#------------------------------------------------------------------------------ #$Date: 2015-11-29 04:17:22 +0200 (Sun, 29 Nov 2015) $ #$Revision: 170598 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/24/13/2241364.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2241364 loop_ _publ_author_name 'Bommagani, Shobanbabu' 'Penthala, Narsimha R.' 'Parkin, Sean' 'Crooks, Peter A.' _publ_section_title ; Crystal structure of (E)-13-(pyrimidin-5-yl)parthenolide ; _journal_coeditor_code ZS2350 _journal_issue 12 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first 1536 _journal_page_last 1538 _journal_paper_doi 10.1107/S2056989015021507 _journal_volume 71 _journal_year 2015 _chemical_formula_iupac 'C19 H22 N2 O3' _chemical_formula_moiety 'C19 H22 N2 O3' _chemical_formula_sum 'C19 H22 N2 O3' _chemical_formula_weight 326.38 _chemical_name_common (E)-13-(Pyrimidin-5-yl)parthenolide _chemical_name_systematic ; (1aR,4E,7aS,8E,10aS,10bR)-1a,5-\ Dimethyl-8-[(pyrimidin-5-yl)methylidene]-2,3,6,7,7a,8,10a,10b-\ octahydrooxireno[2',3':9,10]cyclodeca[1,2-b]furan-9(1aH)-one ; _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_space_group_name_H-M 'P 1 21 1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 108.1210(6) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.3526(2) _cell_length_b 7.26120(10) _cell_length_c 11.9198(2) _cell_measurement_reflns_used 9908 _cell_measurement_temperature 90.0(2) _cell_measurement_theta_max 68.18 _cell_measurement_theta_min 4.49 _cell_volume 851.60(2) _computing_cell_refinement ; SAINT (Bruker, 2006) ; _computing_data_collection ; APEX2 (Bruker, 2006) ; _computing_data_reduction ; SAINT (Bruker, 2006) ; _computing_molecular_graphics ; XP in SHELXTL (Sheldrick, 2008) ; _computing_publication_material ; SHELXTL (Sheldrick, 2008) and CIFFIX (Parkin, 2013) ; _computing_structure_refinement ; SHELXL2014 (Sheldrick, 2015) ; _computing_structure_solution ; SHELXS97 (Sheldrick, 2008) ; _diffrn_ambient_temperature 90.0(2) _diffrn_detector_area_resol_mean 5.6 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.981 _diffrn_measurement_device_type 'Bruker X8 Proteum diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0323 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 11370 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.178 _diffrn_reflns_theta_min 4.494 _exptl_absorpt_coefficient_mu 0.700 _exptl_absorpt_correction_T_max 0.942 _exptl_absorpt_correction_T_min 0.850 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Bruker, 2006) ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.273 _exptl_crystal_description 'solvent-rounded block' _exptl_crystal_F_000 348 _exptl_crystal_size_max 0.250 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.100 _refine_diff_density_max 0.149 _refine_diff_density_min -0.135 _refine_ls_abs_structure_details ; Flack x determined using 1354 quotients [(I^+^)-(I^-^)]/[(I^+^)+(I^-^)] (Parsons et al., 2013). ; _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_extinction_coef 0.010(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL-2014 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 220 _refine_ls_number_reflns 3020 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0267 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0326P)^2^+0.1773P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.0678 _reflns_number_gt 3013 _reflns_number_total 3020 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL x14235 in P2(1) CELL 1.54178 10.3526 7.2612 11.9198 90.000 108.121 90.000 ZERR 2.00 0.00020 0.00010 0.00020 0.0000 0.0006 0.0000 LATT -1 SYMM -X, 1/2+Y, -Z SFAC C H N O UNIT 38 44 4 6 TEMP -183.000 SIZE 0.25 0.13 0.10 REM COLR colourless REM FORM solvent-rounded block REM No classical (i.e. strong) hydrogen bonds. L.S. 10 BOND $H ACTA HTAB CONF LIST 4 FMAP 2 PLAN 10 WGHT 0.032600 0.177300 EXTI 0.010299 FVAR 0.55286 O1 4 0.594278 0.240722 0.489573 11.00000 0.01879 0.03055 = 0.01762 0.00919 0.00351 0.00610 O2 4 0.306326 0.254861 0.438875 11.00000 0.01870 0.02004 = 0.02212 0.00644 0.00975 0.00384 O3 4 0.123966 0.292551 0.498548 11.00000 0.02420 0.03049 = 0.03034 0.00975 0.01619 0.00311 C1 1 0.576795 0.528528 0.199447 11.00000 0.02180 0.01629 = 0.01974 0.00245 0.00998 -0.00063 AFIX 43 H1A 2 0.583261 0.643921 0.238373 11.00000 -1.20000 AFIX 0 C2 1 0.703863 0.413362 0.232888 11.00000 0.01836 0.02084 = 0.02536 -0.00007 0.01014 -0.00184 AFIX 23 H2A 2 0.780879 0.488104 0.225697 11.00000 -1.20000 H2B 2 0.691545 0.307611 0.178133 11.00000 -1.20000 AFIX 0 C3 1 0.736756 0.341705 0.361155 11.00000 0.01574 0.02157 = 0.02279 -0.00044 0.00529 0.00157 AFIX 23 H3A 2 0.814596 0.255450 0.379216 11.00000 -1.20000 H3B 2 0.761535 0.445991 0.417285 11.00000 -1.20000 AFIX 0 C4 1 0.613220 0.244697 0.373448 11.00000 0.01630 0.01835 = 0.01737 0.00396 0.00307 0.00357 