#============================================================================== data_global loop_ _journal_name_full 'European Journal of Chemistry' _journal_coden_ASTM EJCUA9 _journal_volume 11 _journal_issue 1 _journal_year 2020 _journal_page_first 1 _journal_page_last 5 #=============================================================================== data_shelx _audit_creation_method 'SHELXL-2016/4' _shelx_SHELXL_version_number '2016/4' _chemical_name_systematic ? _chemical_name_common '[{VO(sashz)}2(\m-O)(\m-H2O)]' _chemical_melting_point ? _chemical_formula_moiety 'C28 H22 N4 O10 V2, 2(C2 H3 N)' _chemical_formula_sum 'C32 H28 N6 O10 V2' _chemical_formula_weight 758.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' _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+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 12.9655(8) _cell_length_b 14.1902(9) _cell_length_c 18.4379(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3392.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 149 _cell_measurement_theta_min 3.0625 _cell_measurement_theta_max 16.367 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.485 _exptl_crystal_F_000 1552 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.175 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.101 _exptl_absorpt_coefficient_mu 0.616 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.557172 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details 'SADABS' _exptl_absorpt_special_details ? _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source ? _diffrn_measurement_device_type 'X8 APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18803 _diffrn_reflns_av_unetI/netI 0.1020 _diffrn_reflns_av_R_equivalents 0.0473 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.811 _diffrn_reflns_theta_max 28.352 _diffrn_reflns_theta_full 25.242 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measured_fraction_theta_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_point_group_measured_fraction_full 0.998 _reflns_number_total 8263 _reflns_number_gt 4652 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.806 _reflns_Friedel_fraction_max 0.993 _reflns_Friedel_fraction_full 1.000 _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 SOFTWARE' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2016/4 (Sheldrick, 2016)' _computing_molecular_graphics 'ORTEP-3 (Farrugia, 2000)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refined as a 2-component perfect inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0830P)^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 ; Refined as a perfect inversion twin. ; _refine_ls_abs_structure_Flack 0.5 _chemical_absolute_configuration ? _refine_ls_number_reflns 8263 _refine_ls_number_parameters 453 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1147 _refine_ls_R_factor_gt 0.0509 _refine_ls_wR_factor_ref 0.1531 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _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 V1 V 0.84905(7) 0.48474(8) 0.11870(5) 0.0414(3) Uani 1 1 d . . . . . V2 V 0.80703(7) 0.50942(7) -0.05094(5) 0.0372(3) Uani 1 1 d . . . . . O10 O 0.9444(3) 0.5046(4) 0.1697(2) 0.0545(12) Uani 1 1 d . . . . . O20 O 0.8835(3) 0.5343(3) -0.1154(2) 0.0496(11) Uani 1 1 d . . . . . O30 O 0.8882(3) 0.5157(3) 0.02819(19) 0.0368(9) Uani 1 1 d . . . . . O40 O 0.6900(3) 0.4667(3) 0.0442(2) 0.0417(10) Uani 1 1 d . . . . . H40A H 0.663215 0.402957 0.041282 0.050 Uiso 1 1 calc R U . . . H40B H 0.636236 0.512389 0.054017 0.050 Uiso 1 1 calc R U . . . O1 O 0.8504(3) 0.3569(3) 0.1129(2) 0.0492(11) Uani 1 1 d . . . . . O2 O 0.7811(3) 0.6046(3) 0.1332(2) 0.0446(11) Uani 1 1 d . . . . . O3 O 0.5552(4) 0.6475(4) 0.2922(3) 0.0762(16) Uani 1 1 d . . . . . H3 H 0.581972 0.597678 0.279873 0.114 Uiso 1 1 calc R U . . . O4 O 0.7333(3) 0.6183(3) -0.0426(2) 0.0455(11) Uani 1 1 d . . . . . O5 O 0.8130(3) 0.3742(3) -0.0553(2) 0.0405(10) Uani 1 1 d . . . . . O6 O 0.6071(4) 0.2104(4) -0.1783(3) 0.0674(15) Uani 1 1 d . . . . . H6 H 0.610291 0.267968 -0.175435 0.101 Uiso 1 1 calc R U . . . N1 N 0.7368(4) 0.4599(4) 0.1981(3) 0.0394(12) Uani 1 1 d . . . . . N2 N 0.6832(4) 0.5374(4) 0.2222(3) 0.0480(13) Uani 1 1 d . . . . . N3 N 0.6835(4) 0.4682(3) -0.1178(2) 0.0379(11) Uani 1 1 d . . . . . N4 N 0.6757(4) 0.3730(4) -0.1322(3) 0.0417(12) Uani 1 1 d . . . . . C1 C 0.8240(5) 0.2812(5) 0.1520(3) 0.0496(17) Uani 1 1 d . . . . . C2 C 0.8656(6) 0.1935(5) 0.1352(4) 0.0545(18) Uani 1 1 d . . . . . H2 H 0.914989 0.187914 0.098917 0.065 Uiso 1 1 calc R U . . . C3 C 0.8329(7) 0.1139(6) 0.1732(5) 0.075(2) Uani 1 1 d . . . . . H3A H 0.862210 0.055575 0.163024 0.090 Uiso 1 1 calc R U . . . C4 C 0.7575(6) 0.1210(6) 0.2256(5) 0.070(2) Uani 1 1 d . . . . . H4 H 0.733361 0.066820 0.248391 0.084 Uiso 1 1 calc R U . . . C5 C 0.7175(6) 0.2078(6) 0.2447(4) 0.064(2) Uani 1 1 d . . . . . H5 H 0.668088 0.212435 0.281124 0.077 Uiso 1 1 calc R U . . . C6 C 0.7528(5) 0.2904(5) 0.2078(4) 0.0527(18) Uani 1 1 d . . . . . C7 C 0.7101(5) 0.3805(5) 0.2256(4) 0.0481(17) Uani 1 1 d . . . . . H7 H 0.658131 0.381551 0.260387 0.058 Uiso 1 1 calc R U . . . C11 C 0.6706(5) 0.7030(5) 0.1993(4) 0.0531(17) Uani 1 1 d . . . . . C12 C 0.5928(5) 0.7170(6) 0.2523(4) 0.0554(19) Uani 1 1 d . . . . . C13 C 0.5562(6) 0.8054(6) 0.2645(5) 0.067(2) Uani 1 1 d . . . . . H13 H 0.506525 0.814452 0.300161 0.081 Uiso 1 1 calc R U . . . C14 C 0.5904(7) 0.8811(6) 0.2257(5) 0.078(3) Uani 1 1 d . . . . . H14 H 0.563045 0.940632 0.234316 0.094 Uiso 1 1 calc R U . . . C15 C 0.6656(7) 0.8691(6) 0.1739(5) 0.075(2) Uani 1 1 d . . . . . H15 H 0.689537 0.920373 0.147366 0.090 Uiso 1 1 calc R U . . . C16 C 0.7053(6) 0.7805(5) 0.1615(4) 0.062(2) Uani 1 1 d . . . . . H16 H 0.756670 0.772754 0.126821 0.074 Uiso 1 1 calc R U . . . C17 C 0.7139(5) 0.6107(5) 0.1845(3) 0.0463(16) Uani 1 1 d . . . . . C21 C 0.6658(5) 0.6676(5) -0.0842(3) 0.0441(15) Uani 1 1 d . . . . . C22 C 0.6520(5) 0.7611(5) -0.0699(4) 0.0567(18) Uani 1 1 d . . . . . H22 H 0.690977 0.790894 -0.034302 0.068 Uiso 1 1 calc R U . . . C23 C 0.5787(6) 0.8115(5) -0.1096(4) 0.066(2) Uani 1 1 d . . . . . H23 H 0.567860 0.874993 -0.099650 0.080 Uiso 1 1 calc R U . . . C24 C 0.5221(6) 0.7679(6) -0.1634(4) 0.066(2) Uani 1 1 d . . . . . H24 H 0.474829 0.802446 -0.190438 0.079 Uiso 1 1 calc R U . . . C25 C 0.5354(6) 0.6747(6) -0.1767(4) 0.059(2) Uani 1 1 d . . . . . H25 H 0.495895 0.645482 -0.212312 0.070 Uiso 1 1 calc R U . . . C26 C 0.6086(5) 0.6210(5) -0.1372(3) 0.0431(15) Uani 1 1 d . . . . . C27 C 0.6158(5) 0.5222(5) -0.1496(3) 0.0442(15) Uani 1 1 d . . . . . H27 H 0.569841 0.494672 -0.182009 0.053 Uiso 1 1 calc R U . . . C31 C 0.7557(4) 0.2264(4) -0.1006(3) 0.0386(14) Uani 1 1 d . . . . . C32 C 0.6847(5) 0.1717(5) -0.1396(4) 0.0479(16) Uani 1 1 d . . . . . C33 C 0.6947(6) 0.0742(5) -0.1403(4) 0.0609(19) Uani 1 1 d . . . . . H33 H 0.648049 0.037797 -0.166480 0.073 Uiso 1 1 calc R U . . . C34 C 0.7735(6) 0.0310(5) -0.1025(4) 0.067(2) Uani 1 1 d . . . . . H34 H 0.779692 -0.034275 -0.103663 0.081 Uiso 1 1 calc R U . . . C35 C 0.8432(6) 0.0836(5) -0.0630(4) 0.0629(19) Uani 1 1 d . . . . . H35 H 0.895872 0.054285 -0.037163 0.075 Uiso 1 1 calc R U . . . C36 C 0.8332(5) 0.1804(4) -0.0624(4) 0.0486(16) Uani 1 1 d . . . . . H36 H 0.879912 0.216001 -0.035665 0.058 Uiso 1 1 calc R U . . . C37 C 0.7482(4) 0.3285(5) -0.0963(3) 0.0406(15) Uani 1 1 d . . . . . N5 N 0.6027(5) 0.2861(6) 0.0488(4) 0.082(2) Uani 1 1 d . . . . . C51 C 0.5953(5) 0.2072(6) 0.0494(4) 0.061(2) Uani 1 1 d . . . . . C52 C 0.5838(7) 0.1072(6) 0.0520(5) 0.081(3) Uani 1 1 d . . . . . H52A H 0.556447 0.089126 0.098376 0.122 Uiso 1 1 calc R U . . . H52B H 0.649763 0.077846 0.045011 0.122 Uiso 1 1 calc R U . . . H52C H 0.537424 0.087299 0.014422 0.122 Uiso 1 1 calc R U . . . N6 N 0.5256(5) 0.5948(5) 0.0596(5) 0.087(2) Uani 1 1 d . . . . . C61 C 0.4909(5) 0.6671(6) 0.0597(5) 0.067(2) Uani 1 1 d . . . . . C62 C 0.4482(8) 0.7603(6) 0.0607(6) 0.096(3) Uani 1 1 d . . . . . H62A H 0.396661 0.764365 0.097912 0.145 Uiso 1 1 calc R U . . . H62B H 0.417416 0.773747 0.014461 0.145 Uiso 1 1 calc R U . . . H62C H 0.501951 0.805094 0.070259 0.145 