 10.01 6.78 1 9 -3 -17 14.63 7.60 1 8 -3 -17 29.49 8.56 1 7 -3 -17 -8.18 6.10 1 7 3 -17 7.60 7.05 2 6 3 -17 124.17 12.39 2 6 -3 -17 116.86 11.95 1 5 3 -17 3.37 6.86 2 5 -3 -17 7.25 7.65 1 4 3 -17 5.69 7.24 2 4 -3 -17 0.91 6.72 1 3 -3 -17 18.93 8.20 1 3 3 -17 3.86 6.64 2 2 3 -17 -4.62 7.22 2 12 -4 -17 130.09 13.43 1 11 -4 -17 78.43 11.77 1 10 -4 -17 182.55 14.84 1 9 -4 -17 3.00 6.25 1 8 4 -17 13.55 7.92 2 8 -4 -17 26.10 8.36 1 7 4 -17 86.92 12.49 2 7 -4 -17 70.88 9.64 1 6 4 -17 6.18 7.12 2 6 -4 -17 -8.55 6.15 1 5 4 -17 25.65 8.15 2 5 -4 -17 74.38 11.23 1 4 -4 -17 1.82 7.12 1 4 4 -17 24.26 8.80 2 3 4 -17 72.04 12.37 2 10 -5 -17 53.38 11.72 1 9 -5 -17 67.14 11.20 1 9 5 -17 46.71 10.83 2 8 5 -17 -0.15 7.60 2 8 -5 -17 10.55 7.66 1 7 -5 -17 1.22 5.93 1 7 5 -17 13.52 8.25 2 6 5 -17 27.35 9.48 2 6 -5 -17 47.77 10.74 1 5 5 -17 1.27 7.56 2 4 5 -17 282.75 19.45 2 10 6 -17 29.47 10.14 2 9 6 -17 -7.19 8.03 2 8 6 -17 96.59 13.73 2 7 6 -17 -8.61 7.44 2 6 6 -17 43.89 11.02 2 13 0 -18 7.99 8.70 1 12 0 -18 136.71 13.67 1 11 0 -18 13.56 8.18 1 10 0 -18 105.43 11.40 1 9 0 -18 5.75 6.49 1 8 0 -18 50.72 9.46 1 7 0 -18 98.88 10.87 1 6 0 -18 29.27 8.11 1 5 0 -18 171.57 14.48 1 4 0 -18 12.82 7.91 1 13 1 -18 27.37 10.20 1 12 -1 -18 -7.62 6.98 1 12 1 -18 3.04 7.77 1 11 -1 -18 15.94 8.02 1 11 1 -18 4.82 7.43 1 10 1 -18 89.32 10.52 1 10 -1 -18 78.78 10.66 1 9 -1 -18 6.09 7.03 1 9 1 -18 0.61 6.61 1 8 -1 -18 14.05 7.56 1 7 -1 -18 -6.86 6.50 1 6 -1 -18 125.37 13.07 1 5 -1 -18 17.48 8.16 1 11 -2 -18 8.97 7.65 1 10 -2 -18 -0.41 6.76 1 9 -2 -18 39.07 9.09 1 8 -2 -18 6.90 6.45 1 7 -2 -18 5.55 6.71 1 6 -2 -18 -11.04 5.90 1 5 -2 -18 -1.28 7.38 1 4 2 -18 34.26 9.95 2 3 2 -18 7.28 8.32 2 10 -3 -18 98.14 12.20 1 9 -3 -18 10.90 7.19 1 8 -3 -18 141.65 13.01 1 7 -3 -18 16.81 7.57 1 6 -3 -18 415.73 23.23 1 5 3 -18 35.92 10.21 2 4 3 -18 197.89 16.64 2 7 4 -18 32.82 10.08 2 6 4 -18 0.01 7.59 2 5 4 -18 225.20 17.83 2 8 5 -18 55.03 11.66 2 7 5 -18 1.82 8.77 2 10 0 -19 19.61 8.28 1 9 0 -19 0.62 7.03 1 8 0 -19 1.45 7.23 1 7 0 -19 1.74 7.65 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 87786 _database_code_depnum_ccdc_archive 'CCDC 959698' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rah202 _audit_creation_method SHELXL-2013 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H38 Cl2 N10 Ni2 2+,2 Cl -,2 C H4 O, 2 H2 O' _chemical_formula_sum 'C34 H50 Cl4 N10 Ni2 O4' _chemical_formula_weight 922.06 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2913(5) _cell_length_b 10.2003(5) _cell_length_c 12.0495(7) _cell_angle_alpha 83.850(4) _cell_angle_beta 67.556(5) _cell_angle_gamma 82.657(4) _cell_volume 1044.70(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7117 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 29.37 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_density_diffrn 1.466 _exptl_crystal_F_000 480 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_absorpt_coefficient_mu 1.206 _shelx_estimated_absorpt_T_min 0.794 _shelx_estimated_absorpt_T_max 0.889 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.804 _exptl_absorpt_correction_T_max 0.890 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Enhance (Mo) X-ray Source' _diffrn_measurement_device_type 'Oxford Diffraction Gemini A Ultra diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3968 _diffrn_reflns_number 10097 _diffrn_reflns_av_unetI/netI 0.0287 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.910 _diffrn_reflns_theta_max 29.436 