C5 1 0.510350 0.361539 0.400095 11.00000 0.01750 0.01732 = 0.01414 0.00309 0.00425 0.00203 AFIX 13 H5A 2 0.535297 0.494798 0.411770 11.00000 -1.20000 AFIX 0 C6 1 0.359774 0.325206 0.347533 11.00000 0.01728 0.01624 = 0.01545 0.00121 0.00684 0.00021 AFIX 13 H6A 2 0.344541 0.232062 0.282915 11.00000 -1.20000 AFIX 0 C7 1 0.278936 0.503620 0.297832 11.00000 0.01551 0.01474 = 0.01423 -0.00075 0.00410 -0.00114 AFIX 13 H7A 2 0.339580 0.611349 0.329236 11.00000 -1.20000 AFIX 0 C8 1 0.228001 0.518412 0.161744 11.00000 0.01722 0.02012 = 0.01429 0.00027 0.00337 0.00048 AFIX 23 H8A 2 0.143446 0.592283 0.137564 11.00000 -1.20000 H8B 2 0.205817 0.393591 0.127802 11.00000 -1.20000 AFIX 0 C9 1 0.333218 0.607765 0.110620 11.00000 0.02090 0.01951 = 0.01468 0.00436 0.00507 0.00177 AFIX 23 H9A 2 0.288431 0.635795 0.026135 11.00000 -1.20000 H9B 2 0.363772 0.725808 0.151908 11.00000 -1.20000 AFIX 0 C10 1 0.455907 0.488658 0.121759 11.00000 0.02214 0.01903 = 0.01500 0.00259 0.00918 0.00033 C11 1 0.168620 0.502701 0.356047 11.00000 0.01534 0.01697 = 0.01434 -0.00098 0.00311 -0.00207 C12 1 0.191001 0.342513 0.437184 11.00000 0.01659 0.02059 = 0.01873 0.00137 0.00651 0.00038 C13 1 0.068675 0.621192 0.352479 11.00000 0.01442 0.02129 = 0.01753 -0.00182 0.00436 -0.00113 AFIX 43 H13A 2 0.009610 0.587232 0.396080 11.00000 -1.20000 AFIX 0 C14 1 0.428761 0.326714 0.038637 11.00000 0.02582 0.03211 = 0.02190 -0.00612 0.00605 0.00414 AFIX 137 H14A 2 0.513977 0.260932 0.047312 11.00000 -1.50000 H14B 2 0.390787 0.370512 -0.042791 11.00000 -1.50000 H14C 2 0.363862 0.243367 0.057324 11.00000 -1.50000 AFIX 0 C15 1 0.575775 0.064302 0.309335 11.00000 0.02060 0.01773 = 0.03464 0.00051 0.01047 0.00226 AFIX 137 H15A 2 0.501189 0.007200 0.331128 11.00000 -1.50000 H15B 2 0.654776 -0.017890 0.331152 11.00000 -1.50000 H15C 2 0.546982 0.086149 0.223985 11.00000 -1.50000 AFIX 0 C16 1 0.039011 0.797723 0.289280 11.00000 0.01746 0.01905 = 0.01609 -0.00437 0.00321 0.00090 C17 1 0.135680 0.909724 0.266009 11.00000 0.01557 0.01892 = 0.03500 0.00195 0.00241 0.00051 AFIX 43 H17A 2 0.228076 0.871946 0.293337 11.00000 -1.20000 AFIX 0 N18 3 0.105382 1.068806 0.206838 11.00000 0.02091 0.02164 = 0.04086 0.00617 0.00295 -0.00138 C19 1 -0.025328 1.115579 0.172694 11.00000 0.02404 0.01829 = 0.02878 0.00188 0.00158 0.00213 AFIX 43 H19A 2 -0.048508 1.226472 0.128716 11.00000 -1.20000 AFIX 0 N20 3 -0.126970 1.024841 0.193125 11.00000 0.02063 0.02320 = 0.03040 0.00032 0.00425 0.00419 C21 1 -0.092914 0.867350 0.252794 11.00000 0.01937 0.02192 = 0.02530 -0.00241 0.00843 0.00256 AFIX 43 H21A 2 -0.162054 0.799402 0.271288 11.00000 -1.20000 AFIX 0 HKLF 4 REM x14235 in P2(1) REM R1 = 0.0267 for 3013 Fo > 4sig(Fo) and 0.0268 for all 3020 data REM 220 parameters refined using 1 restraints END WGHT 0.0326 0.1770 REM Instructions for potential hydrogen bonds EQIV $1 x, y-1, z HTAB C6 N18_$1 EQIV $2 -x+1, y+1/2, -z+1 HTAB C7 O1_$2 EQIV $3 -x, y+1/2, -z+1 HTAB C21 O3_$3 REM Highest difference peak 0.149, deepest hole -0.135, 1-sigma level 0.032 Q1 1 0.3209 0.4137 0.3087 11.00000 0.05 0.15 Q2 1 0.2805 0.5627 0.1382 11.00000 0.05 0.14 Q3 1 0.5340 0.5555 0.1244 11.00000 0.05 0.14 Q4 1 -0.0217 0.8330 0.2824 11.00000 0.05 0.14 Q5 1 0.2296 0.5321 0.3306 11.00000 0.05 0.13 Q6 1 0.2599 0.5095 0.2328 11.00000 0.05 0.13 Q7 1 0.6725 0.2973 0.3661 11.00000 0.05 0.13 Q8 1 0.5385 0.4947 0.4556 11.00000 0.05 0.13 Q9 1 0.1667 0.4172 0.3714 11.00000 0.05 0.13 Q10 1 0.4348 0.3498 0.3780 11.00000 0.05 0.12 ; _cod_data_source_file zs2350sup1.cif _cod_data_source_block I _cod_database_code 2241364 _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. ; _shelx_estimated_absorpt_t_min 0.844 _shelx_estimated_absorpt_t_max 0.933 _shelx_hkl_file ; -1 0 0 71.74 3.42 -1 0 0 69.88 3.40 -1 0 0 68.29 3.39 -1 0 0 67.82 3.27 -1 0 0 72.24 3.14 -2 0 0 0.73 0.07 -2 0 0 0.78 0.07 -2 0 0 0.77 0.08 2 0 0 0.73 0.08 -2 0 0 0.83 0.08 -2 0 0 0.88 0.09 -2 0 0 0.74 0.08 2 0 0 0.85 0.08 -2 0 0 0.71 0.07 -2 0 0 0.74 0.07 -3 0 0 5.01 0.24 -3 0 0 4.68 0.24 -3 0 0 5.16 0.29 -3 0 0 4.87 0.28 -3 0 0 4.66 0.27 3 0 0 5.04 0.26 -3 0 0 4.69 0.25 -3 0 0 5.05 0.25 -3 0 0 4.92 0.25 -3 0 0 5.17 0.25 3 0 0 5.04 0.26 -4 0 0 240.35 10.97 -4 0 0 241.20 11.94 4 0 0 249.31 10.99 -4 0 0 234.05 11.02 -4 0 0 256.86 12.04 -4 0 0 263.54 12.13 4 0 0 256.24 10.98 -4 0 0 241.79 10.96 -4 0 0 233.76 11.48 -5 0 0 45.13 2.11 -5 0 0 50.48 2.19 5 0 0 44.00 2.12 -5 0 0 50.32 2.31 -5 0 0 46.52 2.29 -5 0 0 49.96 2.29 -5 0 0 48.21 2.22 -5 0 0 43.14 2.12 -6 0 0 31.65 1.65 -6 0 0 32.63 1.55 -6 0 0 32.11 1.49 -6 0 0 34.34 1.49 -6 0 0 36.66 1.69 -6 0 0 33.09 1.55 -7 0 0 96.43 4.49 -7 0 0 92.57 3.91 -7 0 0 92.35 3.23 -7 0 0 95.17 3.71 -7 0 0 95.69 4.12 -7 0 0 91.60 4.10 -7 0 0 81.09 3.76 -8 0 0 0.37 0.11 -8 0 0 0.41 0.08 -8 0 0 0.25 0.10 -8 0 0 0.33 0.10 -8 0 0 0.27 0.03 -8 0 0 0.30 