#------------------------------------------------------------------------------ #$Date: 2019-10-28 02:41:43 +0200 (Mon, 28 Oct 2019) $ #$Revision: 219594 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/24/1552490.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_1552490 loop_ _publ_author_name 'Policarpo, Rocco L.' 'Decultot, Ludovic' 'May, Elizabeth' 'Kuzmi\N-Methyltransferase (NNMT). ; _journal_name_full 'Journal of medicinal chemistry' _journal_paper_doi 10.1021/acs.jmedchem.9b01238 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_sum 'C13 H18 O4' _chemical_formula_weight 238.27 _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 geom _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90 _cell_angle_beta 90.0232(11) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.76180(10) _cell_length_b 19.4824(4) _cell_length_c 11.8204(2) _cell_measurement_reflns_used 9922 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 65.7 _cell_measurement_theta_min 3.73 _cell_volume 1326.88(4) _computing_cell_refinement 'SAINT 8.37A (Bruker-AXS, 2015)' _computing_data_reduction 'SAINT 8.37A (Bruker-AXS, 2015)' _computing_molecular_graphics 'Bruker SHELXTL (Sheldrick, 2015)' _computing_publication_material 'Bruker SHELXTL (Sheldrick, 2015)' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT-2014 (Sheldrick, 2015)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type ; Bruker D8 goniometer with CCD area detector ; _diffrn_measurement_method 'omega and phi scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'I\mS microfocus tube' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_unetI/netI 0.0186 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 26548 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 66.713 _diffrn_reflns_theta_max 66.713 _diffrn_reflns_theta_min 2.268 _exptl_absorpt_coefficient_mu 0.722 _exptl_absorpt_correction_T_max 0.8642 _exptl_absorpt_correction_T_min 0.7968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details sadabs _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.193 _exptl_crystal_description needle _exptl_crystal_F_000 512 _exptl_crystal_size_max 0.140 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.060 _refine_diff_density_max 0.111 _refine_diff_density_min -0.151 _refine_diff_density_rms 0.028 _refine_ls_abs_structure_details ; Flack x determined using 1834 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.02(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 314 _refine_ls_number_reflns 4269 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.058 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0256 _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^)+(0.0375P)^2^+0.1740P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.0638 _reflns_Friedel_coverage 0.934 _reflns_Friedel_fraction_full 0.996 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 4245 _reflns_number_total 4269 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jm9b01238_si_007.cif _cod_data_source_block Cyclopropyl-Alkyne-S30 _cod_database_code 1552490 _shelx_shelxl_version_number 2014/7 _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 0.906 _shelx_estimated_absorpt_t_max 0.958 _refine_ls_abs_structure_hooft 0.04(6) _shelx_res_file ; zsl.res created by SHELXL-2014/7 TITL zsl in P2(1) CELL 1.54178 5.7618 19.4824 11.8204 90 90.0232 90 ZERR 4 0.0001 0.0004 0.0002 0 0.0011 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H O UNIT 52 72 16 L.S. 10 PLAN -1 SIZE 0.06 0.1 0.14 TEMP -173.11 CONF BOND $H fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 1 2 REM REM REM WGHT 0.037500 0.174000 BASF 0.62965 FVAR 0.27388 O1 3 