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 V1 0.0414(5) 0.0443(7) 0.0386(5) 0.0005(5) 0.0024(4) -0.0036(5) V2 0.0394(5) 0.0337(6) 0.0387(5) -0.0003(5) -0.0031(4) -0.0008(5) O10 0.049(2) 0.068(4) 0.046(2) 0.000(3) -0.0052(18) -0.010(3) O20 0.058(2) 0.053(3) 0.038(2) -0.001(2) 0.003(2) -0.008(2) O30 0.0377(19) 0.034(2) 0.0385(19) 0.001(2) -0.0011(15) -0.0042(18) O40 0.039(2) 0.037(2) 0.049(2) -0.0067(19) 0.0014(19) -0.0018(19) O1 0.056(3) 0.041(3) 0.050(3) 0.003(2) 0.008(2) -0.003(2) O2 0.053(3) 0.036(3) 0.045(2) -0.004(2) 0.006(2) -0.0043(19) O3 0.079(4) 0.074(4) 0.076(4) -0.004(3) 0.017(3) 0.022(3) O4 0.051(2) 0.036(3) 0.050(3) 0.000(2) -0.010(2) 0.003(2) O5 0.040(2) 0.034(2) 0.048(2) -0.005(2) -0.010(2) -0.0010(18) O6 0.064(3) 0.050(3) 0.088(4) -0.015(3) -0.033(3) 0.000(3) N1 0.045(3) 0.032(3) 0.040(3) -0.001(2) -0.003(2) 0.002(2) N2 0.061(3) 0.040(3) 0.043(3) 0.002(3) 0.006(3) 0.001(3) N3 0.042(3) 0.034(3) 0.038(2) 0.000(2) -0.003(2) 0.000(2) N4 0.049(3) 0.033(3) 0.043(3) -0.003(2) -0.009(2) 0.001(2) C1 0.054(4) 0.046(4) 0.049(4) -0.004(3) -0.007(3) -0.006(3) C2 0.068(5) 0.039(4) 0.056(4) 0.005(3) -0.005(4) 0.002(3) C3 0.098(6) 0.034(5) 0.092(6) 0.003(4) -0.021(5) 0.007(4) C4 0.084(5) 0.057(6) 0.069(5) 0.015(5) 0.003(4) -0.008(4) C5 0.084(5) 0.042(5) 0.066(5) 0.020(4) -0.009(4) -0.017(4) C6 0.065(4) 0.047(5) 0.046(4) 0.002(4) -0.011(3) -0.007(4) C7 0.045(4) 0.052(5) 0.047(4) 0.002(3) 0.001(3) -0.002(3) C11 0.057(4) 0.050(5) 0.053(4) -0.008(3) -0.006(3) 0.005(3) C12 0.057(4) 0.057(5) 0.052(4) -0.001(4) -0.004(3) 0.008(4) C13 0.066(5) 0.064(6) 0.072(5) -0.009(5) -0.007(4) 0.017(4) C14 0.085(6) 0.056(6) 0.094(6) -0.020(5) -0.016(5) 0.023(5) C15 0.096(6) 0.042(5) 0.087(6) -0.001(4) 0.001(5) 0.002(5) C16 0.072(5) 0.043(5) 0.071(5) -0.004(4) 0.000(4) 0.004(4) C17 0.046(4) 0.052(5) 0.042(3) -0.006(3) -0.002(3) 0.000(3) C21 0.046(4) 0.038(4) 0.048(4) 0.007(3) 0.000(3) 0.003(3) C22 0.063(4) 0.038(4) 0.068(5) 0.005(3) -0.004(4) 0.001(3) C23 0.076(5) 0.044(5) 0.078(6) 0.007(4) -0.009(4) 0.016(4) C24 0.068(5) 0.053(6) 0.077(5) 0.016(4) -0.012(4) 0.012(4) C25 0.061(4) 0.061(6) 0.054(4) 0.007(4) -0.013(4) 0.012(4) C26 0.047(3) 0.041(4) 0.041(3) 0.001(3) -0.005(3) 0.006(3) C27 0.044(3) 0.046(4) 0.043(3) 0.002(3) -0.004(3) 0.004(3) C31 0.039(3) 0.034(4) 0.044(3) -0.008(3) -0.002(3) 0.001(3) C32 0.047(4) 0.041(4) 0.055(4) -0.008(3) -0.003(3) -0.003(3) C33 0.068(4) 0.042(4) 0.073(5) -0.010(4) -0.005(4) -0.009(4) C34 0.076(5) 0.038(4) 0.088(5) -0.010(4) 0.002(4) 0.003(4) C35 0.065(4) 0.045(5) 0.078(5) -0.004(4) -0.002(4) 0.007(4) C36 0.052(4) 0.034(4) 0.060(4) -0.005(3) -0.006(3) 0.002(3) C37 0.039(3) 0.041(4) 0.042(3) -0.004(3) 0.003(3) 0.001(3) N5 0.069(4) 0.070(5) 0.108(6) -0.008(5) 0.020(4) -0.013(4) C51 0.053(4) 0.063(6) 0.066(5) -0.014(5) 0.013(4) -0.014(4) C52 0.084(6) 0.060(6) 0.099(7) -0.011(5) 0.012(5) -0.020(4) N6 0.066(4) 0.061(5) 0.135(7) -0.011(5) 0.015(5) 0.005(4) C61 0.047(4) 0.057(5) 0.098(6) -0.007(5) 0.012(4) 0.004(4) C62 0.085(6) 0.071(7) 0.132(9) -0.006(6) 0.022(6) 0.026(5) _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 V1 O10 1.578(4) . ? V1 O30 1.799(4) . ? V1 O1 1.818(4) . ? V1 O2 1.934(4) . ? V1 N1 2.095(5) . ? V1 O40 2.491(4) . ? V2 O20 1.588(4) . ? V2 O30 1.801(4) . ? V2 O4 1.824(4) . ? V2 O5 1.922(4) . ? V2 N3 2.104(5) . ? V2 O40 2.397(4) . ? O40 H40A 0.9700 . ? O40 H40B 0.9700 . ? O1 C1 1.338(8) . ? O2 C17 1.290(7) . ? O3 C12 1.322(9) . ? O3 H3 0.8200 . ? O4 C21 1.357(7) . ? O5 C37 1.304(7) . ? O6 C32 1.350(8) . ? O6 H6 0.8200 . ? N1 C7 1.284(8) . ? N1 N2 1.374(7) . ? N2 C17 1.312(8) . ? N3 C27 1.304(8) . ? N3 N4 1.380(6) . ? N4 C37 1.312(8) . ? C1 C6 1.389(9) . ? C1 C2 1.392(9) . ? C2 C3 1.394(10) . ? C2 H2 0.9300 . ? C3 C4 1.379(11) . ? C3 H3A 0.9300 . ? C4 C5 1.382(11) . ? C4 H4 0.9300 . ? C5 C6 1.431(10) . ? C5 H5 0.9300 . ? C6 C7 1.431(10) . ? C7 H7 0.9300 . ? C11 C16 1.377(10) . ? C11 C12 1.419(9) . ? C11 C17 1.451(9) . ? C12 C13 1.359(10) . ? C13 C14 1.365(11) . ? C13 H13 0.9300 . ? C14 C15 1.376(12) . ? C14 H14 0.9300 . ? C15 C16 