0.09 -9 0 0 0.14 0.07 -9 0 0 0.19 0.11 -9 0 0 0.12 0.06 -9 0 0 0.17 0.02 -10 0 0 9.49 0.51 -10 0 0 10.52 0.52 -10 0 0 9.74 0.48 -11 0 0 9.81 0.47 -11 0 0 10.34 0.50 0 -1 0 0.02 0.04 0 -1 0 0.06 0.05 0 1 0 0.11 0.03 0 1 0 0.00 0.04 0 1 0 0.04 0.05 -2 -1 0 113.04 5.25 -2 -1 0 113.49 5.50 -2 -1 0 107.98 5.04 -2 -1 0 101.67 5.40 -2 -1 0 101.59 5.23 -2 -1 0 117.51 5.03 2 -1 0 120.57 5.02 2 -1 0 111.28 4.98 -2 -1 0 112.16 5.05 -2 -1 0 115.15 5.01 -2 1 0 105.12 5.02 -2 1 0 106.81 5.46 -2 1 0 107.89 5.04 -2 1 0 112.44 4.99 2 1 0 118.31 5.02 -2 1 0 113.90 5.02 -2 1 0 97.39 5.37 2 1 0 119.56 5.04 -2 1 0 105.32 5.23 -2 1 0 113.32 5.48 -2 1 0 113.12 5.26 3 -1 0 71.64 3.06 -3 -1 0 64.99 3.10 -3 -1 0 71.04 3.06 3 -1 0 69.26 3.06 -3 -1 0 68.32 3.30 -3 -1 0 62.70 3.31 -3 -1 0 70.99 3.06 -3 -1 0 68.96 3.37 -3 -1 0 70.18 3.46 -3 -1 0 71.39 3.16 -3 -1 0 64.67 3.22 3 1 0 73.76 3.06 3 1 0 72.01 3.06 -3 1 0 71.97 3.31 -3 1 0 73.66 3.45 -3 1 0 68.26 3.42 -3 1 0 62.52 3.09 -3 1 0 62.24 3.19 -3 1 0 61.94 3.33 -3 1 0 68.90 3.14 -3 1 0 67.49 3.05 -3 1 0 68.75 3.06 4 -1 0 22.27 1.05 -4 -1 0 23.07 1.12 -4 -1 0 22.87 1.06 -4 -1 0 22.97 1.06 4 -1 0 21.44 1.05 -4 -1 0 24.23 1.14 -4 -1 0 22.41 1.04 -4 -1 0 21.23 1.09 -4 -1 0 21.97 1.02 -4 -1 0 24.30 1.02 -4 -1 0 22.34 1.04 -4 1 0 21.37 1.04 -4 1 0 23.15 1.06 4 1 0 22.60 1.05 -4 1 0 22.94 1.02 -4 1 0 20.90 1.04 -4 1 0 22.81 1.12 -4 1 0 20.82 1.02 -4 1 0 20.59 1.06 4 1 0 22.62 1.04 -4 1 0 23.28 1.13 -5 -1 0 130.98 6.01 -5 -1 0 141.92 6.58 -5 -1 0 126.44 6.21 -5 -1 0 135.33 6.26 -5 -1 0 119.30 5.94 -5 -1 0 134.70 6.55 -5 1 0 121.23 6.22 -5 1 0 139.07 6.62 -5 1 0 123.22 5.98 -5 1 0 138.40 6.05 -5 1 0 132.66 6.60 -5 1 0 142.85 6.30 -6 -1 0 90.74 3.75 -6 -1 0 91.08 4.18 -6 -1 0 94.16 4.29 -6 -1 0 89.83 3.56 -6 -1 0 87.32 3.95 -6 -1 0 83.12 4.15 -6 -1 0 84.66 3.95 -6 -1 0 95.36 4.03 -6 -1 0 87.79 3.09 -6 1 0 91.06 4.05 -6 1 0 76.15 4.13 -6 1 0 90.09 4.29 -6 1 0 87.39 3.93 -6 1 0 91.22 3.96 -6 1 0 88.81 4.21 -6 1 0 93.94 4.30 -6 1 0 82.15 3.97 -6 1 0 89.03 3.09 -6 1 0 88.76 3.75 -7 -1 0 20.54 0.89 -7 -1 0 20.90 0.98 -7 -1 0 19.53 0.97 -7 -1 0 21.19 1.11 -7 -1 0 21.26 0.93 -7 -1 0 20.11 0.74 -7 1 0 21.41 0.99 -7 1 0 20.71 1.09 -7 1 0 21.51 1.13 -7 1 0 21.64 0.94 -7 1 0 21.05 0.75 -7 1 0 21.43 0.98 -7 1 0 19.79 0.90 -8 -1 0 68.11 3.48 -8 -1 0 69.71 3.16 -8 -1 0 70.78 3.02 -8 -1 0 71.74 2.46 -8 -1 0 72.42 2.86 -8 -1 0 71.35 3.18 -8 1 0 70.70 2.91 -8 1 0 72.00 3.17 -8 1 0 65.91 3.48 -8 1 0 69.67 2.47 -8 1 0 71.97 3.18 -8 1 0 70.82 3.02 -9 -1 0 19.45 0.89 -9 -1 0 17.71 0.89 -9 -1 0 18.14 0.65 -9 -1 0 18.84 0.85 -9 1 0 18.92 0.89 -9 1 0 17.30 0.81 -9 1 0 18.58 0.84 -9 1 0 18.83 0.89 -9 1 0 18.32 0.65 -10 -1 0 1.78 0.14 -10 -1 0 1.81 0.16 -10 -1 0 1.66 0.17 -10 1 0 1.70 0.14 -10 1 0 1.66 0.15 -10 1 0 1.56 0.12 -11 -1 0 6.55 0.34 -11 -1 0 6.60 0.33 -11 -1 0 5.94 0.34 -11 1 0 6.43 0.32 -11 1 0 6.95 0.35 0 -2 0 154.33 7.29 0 -2 0 163.83 7.23 0 -2 0 152.65 7.81 0 -2 0 155.92 7.62 0 -2 0 166.69 7.26 0 2 0 155.73 7.61 0 2 0 154.15 7.76 0 2 0 156.44 7.28 0 2 0 164.09 7.24 0 2 0 169.90 7.27 -1 -2 0 58.58 2.63 -1 -2 0 56.74 2.79 -1 -2 0 57.72 2.87 1 -2 0 60.23 2.63 -1 -2 0 60.09 2.63 1 -2 0 54.47 2.71 -1 -2 0 60.16 2.66 1 -2 0 55.43 2.60 1 -2 0 61.45 2.64 1 2 0 52.80 2.71 1 2 0 53.25 2.80 1 2 0 61.91 2.64 -1 2 0 56.21 2.85 1 2 0 55.95 2.60 -1 2 0 57.61 2.77 -1 2 0 61.04 2.64 -1 2 0 59.99 2.63 -1 2 0 59.04 2.61 1 2 0 60.94 2.63 2 -2 0 119.67 5.17 -2 -2 0 122.03 5.18 -2 -2 0 127.49 5.81 2 -2 0 103.53 5.15 -2 -2 0 122.60 5.37 2 -2 0 108.53 5.37 -2 -2 0 114.83 5.52 2 -2 0 120.85 5.17 2 2 0 118.87 5.17 -2 2 0 116.60 5.17 2 2 0 98.80 5.37 -2 2 0 101.98 5.37 2 2 0 122.79 5.19 2 2 0 103.76 5.14 -2 2 0 119.78 5.34 -2 2 0 117.04 5.16 -2 2 0 125.78 5.59 -2 2 0 120.43 5.77 -3 -2 0 455.61 19.72 3 -2 0 447.48 19.71 -3 -2 0 423.43 19.67 -3 -2 0 474.37 21.51 -3 -2 0 411.61 20.62 -3 -2 0 460.64 21.32 -3 -2 0 375.44 19.72 3 -2 0 442.87 19.71 3 2 0 459.91 19.69 -3 2 0 426.08 19.69 3 2 0 437.77 19.69 -3 2 0 433.03 19.68 -3 2 0 452.52 21.40 -3 2 0 471.62 19.85 -3 2 0 460.82 21.39 -4 -2 0 63.15 3.10 -4 -2 0 65.35 3.13 -4 -2 0 62.39 2.95 -4 -2 0 64.90 3.10 -4 2 0 62.30 3.11 -4 2 0 65.46 3.11 -4 2 0 63.17 3.07 -4 2 0 65.74 2.97 -5 -2 0 40.76 1.87 -5 -2 0 38.92 1.79 -5 -2 0 39.96 1.99 -5 -2 0 39.79 1.96 -5 2 0 39.77 1.98 -5 2 0 37.82 1.80 -5 2 0 40.07 1.87 -5 2 0 40.30 1.98 -6 -2 0 12.25 0.59 -6 -2 0 11.75 0.59 -6 -2 0 11.94 0.44 -6 -2 0 12.60 0.57 -6 -2 0 12.73 0.68 -6 -2 0 12.71 0.60 -6 -2 0 11.89 0.48 -6 -2 0 12.09 0.54 -6 -2 0 11.79 0.56 -6 -2 0 13.01 0.70 -6 2 0 11.73 0.58 -6 2 0 11.44 0.48 -6 2 0 11.87 0.54 -6 2 0 11.70 0.45 -6 2 0 12.51 0.69 -6 2 0 12.16 0.60 -6 2 0 12.46 0.69 -6 2 0 12.12 0.60 -6 2 0 11.44 0.59 -6 2 0 11.62 0.56 -7 -2 0 15.01 0.83 -7 -2 0 15.00 0.72 -7 -2 0 12.92 0.70 -7 -2 0 15.31 0.68 -7 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9.27 -1 -3 0 191.79 8.42 1 -3 0 187.37 9.23 1 -3 0 184.49 8.95 1 -3 0 191.75 8.42 1 -3 0 187.21 8.51 1 3 0 173.01 8.88 1 3 0 185.51 8.49 -1 3 0 201.39 9.05 -1 3 0 194.63 9.29 -1 3 0 187.91 8.42 1 3 0 183.78 8.41 -1 3 0 197.95 8.73 1 3 0 170.63 9.08 1 3 0 196.56 8.43 -1 3 0 189.80 8.41 -2 -3 0 15.72 0.74 -2 -3 0 13.05 0.73 2 -3 0 13.12 0.72 -2 -3 0 14.14 0.68 -2 -3 0 14.14 0.72 -2 3 0 13.69 0.67 -2 3 0 12.34 0.71 -2 3 0 12.51 0.72 -2 3 0 13.70 0.72 2 3 0 14.99 0.74 -2 3 0 13.42 0.69 -3 -3 0 316.77 15.70 -3 -3 0 322.52 15.13 -3 -3 0 323.54 14.52 -3 3 0 311.86 14.57 -3 3 0 314.16 15.72 -3 3 0 330.39 15.18 -4 -3 0 102.85 5.00 -4 -3 0 102.10 4.72 -4 -3 0 104.18 4.96 -4 -3 0 101.28 4.98 -4 3 0 97.19 4.63 -4 3 0 105.41 4.95 -4 3 0 103.19 5.02 -5 -3 0 43.86 1.54 -5 -3 0 45.39 1.97 -5 -3 0 45.36 2.07 -5 -3 0 46.17 2.17 -5 -3 0 45.51 2.20 -5 -3 0 42.97 1.87 -5 -3 0 41.48 1.77 -5 -3 0 44.49 1.99 -5 -3 0 41.88 1.68 -5 -3 0 41.57 1.97 -5 3 0 42.80 1.87 -5 3 0 40.93 2.07 -5 3 0 43.59 1.81 -5 3 0 40.26 1.74 -5 3 0 46.31 2.08 -5 3 0 47.18 2.19 -5 3 0 43.21 1.55 -5 3 0 46.70 2.00 -5 3 0 38.32 1.97 -5 3 0 44.71 1.69 -6 -3 0 126.07 5.31 -6 -3 0 128.38 5.69 -6 -3 0 126.64 5.03 -6 -3 0 125.03 4.84 -6 -3 0 124.23 5.60 -6 -3 0 126.43 5.89 -6 -3 0 129.13 6.11 -6 -3 0 125.00 4.39 -6 -3 0 132.18 6.08 -6 3 0 125.25 5.14 -6 3 0 130.34 4.40 -6 3 0 126.23 5.31 -6 3 0 116.54 5.88 -6 3 0 121.24 5.94 -6 3 0 127.40 5.61 -6 3 0 119.80 5.57 -6 3 0 126.38 6.09 -6 3 0 125.38 4.80 -7 -3 0 48.62 2.49 -7 -3 0 51.17 2.24 -7 -3 0 48.82 1.88 -7 -3 0 52.74 1.74 -7 -3 0 52.80 2.13 -7 -3 0 49.65 2.02 -7 -3 0 45.99 2.29 -7 -3 0 47.75 2.47 -7 -3 0 46.72 2.19 -7 3 0 51.58 2.06 -7 3 0 50.44 1.89 -7 3 0 51.21 2.13 -7 3 0 49.54 2.23 -7 3 0 45.77 2.21 -7 3 0 50.13 1.74 -7 3 0 47.70 2.48 -7 3 0 46.04 2.30 -8 -3 0 12.63 0.63 -8 -3 0 13.00 0.47 -8 -3 0 11.97 0.58 -8 -3 0 12.71 0.61 -8 3 0 12.53 0.60 -8 3 0 12.98 0.59 -8 3 0 12.23 0.63 -8 3 0 12.92 0.47 -9 -3 0 45.05 1.62 -9 -3 0 46.99 2.01 -9 -3 0 45.06 2.11 -9 -3 0 46.53 1.90 -9 3 0 46.64 1.62 -9 3 0 45.26 2.00 -9 3 0 48.03 1.94 -9 3 0 46.47 2.10 -10 -3 0 23.64 1.11 -10 -3 0 25.37 1.07 -10 3 0 23.31 1.12 -10 3 0 23.95 1.03 -11 -3 0 1.72 0.11 -11 -3 0 1.91 0.13 -11 3 0 1.64 0.11 0 -4 0 639.21 29.93 0 -4 0 644.32 28.74 0 -4 0 642.53 30.74 0 4 0 612.81 29.92 0 4 0 642.86 30.61 0 4 0 639.24 28.75 -1 -4 0 109.86 5.02 -1 -4 0 116.17 5.23 -1 -4 0 110.36 5.38 -1 4 0 115.52 5.02 -1 4 0 107.07 5.22 -1 4 0 110.60 5.36 -2 -4 0 43.27 1.98 -2 -4 0 42.67 2.11 -2 -4 0 41.92 2.05 -2 4 0 43.41 2.05 -2 4 0 42.45 1.98 -2 4 0 41.91 2.11 -3 -4 0 9.63 0.56 -3 -4 0 10.19 0.54 -3 -4 0 8.84 0.41 -3 -4 0 9.93 0.53 -3 4 0 9.15 0.42 -3 4 0 10.20 0.53 -3 4 0 9.67 0.53 -3 4 0 9.70 0.56 -4 -4 0 43.35 2.08 -4 -4 0 42.30 1.93 -4 -4 0 42.19 2.01 -4 -4 0 39.84 1.68 -4 -4 0 40.36 1.62 -4 -4 0 40.52 1.89 -4 -4 0 41.28 1.49 -4 -4 0 43.15 2.11 -4 4 0 39.96 1.73 -4 4 0 38.30 1.49 -4 4 0 43.40 2.10 -4 4 0 42.38 2.01 -4 4 0 44.46 1.95 -4 4 0 42.09 1.68 -4 4 0 42.02 1.63 -5 -4 0 25.45 1.19 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0 0.93 0.10 -10 -4 0 0.95 0.11 -10 4 0 0.79 0.09 -10 4 0 0.78 0.09 -1 -5 0 108.78 4.37 -1 5 0 108.88 4.37 -2 -5 0 19.19 0.98 -2 -5 0 20.28 1.00 -2 -5 0 17.16 0.78 -2 -5 0 18.84 0.81 -2 5 0 20.06 0.98 -2 5 0 20.23 1.02 -2 5 0 18.74 0.99 -2 5 0 18.74 0.81 -3 -5 0 32.65 1.69 -3 -5 0 33.28 1.59 -3 -5 0 33.45 1.31 -3 -5 0 32.91 1.35 -3 -5 0 33.52 1.64 -3 -5 0 31.13 1.20 -3 5 0 31.75 1.31 -3 5 0 34.64 1.70 -3 5 0 33.86 1.64 -3 5 0 32.96 1.59 -3 5 0 33.86 1.36 -4 -5 0 119.80 4.71 -4 -5 0 123.93 4.15 -4 -5 0 114.52 5.71 -4 -5 0 123.53 4.54 -4 -5 0 120.34 5.27 -4 -5 0 116.82 5.32 -4 -5 0 115.09 5.75 -4 -5 0 112.22 5.54 -4 5 0 120.44 4.15 -4 5 0 115.48 5.54 -4 5 0 118.45 5.74 -4 5 0 116.38 4.72 -4 5 0 122.33 4.54 -4 5 0 112.60 4.82 -4 5 0 118.04 5.33 -5 -5 0 39.62 2.19 -5 -5 0 45.40 1.70 -5 -5 0 44.85 1.89 -5 -5 0 43.65 1.56 -5 -5 0 44.21 1.99 -5 5 0 42.18 1.82 -5 5 0 43.66 1.75 -5 5 0 40.68 2.21 -5 5 0 45.03 1.71 -5 5 0 44.27 2.10 -5 5 0 44.66 1.56 -6 -5 0 113.04 5.15 -6 -5 0 115.42 4.88 -6 -5 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0.89 -6 6 0 22.24 0.83 -7 -6 0 6.94 0.37 -7 -6 0 7.24 0.35 -7 -6 0 7.21 0.28 -7 6 0 7.31 0.29 -7 6 0 6.88 0.34 -7 6 0 6.81 0.38 -8 -6 0 4.09 0.25 -8 -6 0 5.08 0.19 -8 -6 0 4.81 0.25 -8 6 0 4.88 0.24 -8 6 0 5.00 0.19 0 -7 0 0.08 0.06 0 7 0 0.04 0.08 -1 -7 0 45.10 1.80 -1 7 0 42.39 1.80 -2 -7 0 71.34 2.88 -2 -7 0 70.09 3.21 -2 -7 0 69.38 2.77 -2 7 0 74.23 2.88 -3 -7 0 63.31 2.44 -3 -7 0 62.50 2.83 -3 -7 0 62.22 2.52 -3 7 0 64.10 2.45 -3 7 0 61.97 2.53 -4 -7 0 17.16 0.67 -4 -7 0 15.41 0.73 -4 -7 0 16.30 0.62 -4 -7 0 16.50 0.78 -4 7 0 17.01 0.83 -4 7 0 15.96 0.67 -4 7 0 16.32 0.68 -5 -7 0 2.20 0.18 -5 -7 0 1.91 0.14 -5 -7 0 2.30 0.12 -5 -7 0 2.01 0.12 -5 7 0 2.17 0.16 -5 7 0 2.16 0.13 -6 -7 0 9.02 0.34 -6 -7 0 8.48 0.41 -6 -7 0 8.07 0.43 -6 7 0 8.99 0.46 -6 7 0 8.97 0.35 -6 7 0 8.51 0.34 -7 -7 0 7.68 0.28 -7 7 0 7.59 0.29 0 -8 0 47.82 1.98 0 8 0 49.69 1.98 -1 -8 0 13.30 0.63 -1 -8 0 13.61 0.56 1 -8 0 13.33 0.57 1 8 0 11.94 0.57 -1 8 0 12.90 0.56 -2 -8 0 2.99 0.14 -2 -8 0 2.61 0.18 2 -8 0 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190.53 9.30 -3 0 1 29.02 1.32 3 0 -1 29.96 1.32 -3 0 1 27.44 1.35 -3 0 1 29.09 1.41 3 0 -1 29.36 1.33 -3 0 1 29.39 1.30 -3 0 1 26.19 1.30 -3 0 1 30.50 1.37 -3 0 1 29.00 1.32 1 0 -1 131.62 5.73 -1 0 1 132.04 5.73 -1 0 1 116.65 6.11 -1 0 1 129.92 5.97 1 0 -1 124.79 5.97 -1 0 -1 154.55 7.44 -1 0 -1 153.24 7.45 -1 0 -1 154.18 7.40 -1 0 -1 152.46 7.50 -2 0 -1 19.54 0.97 -2 0 -1 19.51 0.98 -2 0 -1 19.69 0.97 -2 0 -1 20.17 0.98 -3 0 -1 59.32 2.92 -3 0 -1 58.19 2.96 -3 0 -1 60.07 2.93 -3 0 -1 62.01 2.96 -4 0 -1 0.44 0.08 -4 0 -1 0.47 0.07 -4 0 -1 0.47 0.08 -4 0 -1 0.59 0.09 -5 0 -1 43.68 2.26 -5 0 -1 47.89 2.28 -5 0 -1 47.44 2.28 -6 0 -1 20.97 1.05 -6 0 -1 19.79 0.84 -6 0 -1 20.57 0.93 -6 0 -1 20.04 0.88 -6 0 -1 19.88 0.92 -6 0 -1 19.39 1.02 -6 0 -1 18.33 0.70 -7 0 -1 36.75 1.49 -7 0 -1 33.15 1.50 -7 0 -1 34.01 1.62 -7 0 -1 36.21 1.83 -7 0 -1 37.25 1.57 -7 0 -1 35.83 1.26 -7 0 -1 37.49 1.65 -7 0 -1 36.73 1.64 -8 0 -1 9.09 0.61 -8 0 -1 9.65 0.51 -8 0 -1 10.22 0.52 -8 0 -1 9.85 0.48 -8 0 -1 9.94 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1.16 -4 2 -11 24.60 1.08 9 -3 -11 20.62 0.85 -9 -3 11 20.02 0.84 -9 3 11 21.16 0.84 9 3 -11 20.73 0.85 8 -3 -11 32.15 1.29 -8 -3 11 31.64 1.29 8 3 -11 31.58 1.29 -8 3 11 30.61 1.30 -7 -3 11 10.78 0.51 7 -3 -11 11.56 0.49 7 3 -11 11.95 0.50 -7 3 11 10.73 0.51 6 -3 -11 1.43 0.12 6 -3 -11 1.30 0.12 6 3 -11 1.44 0.14 6 3 -11 1.59 0.12 5 -3 -11 34.85 1.44 5 -3 -11 36.29 1.41 5 3 -11 36.58 1.41 5 3 -11 34.72 1.44 4 -3 -11 8.79 0.41 4 -3 -11 8.54 0.38 4 -3 -11 7.70 0.34 4 -3 -11 8.30 0.35 4 3 -11 7.92 0.42 4 3 -11 8.02 0.35 4 3 -11 8.46 0.43 4 3 -11 8.81 0.37 3 -3 -11 19.94 0.85 3 -3 -11 18.69 0.93 3 -3 -11 19.86 0.75 3 -3 -11 20.90 0.81 3 3 -11 19.94 0.74 3 3 -11 19.29 0.93 3 3 -11 20.66 0.80 3 3 -11 19.51 0.92 2 -3 -11 11.07 0.56 2 -3 -11 11.06 0.52 2 -3 -11 10.69 0.46 2 -3 -11 11.20 0.45 2 3 -11 11.50 0.56 2 3 -11 11.76 0.56 2 3 -11 12.03 0.44 2 3 -11 11.29 0.46 1 -3 -11 30.68 1.25 1 -3 -11 28.87 1.37 1 -3 -11 30.52 1.08 1 3 -11 29.10 1.14 1 3 -11 29.67 1.08 1 3 -11 30.58 1.35 0 -3 -11 5.69 0.33 0 -3 -11 6.20 0.31 0 -3 -11 5.82 0.24 0 3 -11 5.98 0.24 0 3 -11 6.26 0.34 -1 -3 -11 8.73 0.32 -1 -3 -11 8.64 0.45 -1 -3 -11 8.98 0.41 -1 3 -11 8.60 0.47 -1 3 -11 9.26 0.45 -1 3 -11 9.12 0.32 -2 -3 -11 7.80 0.38 -2 -3 -11 8.85 0.44 -2 3 -11 7.80 0.44 -2 3 -11 9.36 0.43 -3 -3 -11 5.65 0.27 -3 3 -11 5.54 0.31 -3 3 -11 5.77 0.29 8 -4 -11 0.94 0.07 -8 -4 11 0.98 0.07 -8 4 11 0.97 0.07 8 4 -11 0.89 0.07 7 -4 -11 8.60 0.39 7 4 -11 9.62 0.39 6 -4 -11 5.23 0.24 6 -4 -11 5.14 0.26 6 4 -11 5.55 0.24 6 4 -11 5.32 0.25 5 -4 -11 2.34 0.16 5 -4 -11 2.07 0.10 5 -4 -11 2.18 0.16 5 4 -11 2.24 0.11 5 4 -11 2.04 0.15 5 4 -11 2.26 0.14 4 -4 -11 35.27 1.35 4 -4 -11 36.84 1.42 4 -4 -11 34.61 1.24 4 4 -11 32.90 1.55 4 4 -11 35.55 1.35 4 4 -11 30.87 1.52 3 -4 -11 25.34 0.97 3 -4 -11 26.86 1.11 3 -4 -11 25.97 1.04 3 4 -11 27.56 1.04 3 4 -11 27.09 1.20 3 4 -11 25.93 0.96 2 -4 -11 1.67 0.17 2 -4 -11 1.84 0.10 2 -4 -11 1.87 0.12 2 4 -11 1.70 0.12 2 4 -11 1.79 0.10 2 4 -11 1.55 0.14 1 -4 -11 28.08 1.06 1 -4 -11 30.17 1.23 1 4 -11 29.13 1.32 1 4 -11 30.54 1.06 0 -4 -11 1.05 0.12 0 -4 -11 1.07 0.07 0 4 -11 1.10 0.11 0 4 -11 1.15 0.08 -1 -4 -11 5.61 0.27 -1 -4 -11 4.93 0.28 -1 4 -11 5.19 0.19 -1 4 -11 6.17 0.29 -2 4 -11 22.41 1.00 6 -5 -11 29.57 1.21 5 -5 -11 3.41 0.18 5 -5 -11 3.62 0.19 5 5 -11 3.64 0.18 4 -5 -11 28.15 1.17 4 -5 -11 27.62 1.11 4 5 -11 29.51 1.11 3 -5 -11 2.15 0.13 3 -5 -11 2.21 0.14 3 5 -11 1.91 0.11 3 5 -11 2.00 0.10 3 5 -11 2.03 0.14 2 -5 -11 1.09 0.09 2 -5 -11 1.08 0.10 2 5 -11 0.88 0.07 1 -5 -11 3.22 0.14 1 -5 -11 3.34 0.18 1 5 -11 3.10 0.14 1 5 -11 3.37 0.20 0 -5 -11 10.27 0.37 0 5 -11 9.75 0.37 0 5 -11 10.78 0.48 -9 0 12 5.96 0.33 -9 0 12 7.15 0.30 9 0 -12 6.76 0.33 9 0 -12 6.54 0.30 8 0 -12 16.73 0.67 -8 0 12 15.38 0.68 8 0 -12 15.61 0.75 7 0 -12 8.12 0.36 7 0 -12 8.11 0.42 7 0 -12 7.91 0.36 6 0 -12 3.96 0.19 6 0 -12 3.94 0.26 6 0 -12 3.73 0.22 5 0 -12 13.42 0.56 5 0 -12 13.21 0.64 5 0 -12 12.60 0.54 4 0 -12 0.87 0.12 4 0 -12 0.84 0.09 4 0 -12 0.91 0.10 3 0 -12 2.61 0.15 3 0 -12 2.25 0.18 3 0 -12 2.44 0.14 2 0 -12 16.68 0.79 2 0 -12 16.50 0.61 2 0 -12 15.96 0.64 1 0 -12 101.13 4.32 1 0 -12 100.12 3.40 1 0 -12 90.07 4.23 0 0 -12 7.52 0.28 0 0 -12 7.42 0.39 0 0 -12 7.54 0.41 -1 0 -12 3.08 0.21 -1 0 -12 3.10 0.20 -2 0 -12 1.80 0.14 -2 0 -12 2.09 0.15 -3 0 -12 14.39 0.66 9 -1 -12 4.80 0.25 -9 -1 12 5.70 0.29 -9 -1 12 5.62 0.25 9 1 -12 5.51 0.25 -9 1 12 5.66 