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.846 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.846 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.846 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 4900 _reflns_number_gt 4215 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET) (compiled Jan 5 2010,16:28:46) ; _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement SHELXL-2013 _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0347P)^2^] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 4900 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0609 _refine_ls_wR_factor_gt 0.0598 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.66043(2) 0.59550(2) 0.25951(2) 0.01258(6) Uani 1 1 d . . . . . Cl1 Cl 0.69425(4) 0.36684(3) 0.20974(3) 0.02001(8) Uani 1 1 d . . . . . N1 N 0.67862(13) 0.65856(11) 0.08321(10) 0.0169(2) Uani 1 1 d . . . . . N2 N 0.88812(13) 0.62201(11) 0.18046(10) 0.0147(2) Uani 1 1 d . . . . . N3 N 0.72861(13) 0.52052(11) 0.40581(10) 0.0144(2) Uani 1 1 d . . . . . H3N H 0.6894(18) 0.4424(15) 0.4177(13) 0.017(4) Uiso 1 1 d . . . . . N4 N 0.58064(13) 0.39990(11) 0.65656(10) 0.0150(2) Uani 1 1 d . . . . . N5 N 0.40017(13) 0.20466(11) 0.69335(10) 0.0166(2) Uani 1 1 d . . . . . C1 C 0.56903(18) 0.67456(15) 0.03540(13) 0.0240(3) Uani 1 1 d . . . . . H1 H 0.4645 0.6598 0.0858 0.029 Uiso 1 1 calc R U . . . C2 C 0.60230(19) 0.71200(16) -0.08535(14) 0.0282(4) Uani 1 1 d . . . . . H2 H 0.5220 0.7211 -0.1170 0.034 Uiso 1 1 calc R U . . . C3 C 0.7521(2) 0.73561(16) -0.15836(13) 0.0274(3) Uani 1 1 d . . . . . H3 H 0.7768 0.7622 -0.2410 0.033 Uiso 1 1 calc R U . . . C4 C 0.86775(18) 0.72009(14) -0.10996(12) 0.0220(3) Uani 1 1 d . . . . . H4 H 0.9723 0.7368 -0.1585 0.026 Uiso 1 1 calc R U . . . C5 C 0.82681(16) 0.67977(13) 0.01054(12) 0.0161(3) Uani 1 1 d . . . . . C6 C 0.94149(16) 0.65816(13) 0.06956(12) 0.0174(3) Uani 1 1 d . . . . . H6 H 1.0489 0.6706 0.0270 0.021 Uiso 1 1 calc R U . . . C7 C 0.97662(16) 0.59948(14) 0.25902(12) 0.0186(3) Uani 1 1 d . . . . . H7A H 0.9733 0.6823 0.2963 0.022 Uiso 1 1 calc R U . . . H7B H 1.0872 0.5696 0.2125 0.022 Uiso 1 1 calc R U . . . C8 C 0.90152(16) 0.49355(14) 0.35534(12) 0.0186(3) Uani 1 1 d . . . . . H8A H 0.9302 0.4061 0.3202 0.022 Uiso 1 1 calc R U . . . H8B H 0.9419 0.4904 0.4207 0.022 Uiso 1 1 calc R U . . . C9 C 0.66514(16) 0.59291(13) 0.51684(11) 0.0154(3) Uani 1 1 d . . . . . H9A H 0.5540 0.6238 0.5329 0.018 Uiso 1 1 calc R U . . . H9B H 0.7224 0.6722 0.5034 0.018 Uiso 1 1 calc R U . . . C10 C 0.67584(16) 0.51180(14) 0.62769(12) 0.0181(3) Uani 1 1 d . . . . . H10A H 0.7862 0.4786 0.6124 0.022 Uiso 1 1 calc R U . . . H10B H 0.6386 0.5686 0.6968 0.022 Uiso 1 1 calc R U . . . C11 C 0.64998(16) 0.28492(14) 0.62979(12) 0.0198(3) Uani 1 1 d . . . . . H11 H 0.7610 0.2718 0.5970 0.024 Uiso 1 1 calc R U . . . C12 C 0.55634(17) 0.17349(14) 0.65018(12) 0.0197(3) Uani 1 1 d . . . . . C13 C 0.62361(19) 0.04485(15) 0.62599(14) 0.0283(4) Uani 1 1 d . . . . . H13 H 0.7341 0.0257 0.5955 0.034 Uiso 1 1 calc R U . . . C14 C 0.5267(2) -0.05452(15) 0.64712(15) 0.0315(4) Uani 1 1 d . . . . . H14 H 0.5698 -0.1435 0.6322 0.038 Uiso 1 1 calc R U . . . C15 C 0.3674(2) -0.02366(14) 0.68987(14) 0.0277(3) Uani 1 1 d . . . . . H15 H 0.2988 -0.0904 0.7039 0.033 Uiso 1 1 calc R U . . . C16 C 0.30884(18) 0.10756(14) 0.71220(13) 0.0218(3) Uani 1 1 d . . . . . H16 H 0.1987 0.1287 0.7422 0.026 Uiso 1 1 calc R U . . . Cl2 Cl 1.05646(4) 