0.997542 0.578911 0.616215 11.00000 0.02721 0.02161 = 0.01906 -0.00024 0.00011 0.00270 O2 3 0.692208 0.548507 0.827229 11.00000 0.02057 0.02617 = 0.02316 -0.00253 0.00054 -0.00284 O3 3 1.063265 0.475419 0.695489 11.00000 0.03024 0.01894 = 0.01926 -0.00133 0.00197 0.00061 O4 3 0.820951 0.659287 0.871464 11.00000 0.02978 0.02466 = 0.02716 -0.00657 0.00074 0.00166 C1 1 1.104183 0.513529 0.594282 11.00000 0.02397 0.01923 = 0.02005 0.00112 0.00088 0.00051 C2 1 1.020297 0.592746 0.734120 11.00000 0.02366 0.02254 = 0.02021 -0.00056 -0.00045 -0.00187 AFIX 13 H2 2 1.140079 0.628563 0.750361 11.00000 -1.20000 AFIX 0 C3 1 0.783574 0.610492 0.784703 11.00000 0.02256 0.02152 = 0.02149 -0.00121 -0.00337 -0.00078 AFIX 13 H3 2 0.678877 0.629831 0.725212 11.00000 -1.20000 AFIX 0 C4 1 0.882605 0.508587 0.870650 11.00000 0.02656 0.02249 = 0.02267 0.00001 0.00109 0.00062 AFIX 13 H4 2 0.840155 0.458915 0.865524 11.00000 -1.20000 AFIX 0 C5 1 1.080828 0.522437 0.787900 11.00000 0.02572 0.02152 = 0.02181 -0.00029 -0.00325 0.00068 AFIX 13 H5 2 1.236946 0.521900 0.824880 11.00000 -1.20000 AFIX 0 C6 1 1.361725 0.521468 0.571545 11.00000 0.02663 0.02892 = 0.02437 -0.00245 -0.00085 -0.00012 AFIX 137 H6A 2 1.385113 0.554500 0.510071 11.00000 -1.50000 H6B 2 1.427228 0.476964 0.549791 11.00000 -1.50000 H6C 2 1.439313 0.538072 0.640076 11.00000 -1.50000 AFIX 0 C7 1 0.978959 0.478903 0.497366 11.00000 0.02347 0.02811 = 0.02368 -0.00439 0.00007 0.00024 AFIX 137 H7A 2 0.811722 0.478654 0.512436 11.00000 -1.50000 H7B 2 1.034527 0.431587 0.489753 11.00000 -1.50000 H7C 2 1.009486 0.504032 0.427109 11.00000 -1.50000 AFIX 0 C8 1 0.609606 0.678015 0.927350 11.00000 0.03526 0.03587 = 0.03462 -0.00857 0.00587 0.00640 AFIX 137 H8A 2 0.496254 0.693701 0.871182 11.00000 -1.50000 H8B 2 0.640601 0.715044 0.981399 11.00000 -1.50000 H8C 2 0.547412 0.638110 0.967694 11.00000 -1.50000 AFIX 0 C9 1 0.937770 0.525053 0.992462 11.00000 0.03163 0.02697 = 0.01940 -0.00236 0.00005 0.00181 AFIX 13 H9 2 0.994900 0.572571 1.008209 11.00000 -1.20000 AFIX 0 C10 1 1.028318 0.469678 1.067636 11.00000 0.05583 0.04096 = 0.02357 -0.00159 -0.00079 0.01841 AFIX 23 H10A 2 1.140412 0.482821 1.127322 11.00000 -1.20000 H10B 2 1.054854 0.423865 1.033792 11.00000 -1.20000 AFIX 0 C11 1 0.779050 0.493770 1.080514 11.00000 0.05052 0.02896 = 0.02227 -0.00098 0.00486 -0.00532 AFIX 13 H11 2 0.659224 0.461542 1.050092 11.00000 -1.20000 AFIX 0 C12 1 0.706162 0.533939 1.176483 11.00000 0.03612 0.03775 = 0.02775 0.00051 0.00059 -0.00707 C13 1 0.645638 0.567539 1.254356 11.00000 0.03707 0.05111 = 0.02693 -0.01114 0.00479 -0.00624 AFIX 163 H13 2 0.597003 0.594539 1.316932 11.00000 -1.20000 AFIX 0 O5 3 0.417404 0.353842 0.430112 11.00000 0.03142 0.02262 = 0.02552 0.00193 -0.00529 0.00219 O6 3 0.798633 0.278060 0.553034 11.00000 0.02337 0.02386 = 0.02563 0.00140 -0.00021 0.00071 O7 3 0.489620 0.251852 0.347005 11.00000 0.03617 0.02577 = 0.01972 0.00087 0.00001 0.00483 O8 3 0.661336 0.168998 0.600833 11.00000 0.03475 0.02212 = 0.02327 0.00401 -0.00171 0.00257 C21 1 0.380953 0.317026 0.327864 11.00000 0.02547 0.02630 = 0.02302 0.00265 -0.00191 0.00203 C22 1 0.465408 0.236320 0.464506 11.00000 0.02306 0.02344 = 0.02008 0.00205 0.00057 -0.00284 AFIX 13 H22 2 0.343815 0.200804 0.479230 11.00000 -1.20000 AFIX 0 C23 1 0.700995 0.216510 0.512601 11.00000 0.02801 0.02184 = 0.02252 0.00007 0.00080 0.00117 AFIX 13 H23 2 0.801306 0.195818 0.452595 11.00000 -1.20000 AFIX 0 C24 1 0.613813 0.319297 0.599276 11.00000 0.02415 0.01849 = 0.02717 0.00191 -0.00183 -0.00066 AFIX 13 H24 2 0.658118 0.368750 0.592432 11.00000 -1.20000 AFIX 0 C25 1 0.409594 0.305585 0.520990 11.00000 0.01898 0.02763 = 0.02162 0.00373 0.00103 0.00082 AFIX 13 H25 2 0.257189 0.305470 0.561434 11.00000 -1.20000 AFIX 0 C26 1 0.506268 0.353533 0.233817 11.00000 0.02459 0.04445 = 0.03211 0.01054 -0.00161 0.00376 AFIX 137 H26A 2 0.672702 0.355064 0.250750 11.00000 -1.50000 H26B 2 0.446355 0.400423 0.226882 11.00000 -1.50000 H26C 2 0.481371 0.328891 0.162560 11.00000 -1.50000 AFIX 0 C27 1 0.125225 0.308764 0.304472 11.00000 0.02621 0.04118 = 0.02423 -0.00014 -0.00162 -0.00143 AFIX 137 H27A 2 0.103641 0.279867 0.237426 11.00000 -1.50000 H27B 2 0.055673 0.353942 0.291056 11.00000 -1.50000 H27C 2 0.050136 0.287112 0.369729 11.00000 -1.50000 AFIX 0 C28 1 0.871796 0.150203 0.657691 11.00000 0.04412 0.02723 = 0.03088 0.00590 -0.00534 0.00740 AFIX 137 H28A 2 0.987982 0.136116 0.601794 11.00000 -1.50000 H28B 2 0.840933 0.112032 0.709543 11.00000 -1.50000 H28C 2 0.930328 0.189613 0.700601 11.00000 -1.50000 AFIX 0 C29 1 0.567882 0.303629 0.722334 11.00000 0.02504 0.02184 = 0.02536 -0.00060 -0.00241 0.00143 AFIX 13 H29 2 0.500906 0.257541 0.740238 11.00000 -1.20000 AFIX 0 C30 1 0.501698 0.361852 0.798821 11.00000 0.03806 0.03272 = 0.02570 -0.00502 -0.00458 0.00962 AFIX 23 H30A 2 0.394729 0.351817 0.862221 11.00000 -1.20000 H30B 2 0.482663 0.407851 0.764459 11.00000 -1.20000 AFIX 0 C31 1 0.745315 0.332171 0.804717 11.00000 0.03051 0.02517 = 0.02377 -0.00230 -0.00615 0.00118 AFIX 13 H31 2 0.869628 0.361204 0.770168 11.00000 -1.20000 AFIX 0 C32 1 0.815246 0.292671 0.901815 11.00000 0.03088 0.02906 = 0.02548 -0.00365 -0.00097 -0.00012 C33 1 0.875281 0.260413 0.981179 11.00000 0.03377 0.04479 = 0.02928 0.00883 -0.00492 0.00162 AFIX 163 H33 2 0.923579 0.234462 1.045028 11.00000 -1.20000 AFIX 0 HKLF 4 REM zsl in P2(1) REM R1 = 0.0256 for 4245 Fo > 4sig(Fo) and 0.0258 for all 4269 data REM 314 parameters refined using 1 restraints END WGHT 0.0375 0.1741 REM Highest difference peak 0.111, deepest hole -0.151, 1-sigma level 0.028 Q1 1 0.9235 0.3300 0.7501 11.00000 0.05 0.10 ; _shelx_res_checksum 62412 _shelx_hkl_file ; 1 0 0 0.41 0.14 1 0 0 0.32 0.26 1 0 0 0.32 0.23 1 0 0 0.35 0.20 1 0 0 0.14 0.20 -1 0 0 0.16 0.29 -1 0 0 0.38 0.18 -1 0 0 0.22 0.21 -1 0 0 0.45 0.13 -1 0 0 0.65 0.28 2 0 0 114.42 4.27 2 0 0 112.09 4.22 -2 0 0 111.23 3.90 -2 0 0 115.90 3.84 2 0 0 116.44 3.86 2 0 0 117.37 3.82 2 0 0 115.38 4.30 -2 0 0 112.02 3.82 2 0 0 121.10 4.57 2 0 0 116.97 3.83 -2 0 0 114.22 4.60 -2 0 0 112.72 4.26 -2 0 0 118.49 4.18 -2 0 0 114.93 4.53 3 0 0 1.98 0.68 3 0 0 1.34 0.52 3 0 0 1.46 0.29 3 0 0 2.04 0.36 -3 0 0 1.91 0.64 -3 0 0 2.00 0.38 -3 0 0 1.32 0.29 -3 0 0 1.47 0.49 -4 0 0 0.55 0.30 4 0 0 0.77 0.23 -4 0 0 0.37 0.17 4 0 0 0.69 0.37 5 0 0 0.85 0.13 -5 0 0 0.70 0.24 5 0 0 0.59 0.46 5 0 0 1.19 0.31 -5 0 0 0.62 0.36 -6 0 0 1.49 0.17 6 0 0 1.32 0.29 -6 0 0 1.48 0.24 0 -1 0 0.05 0.04 0 -1 0 0.09 0.04 0 -1 0 0.00 0.04 0 -1 0 0.04 0.04 0 -1 0 -0.01 0.04 0 -1 0 -0.02 0.04 1 -1 0 95.52 3.32 -1 -1 0 93.01 3.16 1 -1 0 91.91 3.33 -1 -1 0 93.25 3.14 -1 -1 0 94.11 3.43 1 -1 0 93.37 3.24 -1 -1 0 93.16 3.33 1 -1 0 85.97 3.25 1 1 0 93.99 3.41 -1 1 0 92.89 3.30 -1 1 0 100.48 3.35 -1 1 0 95.30 3.49 1 1 0 96.92 3.37 1 1 0 90.98 3.26 1 1 0 93.77 3.45 -2 -1 0 50.48 2.09 2 -1 0 55.05 2.50 2 -1 0 54.34 1.86 2 -1 0 56.06 2.30 2 -1 0 52.96 1.84 -2 -1 0 52.32 2.41 2 -1 0 52.19 2.31 -2 -1 0 47.43 2.47 -2 -1 0 52.15 1.85 2 -1 0 53.45 1.84 -2 -1 0 50.37 2.24 -2 -1 0 50.74 2.00 2 1 0 53.40 2.40 2 1 0 54.42 2.33 -2 1 0 51.00 2.22 2 1 0 52.23 2.02 2 1 0 51.59 2.47 -2 1 0 52.34 2.55 -2 1 0 50.18 2.18 2 1 0 52.24 2.19 2 1 0 52.71 1.87 -2 1 0 51.86 1.84 3 -1 0 137.21 4.71 3 -1 0 150.73 5.92 3 -1 0 136.11 4.68 -3 -1 0 134.21 4.68 3 -1 0 138.80 5.43 -3 -1 0 134.55 5.35 