#------------------------------------------------------------------------------ #$Date: 2023-11-16 01:36:29 +0200 (Thu, 16 Nov 2023) $ #$Revision: 287626 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/77/7247733.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7247733 loop_ _publ_author_name 'Uvarova, Marina A.' 'Lutsenko, Irina' 'Babeshkin, Konstantin Andreevich' 'Efimov, Nikolay' 'Shmelev, Maxim' 'Alexandrov, Eugeny V.' 'Sokolov, Andrey V.' 'Eremenko, Igor' 'Khoroshilov, Andrey V.' 'Kiskin, Mikhail A.' _publ_section_title ; Solvent effect in the chemical design of coordination polymers of various topologies with Co2+ and Ni2+ ions and 2-furoate anions ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D3CE00813D _journal_year 2023 _chemical_formula_moiety 'C68 H52 N8 Ni2 O12, 0.5(C4 H6 N2)' _chemical_formula_sum 'C70 H55 N9 Ni2 O12' _chemical_formula_weight 1331.657 _space_group_crystal_system orthorhombic _space_group_IT_number 56 _space_group_name_Hall '-P 2ab 2ac' _space_group_name_H-M_alt 'P c c n' _symmetry_Int_Tables_number 56 _audit_creation_date 2022-03-11 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408) ; _audit_update_record ; 2023-05-26 deposited with the CCDC. 2023-11-15 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.4988(3) _cell_length_b 16.7826(4) _cell_length_c 18.4931(5) _cell_measurement_reflns_used 9060 _cell_measurement_temperature 100 _cell_measurement_theta_max 30.23 _cell_measurement_theta_min 2.29 _cell_volume 3258.43(15) _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'olex2.refine 1.3 (Bourhis et al., 2015)' _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.9783 _diffrn_measured_fraction_theta_max 0.9800 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_unetI/netI 0.0325 _diffrn_reflns_Laue_measured_fraction_full 0.9783 _diffrn_reflns_Laue_measured_fraction_max 0.9800 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 44439 _diffrn_reflns_point_group_measured_fraction_full 0.9783 _diffrn_reflns_point_group_measured_fraction_max 0.9800 _diffrn_reflns_theta_full 25.2417 _diffrn_reflns_theta_max 26.00 _diffrn_reflns_theta_min 2.20 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.647 _exptl_absorpt_correction_T_max 0.3812 _exptl_absorpt_correction_T_min 0.3182 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0961 before and 0.0527 after correction. The Ratio of minimum to maximum transmission is 0.8347. The \l/2 correction factor is Not present. ; _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.357 _exptl_crystal_description prism _exptl_crystal_F_000 1382.115 _exptl_crystal_preparation 'Magnetic properties,TGA' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _refine_diff_density_max 0.5746 _refine_diff_density_min -0.4107 _refine_diff_density_rms 0.0818 _refine_ls_d_res_high 0.8107 _refine_ls_d_res_low 9.2465 _refine_ls_goodness_of_fit_ref 1.0700 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_constraints 44 _refine_ls_number_parameters 244 _refine_ls_number_reflns 3140 _refine_ls_number_restraints 106 _refine_ls_restrained_S_all 1.0509 _refine_ls_R_factor_all 0.0728 _refine_ls_R_factor_gt 0.0568 _refine_ls_shift/su_max 0.0009 _refine_ls_shift/su_mean 0.0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0768P)^2^+4.2314P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1510 _refine_ls_wR_factor_ref 0.1651 _reflns_Friedel_coverage 0.0 _reflns_limit_h_max 12 _reflns_limit_h_min 0 _reflns_limit_k_max 20 _reflns_limit_k_min 0 _reflns_limit_l_max 22 _reflns_limit_l_min 0 _reflns_number_gt 2374 _reflns_number_total 3140 _reflns_threshold_expression I>=2u(I) _iucr_refine_instructions_details ; TITL 1_a.res in Pccn REM Old TITL NiFurDPE_0m in Pccn REM SHELXT solution in Pccn REM R1 0.215, Rweak 0.006, Alpha 0.040, Orientation as input REM Formula found by SHELXT: C32 N4 O8 Ni CELL 0.71073 10.4988 16.7826 18.4931 90 90 90 ZERR 2 0.0003 0.0004 0.0005 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,-Y,0.5-Z SFAC C H N Ni O UNIT 140 110 18 4 24 SADI O2 C13 O2A C13 EADP O3A O3 SADI C13 C14 C13 C14A ISOR 0.01 0.02 C17 C17A SADI C14 O3 C14A O3A SADI C14 C15 C14A C15A EADP C16 C16A SADI 0.04 O3 C15 O3A C15A SADI O3 C17 O3A C17A SADI C17 C16 C17A C16A ISOR 0.001 0.002 C15 C15A C16 C16A ISOR 0.01 0.02 O2A O2 SADI 0.04 O3 C16 O3A C16A SADI C15 C16 C15A C16A SADI 0.04 C17 C15 C17A C15A SADI 0.04 C13 O3 C13 O3A SADI 0.04 C13 C15 C13 C15A SADI 0.04 C14 C17 C14A C17A SADI 0.04 C14 C16 C14A C16A ISOR 0.01 0.02 O3 O3A ISOR 0.01 0.02 C14 C14A EADP C15A C15 EADP C17A C17 EADP O2 O2A EADP C19 N3 ISOR 0.01 0.02 C18 EXYZ C19 N3 L.S. 99 PLAN 99 SIZE 0.1 0.1 0.2 TEMP -173.15 CONF BOND $H LIST 4 MORE -1 fmap 2 acta OMIT -4 52 OMIT 2 1 6 OMIT 3 1 0 OMIT 1 2 4 OMIT 0 3 2 OMIT 1 0 4 OMIT 2 4 1 OMIT 1 1 1 OMIT 0 1 2 OMIT 0 2 0 OMIT 2 9 2 OMIT 6 4 1 OMIT 3 10 4 OMIT 5 6 4 OMIT 3 6 9 OMIT 1 2 2 OMIT 1 0 2 OMIT 3 4 3 OMIT 5 3 1 OMIT 2 9 1 OMIT 3 9 3 OMIT 4 2 0 OMIT 1 4 3 OMIT 5 8 4 OMIT 0 2 4 OMIT 1 1 2 OMIT 1 1 4 OMIT 1 2 6 OMIT 0 0 4 OMIT 2 2 0 OMIT 5 2 3 OMIT 3 2 6 OMIT 2 1 2 OMIT 2 2 2 OMIT 5 3 9 OMIT 6 5 7 OMIT 6 1 3 OMIT 3 4 5 OMIT 4 3 7 OMIT 4 4 0 OMIT 0 1 8 OMIT 0 3 6 OMIT 1 1 8 OMIT 2 12 3 OMIT 1 3 7 OMIT 1 6 3 OMIT 7 4 5 OMIT 2 0 0 OMIT 1 2 5 OMIT 4 0 2 OMIT 1 7 2 OMIT 3 2 2 OMIT 3 2 4 OMIT 1 3 3 OMIT 2 4 7 OMIT 3 3 7 OMIT 4 4 1 OMIT 5 2 2 OMIT 1 1 0 OMIT 3 3 3 OMIT 4 3 5 OMIT 3 9 5 OMIT 3 3 1 OMIT 0 1 4 OMIT 5 2 4 WGHT 0.076824 4.231401 FVAR 0.397532 0.61705 REM REM REM Ni1 4 0.25000 0.25000 0.75110 10.50000 0.04352 0.03190 0.02484 = -0.00000 -0.00000 -0.01359 O1 5 0.40873 0.17769 0.74096 11.00000 0.04957 0.05487 0.05320 = -0.00162 -0.00609 0.00149 N1 3 0.16904 0.17819 0.66943 11.00000 0.05530 0.03821 0.03811 = -0.00646 -0.00392 -0.01532 N2 3 0.33921 0.32078 0.82897 11.00000 0.05642 0.04802 0.03194 = -0.00813 -0.00070 -0.01881 C6 1 0.17877 0.09874 0.67161 11.00000 0.06396 0.04429 0.04695 = -0.00974 -0.00198 -0.01599 AFIX 43 H6 2 0.22308 0.07481 0.71078 11.00000 -1.20000 AFIX 0 C1 1 0.10986 0.20938 0.61238 11.00000 0.06634 0.05449 0.04762 = -0.00906 -0.01720 -0.00720 AFIX 43 H1 2 0.10240 0.26574 0.61003 11.00000 -1.20000 AFIX 0 C2 1 0.05881 0.16555 0.55666 11.00000 0.06919 0.07034 0.05189 = -0.01568 -0.01769 -0.00477 AFIX 43 H2 2 0.01969 0.19139 0.51671 11.00000 -1.20000 AFIX 0 PART 1 O2 5 0.51652 0.13883 0.84073 21.00000 0.09619 0.12840 0.07047 = 0.03239 0.00017 0.03576 PART 0 C12 1 0.27795 0.35143 0.88547 11.00000 0.05936 0.07915 0.06216 = -0.02775 0.00901 -0.02261 AFIX 43 H12 2 0.19082 0.33811 0.89225 11.00000 -1.20000 AFIX 0 C5 1 0.12639 0.04992 0.61864 11.00000 0.06995 0.04204 0.06802 = -0.02053 0.00981 -0.01909 AFIX 43 H5 2 0.13218 -0.00641 0.62257 11.00000 -1.20000 AFIX 0 C3 1 0.06509 0.08489 0.55955 11.00000 0.05291 0.07671 0.04668 = -0.01826 0.00038 -0.01962 C13 1 0.50190 0.15135 0.77375 11.00000 0.05868 0.06962 0.05340 = 0.01308 0.00095 -0.00245 C11 1 0.33465 0.40102 0.93396 11.00000 0.06768 0.11984 0.07286 = -0.05602 0.01225 -0.02575 AFIX 43 H11 2 0.28637 0.42161 0.97319 11.00000 -1.20000 AFIX 0 PART 1 C14 1 0.60664 0.11889 0.72835 21.00000 0.04751 0.06335 0.07917 = 0.00669 0.00039 0.00286 PART 0 C7 1 0.46297 0.33886 0.82250 11.00000 0.05682 0.06864 0.06023 = -0.02430 0.00348 -0.01467 AFIX 43 H7 2 0.50977 0.31603 0.78372 11.00000 -1.20000 AFIX 0 C8 1 0.52543 0.38911 0.86962 11.00000 0.05294 0.09124 0.07962 = -0.03904 0.00628 -0.02067 AFIX 43 H8 2 0.61294 0.40111 0.86241 11.00000 -1.20000 AFIX 0 C9 1 0.46085 0.42180 0.92705 11.00000 0.06245 0.09584 0.07221 = -0.03724 0.00081 -0.02416 C4 1 0.00727 0.03796 0.49970 11.00000 0.07327 0.07560 0.05621 = -0.01934 0.00037 -0.02188 AFIX 43 H4 2 -0.02085 0.06618 0.45813 11.00000 -1.20000 AFIX 0 PART 1 O3 5 0.70910 0.08018 0.75522 21.00000 0.07994 0.09913 0.12341 = 0.02078 0.00973 0.02211 PART 0 C10 1 0.52739 0.47744 0.97548 11.00000 0.06206 0.12360 0.08007 = -0.05072 0.00257 -0.02599 AFIX 43 H10 2 0.61734 0.48105 0.97095 11.00000 -1.20000 AFIX 0 PART 1 C17 1 0.78934 0.06332 0.70123 21.00000 0.06295 0.08750 0.12287 = -0.00742 0.01859 0.01024 AFIX 43 H17 2 0.87440 0.04512 0.70707 21.00000 -1.20000 AFIX 0 C15 1 0.61194 0.10880 0.65833 21.00000 0.09784 0.09836 0.09807 = -0.00014 0.00004 0.00019 AFIX 43 H15 2 0.54696 0.12122 0.62441 21.00000 -1.20000 AFIX 0 C16 1 0.73589 0.07503 0.64229 21.00000 0.11196 0.11226 0.11225 = -0.00021 0.00030 0.00019 AFIX 43 H16 2 0.76967 0.06401 0.59570 21.00000 -1.20000 AFIX 0 PART 0 C18 1 0.75000 0.25000 0.95622 10.25000 0.09784 0.10941 0.11311 = -0.00000 -0.00000 -0.01463 PART 4 N3 3 0.70099 0.16986 0.94464 10.25000 0.08276 0.15881 0.08480 = 0.00667 -0.00404 -0.00550 PART 2 C15A 1 0.63668 0.15120 0.65756 -21.00000 0.09784 0.09836 0.09807 = -0.00014 0.00004 0.00019 AFIX 43 H15A 2 0.58498 0.18197 0.62598 -21.00000 -1.20000 AFIX 0 C14A 1 0.61075 0.13161 0.72571 -21.00000 0.05412 0.06167 0.06840 = 0.00814 0.00285 0.00065 O3A 5 0.72527 0.11391 0.75998 -21.00000 0.07994 0.09913 0.12341 = 0.02078 0.00973 0.02211 C16A 1 0.75972 0.11618 0.64111 -21.00000 0.11196 0.11226 0.11225 = -0.00021 0.00030 0.00019 AFIX 43 H16A 2 0.80116 0.11313 0.59553 -21.00000 -1.20000 AFIX 0 C17A 1 0.79841 0.09106 0.70050 -21.00000 0.06295 0.08750 0.12287 = -0.00742 0.01859 0.01024 AFIX 43 H17A 2 0.87226 0.05873 0.70500 -21.00000 -1.20000 AFIX 0 O2A 5 0.51830 0.16723 0.84031 -21.00000 0.09619 0.12840 0.07047 = 0.03239 0.00017 0.03576 PART 3 C19 1 0.70099 0.16986 0.94464 10.25000 0.08276 0.15881 0.08480 = 0.00667 -0.00404 -0.00550 AFIX 137 H19a 2 0.64132 0.17021 0.90389 10.25000 -1.50000 H19b 2 0.77183 0.13371 0.93393 10.25000 -1.50000 H19c 2 0.65682 0.15170 0.98832 10.25000 -1.50000 AFIX 0 HKLF 4 END Q2 1 0.027778 0 0.533333 11 0.05 0.56 Q1 1 0.444444 0.092593 0.816667 11 0.05 0.57 Q4 1 0.166667 0.018519 0.65 11 0.05 0.37 Q3 1 0.5 0.222222 0.85 11 0.05 0.38 Q7 1 0.666667 0.185185 0.683333 11 0.05 0.32 Q5 1 0.75 0.25 0.916667 11 0.05 0.35 Q8 1 0.027778 0.12963 0.583333 11 0.05 0.32 Q9 1 0.805556 0.148148 0.666667 11 0.05 0.31 Q12 1 0.833333 0.092593 0.766667 11 0.05 0.3 Q10 1 0.611111 0.074074 0.683333 11 0.05 0.31 Q13 1 0.083333 0.037037 0.583333 11 0.05 0.29 Q11 1 0.25 0.333333 0.833333 11 0.05 0.31 Q25 1 0.527778 0.148148 0.85 11 0.05 0.21 Q16 1 0.75 0.111111 0.633333 11 0.05 0.25 Q21 1 0.166667 0.203704 0.683333 11 0.05 0.22 Q14 1 0.666667 0.055556 0.733333 11 0.05 0.29 Q26 1 0.25 0.25 0.7 11 0.05 