0.21068(3) 0.48065(3) 0.02215(8) Uani 1 1 d . . . . . C17 C 0.7784(3) 0.0723(2) 0.9793(2) 0.0688(7) Uani 1 1 d . . . . . H17A H 0.8687 0.0136 0.9833 0.103 Uiso 0.820(11) 1 calc R U P A 1 H17B H 0.6940 0.0192 0.9869 0.103 Uiso 0.820(11) 1 calc R U P A 1 H17C H 0.7421 0.1322 1.0449 0.103 Uiso 0.820(11) 1 calc R U P A 1 H17D H 0.7891 0.0820 1.0557 0.103 Uiso 0.180(11) 1 calc R U P A 2 H17E H 0.7482 -0.0163 0.9793 0.103 Uiso 0.180(11) 1 calc R U P A 2 H17F H 0.6980 0.1392 0.9692 0.103 Uiso 0.180(11) 1 calc R U P A 2 O1 O 0.8212(7) 0.1451(2) 0.8710(2) 0.0799(16) Uani 0.820(11) 1 d . . P A 1 H1O H 0.8503 0.0938 0.8147 0.120 Uiso 0.820(11) 1 calc R U P A 1 O1A O 0.921(2) 0.089(2) 0.8843(10) 0.068(7) Uani 0.180(11) 1 d . . P A 2 H1A H 0.9124 0.0811 0.8187 0.102 Uiso 0.180(11) 1 calc R U P A 2 O2 O 1.00676(17) -0.01662(15) 0.68196(12) 0.0409(3) Uani 1 1 d . . . . . H2A H 1.024(2) 0.046(2) 0.6328(19) 0.039(6) Uiso 1 1 d . . . . . H2B H 0.996(3) -0.080(3) 0.644(2) 0.074(8) 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 Ni 0.00985(9) 0.01440(9) 0.01214(9) -0.00024(6) -0.00276(7) -0.00117(6) Cl1 0.01940(18) 0.01714(16) 0.02282(17) -0.00512(13) -0.00596(14) -0.00224(13) N1 0.0150(6) 0.0196(6) 0.0154(6) -0.0005(5) -0.0051(5) -0.0017(5) N2 0.0113(5) 0.0156(5) 0.0158(6) -0.0012(4) -0.0037(5) -0.0013(4) N3 0.0123(6) 0.0157(6) 0.0142(6) -0.0009(4) -0.0034(5) -0.0023(4) N4 0.0118(5) 0.0218(6) 0.0112(5) 0.0005(4) -0.0041(4) -0.0027(4) N5 0.0155(6) 0.0162(6) 0.0154(6) 0.0008(4) -0.0037(5) 0.0001(4) C1 0.0173(7) 0.0347(8) 0.0204(7) 0.0004(6) -0.0075(6) -0.0047(6) C2 0.0276(9) 0.0408(9) 0.0205(8) 0.0000(7) -0.0142(7) -0.0029(7) C3 0.0326(9) 0.0344(9) 0.0146(7) 0.0003(6) -0.0083(7) -0.0039(7) C4 0.0218(8) 0.0259(8) 0.0143(7) -0.0016(6) -0.0017(6) -0.0042(6) C5 0.0162(7) 0.0156(6) 0.0145(6) -0.0021(5) -0.0034(5) -0.0004(5) C6 0.0130(7) 0.0189(7) 0.0173(7) -0.0022(5) -0.0017(5) -0.0022(5) C7 0.0104(7) 0.0273(7) 0.0180(7) -0.0009(6) -0.0052(5) -0.0024(5) C8 0.0129(7) 0.0245(7) 0.0167(7) -0.0009(5) -0.0054(5) 0.0032(5) C9 0.0132(7) 0.0169(6) 0.0152(6) -0.0026(5) -0.0032(5) -0.0036(5) C10 0.0135(7) 0.0270(7) 0.0144(6) -0.0020(6) -0.0041(5) -0.0068(5) C11 0.0116(7) 0.0282(8) 0.0165(7) -0.0009(6) -0.0034(5) 0.0026(6) C12 0.0192(7) 0.0210(7) 0.0162(7) -0.0003(5) -0.0053(6) 0.0033(6) C13 0.0248(8) 0.0247(8) 0.0305(8) -0.0057(6) -0.0076(7) 0.0096(6) C14 0.0412(10) 0.0184(8) 0.0336(9) -0.0057(7) -0.0150(8) 0.0084(7) C15 0.0374(9) 0.0170(7) 0.0289(8) -0.0003(6) -0.0127(7) -0.0035(6) C16 0.0219(8) 0.0187(7) 0.0231(7) -0.0007(6) -0.0068(6) -0.0020(6) Cl2 0.01737(18) 0.02119(18) 0.02528(18) -0.00189(14) -0.00506(14) -0.00154(13) C17 0.0807(18) 0.0488(13) 0.0554(14) -0.0129(11) 0.0006(13) -0.0043(12) O1 0.120(4) 0.0395(12) 0.0490(12) -0.0035(9) 0.0050(15) -0.0139(15) O1A 0.054(9) 0.089(12) 0.052(6) -0.040(6) 0.013(5) -0.046(8) O2 0.0566(9) 0.0440(8) 0.0296(7) 0.0086(6) -0.0217(7) -0.0224(7) _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 Ni Cl1 2.4222(4) . ? Ni N1 2.1014(11) . ? Ni N2 2.0020(11) . ? Ni N3 2.1293(11) . ? Ni N4 2.0726(11) 2_666 ? Ni N5 2.1226(11) 2_666 ? N1 C1 1.3344(18) . ? N1 C5 1.3506(18) . ? N2 C6 1.2660(17) . ? N2 C7 1.4575(17) . ? N3 H3N 0.894(16) . ? N3 C8 1.4844(17) . ? N3 C9 1.4767(17) . ? N4 Ni 2.0726(11) 2_666 ? N4 C10 1.4643(17) . ? N4 C11 1.2744(18) . ? N5 Ni 2.1227(11) 2_666 ? N5 C12 1.3484(18) . ? N5 C16 1.3312(18) . ? C1 H1 0.950 . ? C1 C2 1.388(2) . ? C2 H2 0.950 . ? C2 C3 