3 -1 0 140.56 4.67 3 -1 0 138.17 5.45 3 1 0 143.25 4.69 -3 1 0 135.77 4.70 -3 1 0 131.19 5.81 -3 1 0 134.92 5.30 3 1 0 135.70 5.42 -3 1 0 134.68 4.61 -3 1 0 132.36 5.19 -3 1 0 141.82 4.64 -4 -1 0 9.10 0.45 4 -1 0 9.17 0.51 -4 -1 0 9.04 0.66 4 -1 0 7.93 0.71 4 1 0 9.90 0.78 -4 1 0 9.28 0.69 -4 1 0 9.28 0.46 4 1 0 9.44 0.52 -5 -1 0 1.16 0.41 -5 -1 0 1.25 0.26 5 -1 0 1.05 0.49 5 -1 0 0.93 0.32 5 -1 0 1.65 0.15 5 1 0 0.01 0.44 -5 1 0 1.18 0.26 5 1 0 1.08 0.32 -5 1 0 1.51 0.41 -6 -1 0 0.08 0.11 6 -1 0 0.13 0.05 -6 -1 0 0.16 0.20 6 1 0 -0.15 0.23 -6 1 0 0.16 0.11 0 -2 0 7.47 0.36 0 -2 0 7.75 0.33 0 -2 0 6.97 0.39 0 -2 0 7.11 0.33 0 -2 0 7.96 0.41 0 -2 0 7.09 0.34 -1 -2 0 953.34 30.61 1 -2 0 933.91 30.53 1 -2 0 925.52 30.56 -1 -2 0 966.16 30.54 1 -2 0 975.41 30.63 1 -2 0 1000.00 30.49 -1 -2 0 915.61 30.65 -1 -2 0 923.84 30.50 -1 2 0 939.18 30.55 1 2 0 969.29 30.59 1 2 0 946.24 30.67 1 2 0 960.07 30.40 -1 2 0 910.15 30.54 1 2 0 978.93 30.66 -1 2 0 943.82 30.49 -2 -2 0 74.08 2.76 -2 -2 0 75.47 3.01 2 -2 0 74.60 3.19 2 -2 0 73.58 2.98 2 -2 0 78.50 2.58 -2 -2 0 75.31 2.83 2 -2 0 74.03 2.66 2 -2 0 76.46 2.55 -2 -2 0 80.24 3.23 2 -2 0 74.53 2.57 2 -2 0 71.31 3.08 -2 -2 0 71.02 3.24 -2 -2 0 74.91 2.57 -2 2 0 75.67 2.53 -2 2 0 75.54 2.94 2 2 0 78.26 2.58 -2 2 0 74.84 2.94 2 2 0 70.12 3.18 -2 2 0 72.26 2.51 2 2 0 69.31 3.01 2 2 0 72.25 2.82 -2 2 0 75.85 3.29 2 2 0 72.40 3.13 2 2 0 74.23 2.83 3 -2 0 229.81 7.58 -3 -2 0 227.70 8.31 3 -2 0 231.13 7.60 -3 -2 0 228.61 7.59 3 -2 0 228.71 8.75 3 -2 0 230.62 7.58 3 -2 0 226.96 8.30 3 -2 0 230.97 8.46 -3 2 0 224.37 8.01 -3 2 0 206.12 7.96 -3 2 0 223.21 7.33 3 2 0 216.37 8.16 -3 2 0 212.15 8.58 -3 2 0 228.06 7.44 -3 2 0 222.91 7.33 3 2 0 233.69 7.40 -4 -2 0 2.04 0.26 -4 -2 0 2.88 0.45 4 -2 0 2.35 0.43 4 -2 0 2.10 0.32 4 -2 0 2.28 0.32 4 -2 0 2.33 0.45 4 -2 0 2.35 0.25 4 -2 0 2.23 0.26 -4 2 0 1.95 0.42 -4 2 0 2.11 0.37 -4 2 0 1.90 0.23 4 2 0 1.95 0.32 -4 2 0 1.78 0.19 4 2 0 2.79 0.50 -5 -2 0 3.21 0.24 -5 -2 0 3.89 0.60 5 -2 0 3.65 0.16 5 -2 0 4.23 0.47 -5 -2 0 3.47 0.37 -5 2 0 3.38 0.34 5 2 0 3.15 0.15 5 2 0 4.25 0.69 5 2 0 3.33 0.47 -6 -2 0 8.72 0.36 -6 -2 0 8.01 0.48 6 -2 0 9.09 0.30 6 2 0 7.63 0.51 0 -3 0 0.04 0.14 0 -3 0 0.10 0.08 0 -3 0 0.02 0.12 0 -3 0 0.03 0.13 0 -3 0 0.11 0.16 0 -3 0 0.16 0.12 0 -3 0 0.01 0.08 0 3 0 -0.03 0.05 0 3 0 0.01 0.06 1 -3 0 170.07 5.40 -1 -3 0 167.77 5.65 -1 -3 0 168.82 5.70 -1 -3 0 168.54 5.74 1 -3 0 175.49 5.81 1 -3 0 153.01 5.63 1 -3 0 171.05 5.58 1 -3 0 166.34 5.60 -1 -3 0 170.98 5.39 -1 -3 0 151.96 5.69 -1 3 0 164.58 5.71 1 3 0 165.26 5.44 -1 3 0 166.26 5.60 -1 3 0 159.43 5.63 1 3 0 173.30 5.80 -1 3 0 161.15 5.42 -1 3 0 176.23 5.76 1 3 0 168.91 5.79 1 3 0 170.15 5.74 -2 -3 0 26.11 1.07 2 -3 0 26.61 1.05 -2 -3 0 27.56 1.37 -2 -3 0 30.30 1.49 -2 -3 0 28.00 1.08 -2 -3 0 26.58 1.05 2 -3 0 26.08 1.58 2 -3 0 27.05 1.17 -2 -3 0 27.65 1.07 -2 -3 0 27.11 1.18 2 -3 0 30.80 1.63 2 -3 0 27.51 1.04 -2 -3 0 29.08 1.65 2 -3 0 28.64 1.09 2 -3 0 28.14 1.42 2 3 0 27.10 1.03 -2 3 0 29.69 1.75 2 3 0 27.59 1.42 2 3 0 29.22 1.29 2 3 0 28.30 1.12 -2 3 0 29.70 1.51 2 3 0 28.96 1.66 -2 3 0 29.35 1.07 2 3 0 26.74 1.52 -2 3 0 25.93 1.06 -2 3 0 27.60 1.43 3 -3 0 14.99 0.76 3 -3 0 14.87 1.23 3 -3 0 13.09 0.71 -3 -3 0 16.09 1.24 3 -3 0 12.53 0.51 -3 -3 0 14.50 0.73 3 -3 0 11.97 1.26 3 -3 0 12.57 0.72 3 -3 0 14.66 1.45 -3 -3 0 13.27 0.54 -3 3 0 13.27 0.72 3 3 0 14.03 0.79 -3 3 0 12.26 1.46 3 3 0 14.39 1.36 -3 3 0 14.26 0.73 -3 3 0 13.78 0.82 -3 3 0 14.81 1.20 -3 3 0 13.11 1.15 4 -3 0 12.98 0.87 4 -3 0 13.41 0.66 -4 -3 0 14.36 0.61 4 -3 0 15.06 0.60 4 -3 0 13.57 0.63 -4 -3 0 14.51 0.89 4 -3 0 14.01 0.87 4 -3 0 13.73 0.62 4 3 0 13.56 0.64 4 3 0 15.19 