data_mo_JC_4Pyr_0m # start Validation Reply Form _vrf_THETM01_mo_JC_4Pyr_0m ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The diffraction power of the crystal was very poor. ; _vrf_PLAT201_mo_JC_4Pyr_0m ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 48 Report RESPONSE: The amount of data was not enough to refine all the atoms anisotropic. ; # end Validation Reply Form _audit_creation_method SHELXL-2014 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H14 N4 Ni' _chemical_formula_weight 369.06 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' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _space_group_IT_number 9 _symmetry_space_group_name_H-M Cc _space_group_name_Hall 'C -2yc' _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+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 19.790(11) _cell_length_b 25.183(14) _cell_length_c 6.297(4) _cell_angle_alpha 90 _cell_angle_beta 106.786(16) _cell_angle_gamma 90 _cell_volume 3005(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 475 _cell_measurement_theta_min 3.75 _cell_measurement_theta_max 16.55 _exptl_crystal_description BLock _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.632 _exptl_crystal_F_000 1520 _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 1.301 _shelx_estimated_absorpt_T_min 0.938 _shelx_estimated_absorpt_T_max 0.974 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.679 _exptl_absorpt_correction_T_max 0.974 _exptl_absorpt_process_details ; SADABS Version 2008/1 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_support 'magnetic support with MicroMount' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'Microfocus source E025 IuS' _diffrn_source_type 'Bruker APEX DUO' _diffrn_source_power 50 _diffrn_source_current 0.6 _diffrn_source_size '0.2 mm x 0.2 mm fine focus' _diffrn_radiation_monochromator 'Quazar MX Multilayer Optics' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'APEX DUO Kappa 4-axis goniometer' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_reflns_number 6827 _diffrn_reflns_av_unetI/netI 0.1313 _diffrn_reflns_av_R_equivalents 0.1381 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -5 _diffrn_reflns_limit_l_max 5 _diffrn_reflns_theta_min 1.345 _diffrn_reflns_theta_max 17.360 _diffrn_reflns_theta_full 20.990 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.563 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.563 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_point_group_measured_fraction_full 0.552 _reflns_number_total 1790 _reflns_number_gt 1213 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.954 _reflns_Friedel_fraction_max 0.938 _reflns_Friedel_fraction_full 0.541 _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 APEX2 v2011.4-0' _computing_cell_refinement 'Bruker APEX2 v2011.4-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'Sir2011' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; ? ; _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^)+(0.0687P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 486 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.08(7) _refine_ls_number_reflns 1790 _refine_ls_number_parameters 211 _refine_ls_number_restraints 56 _refine_ls_R_factor_all 0.1146 _refine_ls_R_factor_gt 0.0639 _refine_ls_wR_factor_ref 0.1590 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.055 _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 Ni1A Ni 0.1036(2) 0.1252(2) 0.5075(6) 0.036(2) Uani 1 1 d . . . . . Ni1B Ni 0.0578(2) 0.37072(19) 0.9776(5) 0.035(2) Uani 1 1 d . . . . . N1A N 0.1486(13) 0.1688(10) 0.755(4) 0.026(7) Uiso 1 1 d . U . . . N1B N -0.0060(13) 0.3269(10) 1.090(4) 0.030(7) Uiso 1 1 d . U . . . N2A N 0.0247(15) 0.1392(12) 0.592(5) 0.035(7) Uiso 