1.369(2) . ? C3 H3 0.950 . ? C3 C4 1.391(2) . ? C4 H4 0.950 . ? C4 C5 1.3830(19) . ? C5 C6 1.4747(19) . ? C6 H6 0.950 . ? C7 H7A 0.990 . ? C7 H7B 0.990 . ? C7 C8 1.519(2) . ? C8 H8A 0.990 . ? C8 H8B 0.990 . ? C9 H9A 0.990 . ? C9 H9B 0.990 . ? C9 C10 1.5239(19) . ? C10 H10A 0.990 . ? C10 H10B 0.990 . ? C11 H11 0.950 . ? C11 C12 1.462(2) . ? C12 C13 1.389(2) . ? C13 H13 0.950 . ? C13 C14 1.381(2) . ? C14 H14 0.950 . ? C14 C15 1.374(2) . ? C15 H15 0.950 . ? C15 C16 1.393(2) . ? C16 H16 0.950 . ? C17 H17A 0.980 . ? C17 H17B 0.980 . ? C17 H17C 0.980 . ? C17 H17D 0.980 . ? C17 H17E 0.980 . ? C17 H17F 0.980 . ? C17 O1 1.372(3) . ? C17 O1A 1.400(9) . ? O1 H1O 0.840 . ? O1A H1A 0.840 . ? O2 H2A 0.81(2) . ? O2 H2B 0.87(3) . ? 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 Cl1 Ni N1 90.02(3) . . ? Cl1 Ni N2 94.64(3) . . ? Cl1 Ni N3 85.76(3) . . ? Cl1 Ni N4 94.25(3) . 2_666 ? Cl1 Ni N5 172.57(3) . 2_666 ? N1 Ni N2 78.62(4) . . ? N1 Ni N3 159.78(4) . . ? N1 Ni N4 99.77(4) . 2_666 ? N1 Ni N5 89.03(4) . 2_666 ? N2 Ni N3 82.02(4) . . ? N2 Ni N4 170.96(4) . 2_666 ? N2 Ni N5 92.39(4) . 2_666 ? N3 Ni N4 100.26(4) . 2_666 ? N3 Ni N5 97.60(4) . 2_666 ? N4 Ni N5 78.66(5) 2_666 2_666 ? Ni N1 C1 129.62(10) . . ? Ni N1 C5 112.08(9) . . ? C1 N1 C5 118.24(11) . . ? Ni N2 C6 118.32(9) . . ? Ni N2 C7 115.55(8) . . ? C6 N2 C7 126.12(12) . . ? Ni N3 H3N 96.9(9) . . ? Ni N3 C8 106.71(8) . . ? Ni N3 C9 118.37(8) . . ? H3N N3 C8 106.8(10) . . ? H3N N3 C9 111.2(10) . . ? C8 N3 C9 114.87(10) . . ? Ni N4 C10 127.32(9) 2_666 . ? Ni N4 C11 114.34(10) 2_666 . ? C10 N4 C11 118.33(12) . . ? Ni N5 C12 111.87(9) 2_666 . ? Ni N5 C16 129.71(9) 2_666 . ? C12 N5 C16 117.97(12) . . ? N1 C1 H1 118.8 . . ? N1 C1 C2 122.35(14) . . ? H1 C1 C2 118.8 . . ? C1 C2 H2 120.4 . . ? C1 C2 C3 119.27(14) . . ? H2 C2 C3 120.4 . . ? C2 C3 H3 120.4 . . ? C2 C3 C4 119.18(13) . . ? H3 C3 C4 120.4 . . ? C3 C4 H4 120.8 . . ? C3 C4 C5 118.40(14) . . ? H4 C4 C5 120.8 . . ? N1 C5 C4 122.53(13) . . ? N1 C5 C6 115.01(11) . . ? C4 C5 C6 122.45(13) . . ? N2 C6 C5 115.93(12) . . ? N2 C6 H6 122.0 . . ? C5 C6 H6 122.0 . . ? N2 C7 H7A 110.3 . . ? N2 C7 H7B 110.3 . . ? N2 C7 C8 107.18(11) . . ? H7A C7 H7B 108.5 . . ? H7A C7 C8 110.3 . . ? H7B C7 C8 110.3 . . ? N3 C8 C7 111.24(11) . . ? N3 C8 H8A 109.4 . . ? N3 C8 H8B 109.4 . . ? C7 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N3 C9 H9A 108.7 . . ? N3 C9 H9B 108.7 . . ? N3 C9 C10 114.31(11) . . ? H9A C9 H9B 107.6 . . ? H9A C9 C10 108.7 . . ? H9B C9 C10 108.7 . . ? N4 C10 C9 110.13(10) . . ? N4 C10 H10A 109.6 . . ? N4 C10 H10B 109.6 . . ? C9 C10 H10A 109.6 . . ? C9 C10 H10B 109.6 . . ? H10A C10 H10B 108.1 . . ? N4 C11 H11 120.5 . . ? N4 C11 C12 119.09(12) . . ? H11 C11 C12 120.5 . . ? N5 C12 C11 115.22(12) . . ? N5 C12 C13 122.42(14) . . ? C11 C12 C13 122.35(13) . . ? C12 C13 H13 120.7 . . ? C12 C13 C14 118.65(14) . . ? H13 C13 C14 120.7 . . ? C13 C14 H14 120.3 . . ? C13 C14 C15 119.42(14) . . ? H14 C14 C15 120.3 . . ? C14 C15 H15 120.7 . . ? C14 C15 C16 118.54(15) . . ? H15 C15 C16 120.7 . . ? N5 C16 C15 122.99(14) . . ? N5 C16 H16 118.5 . . ? C15 C16 H16 118.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17A C17 O1 109.5 . . ? H17B C17 H17C 109.5 . . ? H17B C17 O1 109.5 . . ? H17C C17 O1 109.5 . . ? H17D C17 H17E 109.5 . . ? H17D C17 H17F 109.5 . . ? H17D C17 O1A 109.5 . . ? H17E C17 H17F 109.5 . . ? H17E C17 O1A 109.5 . . ? H17F C17 O1A 109.5 . . ? C17 O1 H1O 109.5 . . ? C17 O1A H1A 109.5 . . ? H2A O2 H2B 104(2) . . ? 