0.95 -4 3 0 12.64 0.53 -4 3 0 13.85 0.95 4 3 0 13.58 0.66 -4 3 0 13.77 0.83 -4 3 0 12.87 0.58 -5 -3 0 2.39 0.34 5 -3 0 2.23 0.33 5 -3 0 2.48 0.14 -5 -3 0 2.37 0.22 5 3 0 2.73 0.64 5 3 0 2.86 0.45 6 -3 0 7.50 0.26 -6 -3 0 6.49 0.47 -6 -3 0 7.19 0.32 6 3 0 6.73 0.50 0 -4 0 919.13 29.77 0 -4 0 938.48 29.84 0 -4 0 953.50 29.89 0 -4 0 894.59 29.94 0 -4 0 955.43 30.01 0 4 0 962.92 30.69 0 4 0 973.40 30.54 0 4 0 923.48 30.42 1 -4 0 161.04 5.45 -1 -4 0 162.40 5.20 1 -4 0 160.28 5.51 -1 -4 0 160.91 5.63 1 -4 0 161.08 5.44 -1 -4 0 162.14 5.55 1 -4 0 163.65 5.36 1 -4 0 164.91 5.73 -1 -4 0 163.88 5.66 1 4 0 166.41 5.64 1 4 0 154.26 5.54 -1 4 0 157.95 5.54 -1 4 0 152.82 5.29 -1 4 0 167.98 5.51 1 4 0 163.74 5.61 -1 4 0 168.38 5.42 -1 4 0 150.65 5.40 -2 -4 0 4.00 0.79 2 -4 0 2.60 0.26 2 -4 0 3.09 0.32 -2 -4 0 3.77 0.57 2 -4 0 3.09 0.36 2 -4 0 2.83 0.60 -2 -4 0 3.74 0.63 -2 -4 0 2.88 0.34 2 -4 0 3.33 0.68 -2 -4 0 3.40 0.35 2 -4 0 2.86 0.39 2 -4 0 2.88 0.50 -2 -4 0 3.00 0.33 -2 -4 0 3.07 0.33 2 4 0 2.97 0.34 2 4 0 2.62 0.52 2 4 0 3.81 0.66 2 4 0 1.94 0.53 -2 4 0 3.27 0.55 2 4 0 3.14 0.28 -2 4 0 3.02 0.30 -2 4 0 3.20 0.55 -2 4 0 3.09 0.69 -2 4 0 2.82 0.30 3 -4 0 2.82 0.80 3 -4 0 2.39 0.25 -3 -4 0 2.75 0.71 3 -4 0 2.73 0.37 3 -4 0 2.23 0.19 -3 -4 0 2.78 0.38 -3 -4 0 2.62 0.21 3 -4 0 2.70 0.39 3 -4 0 2.87 0.43 3 -4 0 1.83 0.57 3 -4 0 2.89 0.79 3 -4 0 2.55 0.43 3 4 0 2.86 0.26 -3 4 0 3.28 0.72 -3 4 0 2.39 0.84 -3 4 0 2.93 0.70 3 4 0 3.03 0.42 -3 4 0 2.63 0.18 3 4 0 1.70 0.64 -3 4 0 2.26 0.36 -3 4 0 2.47 0.47 4 -4 0 0.14 0.16 4 -4 0 1.03 0.40 4 -4 0 0.86 0.23 4 -4 0 0.12 0.30 4 -4 0 0.37 0.15 -4 -4 0 0.42 0.19 -4 -4 0 0.12 0.32 4 4 0 0.70 0.25 4 4 0 0.40 0.39 -4 4 0 0.44 0.36 4 4 0 0.17 0.22 -4 4 0 0.44 0.13 -4 4 0 0.19 0.32 5 -4 0 17.41 0.88 5 -4 0 16.22 0.68 -5 -4 0 16.28 0.60 -5 -4 0 17.18 0.73 5 -4 0 15.56 0.55 5 4 0 17.69 0.86 -6 -4 0 2.93 0.21 6 -4 0 3.48 0.15 6 -4 0 3.12 0.40 6 4 0 2.55 0.39 0 -5 0 0.39 0.15 0 -5 0 0.17 0.25 0 -5 0 -0.02 0.13 0 -5 0 -0.14 0.18 0 -5 0 -0.10 0.13 0 5 0 -0.02 0.11 0 5 0 -0.22 0.25 0 5 0 0.09 0.13 0 5 0 -0.09 0.16 0 5 0 0.25 0.18 -1 -5 0 0.60 0.12 -1 -5 0 0.64 0.19 -1 -5 0 0.67 0.32 1 -5 0 0.96 0.24 1 -5 0 1.10 0.31 -1 -5 0 0.77 0.35 1 -5 0 0.52 0.21 1 -5 0 0.51 0.33 1 -5 0 0.46 0.18 -1 -5 0 0.46 0.16 -1 -5 0 1.10 0.34 1 -5 0 0.37 0.20 -1 -5 0 0.66 0.20 1 -5 0 0.94 0.24 -1 5 0 0.42 0.21 -1 5 0 0.38 0.32 -1 5 0 0.73 0.22 1 5 0 0.65 0.35 1 5 0 0.52 0.29 1 5 0 0.75 0.33 -1 5 0 0.74 0.27 -1 5 0 0.68 0.27 1 5 0 0.59 0.12 -2 -5 0 27.47 1.06 2 -5 0 25.82 1.17 -2 -5 0 27.08 1.65 2 -5 0 25.43 0.98 2 -5 0 27.40 1.09 2 -5 0 24.77 1.00 -2 -5 0 24.78 1.04 2 -5 0 27.26 1.68 2 -5 0 25.22 1.34 -2 -5 0 26.16 1.10 -2 -5 0 26.06 1.07 2 -5 0 26.87 1.58 -2 -5 0 27.17 1.49 -2 -5 0 26.40 1.45 2 5 0 26.68 1.51 -2 5 0 25.25 0.95 -2 5 0 27.83 1.49 -2 5 0 25.09 1.63 2 5 0 25.67 1.05 -2 5 0 23.95 1.33 2 5 0 24.56 1.60 2 5 0 23.97 1.48 2 5 0 24.06 0.95 -2 5 0 23.20 0.96 -3 -5 0 11.60 0.49 3 -5 0 11.88 0.66 3 -5 0 11.09 0.51 3 -5 0 12.01 0.52 -3 -5 0 11.10 0.48 3 -5 0 11.17 0.70 3 -5 0 10.83 1.24 3 -5 0 10.32 1.29 -3 -5 0 10.90 0.66 3 -5 0 11.28 0.45 -3 -5 0 11.35 1.12 -3 5 0 12.94 1.24 3 5 0 10.76 0.44 3 5 0 9.95 1.23 -3 5 0 11.17 1.40 -3 5 0 11.74 0.43 3 5 0 10.87 0.74 -3 5 0 11.62 0.79 3 5 0 11.21 0.52 3 5 0 11.73 0.54 -3 5 0 11.98 0.67 4 -5 0 75.14 2.52 4 -5 0 72.46 2.56 -4 -5 0 79.32 2.85 4 -5 0 74.47 2.85 4 -5 0 76.25 2.85 -4 -5 0 73.24 2.53 4 -5 0 75.26 2.57 4 5 0 69.55 2.43 4 5 0 72.72 2.46 -4 5 0 71.21 2.33 -4 5 0 69.64 2.84 4 5 0 69.60 2.77 -4 5 0 67.40 2.66 -5 -5 0 3.23 0.23 5 -5 0 3.78 0.41 5 -5 0 3.40 0.16 5 -5 0 3.49 0.21 5 -5 0 3.71 0.35 -5 -5 0 3.40 0.37 5 -5 0 3.57 0.36 5 5 0 3.19 0.45 -6 -5 0 5.52 0.27 6 -5 0 5.85 0.22 6 -5 0 5.99 0.38 0 -6 0 546.46 16.86 0 -6 0 536.91 16.85 0 -6 0 515.82 17.20 0 -6 0 511.58 16.95 0 -6 0 513.79 17.02 0 -6 0 518.45 16.83 0 6 0 504.04 16.20 0 6 0 500.70 16.16 0 6 0 502.35 16.33 0 6 0 505.99 16.30 0 6 0 499.93 16.56 -1 -6 0 190.34 5.95 1 -6 0 186.42 6.55 1 -6 0 180.75 6.23 -1 -6 0 180.92 6.06 1 -6 0 180.82 6.16 1 -6 0 181.77 6.10 -1 -6 0 185.97 6.40 1 -6 0 185.41 6.02 -1 -6 0 181.47 6.30 1 -6 0 180.84 6.22 -1 -6 0 192.33 6.09 -1 -6 0 180.94 5.98 -1 -6 0 182.38 6.52 -1 6 0 180.31 6.35 1 6 0 180.14 5.95 -1 6 0 177.72 6.13 1 6 0 180.85 6.35 -1 6 0 181.88 6.17 -1 6 0 178.61 6.10 1 6 0 188.96 6.53 1 6 0 184.38 6.37 -1 6 0 179.51 6.17 1 6 0 184.13 5.86 2 -6 0 11.24 1.13 2 -6 0 11.72 0.64 2 -6 0 11.48 0.73 -2 -6 0 11.07 0.61 -2 -6 0 11.01 0.65 2 -6 0 10.64 0.51 -2 -6 0 11.66 1.11 2 -6 0 10.66 0.81 -2 -6 0 11.69 0.95 2 -6 0 10.23 0.98 -2 -6 0 11.33 0.59 -2 -6 0 11.01 0.59 -2 -6 0 11.19 0.98 -2 6 0 11.87 1.14 -2 6 0 11.67 0.53 2 6 0 11.33 0.65 -2 6 0 10.69 0.98 2 6 0 11.33 1.07 -2 6 0 10.53 0.88 2 6 0 12.10 1.13 2 6 0 11.17 1.03 2 6 0 10.80 0.54 3 -6 0 34.19 1.19 3 -6 0 36.43 2.30 -3 -6 0 33.35 1.16 -3 -6 0 32.42 1.15 3 -6 0 32.39 2.21 3 -6 0 31.92 1.18 3 -6 0 31.22 1.12 -3 -6 0 34.47 2.01 3 -6 0 31.06 1.32 3 -6 0 32.22 1.41 -3 -6 0 33.22 1.37 3 6 0 30.70 1.05 3 6 0 31.66 1.16 -3 6 0 31.05 1.97 -3 6 0 32.62 1.48 3 6 0 30.93 1.38 3 6 0 29.01 2.03 -3 6 0 31.60 1.05 -3 6 0 29.20 1.29 -3 6 0 30.21 2.25 4 -6 0 54.69 1.92 -4 -6 0 55.23 2.18 -4 -6 0 53.69 1.87 4 -6 0 54.75 1.86 4 -6 0 53.00 2.18 4 -6 0 54.03 1.92 4 -6 0 54.07 2.20 -4 6 0 51.34 2.31 -4 6 0 53.31 1.78 4 6 0 53.62 2.27 4 6 0 56.41 1.93 4 6 0 50.41 1.89 -5 -6 0 46.93 1.60 5 -6 0 43.18 1.47 -5 -6 0 43.27 1.47 5 -6 0 42.47 1.54 5 -6 0 46.16 1.63 5 -6 0 44.61 1.58 5 6 0 41.69 1.58 -5 6 0 40.11 1.43 6 -6 0 11.76 0.52 6 -6 0 11.51 0.40 -6 -6 0 11.98 0.44 0 -7 0 -0.05 0.19 0 -7 0 0.14 0.16 0 -7 0 -0.20 0.27 0 -7 0 0.16 0.17 0 -7 0 -0.02 0.18 0 -7 0 0.03 0.18 0 -7 0 0.06 0.15 0 7 0 -0.05 0.27 0 7 0 0.19 0.14 0 7 0 0.15 0.21 0 7 0 0.06 0.19 0 7 0 0.01 0.15 -1 -7 0 24.98 1.25 -1 -7 0 26.31 0.93 -1 -7 0 25.47 1.33 1 -7 0 25.80 1.01 1 -7 0 26.47 1.20 -1 -7 0 24.79 0.96 1 -7 0 24.44 1.09 1 -7 0 26.57 1.48 -1 -7 0 26.24 1.09 -1 -7 0 25.90 1.06 1 -7 0 24.35 1.13 1 -7 0 25.58 1.25 -1 -7 0 26.71 1.49 1 7 0 26.55 0.90 -1 7 0 24.86 1.18 1 7 0 24.33 1.50 1 7 0 23.92 0.99 -1 7 0 24.43 1.24 1 7 0 26.25 1.39 -1 7 0 24.95 1.35 1 7 0 25.04 1.35 -1 7 0 25.94 1.19 2 -7 0 26.44 1.59 2 -7 0 26.18 1.25 -2 -7 0 25.89 1.17 -2 -7 0 27.47 1.10 2 -7 0 27.18 1.76 2 -7 0 25.94 1.13 2 -7 0 26.95 1.01 -2 -7 0 28.20 1.10 -2 -7 0 24.74 1.61 -2 -7 0 25.54 1.15 -2 -7 0 28.34 1.58 -2 -7 0 26.54 1.72 -2 7 0 25.12 0.96 2 7 0 26.89 1.65 2 7 0 22.99 1.08 2 7 0 26.17 1.67 -2 7 0 25.01 1.65 -2 7 0 27.92 1.62 2 7 0 27.38 1.74 2 7 0 25.74 1.00 3 -7 0 26.45 1.97 -3 -7 0 27.25 1.79 -3 -7 0 24.78 1.16 -3 -7 0 24.48 0.91 3 -7 0 25.85 0.95 -3 -7 0 23.89 1.14 -3 -7 0 25.54 1.17 -3 -7 0 25.87 0.92 3 -7 0 24.53 0.95 3 -7 0 24.32 1.17 3 -7 0 23.14 0.87 3 -7 0 22.82 1.87 3 -7 0 25.48 1.10 3 7 0 23.17 0.94 3 7 0 24.82 0.83 -3 7 0 24.55 1.09 -3 7 0 22.60 1.97 -3 7 0 27.34 1.88 3 7 0 21.18 1.81 -3 7 0 25.18 1.27 3 7 0 23.74 1.04 -3 7 0 23.18 0.82 3 7 0 24.03 1.18 4 -7 0 7.18 0.38 4 -7 0 6.01 0.70 4 -7 0 7.21 0.47 4 -7 0 6.49 0.47 4 -7 0 6.88 0.67 -4 -7 0 6.62 0.72 -4 -7 0 6.96 0.43 4 7 0 5.99 0.48 -4 7 0 7.19 0.86 -4 7 0 5.94 0.67 4 7 0 6.94 0.80 4 7 0 6.62 0.48 -4 7 0 6.59 0.34 5 -7 0 1.11 0.28 -5 -7 0 1.75 0.20 5 -7 0 1.30 0.23 5 -7 0 1.00 0.21 5 -7 0 1.30 0.18 -5 -7 0 1.49 0.28 -5 -7 0 1.24 0.10 5 7 0 0.70 0.28 -5 7 0 1.14 0.20 6 -7 0 0.17 0.09 6 -7 0 0.12 0.06 6 -7 0 0.05 0.16 -6 -7 0 0.10 0.10 0 -8 0 1.87 0.35 0 -8 0 1.66 0.30 0 -8 0 2.42 0.53 0 -8 0 2.21 0.31 0 -8 0 2.55 0.33 0 8 0 2.36 0.41 0 8 0 2.00 0.51 0 8 0 2.03 0.36 0 8 0 2.02 0.33 -1 -8 0 23.67 1.47 -1 -8 0 21.63 0.85 -1 -8 0 21.60 0.82 1 -8 0 21.16 0.89 -1 -8 0 21.50 1.16 -1 -8 0 22.57 1.00 1 -8 0 21.33 1.08 1 -8 0 22.49 1.38 1 -8 0 20.97 0.99 -1 -8 0 20.33 1.21 -1 -8 0 21.62 0.98 1 8 0 23.52 1.32 -1 8 0 21.21 1.28 1 8 0 22.97 1.33 -1 8 0 21.25 1.36 1 8 0 22.14 0.81 -1 8 0 22.17 1.11 1 8 0 22.52 1.48 1 8 0 21.18 0.92 2 -8 0 144.62 4.83 -2 -8 0 140.66 4.76 2 -8 0 144.38 4.68 2 -8 0 145.09 5.00 -2 -8 0 142.65 5.63 2 -8 0 141.94 5.41 -2 -8 0 138.93 4.77 -2 -8 0 143.53 4.91 -2 -8 0 140.18 4.87 -2 -8 0 142.94 5.35 2 -8 0 144.80 5.73 -2 -8 0 136.88 5.62 2 8 0 134.14 5.52 2 8 0 143.52 5.47 2 8 0 141.16 4.58 -2 8 0 137.79 5.39 -2 8 0 136.79 4.52 2 8 0 137.45 4.71 2 8 0 138.61 5.53 -2 8 0 132.73 5.40 3 -8 0 119.59 4.14 -3 -8 0 118.94 3.94 3 -8 0 123.69 4.05 -3 -8 0 100.62 4.90 3 -8 0 112.15 3.80 3 -8 0 117.50 3.88 -3 -8 0 120.79 4.08 -3 -8 0 119.24 3.85 -3 -8 0 119.35 4.16 3 -8 0 119.91 3.88 -3 -8 0 108.68 3.85 -3 -8 0 121.17 4.13 -3 -8 0 115.55 3.84 -3 8 0 118.28 3.96 3 8 0 116.94 5.14 3 8 0 118.54 5.61 3 8 0 113.70 3.70 3 8 0 114.77 4.10 3 8 0 113.87 3.93 -3 8 0 120.61 4.23 3 8 0 109.74 3.82 -3 8 0 108.37 3.69 -4 -8 0 62.28 2.41 4 -8 0 58.33 2.44 4 -8 0 59.02 2.13 -4 -8 0 61.51 2.09 4 -8 0 60.26 2.14 4 -8 0 63.08 2.43 4 -8 0 60.97 2.07 4 8 0 58.63 2.11 -4 8 0 57.89 2.32 -4 8 0 58.66 2.57 4 8 0 59.61 2.48 4 8 0 57.13 2.08 -4 8 0 58.74 1.96 -5 -8 0 18.45 0.60 5 -8 0 18.22 0.64 -5 -8 0 17.89 0.78 5 -8 0 17.88 0.74 -5 -8 0 17.68 0.65 5 -8 0 17.52 0.75 5 -8 0 17.55 0.81 5 8 0 16.90 0.82 -5 8 0 16.06 0.67 -6 -8 0 -0.04 0.09 6 -8 0 -0.07 0.16 6 -8 0 -0.03 0.08 6 -8 0 -0.02 0.06 0 -9 0 -0.24 0.21 0 -9 0 0.05 0.20 0 -9 0 -0.32 0.33 0 -9 0 -0.11 0.19 0 9 0 0.36 0.38 0 9 0 0.14 0.20 1 -9 0 0.43 0.24 -1 -9 0 0.21 0.25 -1 -9 0 0.14 0.32 1 -9 0 0.64 0.22 -1 -9 0 0.32 0.14 -1 -9 0 0.16 0.23 -1 -9 0 0.06 0.32 -1 -9 0 0.42 0.47 1 -9 0 0.58 0.43 -1 -9 0 0.38 0.19 1 9 0 1.15 0.41 1 9 0 0.33 0.12 -1 9 0 0.48 0.33 -1 9 0 0.38 0.28 1 9 0 0.19 0.38 1 9 0 0.26 0.20 1 9 0 0.40 0.37 2 -9 0 10.39 0.65 -2 -9 0 9.65 0.95 -2 -9 0 10.60 0.71 -2 -9 0 9.35 0.46 2 -9 0 9.27 0.47 2 -9 0 12.64 1.07 -2 -9 0 10.33 0.43 2 -9 0 10.50 0.48 -2 -9 0 12.42 1.23 -2 -9 0 10.13 0.50 -2 -9 0 9.71 0.69 -2 -9 0 10.29 0.60 -2 -9 0 10.44 0.42 2 -9 0 10.09 0.50 -2 -9 0 10.47 0.59 2 -9 0 10.77 1.19 -2 -9 0 10.28 0.47 -2 -9 0 11.89 1.28 2 9 0 9.37 0.64 2 9 0 8.68 1.09 -2 9 0 9.88 1.08 2 9 0 8.46 1.06 2 9 0 9.35 0.36 -2 9 0 9.24 0.46 2 9 0 9.75 0.52 2 9 0 8.50 1.09 -2 9 0 9.79 1.06 -3 -9 0 0.56 0.33 -3 -9 0 0.56 0.16 -3 -9 0 1.23 0.37 3 -9 0 0.67 0.19 -3 -9 0 1.00 0.35 -3 -9 0 0.65 0.22 -3 -9 0 1.01 0.20 3 -9 0 0.61 0.20 3 -9 0 0.72 0.26 3 -9 0 0.59 0.12 3 -9 0 0.98 0.35 -3 -9 0 0.71 0.16 3 9 0 0.68 0.35 3 9 0 0.56 0.11 -3 9 0 0.56 0.28 3 9 0 0.76 0.28 -3 9 0 0.38 0.10 -3 9 0 0.87 0.40 3 9 0 0.69 0.21 4 -9 0 17.91 0.80 4 -9 0 17.13 0.78 4 -9 0 16.59 1.07 -4 -9 0 17.47 1.04 4 -9 0 18.13 1.06 4 -9 0 18.42 0.73 -4 -9 0 17.26 0.73 -4 9 0 18.61 1.25 -4 9 0 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12 5.92 0.25 -1 -4 -12 5.54 0.28 1 4 12 5.95 0.41 -1 4 -12 5.70 0.58 -1 4 -12 5.47 0.28 -1 4 -12 5.59 0.46 -2 -4 -12 6.39 0.29 2 -4 12 6.65 0.24 2 -4 12 6.19 0.27 3 -4 12 1.55 0.09 -3 -5 12 2.56 0.13 -3 5 12 2.47 0.14 -2 -5 12 4.80 0.18 -2 -5 12 4.63 0.25 -2 -5 12 4.94 0.22 -2 5 12 4.44 0.20 -1 -5 12 2.39 0.16 -1 -5 12 2.05 0.30 -1 -5 12 2.39 0.13 -1 -5 12 2.35 0.21 1 -5 -12 1.96 0.19 1 5 -12 2.47 0.44 -1 5 12 2.03 0.14 1 5 -12 