1.377(10) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C21 C22 1.365(9) . ? C21 C26 1.394(9) . ? C22 C23 1.397(9) . ? C22 H22 0.9300 . ? C23 C24 1.380(11) . ? C23 H23 0.9300 . ? C24 C25 1.357(10) . ? C24 H24 0.9300 . ? C25 C26 1.418(9) . ? C25 H25 0.9300 . ? C26 C27 1.424(9) . ? C27 H27 0.9300 . ? C31 C36 1.391(8) . ? C31 C32 1.403(8) . ? C31 C37 1.454(9) . ? C32 C33 1.389(9) . ? C33 C34 1.381(10) . ? C33 H33 0.9300 . ? C34 C35 1.380(10) . ? C34 H34 0.9300 . ? C35 C36 1.380(9) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? N5 C51 1.123(10) . ? C51 C52 1.428(11) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? N6 C61 1.120(9) . ? C61 C62 1.434(11) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O10 V1 O30 106.74(19) . . ? O10 V1 O1 101.9(2) . . ? O30 V1 O1 100.71(19) . . ? O10 V1 O2 96.8(2) . . ? O30 V1 O2 92.42(19) . . ? O1 V1 O2 152.91(18) . . ? O10 V1 N1 99.1(2) . . ? O30 V1 N1 152.35(18) . . ? O1 V1 N1 83.12(19) . . ? O2 V1 N1 74.61(19) . . ? O10 V1 O40 174.4(2) . . ? O30 V1 O40 75.33(14) . . ? O1 V1 O40 82.66(16) . . ? O2 V1 O40 77.87(16) . . ? N1 V1 O40 78.07(16) . . ? O20 V2 O30 103.35(19) . . ? O20 V2 O4 101.7(2) . . ? O30 V2 O4 101.31(19) . . ? O20 V2 O5 99.5(2) . . ? O30 V2 O5 93.41(17) . . ? O4 V2 O5 150.52(18) . . ? O20 V2 N3 95.6(2) . . ? O30 V2 N3 158.91(18) . . ? O4 V2 N3 83.46(19) . . ? O5 V2 N3 74.25(17) . . ? O20 V2 O40 177.93(19) . . ? O30 V2 O40 77.85(15) . . ? O4 V2 O40 79.66(17) . . ? O5 V2 O40 78.67(16) . . ? N3 V2 O40 82.91(16) . . ? V1 O30 V2 125.1(2) . . ? V2 O40 V1 81.59(12) . . ? V2 O40 H40A 115.0 . . ? V1 O40 H40A 115.0 . . ? V2 O40 H40B 115.0 . . ? V1 O40 H40B 115.0 . . ? H40A O40 H40B 112.1 . . ? C1 O1 V1 140.1(4) . . ? C17 O2 V1 117.9(4) . . ? C12 O3 H3 109.5 . . ? C21 O4 V2 136.6(4) . . ? C37 O5 V2 119.7(4) . . ? C32 O6 H6 109.5 . . ? C7 N1 N2 116.1(5) . . ? C7 N1 V1 127.7(5) . . ? N2 N1 V1 116.3(4) . . ? C17 N2 N1 108.1(5) . . ? C27 N3 N4 116.0(5) . . ? C27 N3 V2 127.7(4) . . ? N4 N3 V2 116.2(3) . . ? C37 N4 N3 108.8(5) . . ? O1 C1 C6 119.6(6) . . ? O1 C1 C2 120.0(6) . . ? C6 C1 C2 120.4(7) . . ? C1 C2 C3 119.7(7) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 120.6(8) . . ? C4 C3 H3A 119.7 . . ? C2 C3 H3A 119.7 . . ? C3 C4 C5 120.6(8) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 119.3(8) . . ? C4 C5 H5 120.4 . . ? C6 C5 H5 120.4 . . ? C1 C6 C5 119.2(7) . . ? C1 C6 C7 120.8(7) . . ? C5 C6 C7 119.9(7) . . ? N1 C7 C6 126.1(6) . . ? N1 C7 H7 116.9 . . ? C6 C7 H7 116.9 . . ? C16 C11 C12 118.0(7) . . ? C16 C11 C17 119.9(6) . . ? C12 C11 C17 122.0(7) . . ? O3 C12 C13 117.9(7) . . ? O3 C12 C11 122.7(7) . . ? C13 C12 C11 119.4(7) . . ? C12 C13 C14 121.8(8) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C15 119.7(8) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C14 C15 C16 119.5(8) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C11 C16 C15 121.5(8) . . ? C11 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? O2 C17 N2 122.7(6) . . ? O2 C17 C11 117.4(6) . . ? N2 C17 C11 119.9(6) . . ? O4 C21 C22 118.4(6) . . ? O4 C21 C26 119.7(6) . . ? C22 C21 C26 121.8(6) . . ? C21 C22 C23 119.1(7) . . ? C21 C22 H22 120.5 . . ? C23 C22 H22 120.5 . . ? C24 C23 C22 120.6(7) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 120.0(7) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 121.1(7) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C21 C26 C25 117.5(6) . . ? C21 C26 C27 123.0(6) . . ? C25 C26 C27 119.4(6) . . ? N3 C27 C26 123.4(6) . . ? N3 C27 H27 118.3 . . ? C26 C27 H27 118.3 . . ? C36 C31 C32 118.3(6) . . ? C36 C31 C37 119.2(5) . . ? C32 C31 C37 122.4(6) . . ? O6 C32 C33 118.0(6) . . ? O6 C32 C31 122.3(6) . . ? C33 C32 C31 119.7(6) . . ? C34 C33 C32 120.4(7) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 120.8(7) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C36 118.7(7) . . ? C34 C35 H35 120.6 . . ? C36 C35 H35 120.6 . . ? C35 C36 C31 122.1(6) . . ? C35 C36 H36 118.9 . . ? C31 C36 H36 118.9 . . ? O5 C37 N4 121.0(6) . . ? O5 C37 C31 119.0(5) . . ? N4 C37 C31 120.0(6) . . ? N5 C51 C52 178.3(9) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N6 C61 C62 178.9(10) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? 