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 Ni N1 C1 C2 -177.16(11) . . . . ? C5 N1 C1 C2 0.0(2) . . . . ? N1 C1 C2 C3 -1.1(2) . . . . ? C1 C2 C3 C4 0.7(2) . . . . ? C2 C3 C4 C5 0.7(2) . . . . ? Ni N1 C5 C4 179.12(11) . . . . ? Ni N1 C5 C6 -1.52(14) . . . . ? C1 N1 C5 C4 1.5(2) . . . . ? C1 N1 C5 C6 -179.13(12) . . . . ? C3 C4 C5 N1 -1.8(2) . . . . ? C3 C4 C5 C6 178.84(13) . . . . ? Ni N2 C6 C5 1.25(16) . . . . ? C7 N2 C6 C5 -177.51(12) . . . . ? N1 C5 C6 N2 0.28(18) . . . . ? C4 C5 C6 N2 179.64(13) . . . . ? Ni N2 C7 C8 31.18(13) . . . . ? C6 N2 C7 C8 -150.03(13) . . . . ? Ni N3 C8 C7 38.49(13) . . . . ? C9 N3 C8 C7 -94.82(13) . . . . ? N2 C7 C8 N3 -45.90(15) . . . . ? Ni N3 C9 C10 161.22(9) . . . . ? C8 N3 C9 C10 -71.16(14) . . . . ? Ni N4 C10 C9 -77.28(13) 2_666 . . . ? C11 N4 C10 C9 103.71(14) . . . . ? N3 C9 C10 N4 -63.49(14) . . . . ? Ni N4 C11 C12 5.12(16) 2_666 . . . ? C10 N4 C11 C12 -175.75(11) . . . . ? Ni N5 C12 C11 -7.80(14) 2_666 . . . ? Ni N5 C12 C13 172.63(11) 2_666 . . . ? C16 N5 C12 C11 179.11(12) . . . . ? C16 N5 C12 C13 -0.5(2) . . . . ? N4 C11 C12 N5 2.04(19) . . . . ? N4 C11 C12 C13 -178.39(13) . . . . ? N5 C12 C13 C14 -0.1(2) . . . . ? C11 C12 C13 C14 -179.60(13) . . . . ? C12 C13 C14 C15 0.8(2) . . . . ? C13 C14 C15 C16 -0.9(2) . . . . ? Ni N5 C16 C15 -171.36(11) 2_666 . . . ? C12 N5 C16 C15 0.3(2) . . . . ? C14 C15 C16 N5 0.4(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3N Cl1 0.894(16) 2.682(15) 3.1045(12) 110.1(11) . O1 H1O O2 0.84 2.03 2.822(3) 156 . O1A H1A O2 0.84 1.87 2.571(9) 140 . O2 H2A Cl2 0.81(2) 2.31(2) 3.1122(14) 172.3(19) . O2 H2B Cl2 0.87(3) 2.33(3) 3.1796(14) 167(2) 2_756 _refine_diff_density_max 0.322 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.052 _shelxl_version_number 2013-2 _shelx_res_file ; TITL rah202 in P-1 CELL 0.71073 9.2913 10.2003 12.0495 83.850 67.556 82.657 ZERR 1.00 0.0005 0.0005 0.0007 0.004 0.005 0.004 LATT 1 SFAC C H N CL NI O UNIT 34 50 10 4 2 4 REM red block SIZE 0.20 0.20 0.10 TEMP -123 L.S. 8 ACTA FMAP 2 PLAN 10 BOND $H CONF HTAB N3 Cl1 HTAB O1 O2 HTAB O1A O2 HTAB O2 Cl2 HTAB O2 Cl2_$1 EQIV $1 -x+2, -y, -z+1 rem EXTI 0.000000 WGHT 0.034700 FVAR 0.54540 0.81950 NI 5 0.660429 0.595498 0.259508 11.00000 0.00985 0.01440 = 0.01214 -0.00024 -0.00276 -0.00117 CL1 4 0.694255 0.366838 0.209743 11.00000 0.01940 0.01714 = 0.02282 -0.00512 -0.00596 -0.00224 N1 3 0.678619 0.658558 0.083208 11.00000 0.01500 0.01957 = 0.01537 -0.00050 -0.00510 -0.00175 N2 3 0.888116 0.622007 0.180462 11.00000 0.01132 0.01563 = 0.01580 -0.00116 -0.00368 -0.00130 N3 3 0.728608 0.520521 0.405810 11.00000 0.01232 0.01566 = 0.01419 -0.00088 -0.00345 -0.00226 H3N 2 0.689384 0.442387 0.417691 11.00000 0.01665 N4 3 0.580640 0.399903 0.656563 11.00000 0.01179 0.02184 = 0.01118 0.00049 -0.00409 -0.00273 N5 3 0.400170 0.204655 0.693351 11.00000 0.01553 0.01621 = 0.01539 0.00076 -0.00366 0.00011 C1 1 0.569025 0.674564 0.035399 11.00000 0.01735 0.03465 = 0.02036 0.00045 -0.00745 -0.00473 AFIX 43 H1 2 0.464481 0.659805 0.085826 11.00000 -1.20000 AFIX 0 C2 1 0.602301 0.711999 -0.085349 11.00000 0.02755 0.04076 = 0.02046 -0.00001 -0.01420 -0.00289 AFIX 43 H2 2 0.522019 0.721148 -0.117009 11.00000 -1.20000 AFIX 0 C3 1 0.752148 0.735605 -0.158359 11.00000 0.03258 0.03442 = 0.01462 0.00033 -0.00832 -0.00387 AFIX 43 H3 2 0.776817 0.762248 -0.241040 11.00000 -1.20000 AFIX 0 C4 1 0.867753 0.720092 -0.109965 11.00000 0.02180 0.02587 = 