0.21 Q27 1 0.111111 0.185185 0.45 11 0.05 0.2 Q18 1 0.444444 0.203704 0.766667 11 0.05 0.23 Q17 1 0.75 0.055556 0.666667 11 0.05 0.25 Q30 1 0.138889 0.166667 0.633333 11 0.05 0.19 Q33 1 0.25 0 0.616667 11 0.05 0.19 Q22 1 0.833333 0 0.583333 11 0.05 0.22 Q34 1 0.527778 0.277778 0.666667 11 0.05 0.19 Q42 1 0.222222 0.296296 0.933333 11 0.05 0.17 Q32 1 0.527778 0.351852 0.933333 11 0.05 0.19 Q52 1 0.638889 0.037037 0.55 11 0.05 0.16 Q28 1 0.472222 0.185185 0.9 11 0.05 0.2 Q49 1 0.055556 -0.037037 0.616667 11 0.05 0.17 Q35 1 0.583333 0.240741 0.883333 11 0.05 0.19 Q36 1 0.5 0.314815 0.883333 11 0.05 0.18 Q59 1 0.166667 0.37037 0.666667 11 0.05 0.15 Q45 1 0.444444 0.5 0.966667 11 0.05 0.17 Q56 1 0.111111 0.296296 0.466667 11 0.05 0.16 Q37 1 0.083333 0.037037 0.683333 11 0.05 0.18 Q48 1 0.472222 0.12963 0.733333 11 0.05 0.17 Q69 1 0.055556 0.240741 0.933333 11 0.05 0.14 Q50 1 0.777778 -0.055556 0.6 11 0.05 0.17 Q84 1 0 0.148148 0.633333 11 0.05 0.14 Q60 1 0.861111 0 0.733333 11 0.05 0.15 Q40 1 0.166667 0.351852 0.866667 11 0.05 0.18 Q43 1 0.277778 0.388889 0.983333 11 0.05 0.17 Q54 1 0.25 0.055556 0.816667 11 0.05 0.16 Q85 1 -0.027778 0.166667 0.466667 11 0.05 0.13 Q67 1 0.361111 0.407407 0.883333 11 0.05 0.15 Q39 1 0.75 0 0.816667 11 0.05 0.18 Q89 1 -0.027778 0.203704 0.516667 11 0.05 0.13 Q63 1 0.083333 -0.018519 0.733333 11 0.05 0.15 Q64 1 0.5 0.055556 0.616667 11 0.05 0.15 Q51 1 0.472222 0.425926 0.816667 11 0.05 0.17 Q79 1 0.777778 0.444444 0.983333 11 0.05 0.14 Q82 1 0.694444 0.481481 0.95 11 0.05 0.14 Q47 1 0.111111 0.240741 0.55 11 0.05 0.17 Q83 1 0.055556 0.092593 0.4 11 0.05 0.14 Q70 1 0.083333 0.166667 0.55 11 0.05 0.14 Q58 1 0.444444 0.074074 0.55 11 0.05 0.16 Q76 1 0.805556 0 0.666667 11 0.05 0.14 Q74 1 0.444444 0.444444 0.916667 11 0.05 0.14 Q55 1 0.583333 0.407407 1 11 0.05 0.16 Q75 1 0 0.074074 0.6 11 0.05 0.14 Q61 1 0.055556 0.018519 0.416667 11 0.05 0.15 Q90 1 0.055556 0.240741 0.633333 11 0.05 0.13 Q53 1 0.361111 0.333333 0.85 11 0.05 0.16 Q62 1 0.555556 0.074074 0.816667 11 0.05 0.15 Q91 1 0.138889 0.296296 0.633333 11 0.05 0.13 Q77 1 0.888889 0.185185 1.033333 11 0.05 0.14 Q78 1 0.611111 0.518519 0.95 11 0.05 0.14 Q66 1 0.861111 0.037037 0.633333 11 0.05 0.15 Q92 1 0.277778 0.074074 0.566667 11 0.05 0.12 Q19 1 0.722222 0.148148 0.816667 11 0.05 0.23 Q24 1 0.722222 0.148148 0.733333 11 0.05 0.22 Q23 1 0.75 0.25 0.6 11 0.05 0.22 Q20 1 0.083333 0.074074 0.633333 11 0.05 0.23 Q38 1 0.166667 0.240741 0.933333 11 0.05 0.18 Q44 1 0.722222 0.092593 0.766667 11 0.05 0.17 Q65 1 0.194444 0.111111 0.65 11 0.05 0.15 Q86 1 0.194444 0.37037 0.916667 11 0.05 0.13 Q80 1 0.111111 0.351852 0.516667 11 0.05 0.14 Q87 1 0.75 0.518519 0.983333 11 0.05 0.13 Q68 1 0.638889 -0.037037 0.666667 11 0.05 0.15 Q29 1 0.222222 0.074074 0.7 11 0.05 0.2 Q46 1 0.555556 0.222222 0.583333 11 0.05 0.17 Q57 1 0.638889 0.148148 0.766667 11 0.05 0.16 Q41 1 0.666667 0.222222 0.583333 11 0.05 0.18 Q81 1 0.083333 0.074074 0.533333 11 0.05 0.14 Q93 1 0.416667 0.277778 0.85 11 0.05 0.12 Q88 1 -0.055556 0.240741 0.716667 11 0.05 0.13 Q94 1 0.444444 0 0.633333 11 0.05 0.12 Q95 1 0.527778 0.166667 0.666667 11 0.05 0.12 Q96 1 0.944444 -0.055556 0.766667 11 0.05 0.12 Q6 1 0.777778 0.222222 0.983333 11 0.05 0.33 Q15 1 0.611111 0.12963 0.65 11 0.05 0.28 Q31 1 0.333333 0.222222 0.75 11 0.05 0.19 Q71 1 0.611111 0.407407 0.816667 11 0.05 0.14 Q72 1 0.861111 0.018519 0.8 11 0.05 0.14 Q73 1 0.583333 0.351852 0.75 11 0.05 0.14 Q97 1 0.611111 0.444444 0.866667 11 0.05 0.12 Q98 1 0 0.018519 0.633333 11 0.05 0.12 Q99 1 0.861111 0.12963 0.916667 11 0.05 0.12 REM The information below was added by Olex2. REM REM R1 = 0.0568 for 2374 Fo > 4sig(Fo) and 0.0728 for all 3140 data REM 244 parameters refined using 106 restraints REM Highest difference peak 0.5746, deepest hole -0.4107 REM Mean Shift 0.0000, Max Shift 0.0009. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0728 REM R1_gt = 0.0568 REM wR_ref = 0.1651 REM GOOF = 1.0700 REM Shift_max = 0.0009 REM Shift_mean = 0.0000 REM Reflections_all = 3140 REM Reflections_gt = 2374 REM Parameters = 244 REM Hole = -0.4107 REM Peak = 0.5746 REM Flack = n/a ; _cod_data_source_file d3ce00813d2.cif _cod_data_source_block 1_a_CCDC2 _cod_database_code 7247733 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Shared sites {C19, N3} 3. Restrained distances O2-C13 \\sim O2A-C13 with sigma of 0.02 C13-C14 \\sim C13-C14A with sigma of 0.02 C14-O3 \\sim C14A-O3A with sigma of 0.02 C14-C15 \\sim C14A-C15A with sigma of 0.02 O3-C15 \\sim O3A-C15A with sigma of 0.04 O3-C17 \\sim O3A-C17A with sigma of 0.02 C17-C16 \\sim C17A-C16A with sigma of 0.02 O3-C16 \\sim O3A-C16A with sigma of 0.04 C15-C16 \\sim C15A-C16A with sigma of 0.02 C17-C15 \\sim C17A-C15A with sigma of 0.04 C13-O3 \\sim C13-O3A with sigma of 0.04 C13-C15 \\sim C13-C15A with sigma of 0.04 C14-C17 \\sim C14A-C17A with sigma of 0.04 C14-C16 \\sim C14A-C16A with sigma of 0.04 4. Uiso/Uaniso restraints and constraints Uanis(C17) \\sim Ueq, Uanis(C17A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C15) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C16A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(O2A) \\sim Ueq, Uanis(O2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O3) \\sim Ueq, Uanis(O3A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C14) \\sim Ueq, Uanis(C14A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O3A) = Uanis(O3) Uanis(C16) = Uanis(C16A) Uanis(C15A) = Uanis(C15) Uanis(C17A) = Uanis(C17) Uanis(O2) = Uanis(O2A) Uanis(C19) = Uanis(N3) 5. Others Sof(C15A)=Sof(H15A)=Sof(C14A)=Sof(O3A)=Sof(C16A)=Sof(H16A)=Sof(C17A)= Sof(H17A)=Sof(O2A)=1-FVAR(1) Sof(O2)=Sof(C14)=Sof(O3)=Sof(C17)=Sof(H17)=Sof(C15)=Sof(H15)=Sof(C16)= Sof(H16)=FVAR(1) Fixed Sof: C18(0.25) N3(0.25) C19(0.25) H19a(0.25) H19b(0.25) H19c(0.25) 6.a Aromatic/amide H refined with riding coordinates: C6(H6), C1(H1), C2(H2), C12(H12), C5(H5), C11(H11), C7(H7), C8(H8), C4(H4), C10(H10), C17(H17), C15(H15), C16(H16), C15A(H15A), C16A(H16A), C17A(H17A) 6.b Idealised Me refined as rotating group: C19(H19a,H19b,H19c) ; _iucr_refine_fcf_details ; data_1_a_CCDC3 _computing_structure_refinement 'olex2.refine 1.3 (Bourhis et al., 2015)' _shelx_refln_list_code 4 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 x+1/2,-y,-z+1/2 3 -x,y+1/2,-z+1/2 4 -x+1/2,-y+1/2,z 5 -x,-y,-z 6 -x-1/2,y,z-1/2 7 x,-y-1/2,z-1/2 8 x-1/2,y-1/2,-z _space_group_crystal_system orthorhombic _space_group_IT_number 56 _space_group_name_H-M_alt 'P c c n' _space_group_name_Hall '-P 2ab 2ac' _symmetry_space_group_name_H-M 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' _symmetry_Int_Tables_number 56 _cell_length_a 10.4988(3) _cell_length_b 16.7826(4) _cell_length_c 18.4931(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3258.43(15) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_F_squared_weight _refln_observed_status 0 0 2 60398.900 59055.300 2361.290 0.001 o 0 0 6 3363.630 3608.070 83.872 0.194 o 0 0 8 8449.350 6948.280 159.487 0.041 o 0 0 10 25027.200 24990.400 561.794 0.004 o 0 0 12 12489.900 12980.100 363.877 0.016 o 0 0 14 5820.170 6503.170 189.449 0.064 o 0 0 16 4624.600 4897.030 121.629 0.107 o 0 0 18 275.923 236.556 28.810 7.580 o 0 0 20 84.562 99.942 18.933 22.676 o 0 0 22 839.818 842.955 38.799 1.928 o 0 1 6 93.028 141.339 5.975 31.370 o 0 1 10 188.433 165.423 8.160 17.388 o 0 1 12 0.848 2.461 4.719 632.934 o 0 1 14 89.886 112.598 8.441 33.002 o 0 1 16 36.080 43.297 7.204 79.695 o 0 1 18 29.410 30.047 7.324 96.716 o 0 1 20 30.087 14.226 10.375 82.381 o 0 1 22 21.083 -12.398 10.530 103.841 o 0 2 2 50670.700 43799.800 949.483 0.001 o 0 2 6 8152.760 8768.990 115.200 0.039 o 0 2 8 3099.310 3332.050 56.208 0.234 o 0 2 10 9529.140 9337.720 151.272 0.030 o 0 2 12 5689.460 5763.850 113.380 0.078 o 0 2 14 7378.990 7367.730 134.760 0.048 o 0 2 16 967.287 1018.180 29.529 1.656 o 0 2 18 260.453 266.361 24.921 8.331 o 0 2 20 658.806 667.909 24.500 2.975 o 0 2 22 572.187 610.842 24.129 3.507 o 0 3 4 12528.300 9514.550 124.347 0.021 o 0 3 8 281.700 325.071 8.090 9.699 o 0 3 10 154.398 188.229 6.627 19.638 o 0 3 12 52.128 93.938 5.721 52.689 o 0 3 14 6.043 6.552 5.142 336.361 o 0 3 16 164.450 178.716 10.274 17.982 o 0 3 18 24.168 26.473 10.278 82.907 o 0 3 20 1.273 -4.068 11.417 132.978 o 0 3 22 5.614 -4.768 16.039 65.202 o 0 4 0 56870.700 43394.600 1436.390 0.001 o 0 4 2 5847.650 7249.570 95.902 0.066 o 0 4 4 19235.900 16963.900 234.035 0.008 o 0 4 6 4801.830 5060.360 72.041 0.107 o 0 4 8 12960.500 13552.800 218.313 0.016 o 0 4 10 80.412 68.432 6.475 44.554 o 0 4 12 965.636 891.511 23.273 1.827 o 0 4 14 2376.150 2326.010 54.669 0.389 o 0 4 16 910.615 722.955 29.986 2.040 o 0 4 18 2714.450 2642.180 63.780 0.306 o 0 4 20 1337.490 1273.010 38.149 1.033 o 0 4 22 510.133 496.224 28.314 4.004 o 0 5 2 13772.900 11863.400 190.082 0.016 o 0 5 4 5802.290 5174.090 66.375 0.084 o 0 5 6 3213.040 3639.700 50.374 0.214 o 0 5 8 151.038 202.693 8.183 18.827 o 0 5 10 27.803 60.746 4.948 90.195 o 0 5 12 539.990 515.024 16.541 4.249 o 0 5 14 553.803 513.402 19.293 4.065 o 0 5 16 197.267 235.318 15.464 12.835 o 0 5 18 4.353 -3.981 9.590 170.766 o 0 5 20 132.612 163.815 15.070 18.690 o 0 5 22 58.384 51.756 12.086 44.263 o 0 6 0 707.334 724.715 23.921 2.702 o 0 6 2 995.337 1094.900 17.713 1.633 o 0 6 4 3968.050 4359.660 59.745 0.148 o 0 6 6 17955.200 17287.800 225.907 0.009 o 0 6 8 3426.070 3351.400 62.858 0.206 o 0 6 10 1836.040 1594.640 28.526 0.674 o 0 6 12 748.917 764.858 21.355 2.543 o 0 6 14 41.774 48.701 9.874 60.275 o 0 6 16 2214.820 2372.710 57.350 0.412 o 0 6 18 2190.240 2126.950 64.811 0.433 o 0 6 20 895.432 843.786 29.956 1.943 o 0 7 2 38.516 4.659 3.117 137.729 o 0 7 4 2683.730 2388.440 36.972 0.344 o 0 7 6 221.650 222.951 8.281 13.707 o 0 7 8 850.919 817.957 25.266 2.131 o 0 7 10 783.997 598.763 16.705 2.777 o 0 7 12 774.373 676.266 19.931 2.626 o 0 7 14 384.615 332.528 15.481 6.878 o 0 7 16 1.497 5.393 7.767 246.653 o 0 7 18 160.560 181.211 14.905 16.248 o 0 7 20 47.304 43.400 19.429 30.465 o 0 8 0 310.001 405.809 18.076 7.229 o 0 8 2 2903.500 2271.120 52.674 0.313 o 0 8 4 4714.650 4681.700 68.655 0.115 o 0 8 6 4247.190 4024.560 60.183 0.144 o 0 8 8 5623.480 5901.110 86.533 0.079 o 0 8 10 2597.050 2617.820 43.985 0.336 o 0 8 12 113.764 122.337 7.210 28.464 o 0 8 14 682.415 690.474 21.625 2.902 o 0 8 16 525.522 520.417 