1 1 d . U . . . N2B N 0.1220(14) 0.3545(11) 1.251(5) 0.029(7) Uiso 1 1 d . U . . . N3A N 0.0387(14) 0.0995(12) 0.262(5) 0.031(7) Uiso 1 1 d . U . . . N3B N 0.1367(15) 0.3963(13) 0.928(5) 0.034(7) Uiso 1 1 d . U . . . N4A N 0.1687(14) 0.0932(11) 0.376(4) 0.037(7) Uiso 1 1 d . U . . . N4B N 0.0094(14) 0.4071(11) 0.704(4) 0.030(7) Uiso 1 1 d . U . . . C1A C 0.2181(15) 0.1812(13) 0.833(5) 0.029(8) Uiso 1 1 d . U . . . H1A H 0.2491 0.1718 0.7534 0.035 Uiso 1 1 calc R U . . . C1B C -0.0750(16) 0.3164(13) 0.991(5) 0.036(8) Uiso 1 1 d . U . . . H1B H -0.0953 0.3270 0.8444 0.044 Uiso 1 1 calc R U . . . C2A C 0.2432(16) 0.2085(13) 1.036(5) 0.031(8) Uiso 1 1 d . U . . . H2A H 0.2910 0.2167 1.0874 0.037 Uiso 1 1 calc R U . . . C2B C -0.1139(17) 0.2916(14) 1.096(5) 0.042(8) Uiso 1 1 d . U . . . H2B H -0.1612 0.2853 1.0227 0.051 Uiso 1 1 calc R U . . . C3A C 0.1998(18) 0.2235(13) 1.163(6) 0.033(8) Uiso 1 1 d . U . . . H3A H 0.2173 0.2418 1.2961 0.039 Uiso 1 1 calc R U . . . C3B C -0.0858(17) 0.2738(13) 1.325(5) 0.040(8) Uiso 1 1 d . U . . . H3B H -0.1135 0.2565 1.4002 0.048 Uiso 1 1 calc R U . . . C4A C 0.1301(19) 0.2102(13) 1.084(6) 0.031(9) Uiso 1 1 d . U . . . H4A H 0.0978 0.2185 1.1605 0.038 Uiso 1 1 calc R U . . . C4B C -0.0134(18) 0.2846(13) 1.423(6) 0.031(9) Uiso 1 1 d . U . . . H4B H 0.0091 0.2745 1.5683 0.037 Uiso 1 1 calc R U . . . C5A C 0.1103(18) 0.1839(13) 0.884(6) 0.020(7) Uiso 1 1 d . U . . . C5B C 0.0223(18) 0.3098(14) 1.299(6) 0.026(8) Uiso 1 1 d . U . . . C6A C 0.0308(19) 0.1706(15) 0.779(6) 0.039(8) Uiso 1 1 d . U . . . C6B C 0.1036(18) 0.3226(13) 1.396(6) 0.021(7) Uiso 1 1 d . U . . . C7A C -0.025(2) 0.1860(14) 0.833(6) 0.040(9) Uiso 1 1 d . U . . . H7A H -0.0199 0.2068 0.9582 0.048 Uiso 1 1 calc R U . . . C7B C 0.1486(19) 0.3035(15) 1.580(6) 0.033(9) Uiso 1 1 d . U . . . H7B H 0.1337 0.2821 1.6775 0.040 Uiso 1 1 calc R U . . . C8A C -0.0928(18) 0.1717(14) 0.704(6) 0.047(8) Uiso 1 1 d . U . . . H8A H -0.1327 0.1812 0.7446 0.056 Uiso 1 1 calc R U . . . C8B C 0.2165(17) 0.3167(13) 1.616(5) 0.028(8) Uiso 1 1 d . U . . . H8B H 0.2488 0.3048 1.7462 0.034 Uiso 1 1 calc R U . . . C9A C -0.0982(17) 0.1417(13) 0.505(5) 0.043(8) Uiso 1 1 d . U . . . H9A H -0.1423 0.1339 0.4075 0.051 Uiso 1 1 calc R U . . . C9B C 0.2410(16) 0.3464(12) 1.474(5) 0.035(8) Uiso 1 1 d . U . . . H9B H 0.2889 0.3538 1.5042 0.042 Uiso 1 1 calc R U . . . C10A C -0.037(2) 0.1242(15) 0.458(6) 0.046(8) Uiso 1 1 d . U . . . C10B C 0.1937(17) 0.3652(14) 1.284(5) 0.033(7) Uiso 1 1 d . U . . . C11A C -0.0300(18) 0.0969(15) 0.264(6) 0.036(7) Uiso 1 1 d . U . . . C11B C 0.198(2) 0.3950(14) 1.089(5) 0.031(8) Uiso 1 1 d . U . . . C12A C -0.0804(18) 0.0698(14) 0.102(5) 0.044(8) Uiso 1 1 d . U . . . H12A H -0.1274 0.0695 0.1021 0.053 Uiso 1 1 calc R U . . . C12B C 0.2555(16) 0.4225(12) 1.062(5) 0.038(8) Uiso 1 1 d . U . . . H12B H 0.2985 0.4204 1.1713 0.046 Uiso 1 1 calc R U . . . C13A C -0.060(2) 0.0437(15) -0.055(6) 0.058(9) Uiso 1 1 d . U . . . H13A H -0.0939 0.0267 -0.1672 0.070 Uiso 1 1 calc R U . . . C13B C 0.2501(17) 0.4526(14) 0.878(5) 0.039(8) Uiso 1 1 d . U . . . H13B H 0.2903 0.4703 0.8674 0.046 Uiso 1 1 calc R U . . . C14A C 0.009(2) 0.0407(14) -0.059(6) 0.046(9) Uiso 1 1 d . U . . . H14A H 0.0205 0.0215 -0.1695 0.055 Uiso 1 1 calc R U . . . C14B C 0.191(2) 0.4583(14) 0.711(6) 0.046(9) Uiso 1 1 d . U . . . H14C H 0.1888 0.4784 0.5859 0.055 Uiso 1 1 calc R U . . . C15A C 0.067(2) 0.0692(14) 0.120(6) 0.031(8) Uiso 1 1 d . U . . . C15B C 0.1277(19) 0.4302(14) 0.741(6) 0.039(8) Uiso 1 1 d . U . . . C16A C 0.1351(19) 0.0690(14) 0.165(6) 0.031(8) Uiso 1 1 d . U . . . C16B C 0.061(2) 0.4319(14) 0.611(6) 0.031(8) Uiso 1 1 d . U . . . C17A C 0.177(2) 0.0486(15) 0.029(6) 0.040(9) Uiso 1 1 d . U . . . H17A H 0.1553 0.0351 -0.1111 0.048 Uiso 1 1 calc R U . . . C17B C 0.0347(18) 0.4529(14) 0.406(6) 0.028(9) Uiso 1 1 d . U . . . H17B H 0.0661 0.4679 0.3389 0.034 Uiso 1 1 calc R U . . . C18A C 0.2459(19) 0.0494(14) 0.106(6) 0.044(9) Uiso 1 1 d . U . . . H18A H 0.2726 0.0352 0.0205 0.052 Uiso 1 1 calc R U . . . C18B C -0.0369(19) 0.4534(14) 0.290(7) 0.043(9) Uiso 1 1 d . U . . . H18B H -0.0515 0.4688 0.1500 0.052 Uiso 1 1 calc R U . . . C19A C 0.2796(18) 0.0704(14) 0.308(6) 0.046(9) Uiso 1 1 d . U . . . H19A H 0.3286 0.0700 0.3607 0.055 Uiso 1 1 calc R U . . . C19B C -0.0868(18) 0.4314(13) 0.380(6) 0.034(9) Uiso 1 1 d . U . . . H19B H -0.1348 0.4318 0.3060 0.041 Uiso 1 1 calc R U . . . C20A C 0.2388(18) 0.0928(14) 0.434(6) 0.047(9) Uiso 1 1 d . U . . . H20A H 0.2626 0.1086 0.5681 0.056 Uiso 1 1 calc R U . . . C20B C -0.0603(17) 0.4090(13) 0.586(5) 0.037(8) Uiso 1 1 d . U . . . H20B H -0.0925 0.3939 0.6501 0.044 Uiso 1 1 calc R U . . . 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 Ni1A 0.050(6) 0.030(4) 0.031(4) 0.004(3) 0.014(5) 0.005(4) Ni1B 0.039(5) 0.029(4) 0.039(4) 0.000(3) 0.016(5) -0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1A N3A 1.82(3) . ? Ni1A N2A 1.82(3) . ? Ni1A N1A 1.90(3) . ? Ni1A N4A 1.90(3) . ? Ni1B N3B 1.80(3) . ? Ni1B N2B 1.87(3) . ? Ni1B N4B 1.94(3) . ? Ni1B N1B 1.95(3) . ? N1A C5A 1.32(4) . ? N1A C1A 1.36(3) . ? N1B C5B 1.35(4) . ? N1B C1B 1.35(3) . ? N2A C10A 1.32(4) . ? N2A C6A 1.40(4) . ? N2B C6B 1.34(4) . ? N2B C10B 1.40(4) . ? N3A C11A 1.37(4) . ? N3A C15A 1.41(4) . ? N3B C11B 1.34(4) . ? N3B C15B 1.43(4) . ? N4A C20A 1.33(3) . ? N4A C16A 1.44(4) . ? N4B C20B 1.37(3) . ? N4B C16B 1.46(4) . ? C1A C2A 1.41(4) . ? C1B C2B 1.31(4) . ? C2A C3A 1.38(4) . ? C2B C3B 1.45(4) . ? C3A C4A 1.37(4) . ? C3B C4B 1.41(4) . ? C4A C5A 1.37(4) . ? C4B C5B 1.35(5) . ? C5A C6A 1.56(5) . ? C5B C6B 1.58(5) . ? C6A C7A 1.31(4) . ? C6B C7B 1.33(4) . ? C7A C8A 1.40(4) . ? C7B C8B 1.34(4) . ? C8A C9A 1.44(4) . ? C8B C9B 1.36(4) . ? C9A C10A 1.40(4) . ? C9B C10B 1.37(4) . ? C10A C11A 1.44(5) . ? C10B C11B 1.46(4) . ? C11A C12A 1.38(4) . ? C11B C12B 1.37(4) . ? C12A C13A 1.35(4) . ? C12B C13B 1.36(4) . ? C13A C14A 1.37(4) . ? C13B C14B 1.34(4) . ? C14A C15A 1.53(5) . ? C14B C15B 1.49(4) . ? C15A C16A 1.29(4) . ? C15B C16B 1.33(5) . ? C16A C17A 1.45(5) . ? C16B C17B 1.35(4) . ? C17A C18A 1.31(4) . ? C17B C18B 1.39(4) . ? C18A C19A 1.36(4) . ? C18B C19B 1.39(4) . ? C19A C20A 1.41(4) . ? C19B C20B 1.37(4) . ? 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 N3A Ni1A N2A 82.1(14) . . ? N3A Ni1A N1A 161.7(13) . . ? N2A Ni1A N1A 83.6(13) . . ? N3A Ni1A N4A 83.0(13) . . ? N2A Ni1A N4A 162.6(15) . . ? N1A Ni1A N4A 112.7(12) . . ? N3B Ni1B N2B 81.0(14) . . ? N3B Ni1B N4B 84.7(13) . . ? N2B Ni1B N4B 162.1(13) . . ? N3B Ni1B N1B 161.5(14) . . ? N2B Ni1B N1B 83.2(12) . . ? N4B Ni1B N1B 112.5(11) . . ? C5A N1A C1A 114(3) . . ? C5A N1A Ni1A 117(2) . . ? C1A N1A Ni1A 128(2) . . ? C5B N1B C1B 118(3) . . ? C5B N1B Ni1B 114(2) . . ? C1B N1B Ni1B 128(2) . . ? C10A N2A C6A 123(3) . . ? C10A N2A Ni1A 118(3) . . ? C6A N2A Ni1A 119(2) . . ? C6B N2B C10B 118(3) . . ? C6B N2B Ni1B 121(2) . . ? C10B N2B Ni1B 119(2) . . ? C11A N3A C15A 124(3) . . ? C11A N3A Ni1A 118(2) . . ? C15A N3A Ni1A 115(2) . . ? C11B N3B C15B 120(3) . . ? C11B N3B Ni1B 121(3) . . ? C15B N3B Ni1B 117(2) . . ? C20A N4A C16A 115(3) . . ? C20A N4A Ni1A 132(2) . . ? C16A N4A Ni1A 113(2) . . ? C20B N4B C16B 119(3) . . ? C20B N4B Ni1B 131(2) . . ? C16B N4B Ni1B 110(2) . . ? N1A C1A C2A 120(3) . . ? C2B C1B N1B 121(3) . . ? C3A C2A C1A 123(3) . . ? C1B C2B C3B 122(3) . . ? C4A C3A C2A 117(3) . . ? C4B C3B C2B 115(3) . . ? C3A C4A C5A 116(4) . . ? C5B C4B C3B 118(3) . . ? N1A C5A C4A 130(3) . . ? N1A C5A