0.01434 -0.00159 -0.00165 -0.00422 AFIX 43 H4 2 0.972343 0.736790 -0.158519 11.00000 -1.20000 AFIX 0 C5 1 0.826806 0.679773 0.010543 11.00000 0.01615 0.01562 = 0.01450 -0.00209 -0.00336 -0.00036 C6 1 0.941487 0.658163 0.069560 11.00000 0.01302 0.01890 = 0.01730 -0.00216 -0.00173 -0.00223 AFIX 43 H6 2 1.048872 0.670613 0.026957 11.00000 -1.20000 AFIX 0 C7 1 0.976616 0.599477 0.259021 11.00000 0.01040 0.02728 = 0.01797 -0.00088 -0.00524 -0.00235 AFIX 23 H7A 2 0.973323 0.682271 0.296299 11.00000 -1.20000 H7B 2 1.087215 0.569560 0.212477 11.00000 -1.20000 AFIX 0 C8 1 0.901517 0.493547 0.355335 11.00000 0.01286 0.02451 = 0.01665 -0.00087 -0.00535 0.00323 AFIX 23 H8A 2 0.930209 0.406063 0.320248 11.00000 -1.20000 H8B 2 0.941911 0.490438 0.420726 11.00000 -1.20000 AFIX 0 C9 1 0.665141 0.592914 0.516837 11.00000 0.01321 0.01688 = 0.01521 -0.00264 -0.00324 -0.00362 AFIX 23 H9A 2 0.554021 0.623792 0.532869 11.00000 -1.20000 H9B 2 0.722370 0.672249 0.503432 11.00000 -1.20000 AFIX 0 C10 1 0.675839 0.511804 0.627691 11.00000 0.01346 0.02699 = 0.01444 -0.00201 -0.00410 -0.00676 AFIX 23 H10A 2 0.786179 0.478582 0.612385 11.00000 -1.20000 H10B 2 0.638568 0.568551 0.696792 11.00000 -1.20000 AFIX 0 C11 1 0.649976 0.284916 0.629795 11.00000 0.01157 0.02820 = 0.01652 -0.00091 -0.00343 0.00258 AFIX 43 H11 2 0.760970 0.271758 0.597042 11.00000 -1.20000 AFIX 0 C12 1 0.556340 0.173488 0.650185 11.00000 0.01921 0.02096 = 0.01618 -0.00026 -0.00533 0.00327 C13 1 0.623614 0.044854 0.625986 11.00000 0.02481 0.02469 = 0.03050 -0.00567 -0.00759 0.00960 AFIX 43 H13 2 0.734058 0.025669 0.595519 11.00000 -1.20000 AFIX 0 C14 1 0.526697 -0.054516 0.647116 11.00000 0.04124 0.01840 = 0.03356 -0.00566 -0.01503 0.00844 AFIX 43 H14 2 0.569753 -0.143453 0.632228 11.00000 -1.20000 AFIX 0 C15 1 0.367416 -0.023661 0.689868 11.00000 0.03738 0.01701 = 0.02891 -0.00025 -0.01271 -0.00347 AFIX 43 H15 2 0.298769 -0.090376 0.703886 11.00000 -1.20000 AFIX 0 C16 1 0.308835 0.107560 0.712195 11.00000 0.02191 0.01874 = 0.02314 -0.00067 -0.00678 -0.00198 AFIX 43 H16 2 0.198686 0.128750 0.742240 11.00000 -1.20000 AFIX 0 CL2 4 1.056464 0.210680 0.480652 11.00000 0.01737 0.02119 = 0.02528 -0.00189 -0.00506 -0.00154 C17 1 0.778442 0.072306 0.979255 11.00000 0.08069 0.04875 = 0.05543 -0.01293 0.00056 -0.00431 PART 1 AFIX 33 H17A 2 0.868685 0.013585 0.983251 21.00000 -1.50000 H17B 2 0.694027 0.019154 0.986905 21.00000 -1.50000 H17C 2 0.742104 0.132204 1.044932 21.00000 -1.50000 AFIX 33 PART 2 H17D 2 0.789059 0.082008 1.055743 -21.00000 -1.50000 H17E 2 0.748156 -0.016270 0.979273 -21.00000 -1.50000 H17F 2 0.698005 0.139241 0.969195 -21.00000 -1.50000 AFIX 0 PART 1 O1 6 0.821160 0.145082 0.870992 21.00000 0.12019 0.03950 = 0.04903 -0.00349 0.00497 -0.01386 AFIX 83 H1O 2 0.850321 0.093822 0.814748 21.00000 -1.50000 AFIX 0 PART 2 O1A 6 0.921499 0.089370 0.884300 -21.00000 0.05426 0.08886 = 0.05151 -0.03990 0.01273 -0.04566 AFIX 83 H1A 2 0.912400 0.081050 0.818740 -21.00000 -1.50000 AFIX 0 PART 0 O2 6 1.006758 -0.016617 0.681961 11.00000 0.05658 0.04401 = 0.02965 0.00858 -0.02172 -0.02242 H2A 2 1.024391 0.045782 0.632784 11.00000 0.03940 H2B 2 0.996009 -0.079846 0.643650 11.00000 0.07388 HKLF 4 REM rah202 in P-1 REM R1 = 0.0236 for 4215 Fo > 4sig(Fo) and 0.0289 for all 4900 data REM 266 parameters refined using 0 restraints END WGHT 0.0345 0.0000 REM Highest difference peak 0.322, deepest hole -0.362, 1-sigma level 0.052 Q1 1 0.6001 0.2325 0.6324 11.00000 0.05 