19.706 4.216 o 0 8 18 1285.290 1421.650 45.908 0.979 o 0 8 20 587.447 604.458 32.018 3.174 o 0 9 2 1879.070 2030.460 73.377 0.501 o 0 9 4 600.405 540.236 13.295 3.855 o 0 9 6 133.388 166.761 8.792 21.933 o 0 9 8 43.620 58.997 5.227 71.933 o 0 9 10 396.829 376.396 11.488 6.646 o 0 9 12 112.649 116.201 7.244 29.168 o 0 9 14 4.259 -12.212 6.842 302.528 o 0 9 16 519.455 491.016 20.653 4.324 o 0 9 18 37.275 8.170 9.161 86.849 o 0 9 20 0.307 -18.154 15.105 77.771 o 0 10 0 3514.220 3664.020 116.691 0.172 o 0 10 2 2918.050 3106.790 71.559 0.254 o 0 10 4 4144.450 3823.960 85.531 0.148 o 0 10 6 3047.640 3197.560 64.151 0.241 o 0 10 8 4493.770 4477.000 68.038 0.125 o 0 10 10 259.172 301.513 11.050 10.360 o 0 10 12 1075.620 1327.370 30.584 1.293 o 0 10 14 894.090 814.513 23.826 2.052 o 0 10 16 868.540 792.587 31.824 2.029 o 0 10 18 515.216 473.005 26.686 4.128 o 0 11 2 346.122 420.799 20.806 6.327 o 0 11 4 548.882 569.343 22.183 3.817 o 0 11 6 36.958 80.580 7.254 62.235 o 0 11 8 152.886 208.513 12.043 17.062 o 0 11 10 0.305 5.250 5.306 488.721 o 0 11 12 47.703 17.052 6.795 83.584 o 0 11 14 327.667 348.146 16.787 7.555 o 0 11 16 132.930 112.279 14.957 20.933 o 0 11 18 6.668 8.035 11.363 111.624 o 0 12 0 8894.450 9371.830 396.692 0.026 o 0 12 2 4575.720 4594.960 102.838 0.116 o 0 12 4 3096.130 3225.280 76.445 0.230 o 0 12 6 2286.320 2137.120 42.421 0.437 o 0 12 8 128.494 130.272 10.061 23.882 o 0 12 10 4276.810 4604.790 83.647 0.128 o 0 12 12 2986.200 2505.390 42.580 0.292 o 0 12 14 1267.920 1494.970 42.533 0.981 o 0 12 16 650.348 668.529 26.970 2.945 o 0 12 18 331.625 299.886 21.949 7.274 o 0 13 2 85.500 117.063 13.480 27.724 o 0 13 4 56.354 47.854 10.662 49.882 o 0 13 6 127.853 107.317 13.402 22.891 o 0 13 8 144.650 172.248 14.112 17.994 o 0 13 10 154.123 178.603 13.749 17.273 o 0 13 12 20.312 32.986 7.563 108.224 o 0 13 14 6.534 8.378 5.874 273.785 o 0 13 16 6.410 -2.650 10.063 149.099 o 0 14 0 5265.540 4563.560 147.364 0.093 o 0 14 2 2702.550 2514.030 64.365 0.316 o 0 14 4 2105.430 2060.190 65.870 0.457 o 0 14 6 20.856 31.676 10.790 79.700 o 0 14 8 837.468 896.835 25.666 2.065 o 0 14 10 2353.920 2126.740 41.091 0.424 o 0 14 12 2137.450 2159.800 42.061 0.469 o 0 14 14 871.165 868.303 22.488 2.057 o 0 14 16 563.186 625.380 36.364 3.068 o 0 15 2 77.146 105.311 15.015 28.012 o 0 15 4 60.912 54.284 15.178 35.685 o 0 15 6 0.593 29.205 8.701 149.451 o 0 15 8 50.867 61.403 7.634 58.239 o 0 15 10 64.652 54.432 8.184 51.141 o 0 15 12 2.002 10.137 7.270 244.201 o 0 15 14 26.903 58.906 9.110 71.159 o 0 16 0 625.180 524.918 50.939 2.486 o 0 16 2 1849.720 1643.230 50.832 0.618 o 0 16 4 964.803 892.731 33.916 1.720 o 0 16 6 951.938 1030.910 37.109 1.595 o 0 16 8 1043.020 970.435 31.114 1.562 o 0 16 10 836.120 770.247 21.503 2.278 o 0 16 12 551.621 521.925 30.584 3.591 o 0 16 14 538.202 475.046 22.262 4.179 o 0 17 2 61.029 46.429 16.591 33.510 o 0 17 4 10.270 40.409 13.703 64.490 o 0 17 6 19.063 33.091 12.878 66.059 o 0 17 8 8.430 5.181 12.695 92.485 o 0 17 10 0.034 1.767 11.783 125.930 o 0 17 12 1.643 11.934 8.893 176.849 o 0 18 0 206.527 244.087 31.950 7.984 o 0 18 2 341.530 459.738 27.137 5.558 o 0 18 4 920.787 880.302 36.066 1.781 o 0 18 6 595.790 575.461 31.507 3.219 o 0 18 8 463.318 435.787 27.319 4.584 o 0 18 10 358.837 391.638 26.803 5.764 o 0 19 2 0.615 -3.548 12.775 107.986 o 0 19 4 0.206 2.675 12.970 103.211 o 0 19 6 22.116 35.353 14.955 52.376 o 0 19 8 41.884 76.879 15.631 36.509 o 0 20 0 268.088 255.195 59.134 3.545 o 0 20 2 201.938 280.111 26.265 9.081 o 0 20 4 111.255 175.388 35.834 9.138 o 1 0 6 176.255 195.053 8.843 17.009 o 1 0 8 395.564 426.178 13.487 6.205 o 1 0 10 42.794 79.344 5.487 63.479 o 1 0 12 14.158 19.199 4.629 198.062 o 1 0 14 13.289 31.483 7.238 130.490 o 1 0 16 278.742 228.030 16.032 10.065 o 1 0 18 0.115 10.488 7.033 275.469 o 1 0 20 34.908 17.789 10.837 72.389 o 1 0 22 2.630 -2.327 10.615 148.293 o 1 1 3 187.696 68.816 1.833 23.457 o 1 1 5 347.404 171.165 4.011 10.300 o 1 1 6 4343.470 4176.230 54.110 0.137 o 1 1 7 116.549 91.391 3.705 32.956 o 1 1 9 7.676 5.779 2.192 510.253 o 1 1 10 3513.560 3637.270 45.966 0.194 o 1 1 11 51.615 53.320 3.645 71.197 o 1 1 12 7269.180 7132.860 87.343 0.051 o 1 1 13 4.513 5.195 3.147 591.871 o 1 1 14 7077.500 6612.410 82.002 0.056 o 1 1 15 51.354 39.172 4.358 76.669 o 1 1 16 2663.940 2722.480 40.124 0.321 o 1 1 17 235.900 219.812 9.133 12.976 o 1 1 18 137.366 118.079 6.866 25.358 o 1 1 19 393.753 388.807 12.533 6.539 o 1 1 20 299.035 313.294 11.607 9.065 o 1 1 21 4.986 -1.626 6.240 335.580 o 1 1 22 772.514 743.605 17.268 2.559 o 1 2 1 67.903 26.471 1.099 72.003 o 1 2 3 46535.000 47505.200 1836.150 0.001 o 1 2 7 4944.310 4539.290 47.925 0.112 o 1 2 8 37.345 48.669 3.320 91.340 o 1 2 9 3450.150 3237.650 39.407 0.214 o 1 2 10 44.812 51.162 3.433 79.743 o 1 2 11 134.998 88.454 5.279 28.834 o 1 2 12 49.354 41.726 4.637 76.601 o 1 2 13 249.632 293.573 8.784 11.079 o 1 2 14 19.247 23.008 4.506 162.608 o 1 2 15 879.219 780.698 15.359 2.214 o 1 2 16 46.384 33.241 5.263 82.516 o 1 2 17 155.664 202.710 13.698 16.401 o 1 2 18 53.163 48.690 6.996 62.860 o 1 2 19 289.180 354.379 13.322 8.631 o 1 2 20 7.710 -6.888 8.648 184.206 o 1 2 21 1.387 -7.780 6.762 358.799 o 1 2 22 0.214 -11.925 7.081 351.004 o 1 3 0 30838.400 23046.400 338.092 0.004 o 1 3 1 965.371 755.932 16.048 2.028 o 1 3 2 56035.700 60854.800 1010.120 0.001 o 1 3 4 16352.300 18617.200 175.799 0.010 o 1 3 5 226.816 288.395 6.508 12.283 o 1 3 6 6611.550 6878.690 71.031 0.060 o 1 3 8 17042.300 16826.900 183.137 0.010 o 1 3 9 1493.670 1572.770 19.572 0.871 o 1 3 10 5256.430 5576.140 68.941 0.090 o 1 3 11 291.439 209.039 6.778 11.314 o 1 3 12 3718.320 3996.950 56.425 0.170 o 1 3 13 0.304 0.914 3.777 1085.000 o 1 3 14 2582.180 2706.800 38.539 0.335 o 1 3 15 59.323 68.815 5.439 56.180 o 1 3 16 827.050 829.512 16.039 2.282 o 1 3 17 190.262 184.553 8.788 16.436 o 1 3 18 1472.280 1484.210 26.950 0.898 o 1 3 19 89.893 110.950 8.535 33.084 o 1 3 20 1031.540 1060.440 21.186 1.583 o 1 3 21 32.899 47.921 8.100 75.957 o 1 3 22 423.953 403.488 16.151 5.834 o 1 4 1 3287.490 3097.900 29.422 0.235 o 1 4 2 5796.680 6522.520 59.644 0.073 o 1 4 4 477.796 704.982 8.350 4.220 o 1 4 5 4657.290 4940.450 47.016 0.114 o 1 4 6 1128.640 1141.530 14.185 1.417 o 1 4 7 2830.020 3449.190 37.306 0.259 o 1 4 8 30.902 41.635 3.498 107.845 o 1 4 9 623.702 685.172 11.423 3.357 o 1 4 10 378.529 437.533 8.615 6.609 o 1 4 11 249.865 300.739 7.308 11.114 o 1 4 12 91.905 115.933 6.197 34.245 o 1 4 13 288.783 251.588 8.251 10.549 o 1 4 14 179.372 179.594 7.882 17.609 o 1 4 15 269.085 295.395 10.919 10.174 o 1 4 16 33.961 41.453 5.780 91.095 o 1 4 17 219.336 225.281 9.490 13.538 o 1 4 18 7.845 2.977 5.605 307.237 o 1 4 19 27.342 33.881 5.964 107.534 o 1 4 20 40.063 29.474 7.820 79.646 o 1 4 21 8.252 -7.686 10.195 139.797 o 1 4 22 6.354 -5.720 8.660 191.446 o 1 5 0 744.885 649.575 10.974 2.901 o 1 5 1 2168.460 2432.380 26.044 0.442 o 1 5 2 1913.570 2895.620 29.645 0.445 o 1 5 3 260.995 196.508 3.718 13.041 o 1 5 4 5442.640 6026.100 54.311 0.083 o 1 5 5 3065.440 2595.020 26.875 0.283 o 1 5 6 10520.500 11887.700 125.108 0.023 o 1 5 7 337.585 410.487 7.317 7.554 o 1 5 8 6133.880 6420.170 87.503 0.068 o 1 5 9 438.718 491.897 9.166 5.489 o 1 5 10 2936.730 2859.270 38.116 0.279 o 1 5 11 101.483 138.238 6.579 29.641 o 1 5 12 1608.190 1424.850 21.734 0.842 o 1 5 13 16.671 16.842 4.242 196.950 o 1 5 14 544.470 551.525 12.696 4.201 o 1 5 15 486.975 429.389 11.563 5.232 o 1 5 16 1125.380 1174.970 21.795 1.370 o 1 5 17 0.672 -2.359 4.933 678.980 o 1 5 18 1284.200 1360.370 27.277 1.086 o 1 5 19 21.828 8.893 7.770 130.674 o 1 5 20 705.344 738.822 21.973 2.721 o 1 5 21 0.862 -8.346 8.599 233.188 o 1 5 22 416.719 379.007 28.290 5.126 o 1 6 1 3618.300 2856.770 28.127 0.218 o 1 6 2 18.879 17.271 1.793 215.064 o 1 6 4 248.490 194.815 4.392 13.608 o 1 6 5 293.189 461.686 7.563 7.896 o 1 6 6 987.420 943.861 12.616 1.806 o 1 6 7 17.767 9.537 2.017 258.231 o 1 6 8 5.341 7.289 2.385 569.932 o 1 6 9 12.425 18.242 2.786 255.314 o 1 6 10 11.832 18.045 3.592 244.403 o 1 6 11 87.261 106.002 5.106 37.628 o 1 6 12 748.999 761.787 15.043 2.634 o 1 6 13 236.896 223.496 10.206 12.663 o 1 6 14 12.646 4.045 4.474 287.449 o 1 6 15 136.812 164.801 8.434 21.838 o 1 6 16 91.739 82.338 7.233 37.609 o 1 6 17 178.442 192.973 12.214 15.860 o 1 6 18 8.233 -9.182 8.655 181.156 o 1 6 19 111.820 88.639 10.224 29.249 o 1 6 20 45.174 60.856 10.491 52.645 o 1 6 21 1.313 -4.424 8.359 242.056 o 1 7 0 454.496 476.023 10.886 5.349 o 1 7 1 460.404 444.768 7.030 5.569 o 1 7 3 0.244 13.323 2.295 716.150 o 1 7 4 6625.260 7437.710 77.484 0.056 o 1 7 5 0.338 18.064 2.167 567.978 o 1 7 6 5708.100 5456.460 57.863 0.083 o 1 7 7 110.284 112.525 4.276 31.757 o 1 7 8 918.389 908.040 12.822 1.984 o 1 7 9 301.021 323.767 7.001 9.291 o 1 7 10 1847.400 1804.620 24.804 0.631 o 1 7 11 8.849 5.272 4.155 356.146 o 1 7 12 914.387 939.784 17.908 1.925 o 1 7 13 1079.100 991.131 18.811 1.576 o 1 7 14 403.261 461.714 12.185 5.953 o 1 7 15 6.988 -2.899 4.715 423.372 o 1 7 16 1205.300 1202.470 26.105 1.242 o 1 7 17 79.088 116.198 9.837 33.409 o 1 7 18 1212.660 1097.840 26.929 1.287 o 1 7 19 0.662 7.452 8.982 191.285 o 1 7 20 781.895 792.807 23.407 2.370 o 1 7 21 0.462 3.672 8.912 207.299 o 1 8 1 1172.670 930.253 15.029 1.499 o 1 8 2 290.251 302.899 6.761 9.876 o 1 8 3 37.820 51.743 4.198 85.655 o 1 8 4 48.672 79.101 3.734 62.886 o 1 8 5 139.722 234.784 5.673 19.133 o 1 8 6 18.023 58.204 3.776 116.397 o 1 8 7 694.306 686.773 10.586 3.037 o 1 8 8 82.481 109.193 4.719 38.867 o 1 8 9 31.106 68.479 3.518 85.665 o 1 8 10 375.910 421.680 8.946 6.751 o 1 8 11 330.661 297.945 9.025 8.740 o 1 8 12 165.735 196.581 8.672 17.760 o 1 8 13 293.611 330.263 11.617 8.991 o 1 8 14 2.751 -3.304 4.881 563.639 o 1 8 15 37.588 42.221 5.799 85.528 o 1 8 16 172.008 143.766 11.467 18.258 o 1 8 17 19.225 24.974 7.580 119.096 o 1 8 18 61.521 57.353 8.824 50.364 o 1 8 19 3.297 5.223 8.571 197.404 o 1 8 20 0.094 -3.315 8.739 232.427 o 1 9 0 852.714 593.455 20.747 2.495 o 1 9 1 1319.420 1164.540 20.957 1.165 o 1 9 2 4095.470 3806.090 49.422 0.157 o 1 9 3 130.961 180.533 6.194 22.522 o 1 9 4 3679.950 3902.250 48.639 0.176 o 1 9 5 17.178 48.803 3.725 131.247 o 1 9 6 5120.100 5286.370 61.401 0.097 o 1 9 7 6.121 11.660 3.208 401.311 o 1 9 8 6437.530 6119.270 66.056 0.067 o 1 9 9 18.138 38.775 3.850 