C6A 111(3) . . ? C4A C5A C6A 119(3) . . ? N1B C5B C4B 125(3) . . ? N1B C5B C6B 114(3) . . ? C4B C5B C6B 121(3) . . ? C7A C6A N2A 121(4) . . ? C7A C6A C5A 131(4) . . ? N2A C6A C5A 108(3) . . ? C7B C6B N2B 124(3) . . ? C7B C6B C5B 128(3) . . ? N2B C6B C5B 108(3) . . ? C6A C7A C8A 121(4) . . ? C6B C7B C8B 117(3) . . ? C7A C8A C9A 117(3) . . ? C7B C8B C9B 124(3) . . ? C10A C9A C8A 120(3) . . ? C8B C9B C10B 119(3) . . ? N2A C10A C9A 118(3) . . ? N2A C10A C11A 112(3) . . ? C9A C10A C11A 129(3) . . ? C9B C10B N2B 118(3) . . ? C9B C10B C11B 135(3) . . ? N2B C10B C11B 106(3) . . ? N3A C11A C12A 122(3) . . ? N3A C11A C10A 109(3) . . ? C12A C11A C10A 129(3) . . ? N3B C11B C12B 120(3) . . ? N3B C11B C10B 112(3) . . ? C12B C11B C10B 128(3) . . ? C13A C12A C11A 118(3) . . ? C13B C12B C11B 121(3) . . ? C12A C13A C14A 124(4) . . ? C14B C13B C12B 124(3) . . ? C13A C14A C15A 120(3) . . ? C13B C14B C15B 115(3) . . ? C16A C15A N3A 116(3) . . ? C16A C15A C14A 132(4) . . ? N3A C15A C14A 112(3) . . ? C16B C15B N3B 113(3) . . ? C16B C15B C14B 128(4) . . ? N3B C15B C14B 119(3) . . ? C15A C16A N4A 112(3) . . ? C15A C16A C17A 128(4) . . ? N4A C16A C17A 120(3) . . ? C15B C16B C17B 130(4) . . ? C15B C16B N4B 115(3) . . ? C17B C16B N4B 115(3) . . ? C18A C17A C16A 119(4) . . ? C16B C17B C18B 124(4) . . ? C17A C18A C19A 122(4) . . ? C19B C18B C17B 121(4) . . ? C18A C19A C20A 119(3) . . ? C20B C19B C18B 115(3) . . ? N4A C20A C19A 125(3) . . ? N4B C20B C19B 125(3) . . ? 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 N3A Ni1A N2A C10A 3(3) . . . . ? N1A Ni1A N2A C10A 171(3) . . . . ? N4A Ni1A N2A C10A -29(6) . . . . ? N3A Ni1A N2A C6A -170(3) . . . . ? N1A Ni1A N2A C6A -1(2) . . . . ? N4A Ni1A N2A C6A 159(4) . . . . ? N3B Ni1B N2B C6B -169(3) . . . . ? N4B Ni1B N2B C6B 154(3) . . . . ? N1B Ni1B N2B C6B 2(2) . . . . ? N3B Ni1B N2B C10B -4(2) . . . . ? N4B Ni1B N2B C10B -41(5) . . . . ? N1B Ni1B N2B C10B 167(3) . . . . ? N2A Ni1A N3A C11A -7(3) . . . . ? N1A Ni1A N3A C11A -46(5) . . . . ? N4A Ni1A N3A C11A 164(3) . . . . ? N2A Ni1A N3A C15A -168(3) . . . . ? N1A Ni1A N3A C15A 153(3) . . . . ? N4A Ni1A N3A C15A 3(2) . . . . ? N2B Ni1B N3B C11B -3(3) . . . . ? N4B Ni1B N3B C11B 167(3) . . . . ? N1B Ni1B N3B C11B -34(6) . . . . ? N2B Ni1B N3B C15B -166(3) . . . . ? N4B Ni1B N3B C15B 3(2) . . . . ? N1B Ni1B N3B C15B 163(3) . . . . ? C5A N1A C1A C2A -1(4) . . . . ? Ni1A N1A C1A C2A -172(2) . . . . ? C5B N1B C1B C2B 2(5) . . . . ? Ni1B N1B C1B C2B -172(2) . . . . ? N1A C1A C2A C3A 0(5) . . . . ? N1B C1B C2B C3B 0(5) . . . . ? C1A C2A C3A C4A 1(5) . . . . ? C1B C2B C3B C4B -1(5) . . . . ? C2A C3A C4A C5A -1(4) . . . . ? C2B C3B C4B C5B 0(4) . . . . ? C1A N1A C5A C4A 0(5) . . . . ? Ni1A N1A C5A C4A 172(3) . . . . ? C1A N1A C5A C6A 178(3) . . . . ? Ni1A N1A C5A C6A -10(3) . . . . ? C3A C4A C5A N1A 1(5) . . . . ? C3A C4A C5A C6A -177(3) . . . . ? C1B N1B C5B C4B -3(5) . . . . ? Ni1B N1B C5B C4B 172(3) . . . . ? C1B N1B C5B C6B 178(3) . . . . ? Ni1B N1B C5B C6B -8(3) . . . . ? C3B C4B C5B N1B 2(5) . . . . ? C3B C4B C5B C6B -179(3) . . . . ? C10A N2A C6A C7A 1(5) . . . . ? Ni1A N2A C6A C7A 173(3) . . . . ? C10A N2A C6A C5A -176(3) . . . . ? Ni1A N2A C6A C5A -4(4) . . . . ? N1A C5A C6A C7A -167(4) . . . . ? C4A C5A C6A C7A 10(6) . . . . ? N1A C5A C6A N2A 9(4) . . . . ? C4A C5A C6A N2A -174(3) . . . . ? C10B N2B C6B C7B 5(5) . . . . ? Ni1B N2B C6B C7B 170(3) . . . . ? C10B N2B C6B C5B -171(3) . . . . ? Ni1B N2B C6B C5B -6(3) . . . . ? N1B C5B C6B C7B -168(3) . . . . ? C4B C5B C6B C7B 13(5) . . . . ? N1B C5B C6B N2B 8(4) . . . . ? C4B C5B C6B N2B -171(3) . . . . ? N2A C6A C7A C8A 0(5) . . . . ? C5A C6A C7A C8A 176(3) . . . . ? N2B C6B C7B C8B -1(5) . . . . ? C5B C6B C7B C8B 174(3) . . . . ? C6A C7A C8A C9A -3(5) . . . . ? C6B C7B C8B C9B -2(5) . . . . ? C7A C8A C9A C10A 6(5) . . . . ? C7B C8B C9B C10B 2(5) . . . . ? C6A N2A C10A C9A 2(5) . . . . ? Ni1A N2A C10A C9A -170(3) . . . . ? C6A N2A C10A C11A 174(3) . . . . ? Ni1A N2A C10A C11A 2(4) . . . . ? C8A C9A C10A N2A -5(5) . . . . ? C8A C9A C10A C11A -175(4) . . . . ? C8B C9B C10B N2B 3(5) . . . . ? C8B C9B C10B C11B -176(4) . . . . ? C6B N2B C10B C9B -6(4) . . . . ? Ni1B N2B C10B C9B -171(2) . . . . ? C6B N2B C10B C11B 173(3) . . . . ? Ni1B N2B C10B C11B 8(3) . . . . ? C15A N3A C11A C12A -10(5) . . . . ? Ni1A N3A C11A C12A -169(3) . . . . ? C15A N3A C11A C10A 168(3) . . . . ? Ni1A N3A C11A C10A 9(4) . . . . ? N2A C10A C11A N3A -7(4) . . . . ? C9A C10A C11A N3A 165(3) . . . . ? N2A C10A C11A C12A 171(4) . . . . ? C9A C10A C11A C12A -18(7) . . . . ? C15B N3B C11B C12B -7(5) . . . . ? Ni1B N3B C11B C12B -169(3) . . . . ? C15B N3B C11B C10B 170(3) . . . . ? Ni1B N3B C11B C10B 8(4) . . . . ? C9B C10B C11B N3B 170(4) . . . . ? N2B C10B C11B N3B -9(4) . . . . ? C9B C10B C11B C12B -14(7) . . . . ? N2B C10B C11B C12B 167(3) . . . . ? N3A C11A C12A C13A 3(5) . . . . ? C10A C11A C12A C13A -175(4) . . . . ? N3B C11B C12B C13B 2(5) . . . . ? C10B C11B C12B C13B -174(3) . . . . ? C11A C12A C13A C14A 3(6) . . . . ? C11B C12B C13B C14B 0(5) . . . . ? C12A C13A C14A C15A -1(5) . . . . ? C12B C13B C14B C15B 2(5) . . . . ? C11A N3A C15A C16A -168(3) . . . . ? Ni1A N3A C15A C16A -9(4) . . . . ? C11A N3A C15A C14A 10(4) . . . . ? Ni1A N3A C15A C14A 170(2) . . . . ? C13A C14A C15A C16A 173(4) . . . . ? C13A C14A C15A N3A -5(4) . . . . ? C11B N3B C15B C16B -172(3) . . . . ? Ni1B N3B C15B C16B -9(4) . . . . ? C11B N3B C15B C14B 8(5) . . . . ? Ni1B N3B C15B C14B 172(2) . . . . ? C13B C14B C15B C16B 175(4) . . . . ? C13B C14B C15B N3B -6(4) . . . . ? N3A C15A C16A N4A 10(4) . . . . ? C14A C15A C16A N4A -168(3) . . . . ? N3A C15A C16A C17A -169(3) . . . . ? C14A C15A C16A C17A 13(7) . . . . ? C20A N4A C16A C15A 178(3) . . . . ? Ni1A N4A C16A C15A -7(4) . . . . ? C20A N4A C16A C17A -3(4) . . . . ? Ni1A N4A C16A C17A 172(3) . . . . ? N3B C15B C16B C17B -169(4) . . . . ? C14B C15B C16B C17B 10(7) . . . . ? N3B C15B C16B N4B 11(4) . . . . ? C14B C15B C16B N4B -170(3) . . . . ? C20B N4B C16B C15B 177(3) . . . . ? Ni1B N4B C16B C15B -8(4) . . . . ? C20B N4B C16B C17B -3(4) . . . . ? Ni1B N4B C16B C17B 172(3) . . . . ? C15A C16A C17A C18A -177(4) . . . . ? N4A C16A C17A C18A 4(5) . . . . ? C15B C16B C17B C18B -178(4) . . . . ? N4B C16B C17B C18B 2(5) . . . . ? C16A C17A C18A C19A -2(5) . . . . ? C16B C17B C18B C19B 0(5) . . . . ? C17A C18A C19A C20A -1(5) . . . . ? C17B C18B C19B C20B -1(5) . . . . ? C16A N4A C20A C19A -1(5) . . . . ? Ni1A N4A C20A C19A -175(3) . . . . ? C18A C19A C20A N4A 3(5) . . . . ? C16B N4B C20B C19B 2(4) . . . . ? Ni1B N4B C20B C19B -172(3) . . . . ? C18B C19B C20B N4B 0(5) . . . . ? _refine_diff_density_max 0.414 _refine_diff_density_min -0.332 _refine_diff_density_rms 0.093 _shelxl_version_number 2014-3 _shelx_res_file ; TITL mo_JC_4Pyr_0m in Cc CELL 0.71073 19.79020 25.18250 6.29710 90.0000 106.7862 90.0000 ZERR 8.00 0.01090 0.01430 0.00350 0.0000 0.0158 0.0000 LATT -7 SYMM X, -Y, 0.5+Z SFAC C H N Ni UNIT 160 112 32 8 L.S. 20 BOND FMAP 2 PLAN 25 omit 2 4 2 size 0.05 0.05 0.02 acta 41.98 conf WGHT 0.068700 FVAR 0.06138 NI1A 4 0.103566 0.125237 0.507543 11.00000 0.05010 0.02982 = 0.03062 0.00351 0.01433 0.00524 NI1B 4 0.057800 0.370715 0.977569 11.00000 0.03939 0.02919 = 0.03885 -0.00026 0.01640 -0.00260 simu 0.01 n1a > c20b delu 0.01 n1a > c20b N1A 3 0.148569 0.168771 0.754663 11.00000 0.02611 N1B 3 -0.005986 0.326948 1.089670 11.00000 0.03015 N2A 3 0.024678 0.139164 0.591874 11.00000 0.03527 N2B 3 0.121977 0.354524 1.250853 