0.32 Q2 1 0.6784 0.5448 0.5639 11.00000 0.05 0.30 Q3 1 0.6971 0.5610 0.4670 11.00000 0.05 0.29 Q4 1 0.7978 0.7542 -0.1313 11.00000 0.05 0.29 Q5 1 0.3512 0.0411 0.6768 11.00000 0.05 0.29 Q6 1 0.8386 0.7121 -0.0419 11.00000 0.05 0.29 Q7 1 0.7378 0.1016 0.8681 11.00000 0.05 0.28 Q8 1 0.9404 0.5473 0.3056 11.00000 0.05 0.27 Q9 1 0.6970 0.5542 0.3554 11.00000 0.05 0.27 Q10 1 0.4813 0.1822 0.6616 11.00000 0.05 0.27 ; _shelx_res_checksum 18960 _shelx_hkl_file ; 0 0 -2 986.59 4.64 0 0 2 996.76 4.65 0 0 2 1007.31 5.84 0 0 -3 753.79 5.01 0 0 3 717.49 4.91 0 0 3 724.25 6.15 0 0 -4 177.95 3.14 0 0 4 178.28 3.83 0 0 -5 241.40 3.91 0 0 5 221.08 4.73 0 0 6 4.31 1.98 0 0 -6 3.72 1.76 0 0 -7 189.88 4.09 0 0 7 202.45 5.24 0 0 -7 186.20 5.21 0 0 -8 357.54 5.82 0 0 -8 341.39 7.33 0 0 8 356.16 7.29 0 0 -9 49.17 3.97 0 0 -9 48.87 2.89 0 0 -10 6.65 2.25 0 0 -10 7.33 3.42 0 0 -11 88.12 5.52 0 0 -11 92.04 3.97 0 0 -12 40.10 3.28 0 0 -12 52.47 5.17 0 0 -13 37.01 5.10 0 0 -13 41.02 3.45 0 -1 -13 96.19 4.66 0 -1 -12 12.31 2.72 0 -1 -12 11.83 3.71 0 -1 -11 470.16 10.26 0 -1 -11 504.76 8.44 0 -1 -10 32.84 2.96 0 -1 -10 31.57 3.46 0 -1 -9 141.07 5.48 0 -1 -9 157.09 4.58 0 -1 -8 44.07 2.80 0 -1 -8 37.46 3.52 0 1 8 41.15 3.00 0 1 7 24.98 2.36 0 -1 -7 23.30 2.66 0 -1 -7 26.81 2.29 0 -1 -6 989.52 10.11 0 1 6 1009.67 10.07 0 -1 -6 1000.45 8.51 0 1 5 103.70 3.32 0 -1 -5 101.09 3.38 0 -1 -5 98.57 2.94 0 1 4 218.78 4.09 0 -1 -4 226.80 4.24 0 -1 -4 218.71 3.70 0 1 3 66.48 2.34 0 -1 -3 58.34 2.31 0 -1 -2 23.02 1.44 0 1 2 22.62 1.45 0 1 -2 1278.42 6.06 0 -1 2 1277.95 5.48 0 -1 2 1301.45 6.96 0 1 -2 1280.95 5.49 0 -1 3 619.18 5.88 0 -1 3 605.80 4.48 0 1 -3 588.02 4.74 0 1 -3 595.34 4.54 0 -1 4 2704.00 10.67 0 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629.20 5.27 1 -4 -2 198.02 2.32 1 -4 -2 202.91 3.46 -1 4 2 195.36 2.34 -1 4 2 196.18 3.47 1 -4 -1 2614.78 12.06 -1 4 1 2570.04 14.35 1 -4 0 1.40 1.43 -1 4 0 0.19 1.53 -1 4 0 0.07 1.93 -1 4 0 0.43 1.45 -1 4 -1 1482.38 7.55 -1 4 -1 1488.85 10.50 1 -4 1 1547.71 5.67 -1 4 -1 1503.46 10.88 -1 4 -2 51.83 2.63 1 -4 2 52.47 3.11 1 -4 2 55.80 1.81 -1 4 -2 52.96 2.82 1 -4 2 54.95 1.62 -1 4 -3 472.86 5.37 1 -4 3 473.98 5.28 1 -4 3 454.55 6.38 -1 4 -3 471.38 7.09 -1 4 -3 484.66 6.60 1 -4 4 20.15 1.97 -1 4 -4 21.52 2.39 1 -4 4 20.18 2.16 -1 4 -4 19.27 2.22 1 -4 5 859.44 8.95 1 -4 5 835.00 8.74 -1 4 -5 861.62 9.10 -1 4 -5 884.81 9.06 -1 4 -6 49.24 2.94 -1 4 -6 46.63 3.20 1 -4 6 49.47 2.81 1 -4 6 52.67 2.83 -1 4 -6 52.06 2.81 1 -4 6 51.79 2.72 1 -4 7 1.66 1.85 1 -4 7 2.21 2.13 -1 4 -7 0.36 1.80 -1 4 -7 0.98 1.99 -1 4 -7 1.85 2.30 -1 4 -8 15.63 2.64 -1 4 -8 15.69 2.50 1 -4 8 13.83 2.19 -1 4 -8 16.71 2.29 -1 4 -9 -0.45 2.23 1 -4 9 0.04 1.97 -1 4 -9 1.28 2.64 -1 4 -9 0.54 1.89 -1 4 -10 172.49 6.70 -1 4 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2 281.06 5.72 1 -5 2 286.77 3.48 -1 5 -2 277.35 5.57 1 -5 3 2389.83 11.72 1 -5 3 2396.84 8.68 -1 5 -3 2351.82 15.76 1 -5 3 2319.29 14.83 -1 5 -3 2347.78 16.20 1 -5 4 14.48 1.78 -1 5 -4 18.63 2.44 -1 5 -4 19.47 2.88 1 -5 4 17.85 2.65 1 -5 4 17.75 2.28 1 -5 5 156.15 4.14 1 -5 5 156.33 4.56 1 -5 5 157.45 4.34 -1 5 -5 156.05 4.61 -1 5 -5 161.82 5.42 -1 5 -6 17.75 2.45 1 -5 6 21.10 2.36 1 -5 6 19.04 2.35 -1 5 -6 21.32 2.57 1 -5 6 22.18 2.55 1 -5 7 370.53 7.25 -1 5 -7 370.28 7.51 -1 5 -7 380.60 7.17 1 -5 7 368.59 6.86 1 -5 7 382.69 6.75 -1 5 -8 0.58 2.12 1 -5 8 1.18 1.99 -1 5 -8 -0.32 2.40 -1 5 -9 6.68 2.77 -1 5 -9 5.00 2.52 -1 5 -10 1.74 2.45 -1 5 -10 1.59 3.14 -1 5 -11 85.91 4.48 -1 5 -11 80.07 5.39 -1 5 -12 -0.91 2.68 -1 5 -12 0.62 3.13 -1 5 -13 11.50 3.99 1 -6 -13 44.88 4.73 1 -6 -12 365.07 9.34 1 -6 -12 374.15 9.07 1 -6 -11 -0.09 2.88 1 -6 -11 -0.43 3.22 1 -6 -10 182.86 6.23 1 -6 -9 46.49 3.76 1 -6 -8 310.22 4.82 -1 6 8 345.11 6.83 1 -6 -8 347.21 7.87 1 -6 -7 64.78 2.39 -1 6 7 63.45 3.03 1 -6 -7 59.36 3.93 1 -6 -6 7.46 1.36 1 -6 -6 9.11 2.84 -1 6 6 8.09 1.66 1 -6 -5 143.23 5.03 -1 6 5 158.94 3.48 1 -6 -5 162.01 3.42 1 -6 -4 67.39 3.91 1 -6 -4 68.32 2.42 -1 6 4 71.41 2.04 1 -6 -3 284.10 4.57 -1 6 3 272.53 2.61 -1 6 3 282.28 4.64 1 -6 -3 265.32 6.16 1 -6 -2 13.88 1.69 1 -6 -2 12.37 2.24 -1 6 2 11.42 1.75 -1 6 1 19.85 2.10 -1 6 1 18.09 2.11 1 -6 -1 19.66 2.77 -1 6 0 45.13 2.96 -1 6 0 42.73 2.09 -1 6 0 44.42 2.67 1 -6 0 40.78 2.88 -1 6 -1 153.69 4.54 1 -6 1 150.93 1.67 -1 6 -1 154.34 4.51 1 -6 1 157.81 4.83 -1 6 -2 59.58 3.20 1 -6 2 59.31 3.27 1 -6 2 58.94 3.22 -1 6 -2 60.75 3.36 1 -6 2 59.42 1.79 1 -6 3 536.40 8.02 1 -6 3 586.45 6.00 -1 6 -3 546.00 8.64 1 -6 3 542.49 8.50 -1 6 -3 582.56 8.77 -1 6 -4 168.38 5.02 1 -6 4 161.18 3.81 1 -6 4 153.27 4.55 1 -6 4 146.59 4.71 -1 6 -4 158.91 5.28 1 -6 5 333.27 6.50 -1 6 -5 315.80 6.76 -1 6 -5 335.27 7.60 1 -6 5 307.94 6.70 1 -6 5 335.56 3.52 1 -6 5 330.52 5.86 -1 6 -5 333.40 6.04 1 -6 6 36.96 3.09 -1 6 -6 38.60 3.01 1 -6 6 40.23 2.84 -1 6 -6 39.01 3.85 -1 6 -6 34.76 3.11 1 -6 6 34.80 2.86 1 -6 7 370.69 7.33 1 -6 7 359.12 7.30 -1 6 -7 367.03 8.77 1 -6 7 332.01 6.81 -1 6 -7 353.91 7.44 -1 6 -8 4.25 2.85 -1 6 -8 2.24 3.27 -1 6 -9 136.99 5.95 -1 6 -9 140.85 6.55 -1 6 -10 110.21 6.26 -1 6 -11 171.78 7.64 -1 6 -12 2.14 3.30 1 -7 -12 62.26 4.76 1 -7 -12 72.80 5.35 1 -7 -11 62.48 4.71 1 -7 -10 211.64 7.03 1 -7 -9 39.34 3.93 1 -7 -8 270.78 7.36 -1 7 8 286.10 6.05 -1 7 7 42.30 2.54 1 -7 -7 41.77 2.10 1 -7 -7 37.87 3.74 1 -7 -6 57.80 3.96 1 -7 -6 65.27 2.44 -1 7 6 61.07 2.54 -1 7 5 120.23 2.78 1 -7 -5 115.92 5.03 1 -7 -5 114.10 3.12 1 -7 -4 301.83 7.13 1 -7 -4 295.24 4.89 -1 7 4 309.06 3.18 1 -7 -3 36.79 3.35 -1 7 3 36.86 2.29 -1 7 2 196.99 4.44 1 -7 -2 210.24 6.10 -1 7 1 487.66 8.46 1 -7 -1 481.19 8.60 -1 7 1 472.71 6.92 -1 7 0 305.13 6.05 1 -7 0 275.85 6.77 -1 7 0 304.04 6.75 -1 7 0 291.82 4.62 1 -7 1 1.74 2.74 -1 7 -1 2.77 2.25 -1 7 -1 0.71 2.14 1 -7 2 2.60 0.90 1 -7 2 0.46 1.92 -1 7 -2 2.61 2.07 1 -7 2 2.72 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518.90 7.96 6 6 5 170.79 4.05 -6 -6 -5 164.61 5.09 6 6 5 170.54 4.76 6 6 6 59.40 2.43 6 6 6 69.41 3.33 -6 -6 -6 66.56 3.98 6 6 7 2.98 1.79 6 6 7 3.40 1.17 -6 -6 -7 2.09 2.63 6 6 8 110.88 3.46 6 6 8 111.58 2.36 -6 -6 -8 112.61 5.09 -6 -6 -9 252.46 7.32 -6 -6 -10 1.99 3.29 -6 -6 -11 3.41 3.16 -6 -6 -12 6.83 3.33 -6 -6 -13 253.31 8.60 -6 -5 7 11.70 2.97 6 5 -7 13.52 4.12 6 5 -6 264.74 9.01 -6 -5 6 286.41 7.04 6 5 -5 2.46 3.05 6 5 -4 14.65 3.76 6 5 -3 111.34 5.57 6 5 -2 226.97 7.07 -6 -5 1 22.08 0.85 6 5 -1 21.44 3.38 -6 -5 0 354.83 4.18 6 5 0 351.45 8.11 -6 -5 -1 163.45 3.52 6 5 1 155.39 5.56 6 5 1 161.20 4.59 -6 -5 -2 682.25 7.49 6 5 2 690.11 9.04 6 5 2 720.13 9.58 -6 -5 -3 39.13 2.62 6 5 3 38.22 2.71 6 5 3 39.56 3.62 -6 -5 -4 382.19 6.64 6 5 4 406.09 6.73 -6 -5 -5 72.81 3.75 6 5 5 83.75 3.07 6 5 5 74.34 3.15 -6 -5 -6 317.05 6.79 6 5 6 314.25 5.08 6 5 6 325.24 5.60 -6 -5 -7 23.69 3.17 6 5 7 22.03 1.76 6 5 7 22.16 1.96 6 5 8 236.82 4.13 6 5 8 248.29 4.08 -6 -5 -8 239.86 6.73 -6 -5 -9 7.80 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