0.25 8 -1 -12 11.88 0.54 -8 -1 12 12.59 0.55 -8 1 12 12.54 0.55 8 1 -12 13.50 0.54 7 -1 -12 7.25 0.35 7 -1 -12 7.47 0.39 7 -1 -12 7.73 0.34 7 1 -12 7.54 0.35 7 1 -12 7.67 0.34 6 -1 -12 26.82 1.09 6 -1 -12 27.15 1.22 6 -1 -12 26.62 1.07 6 1 -12 26.81 1.06 6 1 -12 25.89 1.23 6 1 -12 26.09 1.09 5 -1 -12 27.72 1.21 5 -1 -12 26.72 1.04 5 -1 -12 24.37 1.05 5 1 -12 26.11 1.04 5 1 -12 25.38 1.05 5 1 -12 26.18 1.21 4 -1 -12 17.90 0.83 4 -1 -12 16.88 0.70 4 -1 -12 17.08 0.65 4 1 -12 16.44 0.64 4 1 -12 17.27 0.70 4 1 -12 17.12 0.82 3 -1 -12 1.75 0.12 3 -1 -12 1.74 0.16 3 -1 -12 1.67 0.11 3 1 -12 1.80 0.16 3 1 -12 1.71 0.12 3 1 -12 1.69 0.11 2 -1 -12 50.63 1.94 2 -1 -12 50.62 1.79 2 -1 -12 50.56 2.28 2 1 -12 52.26 2.28 2 1 -12 51.73 1.79 2 1 -12 50.29 1.94 2 1 -12 47.43 2.23 1 -1 -12 5.72 0.32 1 -1 -12 5.46 0.23 1 1 -12 5.58 0.32 1 1 -12 5.46 0.23 1 1 -12 5.36 0.30 0 -1 -12 3.24 0.13 0 -1 -12 2.94 0.20 0 -1 -12 3.42 0.24 0 1 -12 3.48 0.21 0 1 -12 3.33 0.14 0 1 -12 2.99 0.21 0 1 -12 3.31 0.22 -1 -1 -12 5.89 0.32 -1 -1 -12 5.59 0.31 -1 1 -12 6.02 0.32 -1 1 -12 5.66 0.30 -1 1 -12 5.29 0.32 -2 -1 -12 12.99 0.56 -2 -1 -12 9.78 0.53 -2 1 -12 11.34 0.54 -3 -1 -12 3.54 0.19 -3 1 -12 3.04 0.18 9 -2 -12 7.89 0.34 -9 -2 12 7.93 0.34 9 2 -12 7.64 0.34 -9 2 12 8.29 0.34 -8 -2 12 5.48 0.26 8 -2 -12 5.49 0.25 8 2 -12 5.54 0.26 7 -2 -12 10.18 0.45 7 -2 -12 10.39 0.44 7 2 -12 10.11 0.44 7 2 -12 9.98 0.44 6 -2 -12 0.58 0.09 6 -2 -12 0.63 0.07 6 2 -12 0.53 0.07 6 2 -12 0.69 0.08 5 -2 -12 42.15 1.96 5 -2 -12 43.29 1.78 5 -2 -12 45.56 1.71 5 2 -12 41.81 1.74 5 2 -12 43.85 1.71 5 2 -12 45.39 1.97 4 -2 -12 50.73 2.14 4 -2 -12 51.72 2.36 4 -2 -12 51.01 1.87 4 -2 -12 54.40 2.04 4 2 -12 54.08 2.04 4 2 -12 54.23 2.36 4 2 -12 51.76 1.87 3 -2 -12 9.54 0.38 3 -2 -12 9.48 0.49 3 -2 -12 9.20 0.44 3 -2 -12 9.76 0.40 3 2 -12 9.66 0.38 3 2 -12 10.21 0.50 3 2 -12 9.01 0.46 3 2 -12 9.43 0.39 2 -2 -12 2.12 0.15 2 -2 -12 2.20 0.17 2 -2 -12 2.32 0.13 2 -2 -12 2.08 0.09 2 2 -12 2.18 0.15 2 2 -12 2.34 0.13 2 2 -12 2.24 0.10 2 2 -12 2.25 0.17 1 -2 -12 1.66 0.09 1 -2 -12 1.48 0.17 1 -2 -12 1.52 0.12 1 2 -12 1.51 0.13 1 2 -12 1.57 0.14 1 2 -12 1.87 0.10 0 -2 -12 6.39 0.24 0 -2 -12 6.56 0.36 0 2 -12 6.72 0.34 0 2 -12 6.50 0.25 0 2 -12 6.47 0.34 -1 -2 -12 10.55 0.50 -1 -2 -12 11.82 0.53 -1 2 -12 10.56 0.54 -1 2 -12 9.78 0.51 -2 -2 -12 9.45 0.45 -2 2 -12 9.44 0.44 -2 2 -12 8.26 0.46 -8 -3 12 14.57 0.61 8 -3 -12 15.62 0.60 -8 3 12 12.77 0.61 8 3 -12 15.41 0.60 7 -3 -12 5.65 0.22 7 -3 -12 5.29 0.24 -7 -3 12 5.18 0.26 -7 3 12 5.23 0.26 7 3 -12 4.89 0.22 7 3 -12 4.29 0.23 6 -3 -12 1.60 0.14 6 -3 -12 1.65 0.12 6 -3 -12 1.37 0.07 6 3 -12 1.78 0.14 6 3 -12 1.54 0.08 6 3 -12 1.74 0.14 5 -3 -12 27.92 1.07 5 -3 -12 25.76 1.12 5 3 -12 26.19 1.23 5 3 -12 28.02 1.07 4 -3 -12 18.69 0.79 4 -3 -12 19.03 0.74 4 -3 -12 18.66 0.69 4 3 -12 18.48 0.68 4 3 -12 18.57 0.86 4 3 -12 17.38 0.74 3 -3 -12 2.84 0.14 3 -3 -12 2.87 0.16 3 -3 -12 2.88 0.20 3 3 -12 2.83 0.18 3 3 -12 3.02 0.16 3 3 -12 2.61 0.18 3 3 -12 2.98 0.15 2 -3 -12 49.94 2.33 2 -3 -12 52.54 1.85 2 -3 -12 54.48 2.13 2 3 -12 48.29 2.33 2 3 -12 53.14 2.30 2 3 -12 55.03 1.85 1 -3 -12 9.97 0.45 1 -3 -12 10.14 0.38 1 -3 -12 9.51 0.50 1 3 -12 10.04 0.49 1 3 -12 10.44 0.38 0 -3 -12 24.22 0.99 0 -3 -12 23.55 1.09 0 -3 -12 23.89 0.84 0 3 -12 23.12 1.07 0 3 -12 24.64 0.84 -1 -3 -12 6.28 0.29 -1 -3 -12 6.21 0.32 6 -4 -12 24.38 0.88 6 4 -12 20.14 1.00 5 -4 -12 3.80 0.20 5 -4 -12 3.95 0.18 5 4 -12 3.88 0.18 5 4 -12 3.29 0.20 4 -4 -12 2.87 0.17 4 -4 -12 2.60 0.15 4 -4 -12 2.98 0.14 4 4 -12 2.92 0.15 4 4 -12 2.60 0.16 4 4 -12 2.88 0.14 3 -4 -12 5.35 0.27 3 -4 -12 4.93 0.21 3 4 -12 4.88 0.21 3 4 -12 5.01 0.21 2 -4 -12 16.07 0.77 2 -4 -12 19.06 0.67 2 4 -12 19.75 0.67 1 -4 -12 2.06 0.13 1 -4 -12 2.14 0.10 1 4 -12 2.09 0.10 0 4 -12 13.12 0.60 8 0 -13 0.19 0.07 8 0 -13 0.29 0.03 7 0 -13 42.10 1.83 7 0 -13 39.38 1.59 6 0 -13 0.13 0.07 6 0 -13 0.08 0.06 5 0 -13 1.81 0.15 5 0 -13 1.74 0.13 5 0 -13 1.75 0.11 4 0 -13 30.31 1.09 4 0 -13 30.34 1.38 4 0 -13 30.20 1.18 3 0 -13 0.99 0.10 3 0 -13 0.64 0.05 3 0 -13 0.80 0.11 2 0 -13 26.83 0.96 2 0 -13 26.61 1.23 1 0 -13 15.39 0.72 1 0 -13 14.72 0.54 0 0 -13 57.91 2.25 0 0 -13 42.26 2.18 -1 0 -13 5.51 0.31 -1 0 -13 7.49 0.33 -8 -1 13 0.48 0.06 8 1 -13 0.39 0.03 8 1 -13 0.47 0.07 7 -1 -13 1.32 0.12 7 -1 -13 1.17 0.10 7 1 -13 1.20 0.12 7 1 -13 1.13 0.11 6 -1 -13 1.19 0.11 6 -1 -13 1.18 0.12 6 1 -13 1.13 0.12 6 1 -13 1.03 0.09 5 -1 -13 17.32 0.67 5 -1 -13 17.17 0.78 5 -1 -13 15.76 0.62 5 1 -13 16.09 0.78 5 1 -13 16.17 0.62 5 1 -13 16.89 0.67 4 -1 -13 3.99 0.19 4 -1 -13 4.08 0.26 4 -1 -13 3.99 0.19 4 1 -13 4.03 0.24 4 1 -13 4.07 0.19 4 1 -13 4.12 0.19 3 -1 -13 7.71 0.31 3 -1 -13 7.78 0.41 3 1 -13 8.07 0.41 3 1 -13 7.40 0.31 2 -1 -13 19.22 0.91 2 -1 -13 19.22 0.70 2 1 -13 19.30 0.91 2 1 -13 19.65 0.70 1 -1 -13 6.55 0.25 1 -1 -13 7.17 0.36 1 1 -13 7.12 0.36 1 1 -13 6.11 0.34 1 1 -13 6.66 0.25 0 -1 -13 10.77 0.50 0 1 -13 9.34 0.48 0 1 -13 9.83 0.47 -1 1 -13 2.20 0.13 7 -2 -13 14.80 0.62 7 2 -13 15.99 0.72 6 -2 -13 0.67 0.08 6 2 -13 0.45 0.08 6 2 -13 0.52 0.06 5 -2 -13 5.90 0.25 5 -2 -13 4.90 0.23 5 2 -13 5.07 0.24 5 2 -13 5.57 0.30 5 2 -13 5.78 0.25 4 -2 -13 11.09 0.43 4 -2 -13 10.89 0.45 4 2 -13 11.01 0.54 4 2 -13 11.35 0.45 4 2 -13 11.12 0.42 3 -2 -13 12.06 0.62 3 -2 -13 13.63 0.49 3 2 -13 13.31 0.49 3 2 -13 13.42 0.63 2 -2 -13 18.06 0.83 2 -2 -13 18.48 0.64 2 2 -13 18.38 0.64 2 2 -13 15.63 0.82 1 -2 -13 0.11 0.02 1 -2 -13 0.21 0.07 1 2 -13 0.14 0.03 1 2 -13 0.08 0.04 1 2 -13 0.20 0.07 0 -2 -13 2.58 0.17 0 2 -13 2.75 0.16 6 3 -13 16.57 0.77 6 3 -13 17.02 0.66 5 -3 -13 9.20 0.38 5 -3 -13 9.49 0.41 5 3 -13 8.89 0.45 5 3 -13 9.82 0.38 4 -3 -13 3.60 0.16 4 -3 -13 3.42 0.14 4 3 -13 3.59 0.20 4 3 -13 3.59 0.15 3 -3 -13 1.54 0.12 3 -3 -13 1.42 0.09 3 3 -13 1.18 0.08 2 -3 -13 4.14 0.21 2 -3 -13 4.61 0.18 2 3 -13 4.52 0.23 2 3 -13 4.80 0.18 1 3 -13 6.40 0.32 6 0 -14 0.76 0.07 5 0 -14 6.70 0.27 5 0 -14 7.52 0.36 5 0 -14 6.67 0.27 4 0 -14 7.01 0.34 4 0 -14 6.27 0.26 3 0 -14 5.82 0.32 3 0 -14 6.53 0.24 2 0 -14 4.25 0.16 2 0 -14 4.45 0.24 6 -1 -14 5.64 0.24 6 1 -14 6.17 0.30 6 1 -14 5.92 0.24 5 -1 -14 14.12 0.53 5 1 -14 14.93 0.68 4 -1 -14 2.69 0.17 4 -1 -14 2.74 0.13 4 1 -14 2.87 0.17 4 1 -14 2.75 0.13 3 -1 -14 10.44 0.41 3 1 -14 11.57 0.42 3 1 -14 11.99 0.55 2 -1 -14 59.46 2.07 2 -1 -14 57.81 2.63 2 1 -14 60.79 2.07 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 92522 _shelx_res_checksum 54045 _shelxl_version_number 2.014 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy O O1 0.59428(12) 0.24072(19) 0.48957(10) 0.0228(3) Uani d 1 O O2 0.30633(12) 0.25486(17) 0.43887(10) 0.0195(3) Uani d 1 O O3 0.12397(13) 0.29255(19) 0.49855(11) 0.0266(3) Uani d 1 C C1 0.57679(17) 0.5285(2) 0.19945(14) 0.0185(4) Uani d 1 H H1A 0.5833 0.6439 0.2384 0.022 Uiso calc 1 C C2 0.70386(17) 0.4134(3) 0.23289(16) 0.0208(4) Uani d 1 H H2A 0.7809 0.4881 0.2257 0.025 Uiso calc 1 H H2B 0.6915 0.3076 0.1781 0.025 Uiso calc 1 C C3 0.73676(17) 0.3417(3) 0.36116(15) 0.0202(4) Uani d 1 H H3A 0.8146 0.2554 0.3792 0.024 Uiso calc 1 H H3B 0.7615 0.4460 0.4173 0.024 Uiso calc 1 C C4 0.61322(17) 0.2447(2) 0.37345(14) 0.0178(4) Uani d 1 C C5 0.51035(16) 0.3615(2) 0.40010(13) 0.0165(3) Uani d 1 H H5A 0.5353 0.4948 0.4118 0.020 Uiso calc 1 C C6 0.35977(16) 0.3252(2) 0.34753(14) 0.0159(3) Uani d 1 H H6A 0.3445 0.2321 0.2829 0.019 Uiso calc 1 C C7 0.27894(16) 0.5036(2) 0.29783(13) 0.0149(3) Uani d 1 H H7A 0.3396 0.6113 0.3292 0.018 Uiso calc 1 C C8 0.22800(16) 0.5184(3) 0.16174(14) 0.0176(4) Uani d 1 H H8A 0.1434 0.5923 0.1376 0.021 Uiso calc 1 H H8B 0.2058 0.3936 0.1278 0.021 Uiso calc 1 C C9 0.33322(17) 0.6078(3) 0.11062(14) 0.0185(4) Uani d 1 H H9A 0.2884 0.6358 0.0261 0.022 Uiso calc 1 H H9B 0.3638 0.7258 0.1519 0.022 Uiso calc 1 C C10 0.45591(17) 0.4887(2) 0.12176(14) 0.0179(4) Uani d 1 C C11 0.16862(16) 0.5027(2) 0.35605(14) 0.0159(3) Uani d 1 C C12 0.19100(17) 0.3425(3) 0.43718(14) 0.0184(4) Uani d 1 C C13 0.06867(17) 0.6212(3) 0.35248(14) 0.0179(4) Uani d 1 H H13A 0.0096 0.5872 0.3961 0.021 Uiso calc 1 C C14 0.42876(19) 0.3267(3) 0.03864(16) 0.0269(4) Uani d 1 H H14A 0.5140 0.2609 0.0473 0.040 Uiso calc 1 H H14B 0.3908 0.3705 -0.0428 0.040 Uiso calc 1 H H14C 0.3639 0.2434 0.0573 0.040 Uiso calc 1 C C15 0.57578(18) 0.0643(2) 0.30934(18) 0.0239(4) Uani d 1 H H15A 0.5012 0.0072 0.3311 0.036 Uiso calc 1 H H15B 0.6548 -0.0179 0.3312 0.036 Uiso calc 1 H H15C 0.5470 0.0861 0.2240 0.036 Uiso calc 1 C C16 0.03901(16) 0.7977(2) 0.28928(14) 0.0180(4) Uani d 1 C C17 0.13568(18) 0.9097(3) 0.26601(18) 0.0244(4) Uani d 1 H H17A 0.2281 0.8719 0.2933 0.029 Uiso calc 1 N N18 0.10538(16) 1.0688(2) 0.20684(16) 0.0293(4) Uani d 1 C C19 -0.02533(19) 1.1156(3) 0.17269(17) 0.0252(4) Uani d 1 H H19A -0.0485 1.2265 0.1287 0.030 Uiso calc 1 N N20 -0.12697(15) 1.0248(2) 0.19312(14) 0.0256(4) Uani d 1 C C21 -0.09291(18) 0.8673(3) 0.25279(15) 0.0219(4) Uani d 1 H H21A -0.1621 0.7994 0.2713 0.026 Uiso calc 1 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 O1 0.0188(6) 0.0306(7) 0.0176(6) 0.0061(5) 0.0035(5) 0.0092(5) O2 0.0187(6) 0.0200(6) 0.0221(6) 0.0038(5) 0.0098(5) 0.0064(5) O3 0.0242(6) 0.0305(8) 0.0303(7) 0.0031(6) 0.0162(5) 0.0097(6) C1 0.0218(8) 0.0163(8) 0.0197(8) -0.0006(7) 0.0100(7) 0.0024(7) C2 0.0184(8) 0.0208(9) 0.0254(9) -0.0018(7) 0.0101(7) -0.0001(7) C3 0.0157(8) 0.0216(9) 0.0228(8) 0.0016(7) 0.0053(6) -0.0004(7) C4 0.0163(8) 0.0184(8) 0.0174(8) 0.0036(7) 0.0031(6) 0.0040(7) C5 0.0175(8) 0.0173(8) 0.0141(7) 0.0020(7) 0.0043(6) 0.0031(6) C6 0.0173(8) 0.0162(8) 0.0154(7) 0.0002(6) 0.0068(6) 0.0012(6) C7 0.0155(7) 0.0147(8) 0.0142(7) -0.0011(6) 0.0041(6) -0.0008(6) C8 0.0172(8) 0.0201(8) 