11.00000 0.02912 N3A 3 0.038709 0.099472 0.261763 11.00000 0.03081 N3B 3 0.136706 0.396296 0.928291 11.00000 0.03414 N4A 3 0.168694 0.093215 0.375828 11.00000 0.03655 N4B 3 0.009402 0.407118 0.703900 11.00000 0.02993 C1A 1 0.218093 0.181243 0.833386 11.00000 0.02927 AFIX 43 H1A 2 0.249102 0.171824 0.753421 11.00000 -1.20000 AFIX 0 C1B 1 -0.075045 0.316419 0.990526 11.00000 0.03642 AFIX 43 H1B 2 -0.095319 0.326971 0.844416 11.00000 -1.20000 AFIX 0 C2A 1 0.243175 0.208477 1.036424 11.00000 0.03100 AFIX 43 H2A 2 0.290962 0.216695 1.087424 11.00000 -1.20000 AFIX 0 C2B 1 -0.113916 0.291647 1.096327 11.00000 0.04243 AFIX 43 H2B 2 -0.161174 0.285285 1.022680 11.00000 -1.20000 AFIX 0 C3A 1 0.199820 0.223516 1.163161 11.00000 0.03289 AFIX 43 H3A 2 0.217261 0.241798 1.296090 11.00000 -1.20000 AFIX 0 C3B 1 -0.085848 0.273762 1.324554 11.00000 0.03974 AFIX 43 H3B 2 -0.113481 0.256518 1.400186 11.00000 -1.20000 AFIX 0 C4A 1 0.130120 0.210219 1.083649 11.00000 0.03131 AFIX 43 H4A 2 0.097827 0.218529 1.160480 11.00000 -1.20000 AFIX 0 C4B 1 -0.013383 0.284554 1.422878 11.00000 0.03065 AFIX 43 H4B 2 0.009058 0.274543 1.568345 11.00000 -1.20000 AFIX 0 C5A 1 0.110295 0.183891 0.883923 11.00000 0.02024 C5B 1 0.022283 0.309820 1.299383 11.00000 0.02617 C6A 1 0.030763 0.170580 0.779011 11.00000 0.03862 C6B 1 0.103622 0.322592 1.396151 11.00000 0.02092 C7A 1 -0.025180 0.186016 0.832514 11.00000 0.04006 AFIX 43 H7A 2 -0.019920 0.206835 0.958240 11.00000 -1.20000 AFIX 0 C7B 1 0.148610 0.303508 1.579505 11.00000 0.03294 AFIX 43 H7B 2 0.133673 0.282083 1.677529 11.00000 -1.20000 AFIX 0 C8A 1 -0.092839 0.171709 0.703616 11.00000 0.04676 AFIX 43 H8A 2 -0.132738 0.181197 0.744600 11.00000 -1.20000 AFIX 0 C8B 1 0.216515 0.316659 1.616101 11.00000 0.02829 AFIX 43 H8B 2 0.248776 0.304839 1.746153 11.00000 -1.20000 AFIX 0 C9A 1 -0.098249 0.141668 0.504705 11.00000 0.04292 AFIX 43 H9A 2 -0.142320 0.133947 0.407480 11.00000 -1.20000 AFIX 0 C9B 1 0.240986 0.346381 1.473521 11.00000 0.03534 AFIX 43 H9B 2 0.288875 0.353819 1.504179 11.00000 -1.20000 AFIX 0 C10A 1 -0.036936 0.124173 0.458483 11.00000 0.04629 C10B 1 0.193660 0.365179 1.283578 11.00000 0.03272 C11A 1 -0.030003 0.096904 0.264140 11.00000 0.03608 C11B 1 0.198491 0.395047 1.089030 11.00000 0.03097 C12A 1 -0.080404 0.069768 0.102368 11.00000 0.04443 AFIX 43 H12A 2 -0.127419 0.069525 0.102122 11.00000 -1.20000 AFIX 0 C12B 1 0.255457 0.422455 1.061934 11.00000 0.03794 AFIX 43 H12B 2 0.298541 0.420408 1.171324 11.00000 -1.20000 AFIX 0 C13A 1 -0.059623 0.043671 -0.054999 11.00000 0.05842 AFIX 43 H13A 2 -0.093887 0.026713 -0.167244 11.00000 -1.20000 AFIX 0 C13B 1 0.250111 0.452606 0.877878 11.00000 0.03868 AFIX 43 H13B 2 0.290276 0.470298 0.867419 11.00000 -1.20000 AFIX 0 C14A 1 0.009025 0.040750 -0.058740 11.00000 0.04562 AFIX 43 H14A 2 0.020529 0.021518 -0.169537 11.00000 -1.20000 AFIX 0 C14B 1 0.190655 0.458326 0.711320 11.00000 0.04575 AFIX 43 H14C 2 0.188785 0.478446 0.585906 11.00000 -1.20000 AFIX 0 C15A 1 0.067022 0.069225 0.119993 11.00000 0.03056 C15B 1 0.127661 0.430233 0.740681 11.00000 0.03910 C16A 1 0.135088 0.069033 0.164899 11.00000 0.03117 C16B 1 0.061191 0.431889 0.610921 11.00000 0.03112 C17A 1 0.177025 0.048627 0.029389 11.00000 0.03961 AFIX 43 H17A 2 0.155253 0.035062 -0.111109 11.00000 -1.20000 AFIX 0 C17B 1 0.034675 0.452885 0.406416 11.00000 0.02848 AFIX 43 H17B 2 0.066131 0.467923 0.338854 11.00000 -1.20000 AFIX 0 C18A 1 0.245922 0.049429 0.106344 11.00000 0.04369 AFIX 43 H18A 2 0.272622 0.035185 0.020516 11.00000 -1.20000 AFIX 0 C18B 1 -0.036912 0.453436 0.290171 11.00000 0.04297 AFIX 43 H18B 2 -0.051475 0.468816 0.150034 11.00000 -1.20000 AFIX 0 C19A 1 0.279568 0.070408 0.307517 11.00000 0.04619 AFIX 43 H19A 2 0.328564 