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 O40 H40A N5 0.97 1.84 2.803(8) 171.4 . O40 H40B N6 0.97 1.85 2.817(8) 171.5 . O3 H3 N2 0.82 1.89 2.619(7) 147.0 . O6 H6 N4 0.82 1.89 2.616(7) 146.7 . _refine_diff_density_max 0.544 _refine_diff_density_min -0.523 _refine_diff_density_rms 0.082 _shelx_res_file ; TITL final1 in P2(1)2(1)2(1) shelx.res created by SHELXL-2016/4 at 19:56:50 on 11-Dec-2019 CELL 0.71073 12.9655 14.1902 18.4379 90.000 90.000 90.000 ZERR 4.00 0.0008 0.0009 0.0010 0.000 0.000 0.000 LATT -1 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SFAC C H N O V UNIT 128 112 24 40 8 MERG 2 ACTA TWIN BIND V1 O40 FMAP 2 PLAN 10 L.S. 10 HTAB O40 N5 HTAB O40 N6 HTAB O3 N2 HTAB O6 N4 BOND $H WGHT 0.083000 FVAR 0.28404 V1 5 0.849049 0.484739 0.118700 11.00000 0.04136 0.04432 = 0.03863 0.00054 0.00244 -0.00364 V2 5 0.807029 0.509420 -0.050943 11.00000 0.03939 0.03365 = 0.03868 -0.00034 -0.00307 -0.00077 O10 4 0.944385 0.504568 0.169674 11.00000 0.04913 0.06828 = 0.04606 -0.00017 -0.00523 -0.00956 O20 4 0.883474 0.534317 -0.115422 11.00000 0.05793 0.05303 = 0.03784 -0.00100 0.00264 -0.00776 O30 4 0.888190 0.515651 0.028190 11.00000 0.03771 0.03407 = 0.03855 0.00077 -0.00109 -0.00415 O40 4 0.690045 0.466658 0.044157 11.00000 0.03908 0.03702 = 0.04898 -0.00667 0.00139 -0.00185 AFIX 23 H40A 2 0.663215 0.402957 0.041282 11.00000 -1.20000 H40B 2 0.636236 0.512389 0.054017 11.00000 -1.20000 AFIX 0 O1 4 0.850353 0.356864 0.112864 11.00000 0.05647 0.04122 = 0.04999 0.00264 0.00809 -0.00269 O2 4 0.781114 0.604579 0.133187 11.00000 0.05328 0.03584 = 0.04460 -0.00421 0.00571 -0.00431 O3 4 0.555218 0.647535 0.292187 11.00000 0.07864 0.07402 = 0.07603 -0.00383 0.01735 0.02188 AFIX 83 H3 2 0.581972 0.597678 0.279873 11.00000 -1.50000 AFIX 0 O4 4 0.733261 0.618307 -0.042553 11.00000 0.05100 0.03563 = 0.04979 0.00011 -0.01033 0.00325 O5 4 0.813027 0.374234 -0.055321 11.00000 0.03956 0.03383 = 0.04800 -0.00538 -0.00995 -0.00100 O6 4 0.607056 0.210377 -0.178292 11.00000 0.06403 0.05025 = 0.08788 -0.01459 -0.03304 0.00003 AFIX 83 H6 2 0.610291 0.267968 -0.175435 11.00000 -1.50000 AFIX 0 N1 3 0.736767 0.459937 0.198132 11.00000 0.04550 0.03231 = 0.04026 -0.00080 -0.00270 0.00151 N2 3 0.683207 0.537429 0.222189 11.00000 0.06056 0.04019 = 0.04310 0.00206 0.00612 0.00108 N3 3 0.683499 0.468175 -0.117816 11.00000 0.04231 0.03358 = 0.03778 0.00029 -0.00260 -0.00001 N4 3 0.675671 0.373041 -0.132214 11.00000 0.04877 0.03319 = 0.04311 -0.00328 -0.00893 0.00069 C1 1 0.823983 0.281213 0.151963 11.00000 0.05424 0.04558 = 0.04886 -0.00386 -0.00744 -0.00627 C2 1 0.865593 0.193461 0.135241 11.00000 0.06844 0.03894 = 0.05624 0.00460 -0.00479 0.00207 AFIX 43 H2 2 0.914989 0.187914 0.098917 11.00000 -1.20000 AFIX 0 C3 1 0.832905 0.113921 0.173179 11.00000 0.09842 0.03377 = 0.09247 0.00344 -0.02143 0.00698 AFIX 43 H3A 2 0.862210 0.055575 0.163024 11.00000 -1.20000 AFIX 0 C4 1 0.757507 0.120985 0.225629 11.00000 0.08428 0.05702 = 0.06886 0.01521 0.00292 -0.00800 AFIX 43 H4 2 0.733361 0.066820 0.248391 11.00000 -1.20000 AFIX 0 C5 1 0.717457 0.207780 0.244708 11.00000 0.08445 0.04246 = 0.06605 0.01993 -0.00884 -0.01650 AFIX 43 H5 2 0.668088 0.212435 0.281124 11.00000 -1.20000 AFIX 0 C6 1 0.752813 0.290407 0.207795 11.00000 0.06465 0.04733 = 0.04624 0.00164 -0.01069 -0.00712 C7 1 0.710090 0.380487 0.225624 11.00000 0.04538 0.05203 = 0.04703 0.00151 0.00074 -0.00178 AFIX 43 H7 2 0.658131 0.381551 0.260387 11.00000 -1.20000 AFIX 0 C11 1 0.670582 0.703021 0.199288 11.00000 0.05657 0.04973 = 0.05286 -0.00770 -0.00556 0.00529 C12 1 0.592769 0.716990 0.252313 11.00000 0.05682 0.05704 = 0.05245 -0.00142 -0.00448 0.00843 C13 1 0.556215 0.805353 0.264466 11.00000 0.06615 0.06372 = 0.07214 -0.00852 -0.00676 0.01686 AFIX 43 H13 2 0.506525 0.814452 0.300161 11.00000 -1.20000 AFIX 0 C14 1 0.590442 0.881102 0.225715 11.00000 0.08503 0.05605 = 0.09405 -0.01992 -0.01593 0.02335 AFIX 43 H14 2 0.563045 0.940632 0.234316 11.00000 -1.20000 AFIX 