143.207 o 1 9 10 1239.110 1227.620 16.137 1.229 o 1 9 11 798.452 760.403 13.071 2.495 o 1 9 12 343.946 405.404 10.064 7.338 o 1 9 13 12.338 15.731 4.854 218.200 o 1 9 14 869.476 993.159 22.303 1.926 o 1 9 15 211.694 250.114 10.884 13.040 o 1 9 16 1162.000 1166.860 27.059 1.305 o 1 9 17 0.761 -10.274 6.949 353.144 o 1 9 18 1172.890 1142.060 26.553 1.309 o 1 9 19 35.206 63.069 10.039 59.223 o 1 9 20 746.039 713.566 22.637 2.614 o 1 10 1 396.957 368.091 11.882 6.682 o 1 10 2 223.913 240.834 11.539 12.583 o 1 10 3 243.951 334.764 9.129 10.555 o 1 10 4 477.110 552.753 11.633 4.749 o 1 10 5 89.894 101.433 5.142 37.500 o 1 10 6 20.315 17.505 3.117 189.619 o 1 10 7 1153.140 1074.660 17.396 1.417 o 1 10 8 26.565 38.916 4.185 116.491 o 1 10 9 1032.660 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643.330 13.439 3.326 o 2 11 5 236.083 237.600 10.895 12.282 o 2 11 6 130.752 158.151 8.727 22.730 o 2 11 7 2289.920 2258.930 32.727 0.430 o 2 11 8 23.822 43.415 4.985 112.213 o 2 11 9 246.051 216.613 8.842 12.657 o 2 11 10 62.706 105.611 7.663 42.450 o 2 11 11 631.932 546.280 14.314 3.630 o 2 11 12 0.925 -3.908 5.213 597.871 o 2 11 13 109.455 107.620 8.688 29.393 o 2 11 14 29.494 41.180 7.026 90.307 o 2 11 15 3.283 2.809 7.425 260.372 o 2 11 16 8.867 17.355 7.883 158.399 o 2 11 17 21.548 18.777 7.474 122.294 o 2 11 18 7.276 -8.711 8.573 189.140 o 2 11 19 99.724 106.628 10.760 29.250 o 2 12 0 3053.340 3120.140 64.840 0.244 o 2 12 1 12.401 13.447 4.633 233.202 o 2 12 2 2344.070 2541.790 36.523 0.389 o 2 12 4 1932.380 1914.080 29.212 0.576 o 2 12 5 125.082 142.600 9.333 23.996 o 2 12 6 523.010 681.416 18.036 3.775 o 2 12 7 114.359 126.473 8.404 27.220 o 2 12 8 2915.950 3027.000 44.888 0.270 o 2 12 9 70.326 114.146 6.522 40.070 o 2 12 10 368.072 295.096 10.011 7.908 o 2 12 11 40.398 54.789 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9.001 106.718 o 7 10 11 2.209 15.530 6.351 259.130 o 7 10 12 31.641 37.364 8.253 82.185 o 7 10 13 46.147 49.156 10.418 55.457 o 7 10 14 0.106 9.313 8.410 211.483 o 7 10 15 4.511 1.241 10.143 151.677 o 7 11 0 590.788 641.487 25.071 3.311 o 7 11 1 396.969 361.893 13.814 6.604 o 7 11 2 1344.380 1424.990 26.853 1.011 o 7 11 3 7.677 24.005 6.326 184.465 o 7 11 4 1837.730 1703.560 28.543 0.651 o 7 11 5 0.175 12.248 5.810 344.950 o 7 11 6 1031.230 964.278 19.455 1.672 o 7 11 7 10.492 12.398 5.436 230.232 o 7 11 8 1001.020 1047.170 26.890 1.602 o 7 11 9 7.295 10.254 6.263 238.520 o 7 11 10 790.521 833.075 20.732 2.326 o 7 11 11 0.004 5.113 6.278 381.788 o 7 11 12 455.750 498.671 16.619 4.990 o 7 11 13 1.551 0.321 10.105 166.544 o 7 11 14 193.085 186.664 13.801 14.676 o 7 12 1 313.756 324.369 15.001 8.239 o 7 12 2 0.045 16.483 7.627 217.947 o 7 12 3 24.530 49.219 7.963 85.481 o 7 12 4 8.977 34.267 6.927 144.309 o 7 12 5 46.758 58.109 7.292 63.133 o 7 12 6 29.315 38.527 6.904 93.302 o 7 12 7 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24.301 7.859 149.994 o 8 3 13 497.866 524.658 20.313 4.373 o 8 3 14 16.112 20.375 10.332 97.456 o 8 3 15 13.097 5.594 10.719 111.043 o 8 3 16 3.632 -9.972 10.459 148.845 o 8 3 17 0.019 14.163 11.412 118.418 o 8 4 0 2278.230 2348.660 39.514 0.418 o 8 4 1 0.208 6.763 4.164 647.700 o 8 4 2 253.448 263.527 8.848 11.460 o 8 4 3 165.044 158.547 7.432 19.768 o 8 4 4 1139.780 1251.220 18.973 1.318 o 8 4 5 323.969 365.469 10.714 8.031 o 8 4 6 825.054 848.523 15.132 2.270 o 8 4 7 331.611 282.687 12.200 8.605 o 8 4 8 264.862 226.263 12.024 11.233 o 8 4 9 1.957 0.448 5.077 557.642 o 8 4 10 639.312 626.621 21.376 3.224 o 8 4 11 47.338 36.128 8.008 68.544 o 8 4 12 761.871 776.852 21.898 2.475 o 8 4 13 69.532 42.413 8.425 51.101 o 8 4 14 741.502 761.712 26.945 2.475 o 8 4 15 3.856 21.366 10.668 114.631 o 8 4 16 703.687 764.788 28.209 2.561 o 8 4 17 1.215 -15.889 16.791 62.416 o 8 5 1 1138.090 1261.710 20.405 1.308 o 8 5 2 165.250 162.352 7.677 19.500 o 8 5 3 956.235 881.081 15.211 1.917 o 8 5 4 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53.826 79.690 7.471 51.917 o 9 8 8 18.985 37.311 6.542 116.643 o 9 8 9 12.716 17.247 7.601 149.461 o 9 8 10 2.548 15.203 7.116 223.931 o 9 8 11 31.100 42.883 9.513 72.416 o 9 8 12 5.264 -4.564 8.199 216.801 o 9 8 13 0.335 5.738 9.314 185.892 o 9 9 0 512.373 451.848 34.524 3.786 o 9 9 1 12.343 14.470 6.037 192.185 o 9 9 2 630.946 655.111 15.537 3.326 o 9 9 3 34.263 35.240 6.529 90.847 o 9 9 4 520.497 557.163 13.964 4.319 o 9 9 5 129.501 136.356 8.317 24.422 o 9 9 6 547.099 557.713 14.440 4.115 o 9 9 7 4.694 3.143 6.130 321.745 o 9 9 8 624.797 626.412 16.328 3.412 o 9 9 9 5.274 0.530 7.629 240.986 o 9 9 10 435.481 420.767 17.511 5.527 o 9 9 11 7.038 12.494 7.698 183.232 o 9 9 12 236.310 215.067 14.138 12.035 o 9 9 13 10.243 22.015 9.253 121.375 o 9 10 1 9.303 11.120 7.517 179.885 o 9 10 2 5.049 7.107 6.345 275.207 o 9 10 3 179.977 182.843 9.813 16.881 o 9 10 4 0.255 -7.361 5.546 565.820 o 9 10 5 41.948 33.568 6.984 79.690 o 9 10 6 5.234 2.895 5.920 329.731 o 9 10 7 148.987 130.001 8.388 22.429 o 9 10 8 0.409 -7.242 6.559 403.202 o 9 10 9 54.834 48.700 8.237 57.891 o 9 10 10 4.286 -0.440 7.585 255.653 o 9 10 11 23.293 29.928 8.717 94.868 o 9 10 12 0.048 19.634 9.734 145.005 o 9 11 0 403.613 489.280 24.889 5.017 o 9 11 1 83.994 86.620 8.883 37.066 o 9 11 2 505.975 476.202 15.251 4.707 o 9 11 3 1.839 2.344 6.962 312.551 o 9 11 4 357.091 364.327 12.724 7.282 o 9 11 5 18.283 15.272 6.746 147.948 o 9 11 6 362.315 366.328 12.960 7.161 o 9 11 7 8.876 0.094 7.234 229.186 o 9 11 8 415.245 402.498 14.165 6.065 o 9 11 9 1.275 -6.803 6.994 339.162 o 9 11 10 190.718 195.501 12.717 14.920 o 9 11 11 0.296 16.397 8.409 187.747 o 9 12 1 18.992 15.500 8.122 124.309 o 9 12 2 77.712 61.338 8.666 43.267 o 9 12 3 81.426 66.502 8.557 41.303 o 9 12 4 5.442 5.001 8.032 204.520 o 9 12 5 135.992 122.277 9.106 24.038 o 9 12 6 5.755 -6.191 6.446 307.750 o 9 12 7 101.738 75.364 9.625 33.172 o 9 12 8 0.176 -5.649 6.535 412.306 o 9 12 9 22.432 8.332 7.757 129.953 o 9 13 0 127.146 132.832 16.620 19.349 o 9 13 1 15.606 0.863 8.424 152.377 o 9 13 2 215.922 232.393 13.626 12.615 o 9 13 3 56.104 41.606 9.710 54.511 o 9 13 4 301.972 277.001 16.799 8.758 o 9 13 5 32.151 10.040 9.534 89.333 o 9 13 6 240.392 198.736 10.899 12.906 o 9 13 7 22.098 24.294 7.184 117.724 o 9 14 1 119.625 111.471 11.439 25.221 o 9 14 2 4.669 -8.807 9.112 185.035 o 9 14 3 4.978 6.046 9.721 151.912 o 9 14 4 24.653 9.155 9.361 103.354 o 9 14 5 58.027 76.995 9.459 46.118 o 10 0 0 220.676 236.227 27.472 8.855 o 10 0 2 20.896 34.387 9.852 85.498 o 10 0 4 27.682 18.457 9.825 87.207 o 10 0 6 145.487 150.616 17.403 16.905 o 10 0 8 21.871 10.889 10.850 90.537 o 10 0 10 612.574 608.372 29.016 3.162 o 10 0 12 377.860 413.322 24.333 5.677 o 10 0 14 222.968 266.033 21.988 9.786 o 10 1 1 2.232 -7.939 6.080 411.544 o 10 1 2 33.491 37.922 7.425 84.690 o 10 1 3 46.584 55.042 7.832 62.541 o 10 1 4 73.552 63.373 7.886 45.890 o 10 1 5 0.906 -0.217 6.289 423.000 o 10 1 6 0.156 4.650 6.533 358.385 o 10 1 7 295.059 313.992 13.670 8.914 o 10 1 8 10.087 5.033 7.397 196.391 o 10 1 9 1.667 2.743 7.531 272.690 o 10 1 10 5.135 4.047 7.644 226.133 o 10 1 11 17.400 8.828 7.303 153.394 o 10 1 12 9.383 26.090 9.839 110.356 o 10 1 13 0.004 -5.150 7.148 348.499 o 10 1 14 13.255 18.595 9.207 118.963 o 10 2 0 663.401 697.919 28.601 2.800 o 10 2 1 22.600 21.850 7.879 111.594 o 10 2 2 665.375 686.641 18.567 3.040 o 10 2 3 23.647 37.024 12.377 64.354 o 10 2 4 683.831 719.554 19.344 2.884 o 10 2 5 20.340 19.491 7.267 127.173 o 10 2 6 70.894 67.573 8.005 45.889 o 10 2 7 11.608 -5.109 7.488 199.742 o 10 2 8 209.747 214.245 12.835 13.473 o 10 2 9 207.437 211.534 12.780 13.657 o 10 2 10 303.158 299.136 12.444 9.043 o 10 2 11 38.482 33.975 8.432 75.585 o 10 2 12 475.997 497.802 17.232 4.788 o 10 2 13 5.018 2.356 7.854 224.695 o 10 2 14 240.303 242.366 14.614 11.301 o 10 3 1 11.950 32.407 7.193 133.681 o 10 3 2 0.534 28.930 7.574 177.630 o 10 3 3 7.621 23.052 7.724 155.363 o 10 3 4 3.341 18.254 7.002 210.521 o 10 3 5 59.840 44.105 9.070 53.831 o 10 3 6 40.922 37.713 7.442 76.315 o 10 3 7 40.812 61.308 7.178 66.828 o 10 3 8 6.271 18.772 9.587 130.274 o 10 3 9 1.976 12.326 6.225 287.836 o 10 3 10 16.215 18.730 7.486 137.103 o 10 3 11 43.100 36.955 7.753 73.067 o 10 3 12 2.638 6.331 14.738 76.221 o 10 3 13 0.444 -2.966 8.500 242.314 o 10 3 14 0.177 -5.714 8.787 229.188 o 10 4 0 712.750 779.221 31.068 2.452 o 10 4 1 38.265 53.643 7.648 70.339 o 10 4 2 1538.760 1533.700 32.008 0.829 o 10 4 3 15.813 31.799 8.456 108.873 o 10 4 4 945.298 991.301 21.573 1.785 o 10 4 5 2.159 7.048 7.216 261.228 o 10 4 6 639.680 683.602 19.211 3.144 o 10 4 7 140.429 176.533 8.796 20.718 o 10 4 8 733.139 735.633 15.941 2.724 o 10 4 9 0.216 5.014 6.311 374.702 o 10 4 10 410.467 407.261 15.389 6.021 o 10 4 11 0.046 -1.122 8.289 258.769 o 10 4 12 304.216 303.594 19.590 8.039 o 10 4 13 5.586 7.797 9.612 149.195 o 10 5 1 0.593 3.999 5.911 421.416 o 10 5 2 20.130 27.606 6.025 131.889 o 10 5 3 97.228 96.749 7.884 33.701 o 10 5 4 41.153 59.220 7.879 64.807 o 10 5 5 43.844 46.879 8.744 64.038 o 10 5 6 13.140 19.371 6.420 166.503 o 10 5 7 0.930 -0.019 6.696 375.257 o 10 5 8 18.179 26.317 7.236 124.260 o 10 5 9 21.769 35.691 7.086 107.244 o 10 5 10 2.533 6.851 8.126 214.740 o 10 5 11 3.469 6.817 8.273 202.467 o 10 5 12 7.953 4.799 14.081 78.200 o 10 5 13 31.277 38.418 10.209 70.308 o 10 6 0 494.841 562.218 22.863 4.151 o 10 6 1 48.429 49.632 7.129 65.600 o 10 6 2 299.861 311.285 14.190 8.771 o 10 6 3 1.424 2.035 6.154 397.765 o 10 6 4 857.647 778.048 17.807 2.252 o 10 6 5 0.836 -4.076 6.173 440.145 o 10 6 6 1262.770 1336.440 25.887 1.120 o 10 6 7 11.351 32.199 7.573 130.234 o 10 6 8 663.210 669.553 17.179 3.112 o 10 6 9 28.858 38.781 7.318 90.980 o 10 6 10 455.122 486.927 16.579 5.052 o 10 6 11 8.738 3.136 10.986 118.701 o 10 6 12 203.952 164.504 12.691 15.052 o 10 7 1 87.930 110.168 9.013 33.087 o 10 7 2 5.601 12.539 7.053 213.035 o 10 7 3 47.207 34.672 7.456 71.649 o 10 7 4 9.514 17.508 6.965 176.486 o 10 7 5 9.358 -2.355 7.724 206.413 o 10 7 6 6.684 6.812 6.727 240.756 o 10 7 7 1.943 11.556 7.417 231.482 o 10 7 8 24.506 20.528 6.634 122.610 o 10 7 9 1.799 9.067 7.686 231.163 o 10 7 10 9.581 9.894 8.076 166.848 o 10 7 11 49.190 49.494 9.667 56.299 o 10 7 12 16.582 31.108 9.451 97.498 o 10 8 0 389.594 444.138 23.356 5.476 o 10 8 1 0.063 2.197 7.371 309.136 o 10 8 2 409.068 408.894 15.287 