0.069960 0.360682 11.00000 -1.20000 AFIX 0 C19B 1 -0.086773 0.431419 0.380104 11.00000 0.03439 AFIX 43 H19B 2 -0.134794 0.431831 0.305983 11.00000 -1.20000 AFIX 0 C20A 1 0.238762 0.092832 0.433811 11.00000 0.04692 AFIX 43 H20A 2 0.262616 0.108590 0.568106 11.00000 -1.20000 AFIX 0 C20B 1 -0.060349 0.409039 0.585629 11.00000 0.03682 AFIX 43 H20B 2 -0.092521 0.393892 0.650087 11.00000 -1.20000 AFIX 0 HKLF 4 REM mo_JC_4Pyr_0m in Cc REM R1 = 0.0639 for 1213 Fo > 4sig(Fo) and 0.1146 for all 1790 data REM 211 parameters refined using 56 restraints END WGHT 0.0718 0.0000 REM Highest difference peak 0.414, deepest hole -0.332, 1-sigma level 0.093 Q1 1 0.0226 0.1303 0.4480 11.00000 0.05 0.41 Q2 1 0.0601 0.3667 1.1689 11.00000 0.05 0.38 Q3 1 0.0589 0.3689 0.7595 11.00000 0.05 0.36 Q4 1 0.1379 0.3758 1.0475 11.00000 0.05 0.35 Q5 1 0.1047 0.1200 0.3137 11.00000 0.05 0.34 Q6 1 0.1363 0.2797 1.7829 11.00000 0.05 0.32 Q7 1 0.1012 0.1153 0.7445 11.00000 0.05 0.31 Q8 1 0.2272 0.1508 0.6592 11.00000 0.05 0.30 Q9 1 -0.0328 0.0738 -0.1619 11.00000 0.05 0.30 Q10 1 0.1155 0.3852 1.0102 11.00000 0.05 0.30 Q11 1 0.0369 0.0110 -0.1919 11.00000 0.05 0.30 Q12 1 0.0023 0.3012 1.5392 11.00000 0.05 0.29 Q13 1 0.0831 0.1725 0.8626 11.00000 0.05 0.29 Q14 1 0.0655 0.4635 0.4957 11.00000 0.05 0.29 Q15 1 0.0717 0.3236 1.3486 11.00000 0.05 0.28 Q16 1 0.0241 0.3758 0.9308 11.00000 0.05 0.28 Q17 1 0.1916 0.3118 1.7007 11.00000 0.05 0.28 Q18 1 0.2172 0.0389 0.0308 11.00000 0.05 0.27 Q19 1 0.1513 0.2051 0.9600 11.00000 0.05 0.27 Q20 1 0.2574 0.2447 1.6584 11.00000 0.05 0.26 Q21 1 0.0323 0.4496 0.3120 11.00000 0.05 0.26 Q22 1 0.1740 -0.0016 -0.1670 11.00000 0.05 0.26 Q23 1 0.1382 0.1183 0.5439 11.00000 0.05 0.26 Q24 1 0.0948 0.0345 -0.0012 11.00000 0.05 0.26 Q25 1 0.0339 0.1379 0.6726 11.00000 0.05 0.25 ; _shelx_res_checksum 82642 _shelx_hkl_file ; -2 0 0 839.36 53.11 -2 0 0 816.34 58.93 2 0 0 808.58 58.78 -2 0 0 789.68 56.51 2 0 0 776.68 56.36 2 0 0 853.38 52.96 4 0 0 43.47 4.30 -4 0 0 36.70 3.51 4 0 0 40.65 3.46 4 0 0 38.10 3.99 -4 0 0 39.60 3.95 -4 0 0 35.71 3.30 -6 0 0 100.20 9.39 -6 0 0 113.25 8.26 6 0 0 106.15 7.45 -6 0 0 104.97 7.71 6 0 0 96.65 9.37 6 0 0 102.67 8.16 -8 0 0 17.74 2.58 8 0 0 16.66 3.10 8 0 0 19.00 2.56 -8 0 0 14.43 2.75 -8 0 0 26.73 4.14 8 0 0 21.43 4.21 -10 0 0 17.03 4.78 10 0 0 20.72 3.82 -10 0 0 21.53 3.30 10 0 0 16.99 5.21 10 0 0 16.22 3.20 -10 0 0 21.54 3.08 12 0 0 5.91 3.06 -12 0 0 0.60 2.94 12 0 0 -2.06 3.56 12 0 0 0.85 5.33 -12 0 0 -1.99 2.68 -12 0 0 4.70 4.31 14 0 0 18.17 6.88 -14 0 0 21.71 4.06 14 0 0 31.25 4.31 14 0 0 12.74 5.05 -14 0 0 17.94 5.72 -14 0 0 23.78 3.87 -1 -1 0 0.20 0.20 -1 -1 0 -0.26 0.38 1 -1 0 -0.21 0.25 -1 -1 0 -0.15 0.39 1 -1 0 0.17 0.40 1 1 0 0.08 0.30 -1 1 0 -0.08 0.23 1 1 0 0.12 0.22 -1 1 0 0.14 0.17 1 1 0 -0.03 0.19 -3 -1 0 1.68 2.13 3 -1 0 0.94 0.95 3 -1 0 2.40 1.22 -3 -1 0 5.91 1.13 -3 -1 0 1.16 1.31 -3 1 0 1.06 0.94 -3 1 0 3.64 1.09 3 1 0 -2.84 1.33 3 1 0 0.06 2.22 -5 -1 0 31.77 3.91 -5 -1 0 28.80 3.40 5 -1 0 29.82 3.84 -5 -1 0 27.69 3.18 5 -1 0 38.16 3.82 5 -1 0 33.56 3.38 -5 1 0 33.60 3.73 5 1 0 31.79 3.56 -5 1 0 29.17 3.24 -5 1 0 34.81 3.40 5 1 0 27.22 3.37 5 1 0 30.98 4.37 7 -1 0 31.74 4.22 -7 -1 0 25.73 2.77 7 -1 0 25.12 2.57 -7 -1 0 23.03 3.91 7 -1 0 27.83 3.18 -7 -1 0 23.07 3.06 -7 1 0 36.95 3.79 -7 1 0 28.84 4.03 7 1 0 20.44 3.31 -7 1 0 24.27 2.71 7 1 0 24.08 4.54 7 1 0 24.43 2.72 -9 -1 0 12.13 2.57 9 -1 0 10.86 4.33 9 -1 0 11.56 2.55 -9 -1 0 12.68 3.90 9 -1 0 10.15 3.19 -9 -1 0 10.20 2.69 -9 1 0 11.23 2.47 -9 1 0 15.31 3.81 9 1 0 15.58 4.73 -9 1 0 11.14 2.69 9 1 0 11.40 2.60 9 1 0 11.92 3.27 -11 -1 0 13.26 4.93 -11 -1 0 9.50 3.20 11 -1 0 6.77 4.89 11 -1 0 9.68 3.76 11 -1 0 12.22 3.09 -11 -1 0 14.10 3.14 11 1 0 8.89 3.81 11 1 0 11.02 