0 C15 1 0.665649 0.869057 0.173864 11.00000 0.09618 0.04167 = 0.08651 -0.00093 0.00119 0.00216 AFIX 43 H15 2 0.689537 0.920373 0.147366 11.00000 -1.20000 AFIX 0 C16 1 0.705275 0.780454 0.161503 11.00000 0.07190 0.04315 = 0.07091 -0.00363 -0.00027 0.00410 AFIX 43 H16 2 0.756670 0.772754 0.126821 11.00000 -1.20000 AFIX 0 C17 1 0.713934 0.610706 0.184544 11.00000 0.04553 0.05174 = 0.04172 -0.00609 -0.00227 0.00007 C21 1 0.665809 0.667552 -0.084172 11.00000 0.04614 0.03811 = 0.04791 0.00742 0.00030 0.00254 C22 1 0.652037 0.761113 -0.069926 11.00000 0.06326 0.03832 = 0.06839 0.00500 -0.00384 0.00074 AFIX 43 H22 2 0.690977 0.790894 -0.034302 11.00000 -1.20000 AFIX 0 C23 1 0.578670 0.811501 -0.109579 11.00000 0.07626 0.04435 = 0.07840 0.00667 -0.00900 0.01646 AFIX 43 H23 2 0.567860 0.874993 -0.099650 11.00000 -1.20000 AFIX 0 C24 1 0.522088 0.767922 -0.163351 11.00000 0.06836 0.05326 = 0.07662 0.01569 -0.01206 0.01234 AFIX 43 H24 2 0.474829 0.802446 -0.190438 11.00000 -1.20000 AFIX 0 C25 1 0.535416 0.674651 -0.176706 11.00000 0.06072 0.06078 = 0.05446 0.00667 -0.01262 0.01235 AFIX 43 H25 2 0.495895 0.645482 -0.212312 11.00000 -1.20000 AFIX 0 C26 1 0.608620 0.620967 -0.137249 11.00000 0.04671 0.04148 = 0.04120 0.00064 -0.00537 0.00578 C27 1 0.615821 0.522160 -0.149587 11.00000 0.04396 0.04561 = 0.04309 0.00155 -0.00375 0.00378 AFIX 43 H27 2 0.569841 0.494672 -0.182009 11.00000 -1.20000 AFIX 0 C31 1 0.755669 0.226424 -0.100624 11.00000 0.03859 0.03352 = 0.04354 -0.00841 -0.00152 0.00109 C32 1 0.684659 0.171664 -0.139573 11.00000 0.04746 0.04148 = 0.05464 -0.00777 -0.00338 -0.00312 C33 1 0.694699 0.074181 -0.140328 11.00000 0.06831 0.04165 = 0.07277 -0.01018 -0.00509 -0.00921 AFIX 43 H33 2 0.648049 0.037797 -0.166480 11.00000 -1.20000 AFIX 0 C34 1 0.773508 0.031001 -0.102490 11.00000 0.07582 0.03813 = 0.08778 -0.01024 0.00195 0.00272 AFIX 43 H34 2 0.779692 -0.034275 -0.103663 11.00000 -1.20000 AFIX 0 C35 1 0.843205 0.083551 -0.062954 11.00000 0.06527 0.04543 = 0.07803 -0.00381 -0.00164 0.00731 AFIX 43 H35 2 0.895872 0.054285 -0.037163 11.00000 -1.20000 AFIX 0 C36 1 0.833247 0.180387 -0.062425 11.00000 0.05175 0.03398 = 0.06000 -0.00505 -0.00649 0.00228 AFIX 43 H36 2 0.879912 0.216001 -0.035665 11.00000 -1.20000 AFIX 0 C37 1 0.748182 0.328512 -0.096325 11.00000 0.03904 0.04051 = 0.04212 -0.00387 0.00264 0.00053 N5 3 0.602743 0.286080 0.048827 11.00000 0.06904 0.07025 = 0.10798 -0.00761 0.01955 -0.01348 C51 1 0.595292 0.207212 0.049447 11.00000 0.05320 0.06350 = 0.06580 -0.01351 0.01293 -0.01377 C52 1 0.583789 0.107172 0.052025 11.00000 0.08443 0.06023 = 0.09946 -0.01114 0.01194 -0.01968 AFIX 137 H52A 2 0.556447 0.089126 0.098376 11.00000 -1.50000 H52B 2 0.649763 0.077846 0.045011 11.00000 -1.50000 H52C 2 0.537424 0.087299 0.014422 11.00000 -1.50000 AFIX 0 N6 3 0.525574 0.594771 0.059554 11.00000 0.06601 0.06079 = 0.13533 -0.01061 0.01490 0.00521 C61 1 0.490874 0.667072 0.059705 11.00000 0.04727 0.05711 = 0.09765 -0.00702 0.01175 0.00360 C62 1 0.448201 0.760267 0.060664 11.00000 0.08548 0.07128 = 0.13230 -0.00603 0.02163 0.02619 AFIX 137 H62A 2 0.396661 0.764365 0.097912 11.00000 -1.50000 H62B 2 0.417416 0.773747 0.014461 11.00000 -1.50000 H62C 2 0.501951 0.805094 0.070259 11.00000 -1.50000 AFIX 0 HKLF 4 REM final1 in P2(1)2(1)2(1) REM R1 = 0.0509 for 4652 Fo > 4sig(Fo) and 0.1147 for all 8263 data REM 453 parameters refined using 0 restraints END WGHT 0.0831 0.0000 REM Highest difference peak 0.544, deepest hole -0.523, 1-sigma level 0.082 Q1 1 0.8154 0.5425 0.1158 11.00000 0.05 0.54 Q2 1 0.6404 0.6250 0.2282 11.00000 0.05 0.30 Q3 1 0.8074 0.4168 0.1156 11.00000 0.05 0.29 Q4 1 0.4568 0.6758 0.0739 11.00000 0.05 0.28 Q5 1 0.5583 0.6421 0.0509 11.00000 0.05 0.27 Q6 1 0.5037 0.6184 0.1470 11.00000 0.05 0.27 Q7 1 0.4860 0.6048 0.0320 11.00000 0.05 0.26 Q8 1 0.5033 0.7639 0.2098 11.00000 0.05 0.26 Q9 1 0.8911 0.4070 0.1223 11.00000 0.05 0.26 Q10 1 0.8067 0.6127 0.1497 11.00000 0.05 0.25 ; _shelx_res_checksum 15885 _shelx_hkl_file ; -1 0 0 -6.66 0.25 -1 0 0 -6.71 0.24 1 0 0 -6.76 0.24 1 0 0 -6.89 0.26 2 0 0 