0.0143(8) 0.0005(7) 0.0034(6) 0.0003(7) C9 0.0209(8) 0.0195(8) 0.0147(7) 0.0018(7) 0.0051(6) 0.0044(7) C10 0.0221(8) 0.0190(9) 0.0150(7) 0.0003(7) 0.0092(7) 0.0026(7) C11 0.0153(7) 0.0170(8) 0.0143(7) -0.0021(7) 0.0031(6) -0.0010(7) C12 0.0166(8) 0.0206(9) 0.0187(8) 0.0004(7) 0.0065(6) 0.0014(7) C13 0.0144(8) 0.0213(9) 0.0175(8) -0.0011(7) 0.0044(6) -0.0018(7) C14 0.0258(9) 0.0321(11) 0.0219(8) 0.0041(8) 0.0061(7) -0.0061(8) C15 0.0206(8) 0.0177(9) 0.0346(10) 0.0023(7) 0.0105(8) 0.0005(7) C16 0.0175(8) 0.0190(9) 0.0161(7) 0.0009(7) 0.0032(6) -0.0044(7) C17 0.0156(8) 0.0189(9) 0.0350(10) 0.0005(7) 0.0024(8) 0.0019(8) N18 0.0209(8) 0.0216(9) 0.0409(10) -0.0014(6) 0.0030(7) 0.0062(7) C19 0.0240(9) 0.0183(9) 0.0288(9) 0.0021(8) 0.0016(7) 0.0019(8) N20 0.0206(8) 0.0232(8) 0.0304(8) 0.0042(6) 0.0043(6) 0.0003(7) C21 0.0194(8) 0.0219(9) 0.0253(9) 0.0026(7) 0.0084(7) -0.0024(7) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C5 O1 C4 60.94(10) C12 O2 C6 111.31(12) C10 C1 C2 128.05(17) C10 C1 H1A 116.0 C2 C1 H1A 116.0 C1 C2 C3 110.73(14) C1 C2 H2A 109.5 C3 C2 H2A 109.5 C1 C2 H2B 109.5 C3 C2 H2B 109.5 H2A C2 H2B 108.1 C4 C3 C2 108.68(14) C4 C3 H3A 110.0 C2 C3 H3A 110.0 C4 C3 H3B 110.0 C2 C3 H3B 110.0 H3A C3 H3B 108.3 O1 C4 C5 59.08(10) O1 C4 C15 112.05(15) C5 C4 C15 121.46(15) O1 C4 C3 118.08(14) C5 C4 C3 116.40(15) C15 C4 C3 116.73(15) O1 C5 C4 59.97(10) O1 C5 C6 120.41(14) C4 C5 C6 122.16(14) O1 C5 H5A 114.5 C4 C5 H5A 114.5 C6 C5 H5A 114.5 O2 C6 C5 109.48(12) O2 C6 C7 106.97(12) C5 C6 C7 112.07(13) O2 C6 H6A 109.4 C5 C6 H6A 109.4 C7 C6 H6A 109.4 C11 C7 C8 115.01(13) C11 C7 C6 102.45(13) C8 C7 C6 115.15(13) C11 C7 H7A 107.9 C8 C7 H7A 107.9 C6 C7 H7A 107.9 C7 C8 C9 112.99(13) C7 C8 H8A 109.0 C9 C8 H8A 109.0 C7 C8 H8B 109.0 C9 C8 H8B 109.0 H8A C8 H8B 107.8 C10 C9 C8 113.70(14) C10 C9 H9A 108.8 C8 C9 H9A 108.8 C10 C9 H9B 108.8 C8 C9 H9B 108.8 H9A C9 H9B 107.7 C1 C10 C14 124.58(16) C1 C10 C9 121.22(16) C14 C10 C9 114.20(15) C13 C11 C12 119.20(15) C13 C11 C7 132.19(16) C12 C11 C7 108.42(13) O3 C12 O2 121.43(16) O3 C12 C11 128.78(16) O2 C12 C11 109.75(13) C11 C13 C16 127.89(16) C11 C13 H13A 116.1 C16 C13 H13A 116.1 C10 C14 H14A 109.5 C10 C14 H14B 109.5 H14A C14 H14B 109.5 C10 C14 H14C 109.5 H14A C14 H14C 109.5 H14B C14 H14C 109.5 C4 C15 H15A 109.5 C4 C15 H15B 109.5 H15A C15 H15B 109.5 C4 C15 H15C 109.5 H15A C15 H15C 109.5 H15B C15 H15C 109.5 C17 C16 C21 115.11(16) C17 C16 C13 124.52(15) C21 C16 C13 120.31(15) N18 C17 C16 123.19(16) N18 C17 H17A 118.4 C16 C17 H17A 118.4 C19 N18 C17 115.52(17) N20 C19 N18 127.34(18) N20 C19 H19A 116.3 N18 C19 H19A 116.3 C19 N20 C21 115.48(15) N20 C21 C16 123.23(17) N20 C21 H21A 118.4 C16 C21 H21A 118.4 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C5 1.444(2) O1 C4 1.457(2) O2 C12 1.348(2) O2 C6 1.4585(19) O3 C12 1.210(2) C1 C10 1.337(2) C1 C2 1.504(2) C1 H1A 0.9500 C2 C3 1.549(2) C2 H2A 0.9900 C2 H2B 0.9900 C3 C4 1.507(2) C3 H3A 0.9900 C3 H3B 0.9900 C4 C5 1.471(2) C4 C15 1.505(3) C5 C6 1.511(2) C5 H5A 1.0000 C6 C7 1.556(2) C6 H6A 1.0000 C7 C11 1.510(2) C7 C8 1.546(2) C7 H7A 1.0000 C8 C9 1.547(2) C8 H8A 0.9900 C8 H8B 0.9900 C9 C10 1.508(2) C9 H9A 0.9900 C9 H9B 0.9900 C10 C14 1.507(3) C11 C13 1.336(2) C11 C12 1.484(2) C13 C16 1.470(2) C13 H13A 0.9500 C14 H14A 0.9800 C14 H14B 0.9800 C14 H14C 0.9800 C15 H15A 0.9800 C15 H15B 0.9800 C15 H15C 0.9800 C16 C17 1.383(3) C16 C21 1.393(2) C17 N18 1.339(2) C17 H17A 0.9500 N18 C19 1.330(2) C19 N20 1.327(3) C19 H19A 0.9500 N20 C21 1.335(3) C21 H21A 0.9500 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 C10 C1 C2 C3 -110.99(19) C1 C2 C3 C4 53.54(19) C5 O1 C4 C15 -114.44(16) C5 O1 C4 C3 105.54(17) C2 C3 C4 O1 -152.28(15) C2 C3 C4 C5 -84.95(18) C2 C3 C4 C15 69.54(18) C4 O1 C5 C6 111.94(17) C15 C4 C5 O1 98.43(17) C3 C4 C5 O1 -108.37(16) O1 C4 C5 C6 -109.10(17) C15 C4 C5 C6 -10.7(2) C3 C4 C5 C6 142.53(15) C12 O2 C6 C5 132.85(14) C12 O2 C6 C7 11.21(17) O1 C5 C6 O2 36.7(2) C4 C5 C6 O2 108.24(17) O1 C5 C6 C7 155.20(14) C4 C5 C6 C7 -133.25(15) O2 C6 C7 C11 -8.19(16) C5 C6 C7 C11 -128.18(14) O2 C6 C7 C8 -133.78(14) C5 C6 C7 C8 106.23(15) C11 C7 C8 C9 153.12(15) C6 C7 C8 C9 -88.08(18) C7 C8 C9 C10 69.71(19) C2 C1 C10 C14 -8.9(3) C2 C1 C10 C9 171.47(16) C8 C9 C10 C1 -107.23(18) C8 C9 C10 C14 73.07(19) C8 C7 C11 C13 -56.5(2) C6 C7 C11 C13 177.78(17) C8 C7 C11 C12 128.73(15) C6 C7 C11 C12 3.06(16) C6 O2 C12 O3 172.90(16) C6 O2 C12 C11 -9.33(18) C13 C11 C12 O3 5.6(3) C7 C11 C12 O3 -178.86(18) C13 C11 C12 O2 -171.94(15) C7 C11 C12 O2 3.59(18) C12 C11 C13 C16 172.57(15) C7 C11 C13 C16 -1.7(3) C11 C13 C16 C17 -29.8(3) C11 C13 C16 C21 153.17(17) C21 C16 C17 N18 -3.7(3) C13 C16 C17 N18 179.10(17) C16 C17 N18 C19 1.1(3) C17 N18 C19 N20 1.7(3) N18 C19 N20 C21 -1.4(3) C19 N20 C21 C16 -1.7(3) C17 C16 C21 N20 4.0(2) C13 C16 C21 N20 -178.66(16) _cod_database_fobs_code 2241364