6.034 o 10 8 3 54.385 100.079 9.750 42.585 o 10 8 4 574.060 576.664 16.984 3.812 o 10 8 5 37.240 32.266 7.083 85.548 o 10 8 6 622.624 630.854 16.691 3.404 o 10 8 7 0.201 3.716 6.400 380.745 o 10 8 8 673.097 717.237 17.843 2.958 o 10 8 9 0.916 -6.513 6.515 395.570 o 10 8 10 224.765 253.119 13.166 11.968 o 10 8 11 2.364 4.197 8.415 213.430 o 10 9 1 65.725 62.608 9.258 46.368 o 10 9 2 11.248 22.108 7.992 139.053 o 10 9 3 0.237 3.616 6.637 357.476 o 10 9 4 10.928 21.236 7.542 149.819 o 10 9 5 1.406 -16.709 6.608 373.909 o 10 9 6 5.458 -5.270 6.925 280.776 o 10 9 7 99.245 48.386 7.964 39.439 o 10 9 8 2.147 10.002 7.234 245.258 o 10 9 9 84.278 63.126 9.892 38.734 o 10 9 10 3.436 11.965 9.133 161.599 o 10 10 0 264.820 229.579 30.604 7.466 o 10 10 1 106.380 126.134 11.185 26.253 o 10 10 2 370.070 381.760 14.427 6.809 o 10 10 3 0.174 -9.704 7.382 323.919 o 10 10 4 205.708 187.252 10.881 14.869 o 10 10 5 7.619 -2.502 9.091 170.780 o 10 10 6 289.901 312.380 13.415 9.086 o 10 10 7 0.043 -8.455 7.657 303.163 o 10 10 8 304.147 275.154 12.621 9.290 o 10 10 9 8.291 25.206 8.676 131.587 o 10 11 1 8.479 9.236 9.486 139.829 o 10 11 2 2.146 -8.146 8.020 253.037 o 10 11 3 146.702 159.570 11.300 19.765 o 10 11 4 10.218 8.044 8.251 163.730 o 10 11 5 166.711 170.909 11.007 17.823 o 10 11 6 0.138 -9.225 8.302 256.950 o 10 11 7 120.314 121.675 10.142 25.446 o 10 12 0 303.435 345.099 25.265 6.916 o 10 12 1 18.605 36.359 8.358 100.526 o 10 12 2 119.574 121.980 13.277 23.096 o 10 12 3 7.976 6.492 9.600 143.462 o 10 12 4 231.098 213.162 13.264 12.476 o 10 12 5 0.677 -8.031 7.772 285.827 o 10 13 1 16.423 -2.948 11.116 104.402 o 10 13 2 8.786 10.782 12.127 94.952 o 11 0 2 13.605 36.914 12.740 69.722 o 11 0 4 7.635 19.298 10.935 105.312 o 11 0 6 159.714 169.401 17.424 15.491 o 11 0 8 15.824 16.484 12.257 81.092 o 11 0 10 49.460 41.195 14.211 43.182 o 11 0 12 14.162 -5.929 13.426 80.688 o 11 1 0 1324.050 1447.920 44.372 0.950 o 11 1 1 42.997 50.498 8.680 63.593 o 11 1 2 646.412 698.084 19.490 3.078 o 11 1 3 4.957 2.911 9.466 165.204 o 11 1 4 486.773 524.991 18.056 4.553 o 11 1 5 16.651 17.859 7.988 129.360 o 11 1 6 170.414 135.509 10.860 18.976 o 11 1 7 24.623 32.424 9.292 86.502 o 11 1 8 73.837 59.800 9.650 43.024 o 11 1 9 2.755 9.941 8.986 173.435 o 11 1 10 608.309 706.650 22.717 3.150 o 11 1 11 25.072 18.083 9.329 95.601 o 11 2 1 88.632 66.915 9.257 37.961 o 11 2 2 0.537 7.050 7.367 270.807 o 11 2 3 2.690 6.790 7.540 240.331 o 11 2 4 4.471 14.401 8.035 182.044 o 11 2 5 75.233 22.854 8.848 52.010 o 11 2 6 0.008 6.048 8.222 233.816 o 11 2 7 51.947 29.515 8.862 63.984 o 11 2 8 23.173 25.281 8.204 103.736 o 11 2 9 1.620 5.690 8.504 209.643 o 11 2 10 3.297 9.908 8.820 175.911 o 11 2 11 7.591 17.675 9.802 124.437 o 11 3 0 8.253 -10.822 11.124 120.987 o 11 3 1 10.918 13.930 8.134 151.647 o 11 3 2 290.651 283.413 15.342 9.155 o 11 3 3 176.863 167.954 11.581 16.989 o 11 3 4 252.862 255.624 13.581 10.871 o 11 3 5 0.760 4.825 7.744 258.344 o 11 3 6 150.796 130.175 10.833 20.988 o 11 3 7 25.634 34.011 8.792 88.021 o 11 3 8 294.510 311.094 13.646 8.963 o 11 3 9 1.072 -5.258 7.729 283.773 o 11 3 10 144.811 110.962 12.582 21.497 o 11 3 11 2.471 -1.244 9.864 170.783 o 11 4 1 23.788 20.960 9.119 97.373 o 11 4 2 6.028 -3.042 7.529 241.401 o 11 4 3 32.479 37.467 8.497 79.677 o 11 4 4 0.444 11.333 8.520 198.076 o 11 4 5 17.586 33.407 8.358 104.970 o 11 4 6 65.242 89.758 10.245 39.808 o 11 4 7 7.369 10.662 8.566 162.463 o 11 4 8 10.945 15.880 7.635 158.305 o 11 4 9 0.038 4.745 8.089 246.499 o 11 4 10 4.988 -3.676 8.116 222.598 o 11 4 11 2.873 -0.716 8.209 235.839 o 11 5 0 118.283 102.825 16.645 21.425 o 11 5 1 0.427 7.325 9.079 189.473 o 11 5 2 281.995 264.530 13.956 9.821 o 11 5 3 3.340 -0.099 8.031 240.849 o 11 5 4 475.230 518.908 18.694 4.641 o 11 5 5 0.508 5.761 8.061 238.867 o 11 5 6 382.079 448.356 17.857 5.950 o 11 5 7 0.527 3.781 8.452 227.549 o 11 5 8 253.759 270.522 17.881 9.818 o 11 5 9 0.026 1.339 7.594 298.676 o 11 5 10 145.048 111.199 10.600 22.719 o 11 6 1 12.117 18.075 8.618 131.819 o 11 6 2 0.365 11.886 7.478 241.283 o 11 6 3 3.537 -2.866 8.192 230.947 o 11 6 4 2.225 13.191 8.159 194.311 o 11 6 5 1.052 10.715 8.501 196.890 o 11 6 6 39.557 63.007 9.336 59.200 o 11 6 7 19.351 12.907 8.820 116.924 o 11 6 8 7.831 29.942 9.007 121.324 o 11 6 9 9.836 -14.904 7.705 203.863 o 11 6 10 8.766 3.911 7.923 190.841 o 11 7 0 449.703 471.264 34.729 4.074 o 11 7 1 1.452 5.249 8.610 207.899 o 11 7 2 331.078 347.303 14.034 7.781 o 11 7 3 36.736 60.490 7.693 68.532 o 11 7 4 225.011 263.041 12.176 11.974 o 11 7 5 0.001 5.164 7.861 257.776 o 11 7 6 490.545 500.380 18.450 4.603 o 11 7 7 0.014 1.061 8.649 233.285 o 11 7 8 460.779 452.939 15.416 5.215 o 11 7 9 11.533 11.812 7.787 160.987 o 11 8 1 219.770 248.361 13.226 12.237 o 11 8 2 3.240 9.343 8.159 199.996 o 11 8 3 32.881 52.502 9.173 68.469 o 11 8 4 7.977 28.678 8.127 136.680 o 11 8 5 26.691 30.812 10.344 77.306 o 11 8 6 9.423 24.048 8.067 140.480 o 11 8 7 76.503 85.393 10.778 36.371 o 11 8 8 3.130 12.116 8.314 186.950 o 11 9 0 123.941 181.103 17.325 17.361 o 11 9 1 6.349 15.732 8.357 161.226 o 11 9 2 201.097 180.218 13.526 14.518 o 11 9 3 3.808 -8.560 7.580 261.019 o 11 9 4 228.368 192.918 11.616 13.412 o 11 9 5 10.556 22.631 8.943 124.608 o 11 9 6 322.554 317.023 19.583 7.587 o 11 10 1 22.319 15.420 8.914 106.950 o 11 10 2 3.298 -5.806 8.620 212.966 o 11 10 3 56.434 64.393 9.617 49.052 o 11 10 4 5.041 12.807 8.720 163.913 o 12 0 0 267.841 293.762 32.216 6.699 o 12 0 2 413.310 384.578 27.005 5.239 o 12 0 4 449.686 430.576 32.484 4.354 o 12 0 6 80.086 86.987 15.219 28.714 o 12 0 8 147.276 115.975 18.627 17.183 o 12 1 1 0.329 -15.750 10.965 146.993 o 12 1 2 3.180 17.032 8.396 171.525 o 12 1 3 47.982 42.029 9.145 61.257 o 12 1 4 1.218 4.499 8.450 219.304 o 12 1 5 13.190 21.611 9.170 116.184 o 12 1 6 2.988 0.999 8.590 212.908 o 12 1 7 0.072 -3.213 10.371 165.269 o 12 1 8 14.700 10.335 9.857 115.480 o 12 2 0 496.709 615.995 29.962 3.660 o 12 2 1 2.169 21.601 9.321 143.741 o 12 2 2 483.512 537.185 18.438 4.514 o 12 2 3 60.491 49.636 9.631 50.528 o 12 2 4 277.772 296.178 15.198 9.335 o 12 2 5 0.065 3.464 8.425 234.151 o 12 2 6 202.636 219.242 14.284 13.285 o 12 2 7 38.087 35.476 10.008 67.007 o 12 2 8 192.041 194.845 14.290 14.357 o 12 3 1 1.104 4.078 9.273 187.714 o 12 3 2 0.006 9.006 8.840 195.890 o 12 3 3 4.700 3.077 8.349 203.766 o 12 3 4 8.517 26.757 9.078 122.473 o 12 3 5 0.523 -6.719 11.929 123.888 o 12 3 6 0.025 31.546 9.204 137.069 o 12 3 7 3.473 11.924 9.503 152.028 o 12 4 0 191.463 219.573 23.775 10.774 o 12 4 1 0.005 -4.661 13.890 92.315 o 12 4 2 170.739 194.766 13.559 15.779 o 12 4 3 0.002 2.507 8.494 235.300 o 12 4 4 178.322 162.434 14.037 16.106 o 12 4 5 25.498 56.971 9.887 69.121 o 12 4 6 183.656 190.360 12.971 15.371 o 12 4 7 2.317 3.124 8.732 204.186 o 12 5 1 0.792 -0.258 10.297 164.514 o 12 5 2 16.450 14.153 9.937 106.930 o 12 5 3 11.953 2.640 8.459 162.716 o 12 5 4 15.917 17.457 9.493 110.465 o 12 5 5 0.083 -9.404 8.538 243.528 o 12 5 6 12.408 12.750 9.145 129.499 o 12 6 0 52.325 30.275 16.019 38.816 o 12 6 1 0.092 -12.816 10.471 162.073 o 12 6 2 24.014 7.189 9.880 100.346 o 12 6 3 19.513 17.244 10.441 93.516 o 12 6 4 68.065 55.316 11.838 41.020 o 12 6 5 1.355 -7.270 8.916 213.776 o 12 7 1 9.791 14.248 10.849 107.183 o 12 7 2 1.127 -3.653 10.583 154.633 o 12 7 3 3.056 -5.949 9.808 169.889 o ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 x+1/2,-y,-z+1/2 3 -x,y+1/2,-z+1/2 4 -x+1/2,-y+1/2,z 5 -x,-y,-z 6 -x-1/2,y,z-1/2 7 x,-y-1/2,z-1/2 8 x-1/2,y-1/2,-z 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_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_group Ni1 Ni 0.25 0.25 0.75110(2) 0.0334(2) Uani 1.000000 2 S T P . O1 O 0.4087(3) 0.17769(16) 0.74096(13) 0.0525(6) Uani 1.000000 1 . . . . N1 N 0.1690(3) 0.17819(16) 0.66943(14) 0.0439(7) Uani 1.000000 1 . . . . N2 N 0.3392(3) 0.32078(17) 0.82897(14) 0.0455(7) Uani 1.000000 1 . . . . C6 C 0.1788(4) 0.0987(2) 0.67161(19) 0.0517(9) Uani 1.000000 1 . . . . H6 H 0.2231(4) 0.0748(2) 0.71078(19) 0.0621(11) Uiso 1.000000 1 R . . . C1 C 0.1099(4) 0.2094(2) 0.61238(19) 0.0561(10) Uani 1.000000 1 . . . . H1 H 0.1024(4) 0.2657(2) 0.61003(19) 0.0674(12) Uiso 1.000000 1 R . . . C2 C 0.0588(4) 0.1656(3) 0.5567(2) 0.0638(11) Uani 1.000000 1 . . . . H2 H 0.0197(4) 0.1914(3) 0.5167(2) 0.0766(13) Uiso 1.000000 1 R . . . O2 O 0.5165(18) 0.1388(8) 0.8407(7) 0.098(3) Uani 0.617(12) 1 D U . 1 C12 C 0.2779(4) 0.3514(3) 0.8855(2) 0.0669(12) Uani 1.000000 1 . . . . H12 H 0.1908(4) 0.3381(3) 0.8922(2) 0.0803(14) Uiso 1.000000 1 R . . . C5 C 0.1264(4) 0.0499(2) 0.6186(2) 0.0600(10) Uani 1.000000 1 . . . . H5 H 0.1322(4) -0.0064(2) 0.6226(2) 0.0720(12) Uiso 1.000000 1 R . . . C3 C 0.0651(4) 0.0849(3) 0.5595(2) 0.0588(10) Uani 1.000000 1 . . . . C13 C 0.5019(4) 0.1513(3) 0.7737(2) 0.0606(10) Uani 1.000000 1 D . . . C11 C 0.3346(5) 0.4010(3) 0.9340(3) 0.0868(16) Uani 1.000000 1 . . . . H11 H 0.2864(5) 0.4216(3) 0.9732(3) 0.1042(19) Uiso 1.000000 1 R . . . C14 C 0.6066(15) 0.1189(16) 0.7284(9) 0.063(5) Uani 0.617(12) 1 D U . 1 C7 C 0.4630(4) 0.3389(3) 0.8225(2) 0.0619(11) Uani 1.000000 1 . . . . H7 H 0.5098(4) 0.3160(3) 0.7837(2) 0.0743(13) Uiso 1.000000 1 R . . . C8 C 0.5254(4) 0.3891(3) 0.8696(3) 0.0746(13) Uani 1.000000 1 . . . . H8 H 0.6129(4) 0.4011(3) 0.8624(3) 0.0895(16) Uiso 1.000000 1 R . . . C9 C 0.4609(4) 0.4218(3) 0.9271(3) 0.0768(14) Uani 1.000000 1 . . . . C4 C 0.0073(5) 0.0380(3) 0.4997(2) 0.0684(12) Uani 1.000000 1 . . . . H4 H -0.0209(5) 0.0662(3) 0.4581(2) 0.0820(15) Uiso 1.000000 1 R . . . O3 O 0.7091(9) 0.0802(7) 0.7552(5) 0.101(2) Uani 0.617(12) 1 D U . 1 C10 C 0.5274(5) 0.4774(4) 0.9755(3) 0.0886(16) Uani 1.000000 1 . . . . H10 H 0.6173(5) 0.4811(4) 0.9710(3) 0.106(2) Uiso 1.000000 1 R . . . C17 C 0.7893(12) 0.0633(7) 0.7012(8) 0.091(3) Uani 0.617(12) 1 D U . 1 H17 H 0.8744(12) 0.0451(7) 0.7071(8) 0.109(4) Uiso 0.617(12) 1 R . . 1 C15 C 0.6119(11) 0.1088(8) 0.6583(6) 0.098(3) Uani 0.617(12) 1 D U . 1 H15 H 0.5470(11) 0.1212(8) 0.6244(6) 0.118(3) Uiso 0.617(12) 1 R . . 1 C16 C 0.7359(12) 0.0750(9) 0.6423(7) 0.112(3) Uani 0.617(12) 1 D U . 1 H16 H 0.7697(12) 0.0640(9) 0.5957(7) 0.135(4) Uiso 0.617(12) 1 R . . 1 C18 C 0.75 0.25 0.9562(11) 0.107(5) Uani 0.500000 2 S TU P . N3 N 0.7010(11) 0.1699(8) 0.9446(6) 0.109(3) Uani 0.250000 1 . . . 