4484.27 250.38 -3 0 0 -0.61 0.90 -3 0 0 -0.30 0.83 3 0 0 -0.97 0.86 4 0 0 590.38 33.56 -4 0 0 602.46 33.60 5 0 0 4.21 1.32 -5 0 0 0.69 1.35 6 0 0 372.29 21.26 -6 0 0 372.75 21.32 -7 0 0 3.69 2.18 7 0 0 -0.11 1.86 -8 0 0 197.29 11.52 8 0 0 182.71 11.38 9 0 0 1.14 2.48 -9 0 0 1.44 2.54 -10 0 0 10.07 3.23 10 0 0 8.53 3.32 -11 0 0 0.21 3.74 11 0 0 0.18 3.69 12 0 0 19.57 4.59 -12 0 0 8.05 4.35 -13 0 0 -1.18 4.36 -14 0 0 46.91 6.33 -15 0 0 3.65 5.87 -16 0 0 4.06 6.78 -17 0 0 1.32 7.76 0 1 0 -0.06 0.23 0 -1 0 -0.02 0.22 2 -1 0 1522.52 85.85 2 1 0 1545.34 85.85 2 1 0 1511.89 85.84 -2 1 0 1549.85 85.86 -2 -1 0 1510.87 86.86 -2 -1 0 1533.41 85.86 2 -1 0 1576.37 85.86 -3 -1 0 21.87 1.82 -3 1 0 21.21 1.85 3 -1 0 24.83 1.83 -3 1 0 20.33 1.83 3 1 0 25.68 1.78 -3 -1 0 23.64 1.92 4 1 0 155.70 8.65 -4 -1 0 146.36 8.66 4 -1 0 142.36 8.63 -4 1 0 146.46 8.66 -5 -1 0 322.29 17.68 5 1 0 300.99 17.59 5 -1 0 319.03 17.64 -5 1 0 292.53 17.63 6 -1 0 15.32 2.23 6 1 0 25.82 2.37 -6 1 0 23.57 2.52 -6 -1 0 21.84 2.46 7 -1 0 373.25 21.60 -7 -1 0 391.95 21.69 7 1 0 358.85 21.55 -7 1 0 384.08 21.65 8 1 0 313.31 17.03 -8 1 0 307.90 17.18 8 -1 0 292.88 17.08 -8 -1 0 254.61 17.02 9 1 0 8.83 2.86 -9 -1 0 15.20 2.90 9 -1 0 9.59 2.79 -9 1 0 6.76 2.74 -10 -1 0 9.60 3.15 10 -1 0 1.17 3.24 10 1 0 6.27 2.97 -10 1 0 10.37 3.40 11 1 0 27.96 4.27 -11 1 0 24.57 4.05 -11 -1 0 21.95 4.25 11 -1 0 23.57 4.08 -12 1 0 26.39 4.48 12 1 0 13.83 4.60 -12 -1 0 24.38 4.44 12 -1 0 16.77 4.74 -13 1 0 2.78 4.81 -13 -1 0 -0.31 4.80 -14 -1 0 9.53 5.23 -14 1 0 7.59 5.58 -15 1 0 19.40 6.18 -15 -1 0 1.58 7.12 -15 -1 0 12.84 6.57 -16 1 0 -1.23 7.30 -16 -1 0 5.04 7.36 -17 -1 0 4.92 7.87 -17 1 0 3.72 8.43 -1 -2 0 276.44 15.61 1 -2 0 276.76 15.61 -2 -2 0 1373.99 79.12 2 2 0 1479.60 79.13 -2 2 0 1412.99 79.12 2 2 0 1436.90 80.05 2 -2 0 1428.56 79.12 2 2 0 1412.75 79.11 -2 -2 0 1394.88 80.05 -2 2 0 1371.73 79.11 2 -2 0 1415.73 79.13 3 2 0 188.88 11.63 3 -2 0 211.39 11.69 -3 -2 0 201.95 11.69 -3 -2 0 209.79 11.71 -3 2 0 208.15 11.71 -3 2 0 198.46 11.66 -3 -2 0 208.83 11.82 -4 2 0 183.85 10.90 -4 -2 0 183.67 10.91 4 2 0 192.50 10.90 -4 -2 0 178.46 11.03 4 -2 0 202.87 10.94 5 2 0 5.88 1.42 5 -2 0 1.37 1.44 -5 2 0 3.34 1.45 -5 -2 0 2.36 1.42 -5 -2 0 4.00 1.50 -6 2 0 508.65 29.17 -6 -2 0 553.87 29.24 -6 -2 0 496.01 29.53 6 -2 0 515.01 29.15 6 2 0 498.83 29.11 7 -2 0 27.84 2.87 7 2 0 22.35 2.68 -7 2 0 22.49 2.68 -7 -2 0 20.96 2.78 8 2 0 115.81 7.59 -8 2 0 123.05 7.71 -8 -2 0 111.79 7.62 8 -2 0 121.49 7.69 -9 -2 0 -2.63 2.79 -9 2 0 0.85 2.62 9 -2 0 -0.52 2.86 9 2 0 -0.16 2.75 -10 2 0 16.10 3.49 10 2 0 20.16 3.46 10 -2 0 22.67 3.89 -10 -2 0 23.19 3.86 -11 2 0 -1.50 3.43 -11 -2 0 0.10 3.73 -11 -2 0 -5.49 3.32 11 2 0 1.29 3.66 11 -2 0 3.22 3.93 12 -2 0 30.19 5.29 -12 -2 0 41.18 5.06 -12 -2 0 42.69 5.47 12 2 0 35.94 5.18 -12 2 0 37.12 4.96 -13 -2 0 -2.66 4.36 -13 -2 0 -0.34 5.05 -13 2 0 2.98 4.50 -14 -2 0 1.96 5.20 -14 -2 0 5.04 6.04 -14 2 0 -0.89 5.48 -15 -2 0 -1.37 7.04 -15 -2 0 -2.45 5.89 -15 2 0 -3.20 6.28 -16 -2 0 7.00 7.49 -16 2 0 2.70 7.39 -17 -2 0 4.88 8.68 -17 2 0 8.53 8.48 0 -3 0 -2.35 0.81 0 3 0 -1.57 0.90 -1 -3 0 2661.48 151.67 -1 3 0 2788.37 151.68 1 -3 0 2687.99 151.67 1 3 0 2721.68 151.66 2 -3 0 35.49 2.50 -2 -3 0 33.29 2.54 -2 3 0 39.11 2.60 -2 3 0 38.56 2.49 2 3 0 33.01 2.52 -3 3 0 595.16 33.52 3 -3 0 589.05 33.53 3 3 0 623.35 33.95 -3 -3 0 597.96 33.54 3 3 0 587.13 33.51 -3 -3 0 579.85 33.92 -4 -3 0 262.86 14.23 4 -3 0 241.32 14.01 -4 3 0 243.65 14.01 4 3 0 242.39 13.98 -4 -3 0 240.95 14.03 4 3 0 229.45 14.20 -5 3 0 643.92 36.48 -5 -3 0 676.69 36.94 5 3 0 630.20 36.43 -5 -3 0 648.76 36.49 5 -3 0 632.71 36.46 -6 3 0 127.45 8.15 -6 -3 0 135.70 8.22 6 3 0 144.79 8.13 6 -3 0 133.08 8.16 -6 -3 0 123.18 8.26 -7 3 0 99.19 6.62 7 3 0 111.66 6.72 7 -3 0 103.73 6.70 -7 -3 0 96.51 6.64 -7 -3 0 97.92 6.72 -8 -3 0 5.60 2.56 8 3 0 8.95 2.45 8 -3 0 10.23 2.62 -8 3 0 7.94 2.73 -8 -3 0 11.05 2.65 9 -3 0 67.33 5.24 9 3 0 65.64 5.08 -9 -3 0 77.85 5.43 -9 -3 0 57.17 5.33 -9 3 0 63.17 5.21 -10 -3 0 8.23 3.23 10 -3 0 10.77 3.65 -10 3 0 6.91 3.19 -10 -3 0 2.53 3.34 10 3 0 4.37 