3.18 -11 1 0 14.76 2.91 -11 1 0 13.91 3.13 11 1 0 10.94 5.57 -11 1 0 11.62 4.50 -13 -1 0 16.50 5.37 13 -1 0 19.73 3.88 -13 -1 0 17.75 3.76 13 -1 0 17.83 6.34 -13 -1 0 15.93 3.57 13 -1 0 19.02 4.49 13 1 0 16.14 3.73 -13 1 0 14.31 4.96 -13 1 0 18.94 3.57 -13 1 0 25.33 3.46 13 1 0 8.57 6.40 13 1 0 16.30 4.52 -15 -1 0 29.87 4.71 15 -1 0 26.88 4.65 15 1 0 27.06 4.56 -15 1 0 35.78 4.53 0 -2 0 -0.07 0.05 0 2 0 -0.11 0.21 -2 -2 0 0.85 0.80 -2 -2 0 0.21 0.77 2 -2 0 0.93 0.91 -2 -2 0 0.55 1.61 2 -2 0 0.27 0.56 -2 2 0 0.50 0.64 2 2 0 0.89 0.82 2 2 0 -0.19 0.60 -2 2 0 0.87 0.93 2 2 0 0.63 0.69 4 -2 0 20.33 2.01 -4 -2 0 18.39 2.12 4 -2 0 16.18 2.86 4 -2 0 15.24 2.22 -4 -2 0 20.16 3.52 -4 -2 0 20.69 2.46 4 2 0 14.69 3.90 -4 2 0 17.28 1.89 -4 2 0 18.51 2.83 4 2 0 16.56 2.44 -4 2 0 14.24 2.03 4 2 0 16.32 2.24 6 -2 0 3.05 2.81 6 -2 0 5.68 1.94 6 -2 0 6.94 1.62 -6 -2 0 0.46 1.87 -6 -2 0 -3.05 1.73 -6 -2 0 -0.12 2.89 -6 2 0 6.48 2.57 6 2 0 1.55 2.23 -6 2 0 4.51 1.47 6 2 0 -2.67 1.86 6 2 0 -1.76 3.69 -8 -2 0 29.36 3.12 8 -2 0 23.02 3.39 8 -2 0 20.29 4.20 8 -2 0 19.37 2.71 -8 -2 0 21.95 3.31 -8 -2 0 31.66 4.64 -8 2 0 24.44 3.20 8 2 0 23.58 2.98 8 2 0 29.24 5.37 -8 2 0 26.30 4.09 8 2 0 27.08 3.79 -8 2 0 23.87 2.84 -10 -2 0 24.48 4.70 10 -2 0 13.48 4.90 10 -2 0 17.50 3.76 10 -2 0 16.01 2.93 -10 -2 0 20.73 3.45 -10 -2 0 22.36 3.30 -10 2 0 17.60 3.15 10 2 0 22.21 3.93 -10 2 0 18.78 4.31 10 2 0 18.61 5.54 10 2 0 19.22 3.13 -10 2 0 18.88 2.92 -12 -2 0 -1.90 3.14 -12 -2 0 0.52 4.57 12 -2 0 11.88 5.20 12 -2 0 11.18 3.98 -12 -2 0 1.91 3.03 12 -2 0 7.46 3.15 -12 2 0 11.67 4.40 12 2 0 7.39 6.14 12 2 0 1.41 3.92 -12 2 0 10.69 3.06 -12 2 0 9.51 2.79 12 2 0 3.00 3.15 -14 -2 0 -1.09 3.58 -14 -2 0 -3.27 5.28 14 -2 0 -5.60 3.52 14 -2 0 -1.58 4.33 14 -2 0 -6.36 5.81 -14 -2 0 -0.20 3.43 -14 2 0 0.65 3.25 14 2 0 -3.31 4.45 -14 2 0 -2.37 4.40 -14 2 0 -1.71 3.05 14 2 0 0.93 6.86 14 2 0 -5.33 3.43 -1 -3 0 0.99 0.71 1 -3 0 1.07 0.65 -1 -3 0 0.80 1.64 -1 3 0 0.47 0.62 1 3 0 0.19 1.47 1 3 0 0.87 0.72 3 -3 0 6.21 1.12 -3 -3 0 8.96 1.58 3 -3 0 5.56 1.72 -3 3 0 4.76 1.72 -3 3 0 7.02 1.32 3 3 0 2.42 1.36 -5 -3 0 41.20 4.29 -5 3 0 26.56 3.42 -7 -3 0 35.85 4.74 7 -3 0 27.95 3.19 -7 -3 0 28.18 3.11 7 -3 0 23.06 2.85 7 -3 0 21.12 4.03 -7 -3 0 25.95 3.19 7 3 0 25.86 3.52 7 3 0 29.37 5.13 -7 3 0 29.56 3.38 -7 3 0 24.86 2.74 -7 3 0 21.07 3.77 7 3 0 25.25 2.99 9 -3 0 16.76 4.25 -9 -3 0 27.49 3.45 9 -3 0 15.63 3.59 -9 -3 0 19.19 3.33 -9 -3 0 30.36 5.09 9 -3 0 15.09 2.97 -9 3 0 20.17 3.88 9 3 0 38.15 5.88 -9 3 0 14.87 2.95 9 3 0 25.42 3.20 9 3 0 17.01 4.08 -9 3 0 16.15 2.73 -11 -3 0 8.76 4.87 11 -3 0 15.33 3.73 -11 -3 0 8.13 2.99 11 -3 0 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0 31.97 4.36 -11 -7 0 35.97 4.41 11 -7 0 19.67 3.59 -11 7 0 18.07 3.01 -11 7 0 16.88 4.54 -11 7 0 30.28 3.85 11 7 0 24.22 5.03 11 7 0 34.52 7.12 -13 -7 0 21.24 4.36 13 -7 0 8.87 5.28 -13 -7 0 17.15 6.58 13 -7 0 19.60 3.94 -13 -7 0 20.11 4.46 -13 7 0 11.47 3.63 13 7 0 13.57 5.02 13 7 0 11.00 7.73 -13 7 0 13.17 3.06 -13 7 0 10.62 4.47 -15 7 0 14.08 4.09 -2 -8 0 79.64 8.84 -2 -8 0 57.13 5.16 2 -8 0 58.56 4.86 2 8 0 53.19 5.22 -2 8 0 54.51 4.39 -4 -8 0 92.99 10.09 -4 -8 0 86.00 7.33 4 -8 0 91.85 7.79 4 -8 0 96.90 6.88 4 8 0 83.24 7.54 -4 8 0 93.24 6.92 6 -8 0 6.43 2.03 6 -8 0 6.55 2.82 -6 -8 0 14.08 2.79 -6 -8 0 20.23 5.22 -6 -8 0 18.96 3.00 -6 8 0 11.24 2.85 -6 8 0 10.77 2.51 6 8 0 21.06 3.19 -8 -8 0 39.99 6.96 -8 -8 0 43.74 5.02 8 -8 0 29.07 4.49 8 -8 0 29.78 3.36 -8 -8 0 39.77 4.25 -8 8 0 33.11 4.86 8 8 0 34.81 4.42 8 8 0 20.86 5.45 -8 8 0 35.28 4.08 -10 -8 0 11.94 5.21 10 -8 0 8.83 2.74 -10 -8 0 8.35 3.14 10 -8 0 2.16 3.74 -10 -8 0 7.73 3.18 -10 8 0 7.90 2.80 10 8 0 8.38 3.89 -10 8 0 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