4 C15A C 0.6367(16) 0.1512(13) 0.6576(9) 0.098(3) Uani 0.383(12) 1 D U . 2 H15A H 0.5850(16) 0.1820(13) 0.6260(9) 0.118(3) Uiso 0.383(12) 1 R . . 2 C14A C 0.611(2) 0.132(3) 0.7257(14) 0.061(8) Uani 0.383(12) 1 D U . 2 O3A O 0.7253(15) 0.1139(11) 0.7600(9) 0.101(2) Uani 0.383(12) 1 D U . 2 C16A C 0.7597(18) 0.1162(14) 0.6411(11) 0.112(3) Uani 0.383(12) 1 D U . 2 H16A H 0.8012(18) 0.1131(14) 0.5955(11) 0.135(4) Uiso 0.383(12) 1 R . . 2 C17A C 0.798(2) 0.0911(14) 0.7005(12) 0.091(3) Uani 0.383(12) 1 D U . 2 H17A H 0.872(2) 0.0587(14) 0.7050(12) 0.109(4) Uiso 0.383(12) 1 R . . 2 O2A O 0.518(3) 0.1672(16) 0.8403(13) 0.098(3) Uani 0.383(12) 1 D U . 2 C19 C 0.7010(11) 0.1699(8) 0.9446(6) 0.109(3) Uani 0.250000 1 . . . 3 H19a H 0.641(14) 0.170(2) 0.904(7) 0.163(5) Uiso 0.250000 1 GR . . 3 H19b H 0.772(2) 0.134(2) 0.934(10) 0.163(5) Uiso 0.250000 1 GR . . 3 H19c H 0.657(16) 0.152(5) 0.988(4) 0.163(5) Uiso 0.250000 1 GR . . 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ni1 0.0435(3) 0.0319(3) 0.0248(3) -0.0136(2) -0.000000 0.000000 O1 0.0496(14) 0.0549(15) 0.0532(14) 0.0015(12) -0.0061(12) -0.0016(11) N1 0.0553(17) 0.0382(14) 0.0381(14) -0.0153(12) -0.0039(13) -0.0065(11) N2 0.0564(17) 0.0480(16) 0.0319(13) -0.0188(13) -0.0007(12) -0.0081(11) C6 0.064(2) 0.0443(19) 0.0469(19) -0.0160(17) -0.0020(17) -0.0097(15) C1 0.066(2) 0.054(2) 0.048(2) -0.0072(19) -0.0172(18) -0.0091(16) C2 0.069(3) 0.070(3) 0.052(2) -0.005(2) -0.0177(19) -0.0157(19) O2 0.096(3) 0.128(10) 0.070(2) 0.036(6) 0.000(2) 0.032(5) C12 0.059(2) 0.079(3) 0.062(2) -0.023(2) 0.0090(19) -0.028(2) C5 0.070(2) 0.042(2) 0.068(2) -0.0191(18) 0.010(2) -0.0205(18) C3 0.053(2) 0.077(3) 0.047(2) -0.020(2) 0.0004(17) -0.0183(19) C13 0.059(2) 0.070(3) 0.053(2) -0.002(2) 0.001(2) 0.013(2) C11 0.068(3) 0.120(4) 0.073(3) -0.026(3) 0.012(2) -0.056(3) C14 0.048(6) 0.063(8) 0.079(7) 0.003(4) 0.000(3) 0.007(4) C7 0.057(2) 0.069(3) 0.060(2) -0.015(2) 0.0035(19) -0.0243(19) C8 0.053(2) 0.091(3) 0.080(3) -0.021(2) 0.006(2) -0.039(3) C9 0.062(3) 0.096(3) 0.072(3) -0.024(2) 0.001(2) -0.037(3) C4 0.073(3) 0.076(3) 0.056(2) -0.022(2) 0.000(2) -0.019(2) O3 0.080(3) 0.099(6) 0.123(4) 0.022(3) 0.010(2) 0.021(3) C10 0.062(3) 0.124(4) 0.080(3) -0.026(3) 0.003(2) -0.051(3) C17 0.063(3) 0.088(7) 0.123(4) 0.010(3) 0.019(2) -0.007(3) C15 0.098(3) 0.098(3) 0.098(3) 0.0002(3) 0.0000(3) -0.0001(3) C16 0.112(3) 0.112(3) 0.112(3) 0.0002(3) 0.0003(3) -0.0002(3) C18 0.098(8) 0.109(9) 0.113(9) -0.015(4) -0.000000 0.000000 N3 0.083(7) 0.159(10) 0.085(7) -0.006(7) -0.004(6) 0.007(7) C15A 0.098(3) 0.098(3) 0.098(3) 0.0002(3) 0.0000(3) -0.0001(3) C14A 0.054(11) 0.062(11) 0.068(10) 0.001(4) 0.003(4) 0.008(4) O3A 0.080(3) 0.099(6) 0.123(4) 0.022(3) 0.010(2) 0.021(3) C16A 0.112(3) 0.112(3) 0.112(3) 0.0002(3) 0.0003(3) -0.0002(3) C17A 0.063(3) 0.088(7) 0.123(4) 0.010(3) 0.019(2) -0.007(3) O2A 0.096(3) 0.128(10) 0.070(2) 0.036(6) 0.000(2) 0.032(5) C19 0.083(7) 0.159(10) 0.085(7) -0.006(7) -0.004(6) 0.007(7) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source _atom_type_scat_dispersion_source H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236 57.79970 0.0030380000826 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870 51.65120 0.215599998832 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750 0.58260 -11.5290002823 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' O 0.01158 0.00611 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390 32.90890 0.250800013542 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' Ni 0.35663 1.12491 12.83760 7.29200 4.44380 2.38000 3.87850 0.25650 12.17630 66.34210 1.03410005569 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u 1 0 0 1.8 0.4 1 0 0 1.5 0.4 1 0 0 2.5 0.4 -2 0 0 273.87 11.3 -2 0 0 265.77 11.1 2 0 0 274.57 11.3 2 0 0 265.17 11.1 3 0 0 1.6 1 -3 0 0 2.1 1 3 0 0 1.4 0.9 -3 0 0 2.1 1.2 3 0 0 3.7 1.3 -3 0 0 2.3 1 4 0 0 3038 119.09 4 0 0 3053.89 119.69 -4 0 0 3054.49 118.99 -4 0 0 3024.4 119.19 4 0 0 3076.59 118.99 5 0 0 4.2 1.7 5 0 0 2.6 1.7 5 0 0 3.9 1.7 -5 0 0 4.9 1.9 6 0 0 41.9 3.9 6 0 0 44.7 4.7 6 0 0 41.1 4 7 0 0 -1.7 1.6 7 0 0 0.3 1.7 7 0 0 -4.3 1.9 8 0 0 319.07 16 8 0 0 337.27 17.2 8 0 0 321.07 15.9 9 0 0 -0.8 3.5 9 0 0 -1.5 2.7 9 0 0 2.3 2.7 10 0 0 39.6 6.7 10 0 0 35.5 5.7 11 0 0 6.7 3.8 11 0 0 9.8 4.3 12 0 0 44.5 7.2 12 0 0 48.2 7.2 13 0 0 10.6 5.1 13 0 0 10.6 4.6 14 0 0 45.5 10.3 14 0 0 31.1 7 15 0 0 -7.3 5.2 15 0 0 1.8 6.4 1 -1 0 5654.63 247.98 -1 1 0 5603.24 248.28 -1 -1 0 5637.64 233.68 -2 -1 0 6.7 1.1 -2 1 0 8 1.3 2 -1 0 6 1.4 2 -1 0 8.7 1.4 2 -1 0 7.5 1.1 -2 1 0 7.8 1 -2 -1 0 7.8 1.2 2 1 0 8 1.2 2 1 0 8.5 1.3 2 1 0 6.6 1.2 -2 1 0 8.9 1.1 -2 1 0 5.6 1.5 -2 -1 0 7.8 1.3 -3 -1 0 240.68 10.7 -3 1 0 247.68 11.2 -3 1 0 258.27 11.2 3 1 0 248.88 11.1 3 -1 0 257.37 11.3 3 -1 0 228.58 10.6 -3 1 0 253.87 10.2 -3 1 0 244.38 10.6 3 -1 0 256.17 10.9 3 -1 0 253.27 10.2 3 1 0 234.68 10.7 -3 -1 0 235.88 10.8 -3 -1 0 256.87 11 3 1 0 248.28 10.9 4 -1 0 2.5 1.4 -4 -1 0 1.5 1.4 -4 1 0 2.6 1.9 4 -1 0 2.4 1.3 -4 -1 0 -0.3 1.2 4 1 0 0.7 0.9 4 -1 0 0.5 1.2 -4 1 0 2.3 0.8 -4 1 0 0.2 1.2 4 1 0 1.8 1.1 -4 1 0 2.1 1.2 -4 -1 0 1.6 1.1 4 1 0 1.7 1.3 4 -1 0 1.5 0.9 5 -1 0 221.68 10.3 -5 1 0 209.08 10.8 5 1 0 203.08 10.1 5 -1 0 213.58 10.9 5 1 0 201.08 10.8 6 -1 0 5.5 2.1 6 -1 0 5.8 2.1 6 1 0 5.5 2 6 -1 0 5.6 2.1 6 1 0 6.6 2.1 6 1 0 7 2.7 7 -1 0 95.49 7.5 7 1 0 112.29 7.2 7 -1 0 105.49 6.8 7 -1 0 108.09 7.2 7 1 0 112.79 7.8 7 1 0 103.59 6.9 8 -1 0 -0.9 2.1 8 -1 0 -1.7 2.3 8 1 0 3.6 2.9 8 1 0 4.1 2.4 8 -1 0 -2.5 2 8 1 0 0.4 2.7 9 -1 0 63.79 6.8 9 1 0 64.79 6.6 9 1 0 62.19 6.9 9 1 0 60.79 7.2 9 -1 0 53.49 5.8 9 -1 0 61.69 6.3 10 -1 0 2.9 3.1 10 1 0 3.6 4 10 1 0 0.9 3.5 10 1 0 -1.3 2.4 10 -1 0 1.3 2.1 11 1 0 238.08 14.1 11 -1 0 225.78 14 11 -1 0 230.38 14.1 11 1 0 220.58 13.9 12 1 0 5.1 4.7 12 1 0 3.1 4 12 -1 0 0.6 4.9 12 -1 0 0.2 4.2 13 -1 0 33.1 6.8 13 -1 0 33.5 6.9 13 1 0 41.4 6.3 13 1 0 32.4 7.2 14 1 0 -4.9 4.5 14 -1 0 -3.8 5.4 14 -1 0 -0.1 4.5 0 -2 0 2311.37 116.09 0 2 0 2310.17 116.69 1 -2 0 1.7 0.5 1 2 0 1 0.5 1 -2 0 1 0.6 1 -2 0 0 0.4 -1 2 0 1.4 0.5 1 2 0 0.9 0.5 -1 -2 0 1.9 0.5 -1 -2 0 0.5 0.3 -1 -2 0 0.9 0.6 -1 2 0 1 0.5 1 2 0 1.3 0.4 -1 2 0 1.8 0.6 -2 2 0 2661.13 102.59 -2 -2 0 2615.54 102.19 2 -2 0 2668.73 102.79 -2 2 0 2638.74 102.69 2 2 0 2678.93 102.29 -2 2 0 2580.84 102.29 2 2 0 2643.74 102.49 2 -2 0 2691.93 102.59 2 2 0 2639.84 102.39 -2 -2 0 2663.03 102.39 2 2 0 2660.23 102.59 -2 -2 0 2582.44 102.59 -2 -2 0 2612.24 102.49 2 -2 0 2559.84 102.29 3 2 0 2.2 1 -3 2 0 3 1.2 3 -2 0 1.3 1.1 -3 -2 0 2.7 1.1 -3 -2 0 1.9 0.7 -3 -2 0 2 1.1 -3 2 0 2.7 0.9 3 2 0 1.7 1.1 3 -2 0 4.6 1.6 3 2 0 4 1.3 -3 2 0 4.1 1.2 3 -2 0 3.8 1.1 3 -2 0 2.9 1.2 -3 -2 0 2.2 1 4 -2 0 159.88 8.3 -4 2 0 141.59 7.9 -4 2 0 159.08 7.5 4 2 0 149.88 7.8 4 -2 0 152.98 7.8 4 2 0 157.18 7.8 -4 -2 0 154.08 7.8 4 -2 0 160.98 7.2 4 2 0 157.98 8 -4 2 0 153.78 7.2 4 -2 0 163.08 7.6 -4 -2 0 160.28 7.9 -4 -2 0 150.78 7.6 5 -2 0 1.5 1.6 -5 2 0 4.1 2.4 -5 2 0 1.1 1.1 5 2 0 1.7 1.6 5 -2 0 0.2 1.7 5 -2 0 2.3 1.2 5 2 0 2.9 1.6 5 -2 0 4.5 1.8 6 -2 0 768.12 32.6 6 -2 0 741.83 31.2 6 2 0 732.43 31.4 6 -2 0 749.82 29.8 6 2 0 752.22 32.1 6 2 0 742.63 31.7 6 -2 0 760.12 31.4 -6 2 0 745.13 30.1 7 -2 0 6.7 2.7 7 -2 0 6.2 2.3 7 2 0 0.6 2.3 7 2 0 1 2.2 7 2 0 1.5 1.9 7 -2 0 4.9 2.3 8 2 0 202.38 12.2 8 2 0 201.08 11.6 8 -2 0 195.28 12.3 8 -2 0 210.48 11.6 8 -2 0 218.28 11.4 8 2 0 221.58 11.9 9 2 0 2.7 2.6 9 2 0 2.7 3.3 9 -2 0 2 3.5 9 2 0 -0.7 3 9 -2 0 0.7 2.7 9 -2 0 1.8 2.5 10 -2 0 103.79 9.4 10 2 0 108.49 8.7 10 -2 0 111.39 9 10 2 0 116.49 9.1 11 -2 0 3.4 4 11 2 0 -0.5 4.1 11 -2 0 0.5 3.4 11 2 0 6.6 3.2 12 2 0 89.39 9.2 12 -2 0 106.89 9.7 12 -2 0 100.49 9.5 12 2 0 91.49 9.5 13 -2 0 1.7 4.6 13 2 0 1.2 6 13 2 0 1.3 4.2 13 -2 0 2.7 5 14 -2 0 1.9 4.9 14 2 0 17.5 5.5 14 -2 0 1.7 6 0 -3 0 4.5 0.9 0 3 0 3.8 1.1 0 3 0 4.3 0.9 0 -3 0 2.3 1 -1 -3 0 3678.73 141.49 -1 -3 0 3630.24 141.29 1 3 0 3737.93 141.49 1 -3 0 3626.04 140.99 -1 3 0 3553.14 140.99 1 -3 0 3663.03 141.69 -1 3 0 3600.34 141.59 -2 3 0 1 1 2 -3 0 6 1.5 2 3 0 0 0.8 -2 -3 0 1.3 0.8 -2 -3 0 0.6 0.8 2 -3 0 1.4 1 -2 -3 0 0.3 0.6 -2 3 0 0.6 0.9 2 3 0 1.6 0.9 -2 -3 0 0.5 0.9 2 3 0 -0.1 0.7 -2 3 0 -0.1 0.8 2 -3 0 -0.4 0.8 3 -3 0 1445.86 58.19 3 -3 0 1444.36 57.99 3 3 0 1447.56 57.49 -3 -3 0 1451.25 57.79 -3 -3 0 1481.95 57.99 -3 3 0 1446.46 57.79 3 -3 0 1486.15 58.39 -3 -3 0 1496.05 57.59 3 3 0 1472.65 57.89 3 3 0 1485.55 58.19 -3 3 0 1484.95 58.89 3 3 0 1470.45 57.99 -3 -3 0 1432.96 58.09 -3 3 0 1492.35 58.09 3 -3 0 1451.45 57.69 4 -3 0 1.6 1.2 -4 -3 0 3.7 1.4 4 -3 0 4.4 1.7 4 3 0 1 1.4 4 3 0 3.8 1.4 -4 -3 0 4.2 1.2 -4 -3 0 1.9 1.1 4 -3 0 3.2 1.8 -4 -3 0 2.5 1 -4 3 0 1.6 1.3 -4 3 0 2 1.4 4 3 0 2.1 1.3 -4 3 0 2.5 1.2 4 -3 0 1.8 1.3 5 3 0 757.52 30.6 5 -3 0 735.63 30 5 -3 0 715.63 31 5 3 0 734.73 30.3 5 -3 0 731.83 29.6 -5 3 0 710.73 29.7 5 -3 0 721.03 30.2 5 3 0 695.83 30.5 6 3 0 2.1 1.9 6 -3 0 1.4 2.4 -6 3 0 1.5 1.4 6 -3 0 2.6 2.1 6 3 0 1.9 1.7 6 -3 0 0.2 1.8 6 3 0 -1.6 1.5 6 -3 0 3.3 1.8 7 -3 0 962.1 38.9 7 -3 0 975.7 42 7 3 0 1007.4 41.6 -7 3 0 971.4 39.3 7 -3 0 973.7 40.6 7 3 0 981 41.1 7 3 0 971.2 40.8 7 -3 0 978.4 40.5 8 -3 0 2.2 2.4 8 3 0 3.3 2.4 8 -3 0 0.3 2.4 8 -3 0 -2 2.4 8 3 0 -0.5 2.6 8 3 0 1.9 2.3 9 3 0 156.98 10.1 9 3 0 127.09 9.6 9 -3 0 157.38 9.9 9 -3 0 138.49 10.7 9 -3 0 155.38 9.7 9 3 0 155.48 10.6 10 -3 0 4 3.5 10 3 0 -0.8 3.2 10 -3 0 5.8 3.2 11 -3 0 -7.5 3.2 11 3 0 1.7 3.2 11 3 0 -0.9 4 11 -3 0 0.4 3.9 12 -3 0 -0.9 3.9 12 3 0 3.4 3.4 12 3 0 5.5 4.7 12 -3 0 -2.5 4.1 13 3 0 21.1 6.4 13 -3 0 23.3 6.3 13 3 0 25.8 6.3 13 -3 0 27.6 6.1 14 -3 0 -3.4 5 14 3 0 0.1 4.4 14 -3 0 0.7 6.6 0 -4 0 6937.61 321.17 0 4 0 6776.12 320.87 -1 -4 0 2.3 1.2 1 4 0 2.7 1.2 1 -4 0 4 1.2 1 -4 0 3.3 0.8 -1 -4 0 3 1 1 -4 0 5.7 1.7 1 4 0 3.5 1.1 -1 4 0 6 1.6 -1 4 0 2.9 0.9 -1 4 0 4.1 1.1 2 4 0 1064.59 42.2 2 4 0 1070.59 42.2 -2 -4 0 1030.5 42.1 2 -4 0 1082.39 41.8 2 -4 0 1039.2 41.9 -2 4 0 1065.99 42.5 -2 -4 0 1043.7 41.3 2 -4 0 1040.2 42.5 -2 4 0 1046.8 41.8 -2 -4 0 1063.29 42.2 -2 4 0 1031.4 41.8 2 4 0 1050.79 41.3 3 4 0 3.2 1.1 3 4 0 1.7 0.9 3 -4 0 4.3 1.4 -3 -4 0 5 1.3 -3 4 0 1.4 1 -3 -4 0 2.9 1.2 -3 -4 0 3.2 1 -3 -4 0 2.4 1.1 3 -4 0 5.4 1.7 3 -4 0 3.7 1.5 3 4 0 5.9 1.4 -3 4 0 4.1 1.3 -4 4 0 275.87 12.7 4 -4 0 271.37 12.2 4 -4 0 272.27 13 -4 -4 0 285.37 12.9 4 -4 0 248.58 12.9 4 -4 0 275.17 12.7 4 4 0 288.67 12.5 -4 4 0 269.07 12.3 -4 -4 0 280.17 12 -5 4 0 0.6 1.3 5 -4 0 -1.2 1.4 5 4 0 -0.7 1.5 5 -4 0 -1.2 