3.32 11 3 0 14.11 4.04 11 -3 0 13.22 4.21 -11 -3 0 13.85 3.89 -11 3 0 14.56 3.86 -11 -3 0 11.27 4.03 -12 -3 0 8.56 4.61 12 -3 0 0.93 4.26 -12 -3 0 1.96 4.03 -12 3 0 6.09 4.42 12 3 0 6.46 4.44 -13 -3 0 -1.57 5.17 -13 3 0 0.96 4.93 -13 -3 0 -2.27 4.97 -14 -3 0 3.48 6.18 -14 3 0 7.83 5.69 -14 -3 0 3.58 5.26 -15 -3 0 0.74 7.08 -15 -3 0 0.63 6.12 -15 3 0 1.65 5.95 -16 3 0 -1.91 7.34 -16 -3 0 -8.25 6.86 -17 3 0 13.36 8.72 -17 -3 0 12.30 8.23 0 -4 0 1064.51 59.77 1 -4 0 51.97 3.31 -1 -4 0 47.42 3.29 2 4 0 19.31 1.88 2 -4 0 22.52 1.90 -2 -4 0 19.54 1.88 3 4 0 321.97 18.88 3 -4 0 319.01 18.64 -3 4 0 346.72 18.67 -3 -4 0 320.97 18.66 4 4 0 570.02 31.12 -4 -4 0 521.35 31.12 -4 4 0 534.98 31.11 4 -4 0 571.61 31.15 -4 -4 0 533.76 31.49 4 4 0 571.67 31.54 -5 4 0 93.91 5.98 5 -4 0 94.09 6.02 -5 -4 0 96.36 6.05 5 4 0 87.92 5.89 -5 -4 0 94.68 6.14 6 -4 0 47.64 3.64 -6 -4 0 38.48 3.44 -6 -4 0 34.88 3.40 -6 4 0 42.25 3.37 6 4 0 41.61 3.45 -7 4 0 52.86 3.90 7 -4 0 47.92 3.90 7 4 0 37.97 3.54 -7 -4 0 38.11 3.69 -7 -4 0 36.50 3.71 8 -4 0 10.01 2.79 8 4 0 9.23 2.74 -8 -4 0 10.17 2.80 -8 4 0 14.34 2.90 -8 -4 0 9.97 2.76 -9 -4 0 10.97 3.14 -9 4 0 9.79 3.00 -9 -4 0 8.33 3.04 9 -4 0 7.45 3.08 9 4 0 6.17 2.85 10 4 0 -0.56 3.34 -10 -4 0 2.84 3.33 -10 4 0 3.51 3.26 10 -4 0 5.44 3.71 -10 -4 0 -1.35 3.32 -11 -4 0 32.05 4.69 -11 -4 0 23.04 4.28 -11 4 0 19.81 4.14 11 -4 0 25.04 4.76 11 4 0 27.07 4.23 12 -4 0 3.00 4.85 -12 -4 0 6.18 4.62 -12 -4 0 0.23 4.13 -12 4 0 5.56 4.15 12 4 0 1.71 4.60 -13 -4 0 12.75 5.00 -13 4 0 4.06 4.72 -13 -4 0 5.02 5.35 -14 -4 0 4.07 6.23 -14 -4 0 -1.68 5.44 -14 4 0 1.73 5.70 -15 -4 0 -1.83 7.31 -15 -4 0 0.00 6.74 -15 4 0 3.82 6.55 -16 4 0 -4.79 7.50 -16 -4 0 5.28 7.27 0 -5 0 -2.07 1.41 -1 -5 0 549.88 32.22 1 -5 0 593.22 32.26 2 -5 0 624.45 36.09 -2 -5 0 655.77 36.11 3 -5 0 231.47 13.09 3 5 0 222.28 13.25 -3 -5 0 221.26 13.08 4 5 0 7.64 1.95 4 -5 0 6.67 1.84 -4 5 0 5.96 1.63 -4 -5 0 6.14 1.82 4 5 0 4.22 1.78 5 5 0 521.33 29.68 -5 -5 0 495.00 29.27 -5 5 0 506.16 29.25 -5 -5 0 527.15 29.64 5 -5 0 480.83 29.23 5 5 0 558.33 29.28 6 5 0 33.87 3.08 6 -5 0 37.76 3.21 -6 -5 0 28.62 3.16 -6 5 0 29.49 3.08 -6 -5 0 27.31 3.14 -7 -5 0 163.92 9.63 7 5 0 152.70 9.34 -7 -5 0 136.25 9.35 7 -5 0 145.59 9.44 -7 5 0 148.38 9.33 -8 -5 0 44.39 4.35 -8 5 0 44.68 4.15 8 5 0 40.65 4.18 -8 -5 0 43.65 4.24 8 -5 0 54.89 4.50 9 5 0 13.19 3.32 -9 5 0 7.02 3.04 9 -5 0 4.57 3.48 -9 -5 0 10.18 3.50 -9 -5 0 8.44 3.36 -10 5 0 7.63 3.42 -10 -5 0 9.38 3.75 10 -5 0 -1.65 3.88 -10 -5 0 5.11 3.59 10 5 0 9.04 3.69 -11 -5 0 16.86 4.63 -11 5 0 22.06 4.29 11 5 0 19.10 4.15 11 -5 0 19.23 4.79 -11 -5 0 25.67 4.48 -12 -5 0 7.04 4.88 12 5 0 9.57 4.81 -12 -5 0 17.53 4.75 -12 5 0 18.13 4.60 -13 5 0 10.88 5.31 -13 -5 0 3.17 5.66 -13 -5 0 3.70 5.36 -14 5 0 20.72 6.19 -14 -5 0 13.68 6.38 -14 -5 0 15.54 6.74 -15 -5 0 9.34 7.12 -15 5 0 3.91 6.18 -16 -5 0 -4.83 7.41 -16 5 0 -4.18 7.05 0 -6 0 1604.05 89.91 -1 -6 0 230.73 13.67 1 -6 0 239.79 13.68 2 -6 0 63.76 4.24 -2 -6 0 57.56 4.21 3 -6 0 45.42 3.53 3 6 0 47.95 3.71 -3 -6 0 45.50 3.53 -4 -6 0 242.21 13.64 4 6 0 229.77 13.85 4 -6 0 221.68 13.56 5 6 0 23.17 2.95 5 6 0 22.10 2.57 -5 -6 0 20.66 2.72 5 -6 0 21.60 2.79 -5 6 0 21.79 2.65 6 6 0 234.48 13.70 6 -6 0 233.70 13.76 6 6 0 227.37 14.06 -6 6 0 220.90 13.65 -6 -6 0 246.14 13.92 -6 -6 0 217.42 13.71 -7 6 0 84.63 6.25 7 -6 0 96.96 6.29 7 6 0 85.02 6.20 -7 -6 0 81.35 6.28 -7 -6 0 92.98 6.42 -8 -6 0 76.13 5.69 8 -6 0 67.06 5.65 8 6 0 70.92 5.35 -8 -6 0 66.02 5.47 -8 6 0 63.83 5.38 -9 -6 0 26.55 3.96 -9 6 0 27.62 3.97 -9 -6 0 22.49 3.99 9 6 0 26.02 3.64 9 -6 0 10.69 3.72 -10 -6 0 -1.17 3.85 10 -6 0 3.93 4.20 -10 -6 0 6.92 3.79 10 6 0 9.81 3.85 -10 6 0 4.93 3.54 -11 6 0 4.71 4.00 11 -6 0 2.46 4.33 -11 -6 0 5.12 4.47 -11 -6 0 11.17 4.62 11 6 0 4.26 4.31 -12 6 0 4.86 4.43 12 6 0 -6.07 4.70 -12 -6 0 -2.69 4.95 -12 -6 0 5.58 5.17 -13 -6 0 19.21 5.70 -13 6 0 29.66 5.62 -13 -6 0 29.99 6.62 -14 -6 0 1.66 6.83 -14 -6 0 -2.65 6.33 -14 6 0 5.04 5.66 -15 -6 0 -1.49 7.28 -15 6 0 5.18 6.49 -16 6 0 15.97 7.59 -16 -6 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