1.6 -5 -4 0 1.5 1.4 5 4 0 -0.4 1.5 -5 -4 0 4 1.5 5 4 0 -0.2 1.2 5 -4 0 3.2 2.3 5 -4 0 -1.6 1.5 6 -4 0 667.93 28.2 6 -4 0 648.84 27.3 6 -4 0 649.64 29.1 6 4 0 685.43 28.6 -6 4 0 655.83 27.6 6 -4 0 653.03 27.7 6 4 0 640.54 28.2 6 4 0 651.63 28.3 -7 4 0 6.4 1.9 7 4 0 4.2 2.5 7 -4 0 1 1.8 7 -4 0 2.7 2.2 7 4 0 9.1 3.2 7 4 0 9.2 3.2 7 -4 0 5.5 2.6 7 -4 0 10 2.8 8 4 0 359.46 18 8 -4 0 358.56 17.8 8 -4 0 396.06 19.4 8 -4 0 365.26 17.6 8 4 0 376.76 18.5 -8 4 0 371.86 16.4 8 -4 0 358.36 15.9 8 4 0 387.96 18.5 9 -4 0 6.3 3.5 9 -4 0 2.8 1.4 9 -4 0 -1.3 3 9 4 0 -1.3 2.2 9 -4 0 1.6 3 9 4 0 4.8 3.7 10 -4 0 118.29 10.1 10 4 0 131.39 9.9 10 -4 0 129.59 9.7 10 4 0 111.29 9.6 11 4 0 -2.2 3.3 11 -4 0 0.4 3.5 11 -4 0 2.8 4 11 4 0 0.2 4.2 12 -4 0 34.8 6.4 12 -4 0 30.5 6.2 12 4 0 38.8 7 13 -4 0 -4.3 4.9 13 4 0 16.3 5.5 13 -4 0 -4 4 14 -4 0 7.2 4.8 14 4 0 2.1 5 14 -4 0 -5 6.6 0 -5 0 3.7 1.1 0 5 0 3.3 1.2 0 5 0 2.4 0.9 0 -5 0 4.9 1.6 1 -5 0 96.79 5.2 1 -5 0 115.39 5.4 -1 5 0 102.59 6.4 1 -5 0 102.59 4.9 -1 5 0 101.59 4.8 -1 -5 0 94.29 5.8 1 -5 0 106.39 6.1 -1 -5 0 98.79 5.4 1 5 0 108.49 6 1 5 0 97.69 5.5 2 5 0 5.5 1.5 2 -5 0 9.1 1.7 2 -5 0 3.2 1.7 -2 5 0 3.9 1.3 -2 -5 0 7.3 1.9 -2 -5 0 6.5 1.5 -2 5 0 1.7 1.2 2 5 0 5 1.5 2 -5 0 3.7 1.3 -2 5 0 8 1.6 -3 5 0 154.98 8.1 3 5 0 150.38 7.1 -3 -5 0 146.89 7.6 3 5 0 155.58 7.8 -3 -5 0 153.58 7 3 -5 0 148.99 7.4 -3 -5 0 140.29 7.7 -3 -5 0 147.69 7.7 3 -5 0 149.29 7.8 3 5 0 157.08 8 -3 5 0 163.68 7.8 -3 5 0 149.69 7.4 3 -5 0 159.98 8.3 -4 5 0 1.4 1.7 -4 -5 0 2.2 1.4 4 -5 0 3.2 1.5 4 5 0 -0.3 1.2 4 -5 0 3.8 2.2 -4 -5 0 2.2 1.1 4 5 0 1 1.3 -4 5 0 1.2 1.2 4 5 0 1.3 1.3 5 -5 0 375.16 16.6 -5 -5 0 358.96 16.5 5 5 0 370.96 16.8 -5 5 0 374.56 17.1 -5 -5 0 377.36 16.2 5 -5 0 371.16 17.6 5 -5 0 392.56 17.2 5 5 0 379.06 17.4 -6 -5 0 4.5 1.9 6 -5 0 4.1 2.7 6 -5 0 2.3 2.3 6 -5 0 2.7 2.6 6 5 0 5.6 2 6 -5 0 4.4 1.9 6 5 0 4.3 2.3 -6 5 0 0 1.7 7 -5 0 621.54 26.3 7 -5 0 630.24 28.4 7 5 0 627.64 27.8 7 5 0 629.14 27.5 7 -5 0 630.94 27.2 -7 5 0 592.84 26.5 7 -5 0 610.84 26.7 8 5 0 -1.5 2.3 8 -5 0 -2.2 2.1 8 5 0 0.8 2.1 8 -5 0 1.4 2.4 -8 5 0 2.8 2.2 8 -5 0 1.1 2.9 8 -5 0 -1.1 2.1 9 -5 0 245.58 16.8 9 5 0 254.87 14.6 9 -5 0 252.57 11.9 9 -5 0 269.57 14.2 9 -5 0 259.77 13.9 10 -5 0 -2 3.2 10 5 0 5.4 3.5 10 -5 0 1.4 3.5 11 -5 0 20.1 5.1 11 -5 0 10.7 4.2 11 5 0 17.4 4.5 12 5 0 -1 3.8 12 -5 0 2.7 4.6 12 -5 0 -1.4 4.2 13 5 0 9.2 4.7 13 -5 0 17.7 5.7 13 -5 0 24.5 6.4 14 -5 0 -3.7 4.8 14 5 0 6.1 8.8 0 6 0 117.69 6.2 0 -6 0 118.09 6.9 0 6 0 106.99 6.6 -1 6 0 0.4 0.8 1 -6 0 1.2 1.4 1 -6 0 2.4 1.1 -1 -6 0 0.4 1.3 1 6 0 4.5 1.3 1 -6 0 1.6 1.3 -1 6 0 1.9 1.5 1 -6 0 0.8 0.9 1 6 0 1.6 1.3 -1 -6 0 4 1.3 -2 6 0 3934.21 153.98 -2 6 0 3873.01 155.38 2 -6 0 3976 154.18 -2 -6 0 3902.91 154.58 -2 6 0 3882.71 154.18 2 -6 0 3988.4 155.38 2 6 0 4046.7 154.88 2 6 0 3960.2 155.08 2 -6 0 3995.9 154.18 -2 -6 0 4052.09 155.18 3 -6 0 4.3 1.7 -3 -6 0 3.2 1 -3 -6 0 2.4 1.4 3 6 0 2.7 1.5 3 -6 0 6.3 1.9 -3 6 0 5.5 1.7 -3 6 0 4 1.6 -3 6 0 1.4 1.4 3 -6 0 6.8 2.6 3 6 0 2.3 1.1 4 6 0 895.91 37.8 4 -6 0 918.61 38 -4 6 0 899.51 38 -4 -6 0 911.81 37.3 4 6 0 948.41 36.8 4 -6 0 925.71 37.6 -4 -6 0 882.31 36.5 4 -6 0 875.51 37.8 5 6 0 2 1.5 -5 -6 0 1.7 1.6 5 -6 0 0.4 1.7 5 -6 0 4.7 2.9 5 -6 0 1.7 2.4 -5 6 0 4.2 2.2 -5 -6 0 4 2 5 -6 0 0.8 1.6 5 6 0 0.1 1.6 6 6 0 994.1 40.7 -6 -6 0 999.6 39.8 6 6 0 970.4 41.5 6 -6 0 963.4 41.2 6 -6 0 985.9 41.8 6 -6 0 962.5 40.3 6 -6 0 982.3 40.8 -7 -6 0 -2.4 1.7 7 -6 0 4.7 3.3 7 -6 0 -0.4 2.4 7 6 0 1 2 7 -6 0 1.6 2 7 -6 0 -2.1 2.5 8 -6 0 137.39 10.8 8 -6 0 114.39 9.1 8 6 0 123.79 9 8 -6 0 125.69 8.2 8 -6 0 128.69 9.1 9 -6 0 2.2 3.8 9 6 0 2.8 3.4 9 -6 0 2.6 2.5 9 -6 0 2.1 3.1 9 -6 0 2 3.3 10 6 0 90.09 8.2 10 -6 0 89.99 8.3 10 -6 0 88.09 5.7 10 -6 0 88.09 7.8 11 6 0 0.6 3.2 11 -6 0 0.2 3.6 11 -6 0 -0.9 3.8 12 -6 0 1.5 4.3 12 -6 0 5 4.7 12 6 0 7.8 4.2 13 -6 0 -3.7 4.4 13 -6 0 -3.3 5.1 13 6 0 2.1 4.3 14 6 0 16 5.7 14 -6 0 10.8 5.8 0 7 0 6 1.6 0 -7 0 3.5 1.3 0 -7 0 6.6 2.1 0 7 0 5.1 1.9 -1 -7 0 79.49 5.7 1 -7 0 77.19 4.7 1 -7 0 75.69 4.7 1 -7 0 81.39 5.8 -1 -7 0 74.99 4.9 1 7 0 72.79 4.9 -1 7 0 70.29 3.8 1 7 0 74.59 5.4 -2 7 0 0.5 1.1 2 -7 0 -0.2 1.3 2 -7 0 0.7 1.2 2 -7 0 0.8 1.2 -2 -7 0 1.6 1.9 2 7 0 2.6 1.7 2 -7 0 3.1 2.3 -3 -7 0 2213.38 86.99 3 -7 0 2191.88 86.29 3 -7 0 2203.88 86.69 3 7 0 2169.38 86.89 3 7 0 2140.69 86.79 -3 -7 0 2172.08 84.89 -3 7 0 2162.38 86.09 3 -7 0 2190.88 88.69 4 7 0 3.6 1.6 4 -7 0 4.1 2.7 4 -7 0 2.2 2.1 -4 -7 0 5 1.3 4 7 0 1 1.6 -4 -7 0 1.5 2 4 -7 0 2.4 1.8 -5 -7 0 498.35 22.2 -5 -7 0 540.95 23.1 5 -7 0 538.15 23.9 5 7 0 546.55 23.9 5 7 0 510.25 22.8 5 -7 0 539.05 23.8 5 -7 0 528.25 22.8 6 -7 0 -0.5 3.4 6 7 0 3.5 2.2 6 -7 0 0.1 2.7 -6 -7 0 1.6 2.2 6 -7 0 -1.1 1.7 6 -7 0 5 2.1 7 -7 0 63.39 6.3 7 -7 0 73.19 7.5 -7 -7 0 66.79 5.2 7 -7 0 77.99 6.9 7 -7 0 78.69 5.8 7 7 0 70.09 6.5 8 -7 0 1.2 3 8 -7 0 3.7 2.5 8 -7 0 2.3 3.3 8 -7 0 8.2 3.9 -8 -7 0 1.1 2.1 8 7 0 1.7 2.6 9 -7 0 99.29 7.3 9 -7 0 111.49 8.2 9 -7 0 109.99 9.7 9 7 0 104.09 9.1 9 -7 0 108.99 8.6 10 -7 0 3.2 3.6 10 7 0 1.7 3.1 10 -7 0 0.2 2.4 10 -7 0 1.4 3.5 11 -7 0 84.09 8.1 11 7 0 61.49 8.3 11 -7 0 73.79 8.3 12 7 0 -1.9 3.3 12 -7 0 -1.3 4.2 12 -7 0 0 4.1 13 7 0 3.2 4.7 13 -7 0 5.1 4.9 13 -7 0 11.1 5.6 14 7 0 24.2 6.2 14 -7 0 -0.5 5.1 14 -7 0 -11.6 6 0 8 0 61.29 4.6 0 -8 0 67.19 4.8 0 -8 0 63.79 5.6 1 -8 0 -0.6 1.8 1 -8 0 -2.2 1.1 -1 -8 0 0.2 1.9 -1 8 0 0.4 0.9 1 8 0 0.4 1.4 1 -8 0 -1 1 2 -8 0 577.94 25.4 -2 8 0 539.75 23 -2 -8 0 553.24 25 2 -8 0 537.95 23.7 2 -8 0 567.24 23.2 2 8 0 569.64 24.3 3 -8 0 1.5 1.9 3 -8 0 5.1 2.8 -3 8 0 4.5 1.8 3 8 0 4 1.6 3 -8 0 6.4 1.9 -4 -8 0 1282.17 51.99 -4 -8 0 1307.27 55.09 4 -8 0 1319.57 53.19 4 8 0 1361.46 54.29 4 -8 0 1317.27 54.59 4 -8 0 1315.87 53.69 5 -8 0 4 2.1 5 8 0 2.7 2 5 -8 0 1.5 2 5 -8 0 1.4 2.9 -5 -8 0 4.7 1.6 -5 -8 0 1.7 2.3 6 -8 0 410.56 19.2 6 -8 0 391.06 19.4 6 -8 0 374.56 17.7 6 8 0 399.66 19.3 6 -8 0 373.76 18.9 -6 -8 0 394.86 18.1 7 -8 0 4.8 3.8 7 -8 0 -3.4 3.1 7 -8 0 1.3 2.4 7 -8 0 -1.4 2.2 7 8 0 0.2 2 -7 -8 0 0.6 2.6 8 -8 0 417.26 19.7 8 8 0 394.26 20.9 8 -8 0 417.46 20.1 -8 -8 0 423.56 18.4 8 -8 0 429.66 20.6 8 -8 0 408.76 21.4 9 -8 0 1 3.3 9 -8 0 -0.6 3.3 9 8 0 -1.9 3 9 -8 0 2.3 3.6 10 -8 0 68.39 6.3 10 -8 0 64.19 7.6 10 -8 0 75.29 7.9 10 8 0 73.49 8.2 11 -8 0 -1.3 4 11 8 0 6.2 3.9 11 -8 0 8.8 3 11 -8 0 -2.1 3.7 12 -8 0 10.3 5 12 -8 0 21.8 5.5 12 8 0 8.1 4.1 13 8 0 -3.5 4.9 13 -8 0 -3.2 5.2 13 -8 0 -2.7 4.8 14 8 0 8.8 5.3 14 -8 0 6.2 5.9 14 -8 0 4.7 6.3 0 9 0 1.4 1.3 0 -9 0 1.8 2.2 1 -9 0 89.29 5.8 1 9 0 96.79 6.3 -1 -9 0 89.79 7.1 1 -9 0 100.19 7.4 2 -9 0 -0.5 1.6 2 -9 0 -1 2.3 -2 9 0 0.4 1.3 2 9 0 3.3 1.7 -2 -9 0 2.3 2.4 3 -9 0 2350.16 92.99 3 -9 0 2378.46 92.89 3 -9 0 2352.46 94.69 -3 9 0 2271.17 92.49 -3 -9 0 2378.86 94.39 3 9 0 2347.57 93.89 -4 -9 0 3.1 2.7 4 9 0 0 1.6 4 -9 0 2.5 1.8 4 -9 0 4.2 2.1 4 -9 0 5.3 3.3 5 -9 0 523.25 24.5 5 9 0 527.45 24.1 5 -9 0 517.55 23.6 5 -9 0 524.45 22.9 -5 -9 0 537.25 23.9 -5 -9 0 500.05 21.8 6 9 0 -0.4 2 6 -9 0 -2.5 1.9 6 -9 0 1.8 2.1 6 -9 0 2 3.5 -6 -9 0 -2 2.5 -7 -9 0 363.36 19.3 7 -9 0 372.06 18.4 7 -9 0 341.07 17.9 7 -9 0 345.17 18.5 7 -9 0 349.77 16.9 7 9 0 343.87 18.4 8 -9 0 4.5 3.3 8 -9 0 7.2 4.1 8 9 0 5.1 3.6 8 -9 0 4.3 4.1 -8 -9 0 1 3.2 9 -9 0 82.29 8.4 -9 -9 0 75.49 5.2 9 9 0 55.39 7.6 9 -9 0 64.59 7.1 10 -9 0 -0.8 3.8 10 -9 0 2.1 3.6 10 9 0 4.4 4 10 -9 0 -2.6 3.5 11 -9 0 34.2 6.1 11 -9 0 26 5.3 11 9 0 28.2 6.5 11 -9 0 26.7 4.6 12 9 0 -3.6 3.9 12 -9 0 7.6 2.9 12 -9 0 10.5 5.4 12 -9 0 2.1 4.7 13 9 0 -4.1 4.4 13 -9 0 -5.8 5.1 13 -9 0 -4.2 4.6 0 10 0 586.74 25.5 0 -10 0 570.34 26.7 1 10 0 0.7 1.2 -1 -10 0 -0.5 2.3 1 -10 0 -1.5 1.5 1 -10 0 1.4 2.5 2 -10 0 226.48 11.4 2 10 0 229.08 12.1 2 -10 0 231.18 13.3 -2 -10 0 220.38 12.8 -3 10 0 2 1.6 3 -10 0 0.1 1.7 3 -10 0 6.3 3 -3 -10 0 0.6 2.7 3 10 0 -0.2 1.6 4 -10 0 1018.2 41.4 4 10 0 978.5 42.3 4 -10 0 977.6 43.1 -4 -10 0 1001.6 42.6 5 -10 0 2 2.3 -5 -10 0 -1.4 2.8 5 -10 0 5.9 3.9 5 -10 0 -1 2 5 10 0 0.9 2.2 -5 -10 0 1.9 1.3 -6 -10 0 265.47 12.6 -6 -10 0 271.27 14.7 6 -10 0 274.47 15.6 6 -10 0 273.37 13.9 6 10 0 286.77 15.3 7 -10 0 -0.9 4.4 7 10 0 0.7 2.8 7 -10 0 1.2 3.6 -7 -10 0 1.5 3.4 7 -10 0 3.6 3.1 8 10 0 185.08 13.1 -8 -10 0 213.68 11.8 8 -10 0 208.18 13.6 8 -10 0 213.08 12.1 8 -10 0 226.28 13.1 9 10 0 1 3.5 9 -10 0 -1.7 3.8 9 -10 0 -0.9 3.5 -9 -10 0 -2 2.8 9 -10 0 -0.2 3.5 10 -10 0 36.8 5.7 10 10 0 23.4 6 10 -10 0 43.4 6.3 11 10 0 5.4 4.3 11 -10 0 10.8 3.8 11 -10 0 6 4.4 11 -10 0 -3.8 4.3 12 10 0 0 4.1 12 -10 0 6.4 5.5 12 -10 0 12.9 3.9 12 -10 0 2.6 4.9 13 10 0 -2.9 4.3 13 -10 0 2.8 5.6 13 -10 0 -6.4 4.2 0 11 0 12.6 2.6 0 -11 0 12.6 3.6 1 -11 0 675.63 31.1 -1 -11 0 656.53 30.8 1 11 0 689.93 29.6 1 -11 0 669.13 28.9 2 -11 0 -1.8 1.7 -2 11 0 -0.9 1.9 2 -11 0 2.6 3 -2 -11 0 3.7 3.2 2 11 0 2.1 2 3 11 0 94.59 7.3 3 -11 0 82.19 6.3 -3 -11 0 94.49 8 3 -11 0 101.39 8.3 -4 -11 0 2.9 3.2 4 11 0 1.8 2.5 4 -11 0 3.5 3.4 4 -11 0 0.3 2.1 5 -11 0 695.63 32.5 5 11 0 695.33 31.8 -5 -11 0 707.33 31.8 5 -11 0 716.53 30.6 6 -11 0 -0.5 2.6 -6 -11 0 -0.6 3.5 6 -11 0 4.4 4.1 6 11 0 -1.8 2.4 7 -11 0 100.19 7.7 7 11 0 95.49 8.9 7 -11 0 103.09 9.5 7 -11 0 108.59 10.2 -7 -11 0 101.09 8.6 -8 -11 0 -1.9 3.5 8 -11 0 -0.6 3.1 8 11 0 -0.8 2.5 8 -11 0 2.6 4.6 8 -11 0 6.2 4.3 9 -11 0 70.39 8.5 9 -11 0 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4 -12 6 361.06 16.7 4 -12 6 366.96 18 4 -12 -6 375.76 20 -4 -12 6 357.16 20.1 4 12 6 381.16 18.9 4 -12 -6 380.06 18.9 4 -12 -6 369.76 18.7 5 12 -6 -2.5 3.6 5 -12 6 2.9 2.3 -5 -12 -6 0.4 2 -5 -12 -6 2.4 3.7 5 -12 6 4.6 3.5 5 -12 6 -0.6 2.5 5 12 6 3.5 2.2 5 12 6 1.9 2.8 -5 -12 6 1.9 3.1 5 -12 -6 -1.8 3.9 -5 -12 6 0 1.6 -5 -12 6 1.1 2.2 -6 -12 -6 208.18 12.9 6 -12 6 226.88 13.3 6 12 -6 221.08 14 6 -12 6 225.98 11.2 6 -12 6 201.88 14.3 6 -12 -6 210.78 14 6 12 6 233.18 14 6 12 6 215.48 11.2 -6 -12 6 229.08 14.6 6 -12 -6 214.78 13 6 -12 -6 222.58 12.3 7 -12 6 7.7 4.5 7 12 -6 6.5 3.6 7 -12 6 8.8 2.9 -7 -12 -6 6.7 3.6 7 -12 6 4.2 3.7 -7 -12 6 4.5 4 7 12 6 4.7 3.3 7 12 6 9.2 3.4 7 -12 -6 5.4 5.2 7 -12 -6 3.7 3.1 7 -12 -6 5 4 8 -12 6 61.39 10.1 8 -12 6 81.79 9.3 -8 -12 -6 93.39 7.2 8 -12 6 84.09 6.4 8 12 -6 63.79 8.3 8 -12 6 75.19 9.9 8 -12 -6 69.59 8 -8 -12 6 86.59 8.4 8 -12 -6 77.29 6.3 8 -12 -6 79.99 8 8 12 6 78.39 7 8 12 6 62.19 8.2 9 -12 6 1 3.3 9 -12 6 -2 6.1 9 -12 6 -3.4 4.3 -9 -12 -6 7.5 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34.1 6.7 2 -13 -6 30.1 5 2 13 6 31.9 4.8 3 -13 6 95.79 6.7 3 -13 6 96.99 9.5 -3 -13 -6 118.19 9.3 3 13 -6 106.89 8.8 3 -13 6 99.89 7 -3 -13 6 102.69 9.3 3 13 6 111.29 8.2 3 -13 -6 99.89 8.4 3 -13 -6 108.89 9.8 4 -13 6 29.9 4.3 4 -13 6 33 5.1 4 13 -6 30.8 7.5 4 -13 6 27.8 6.2 -4 -13 -6 33.3 5.9 -4 -13 6 32.2 6.3 4 13 6 39.6 5.8 4 -13 -6 29.6 6.3 -5 -13 -6 275.27 16 5 -13 6 279.17 15.1 5 -13 6 280.67 13.6 5 -13 6 279.67 17.4 5 13 -6 271.87 16.3 5 13 6 297.67 17.7 5 -13 -6 285.97 15.8 -5 -13 6 281.57 17 6 -13 6 7.9 6.8 6 -13 6 1.1 2.4 -6 -13 -6 3.1 3.8 6 13 -6 2.3 2.7 6 -13 6 2.1 2.9 -6 -13 6 1.9 4 6 -13 -6 -0.6 3.6 6 -13 -6 3.3 3.7 6 -13 -6 -3.6 4 6 13 6 3.9 3.7 7 -13 6 188.78 15.7 -7 -13 -6 202.38 12.4 7 -13 6 180.38 13.2 7 -13 6 210.28 10.9 7 13 -6 202.38 13.9 -7 -13 6 213.28 14 7 13 6 195.08 10.7 7 13 6 196.48 13.5 7 -13 -6 188.68 12.8 7 -13 -6 200.98 13.8 7 -13 -6 174.68 10.9 8 13 -6 -0.9 3.2 8 -13 6 1.8 5.4 8 -13 6 -8.7 4.3 8 -13 6 -2.1 2.9 -8 -13 -6 5.8 3.7 8 -13 6 0.4 3.6 8 -13 -6 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8 14 -6 64.99 8.8 8 14 6 58.59 8 8 -14 -6 55.19 6 8 -14 -6 81.29 8.9 8 -14 -6 80.39 9 -8 -14 6 53.59 8.6 9 -14 6 7.5 5.5 9 -14 6 8.9 6.1 -9 -14 -6 10 4 9 -14 6 11.1 7.7 9 -14 6 6.2 4.8 9 14 -6 2.5 3.7 9 -14 -6 -0.2 4.6 9 -14 -6 12.2 4.8 9 14 6 -0.9 3.8 9 -14 -6 -2.7 3.1 -9 -14 6 -1.7 5.6 10 -14 6 -1.5 6.2 10 -14 6 10.5 4.5 10 -14 6 -1.8 7.3 10 14 -6 11.3 5.3 10 -14 6 18.2 5.8 -10 -14 -6 20.3 4 10 -14 -6 8.2 5.4 -10 -14 6 1 6 10 14 6 11.4 6.7 10 -14 -6 5.6 4 10 -14 -6 15 5.5 11 -14 6 6 9.6 11 -14 6 -5.3 5.8 11 14 -6 -2.7 4.6 11 -14 6 -6.1 4.4 11 -14 6 -11 6.4 11 -14 -6 1.5 5.2 11 14 6 0.5 4.2 11 -14 -6 -0.6 4.1 0 -15 6 4.9 3.9 0 -15 -6 0.6 2.7 0 -15 6 4.9 2.8 0 -15 -6 9.3 5.1 0 15 6 5.6 2.5 -1 -15 -6 78.89 10.1 1 -15 6 70.39 6.2 1 -15 6 77.49 10.5 -1 -15 -6 75.59 7.7 1 -15 -6 63.99 7.1 -1 -15 6 66.29 9.6 1 15 6 73.39 6.8 1 -15 -6 73.39 10 -2 -15 -6 33.4 7 2 -15 6 47.1 4.9 2 -15 6 42.2 5.2 2 -15 6 27.5 6.7 -2 -15 6 30.8 7 2 -15 -6 36.8 6.1 2 -15 -6 34.9 6.8 2 15 6 36.5 5.3 3 -15 6 132.79 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-7 25 -11 8.4 2 -7 25 13.5 6.3 -2 -7 25 0.4 5.6 2 -7 -25 9.4 5.3 2 7 25 10.5 5.7 0 0 26 48.7 8.6 0 0 26 32 6.4 -1 0 26 -1.6 5.3 -1 0 26 -11.6 4.3 1 0 26 3.7 4.4 1 0 26 -3.6 4.6 -2 0 26 42.8 8.3 2 0 26 45.7 8.4 2 0 26 36.7 6.9 0 -1 26 3.1 4.5 0 -1 26 -8.4 4.3 0 1 26 4.6 4.7 1 -1 26 41.5 8.1 -1 1 26 41.5 8.3 1 -1 26 39.1 7.7 1 1 26 48.2 8.1 1 1 26 27.3 6.1 -1 -1 26 37 8.3 2 -1 26 -3.1 4.3 2 -1 26 -2 5.2 -2 1 26 4.5 5.6 2 1 26 -12.8 4.2 -2 -1 26 0.5 5.3 2 -1 -26 -1.3 7.7 2 1 26 -2.6 5.1 0 -2 26 37.2 7.8 0 -2 26 45.7 8.6 0 2 26 40.3 8.1 1 -2 26 0.4 5.6 -1 2 26 6.2 5.7 1 -2 26 -10.5 5 -1 -2 26 -1.6 4.8 1 2 26 3 4.7 2 -2 26 14.2 6.7 2 -2 26 30.8 6.9 -2 2 26 23.2 6.8 -2 -2 26 22.4 7.9 2 2 26 30 7.5 2 2 26 29.2 6.2 0 -3 26 -1.5 5.6 0 3 26 -5.2 5.2 0 -3 26 -1.7 4.9 -1 3 26 24.5 7.1 1 -3 26 15.7 7.6 1 -3 26 20 6.4 -1 -3 26 16 6.8 1 -3 -26 22 7 1 3 26 8.4 6.1 1 3 26 21 6.6 -1 -3 26 -0.1 6 -2 -3 26 -16.9 5.2 0 4 26 6.1 5.8 0 -4 -26 1.3 7.7 0 -4 26 -0.2 6.7 0 -4 26 4.8 5.1 1 -4 26 -11.2 5.5 -1 -4 26 -10.9 5.7 1 -4 -26 -8 5.1 loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ni1 O1 169.61(13) 4 . ? N1 Ni1 O1 85.68(11) 4 4 ? N1 Ni1 O1 85.68(11) . . ? N1 Ni1 O1 86.89(11) 4 . ? N1 Ni1 O1 86.89(11) . 4 ? N1 Ni1 N1 88.63(14) . 4 ? N2 Ni1 O1 95.16(11) 4 . ? N2 Ni1 O1 92.00(11) 4 4 ? N2 Ni1 O1 95.16(11) . 4 ? N2 Ni1 O1 92.00(11) . . ? N2 Ni1 N1 89.32(11) 4 . ? N2 Ni1 N1 176.98(11) . . ? N2 Ni1 N1 89.32(11) . 4 ? N2 Ni1 N1 176.98(11) 4 4 ? N2 Ni1 N2 92.82(14) 4 . ? C13 O1 Ni1 143.6(3) . . ? C6 N1 Ni1 121.1(2) . 4 ? C1 N1 Ni1 122.0(2) . 4 ? C1 N1 C6 116.8(3) . . ? C12 N2 Ni1 123.0(2) . . ? C7 N2 Ni1 120.1(2) . . ? C7 N2 C12 116.8(3) . . ? H6 C6 N1 118.8(2) . . ? C5 C6 N1 122.4(4) . . ? C5 C6 H6 118.8(2) . . ? H1 C1 N1 117.79(19) . . ? C2 C1 N1 124.4(4) . . ? C2 C1 H1 117.8(3) . . ? H2 C2 C1 120.5(3) . . ? C3 C2 C1 119.1(4) . . ? C3 C2 H2 120.5(2) . . ? H12 C12 N2 118.6(2) . . ? C11 C12 N2 122.9(4) . . ? C11 C12 H12 118.6(3) . . ? H5 C5 C6 120.5(2) . . ? C3 C5 C6 119.0(4) . . ? C3 C5 H5 120.5(2) . . ? C5 C3 C2 118.2(3) . . ? C4 C3 C2 118.6(4) . . ? C4 C3 C5 123.2(4) . . ? O2 C13 O1 129.6(9) . . ? C14 C13 O1 116.1(7) . . ? C14 C13 O2 113.7(11) . . ? C14A C13 O1 113.3(11) . . ? C14A C13 O2 117.1(13) . . ? C14A C13 C14 9(3) . . ? O2A C13 O1 120.6(13) . . ? O2A C13 O2 21.7(16) . . ? O2A C13 C14 121.6(16) . . ? O2A C13 C14A 121.5(19) . . ? H11 C11 C12 119.5(3) . . ? C9 C11 C12 121.0(4) . . ? C9 C11 H11 119.5(2) . . ? O3 C14 C13 123.9(13) . . ? C15 C14 C13 129.7(13) . . ? C15 C14 O3 105.6(13) . . ? H7 C7 N2 118.5(2) . . ? C8 C7 N2 122.9(4) . . ? C8 C7 H7 118.5(3) . . ? H8 C8 C7 120.1(3) . . ? C9 C8 C7 119.9(4) . . ? C9 C8 H8 120.1(2) . . ? C8 C9 C11 116.5(4) . . ? C10 C9 C11 124.2(4) . . ? C10 C9 C8 119.3(4) . . ? C4 C4 C3 124.6(6) 5_556 . ? H4 C4 C3 117.7(3) . . ? C17 O3 C14 109.2(11) . . ? C10 C10 C9 125.3(6) 5_667 . ? H10 C10 C9 117.3(3) . . ? H17 C17 O3 125.1(7) . . ? C16 C17 O3 109.7(12) . . ? C16 C17 H17 125.1(8) . . ? H15 C15 C14 126.5(8) . . ? C16 C15 C14 106.9(11) . . ? C16 C15 H15 126.5(7) . . ? C15 C16 C17 106.7(11) . . ? H16 C16 C17 126.6(8) . . ? H16 C16 C15 126.6(7) . . ? N3 C18 N3 163.1(19) . 4_655 ? C19 C18 N3 163.1(19) . 4_655 ? C19 C18 N3 163.1(19) 4_655 . ? C19 C18 N3 0.0 4_655 4_655 ? C19 C18 N3 0.0 . . ? C19 C18 C19 163.1(19) . 4_655 ? C14A C15A H15A 126.9(13) . . ? C16A C15A H15A 126.9(10) . . ? C16A C15A C14A 106.3(17) . . ? C15A C14A C13 132(2) . . ? O3A C14A C13 116.1(19) . . ? O3A C14A C15A 107.9(19) . . ? C17A O3A C14A 100.1(17) . . ? H16A C16A C15A 128.0(10) . . ? C17A C16A C15A 104.0(18) . . ? C17A C16A H16A 128.0(13) . . ? C16A C17A O3A 115.0(19) . . ? H17A C17A O3A 122.5(11) . . ? H17A C17A C16A 122.5(13) . . ? H19a C19 C18 109.5 . 4_655 ? H19b C19 C18 109.5 . 4_655 ? H19b C19 H19a 109.5 . . ? H19c C19 C18 109.5 . 4_655 ? H19c C19 H19a 109.5 . . ? H19c C19 H19b 109.5 . . ? 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 Ni1 O1 2.070(3) . ? Ni1 O1 2.070(3) 4 ? Ni1 N1 2.111(3) 4 ? Ni1 N1 2.111(3) . ? Ni1 N2 2.089(3) 4 ? Ni1 N2 2.089(3) . ? O1 C13 1.233(5) . ? N1 C6 1.338(4) . ? N1 C1 1.332(5) . ? N2 C12 1.330(5) . ? N2 C7 1.340(5) . ? C6 H6 0.9500 . ? C6 C5 1.390(5) . ? C1 H1 0.9500 . ? C1 C2 1.375(5) . ? C2 H2 0.9500 . ? C2 C3 1.356(6) . ? O2 C13 1.266(14) . ? C12 H12 0.9500 . ? C12 C11 1.361(6) . ? C5 H5 0.9500 . ? C5 C3 1.398(6) . ? C3 C4 1.488(5) . ? C13 C14 1.487(15) . ? C13 C14A 1.48(2) . ? C13 O2A 1.27(2) . ? C11 H11 0.9500 . ? C11 C9 1.376(6) . ? C14 O3 1.351(17) . ? C14 C15 1.307(18) . ? C7 H7 0.9500 . ? C7 C8 1.379(5) . ? C8 H8 0.9500 . ? C8 C9 1.374(6) . ? C9 C10 1.470(6) . ? C4 C4 1.283(10) 5_556 ? C4 H4 0.9500 . ? O3 C17 1.337(14) . ? C10 C10 1.314(10) 5_667 ? C10 H10 0.9500 . ? C17 H17 0.9500 . ? C17 C16 1.242(16) . ? C15 H15 0.9500 . ? C15 C16 1.450(14) . ? C16 H16 0.9500 . ? C18 N3 1.456(14) 4_655 ? C18 N3 1.456(14) . ? C18 C19 1.456(14) 4_655 ? C18 C19 1.456(14) . ? C15A H15A 0.9500 . ? C15A C14A 1.33(3) . ? C15A C16A 1.45(2) . ? C14A O3A 1.39(3) . ? O3A C17A 1.40(2) . ? C16A H16A 0.9500 . ? C16A C17A 1.24(2) . ? C17A H17A 0.9500 . ? C19 H19a 0.9800 . ? C19 H19b 0.9800 . ? C19 H19c 0.9800 . ? 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 Ni1 O1 C13 O2 27.5(10) . . . . ? Ni1 O1 C13 O2 27.5(10) 4 . . . ? Ni1 O1 C13 C14 -161.9(12) 4 . . . ? Ni1 O1 C13 C14 -161.9(12) . . . . ? Ni1 O1 C13 C14A -152.9(19) . . . . ? Ni1 O1 C13 C14A -152.9(19) 4 . . . ? Ni1 O1 C13 O2A 3.3(16) 4 . . . ? Ni1 O1 C13 O2A 3.3(16) . . . . ? Ni1 N1 C6 C5 180.0(3) 4 . . . ? Ni1 N1 C6 C5 180.0(3) . . . . ? Ni1 N1 C1 C2 178.0(3) . . . . ? Ni1 N1 C1 C2 178.0(3) 4 . . . ? Ni1 N2 C12 C11 -176.3(4) 4 . . . ? Ni1 N2 C12 C11 -176.3(4) . . . . ? Ni1 N2 C7 C8 176.0(4) 4 . . . ? Ni1 N2 C7 C8 176.0(4) . . . . ? O1 C13 C14 O3 -172.7(13) . . . . ? O1 C13 C14 C15 -5.3(9) . . . . ? O1 C13 C14A C15A 15.6(14) . . . . ? O1 C13 C14A O3A 170(2) . . . . ? N1 C6 C5 C3 2.3(4) . . . . ? N1 C1 C2 C3 1.7(5) . . . . ? N2 C12 C11 C9 -0.5(6) . . . . ? N2 C7 C8 C9 1.3(6) . . . . ? C6 C5 C3 C2 -0.3(5) . . . . ? C6 C5 C3 C4 179.3(4) . . . . ? C1 C2 C3 C5 -1.5(5) . . . . ? C1 C2 C3 C4 178.8(4) . . . . ? C2 C3 C4 C4 -170.9(6) . . . 5_556 ? O2 C13 C14 O3 -0.6(12) . . . . ? O2 C13 C14 C15 166.8(15) . . . . ? O2 C13 C14A C15A -165(2) . . . . ? O2 C13 C14A O3A -10.4(14) . . . . ? C12 C11 C9 C8 -0.8(7) . . . . ? C12 C11 C9 C10 177.5(6) . . . . ? C5 C3 C4 C4 9.5(5) . . . 5_556 ? C3 C4 C4 C3 180.0(6) . . 5_556 5_556 ? C13 C14 O3 C17 -175.9(18) . . . . ? C13 C14 C15 C16 -180(2) . . . . ? C13 C14A C15A C16A 178(4) . . . . ? C13 C14A O3A C17A 174(3) . . . . ? C11 C9 C8 C7 0.4(7) . . . . ? C11 C9 C10 C10 -10.1(8) . . . 5_667 ? C14 O3 C17 C16 -12.0(15) . . . . ? C14 C15 C16 C17 4.0(17) . . . . ? C7 C8 C9 C10 -177.9(5) . . . . ? C8 C9 C10 C10 168.1(8) . . . 5_667 ? C9 C10 C10 C9 -180.0(8) . . 5_667 5_667 ? O3 C17 C16 C15 4.8(11) . . . . ? C15A C14A O3A C17A -26(3) . . . . ? C15A C16A C17A O3A -9(2) . . . . ? C14A O3A C17A C16A 21(2) . . . . ? loop_ _restr_equal_distance_atom_site_label_1 _restr_equal_distance_atom_site_label_2 _restr_equal_distance_site_symmetry_2 _restr_equal_distance_class_id O2 C13 1 1 C13 C14 1 2 C13 O3 1 11 C13 C15 1 12 C13 C15A 1 12 C13 C14A 1 2 C13 O3A 1 11 C14 O3 1 3 C14 C17 1 13 C14 C15 1 4 C14 C16 1 14 O3 C17 1 6 O3 C15 1 5 O3 C16 1 8 C17 C15 1 10 C17 C16 1 7 C15 C16 1 9 C15A C16A 1 9 C14A C15A 1 4 C14A O3A 1 3 C14A C16A 1 14 C14A C17A 1 13 O3A C15A 1 5 O3A C16A 1 8 O3A C17A 1 6 C17A C15A 1 10 C17A C16A 1 7 O2A C13 1 1 loop_ _restr_equal_distance_class_class_id _restr_equal_distance_class_target_weight_param _restr_equal_distance_class_average _restr_equal_distance_class_esd _restr_equal_distance_class_diff_max 1 0.0200 1.2685 0.0027 0.0027 2 0.0200 1.4859 0.0010 0.0010 3 0.0200 1.3712 0.0200 0.0200 4 0.0200 1.3188 0.0117 0.0117 5 0.0400 2.1589 0.0420 0.0420 6 0.0200 1.3659 0.0293 0.0293 7 0.0200 1.2431 0.0015 0.0015 8 0.0400 2.1686 0.0596 0.0596 9 0.0200 1.4507 0.0007 0.0007 10 0.0400 2.1462 0.0173 0.0173 11 0.0400 2.4732 0.0320 0.0320 12 0.0400 2.5513 0.0214 0.0214 13 0.0400 2.1634 0.0275 0.0275 14 0.0400 2.2222 0.0050 0.0050 loop_ _restr_U_iso_atom_site_label _restr_U_iso_weight_param O2 0.0200 C14 0.0100 O3 0.0100 C17 0.0100 C15 0.0010 C16 0.0010 C18 0.0100 C15A 0.0010 C14A 0.0100 O3A 0.0100 C16A 0.0010 C17A 0.0100 O2A 0.0200