2.11 0.36 0 -5 12 2.62 0.14 0 -5 12 2.13 0.30 0 -5 12 2.67 0.18 0 -5 -12 2.78 0.21 0 -5 -12 1.86 0.30 0 -5 12 2.32 0.22 0 -5 12 2.49 0.37 0 5 -12 1.98 0.36 0 5 -12 2.47 0.34 0 5 12 2.28 0.33 -1 -5 -12 3.47 0.23 1 -5 12 3.61 0.21 1 -5 12 3.72 0.16 -1 5 -12 3.75 0.23 1 5 12 2.82 0.33 -1 5 -12 3.07 0.39 -2 -5 -12 7.74 0.32 2 -5 12 7.54 0.27 2 -5 12 7.10 0.30 3 -5 12 1.85 0.10 3 -5 12 1.66 0.13 3 -5 12 1.53 0.15 -3 6 12 1.95 0.12 -2 -6 12 6.00 0.22 -2 -6 12 5.95 0.24 -2 -6 12 5.53 0.27 -2 6 12 5.40 0.22 -1 -6 12 2.28 0.13 -1 -6 12 2.41 0.22 1 -6 -12 2.19 0.19 -1 -6 12 2.23 0.16 0 -6 -12 4.75 0.26 0 -6 12 5.48 0.44 0 -6 12 4.17 0.26 0 -6 12 4.60 0.19 0 -6 12 4.65 0.22 0 -6 12 3.92 0.39 0 6 12 3.83 0.36 0 6 -12 3.89 0.41 1 -6 12 3.39 0.20 -1 -6 -12 3.65 0.22 1 -6 12 3.55 0.16 -1 6 -12 3.29 0.22 2 -6 12 5.32 0.26 2 -6 12 5.06 0.24 -2 -6 -12 5.30 0.25 2 -6 12 5.34 0.20 3 -6 12 2.37 0.14 3 -6 12 2.55 0.11 3 -6 12 2.41 0.17 -2 -7 12 5.10 0.26 -2 -7 12 4.99 0.22 -2 -7 12 5.36 0.20 -2 7 12 5.37 0.21 -1 -7 12 5.38 0.21 -1 -7 12 5.17 0.24 -1 -7 12 5.64 0.29 1 -7 -12 5.44 0.26 0 -7 12 2.94 0.21 0 -7 12 2.97 0.15 0 -7 12 2.85 0.18 0 -7 -12 2.96 0.21 1 -7 12 3.93 0.17 1 -7 12 3.98 0.23 1 -7 12 4.42 0.22 -1 -7 -12 3.88 0.24 -1 7 -12 3.86 0.22 2 -7 12 4.25 0.21 -2 -7 -12 4.26 0.23 2 -7 12 4.21 0.23 2 -7 12 4.38 0.17 -2 -8 12 3.88 0.22 -2 -8 12 3.90 0.16 -1 -8 12 2.85 0.21 -1 -8 12 2.92 0.16 -1 -8 12 2.81 0.14 0 -8 12 0.93 0.13 0 -8 12 0.93 0.10 0 -8 12 1.43 0.19 0 -8 -12 1.18 0.16 0 -8 12 0.95 0.11 1 -8 12 4.34 0.21 -1 -8 -12 4.32 0.23 1 -8 12 3.86 0.23 1 -8 12 4.03 0.17 -2 -8 -12 4.09 0.21 2 -8 12 4.39 0.20 2 -8 12 3.95 0.22 2 -8 12 4.08 0.16 -2 -9 12 0.86 0.15 -2 -9 12 1.04 0.09 -1 -9 12 1.01 0.12 -1 -9 12 0.80 0.13 -1 -9 12 1.10 0.09 0 -9 12 0.52 0.07 0 -9 12 0.62 0.12 0 -9 12 0.68 0.13 0 -9 -12 0.69 0.12 0 -9 12 0.58 0.09 -1 -9 -12 1.43 0.16 1 -9 12 1.29 0.17 1 -9 12 1.15 0.10 1 -9 12 1.30 0.14 2 -9 12 1.14 0.09 2 -9 12 0.90 0.16 -2 -9 -12 1.28 0.15 2 -9 12 1.37 0.13 -2 -10 12 0.32 0.10 -2 -10 12 0.27 0.05 -1 -10 12 1.27 0.11 -1 -10 12 1.20 0.09 -1 -10 12 1.12 0.15 -1 -10 12 1.10 0.17 0 -10 12 0.63 0.09 0 -10 12 0.85 0.12 0 -10 12 0.72 0.09 0 -10 12 0.71 0.12 0 -10 -12 0.61 0.10 1 -10 12 0.98 0.16 1 -10 12 1.03 0.13 -1 -10 -12 1.07 0.15 2 -10 12 0.45 0.09 2 -10 12 0.30 0.05 2 -10 12 0.27 0.10 -2 -10 -12 0.57 0.10 -1 -11 12 0.68 0.08 -1 -11 12 0.86 0.12 -1 -11 12 0.77 0.14 0 -11 12 0.29 0.08 0 -11 12 0.40 0.11 0 -11 12 0.45 0.11 0 -11 12 0.33 0.07 0 -11 -12 0.40 0.09 -1 -11 -12 1.31 0.14 1 -11 12 1.39 0.13 1 -11 12 1.28 0.15 0 -12 12 0.39 0.09 0 -12 -12 0.45 0.08 0 -12 12 0.42 0.10 0 -12 12 0.42 0.06 -2 0 13 2.45 0.15 -1 0 13 4.63 0.21 1 0 -13 4.83 0.24 0 0 13 0.13 0.08 0 0 -13 -0.06 0.10 -1 0 -13 3.63 0.22 1 0 13 3.44 0.17 -2 0 -13 1.61 0.15 -2 -1 13 2.74 0.15 2 1 -13 2.52 0.16 -2 1 13 2.84 0.15 -1 -1 13 0.97 0.13 1 -1 -13 0.94 0.16 1 1 -13 1.09 0.17 -1 1 13 1.22 0.13 0 -1 13 9.05 0.34 0 -1 -13 9.72 0.38 0 -1 13 8.91 0.31 0 1 -13 9.45 0.38 0 1 13 8.95 0.34 1 -1 13 1.20 0.13 -1 -1 -13 1.26 0.17 1 -1 13 1.19 0.08 -1 1 -13 1.13 0.17 -2 -1 -13 2.96 0.18 -2 -2 13 1.47 0.12 -2 2 13 1.17 0.11 2 2 -13 1.42 0.14 1 -2 -13 3.92 0.22 -1 -2 13 3.93 0.19 -1 2 13 3.72 0.18 1 2 -13 4.09 0.22 0 -2 -13 1.52 0.18 0 -2 13 1.44 0.09 0 -2 13 1.34 0.13 0 2 13 1.31 0.13 0 2 -13 1.31 0.18 1 -2 13 3.30 0.13 -1 -2 -13 3.24 0.21 1 -2 13 3.41 0.18 -1 2 -13 3.16 0.20 2 -2 13 0.92 0.07 -2 -2 -13 0.97 0.14 -2 -3 13 2.42 0.14 2 3 -13 2.29 0.16 -2 3 13 2.45 0.14 -1 -3 13 0.55 0.06 -1 -3 13 0.32 0.08 1 -3 -13 0.32 0.10 1 3 -13 0.19 0.11 -1 3 13 0.37 0.07 0 -3 13 0.96 0.09 0 -3 13 1.17 0.13 0 -3 -13 1.37 0.17 0 3 -13 0.95 0.17 1 -3 13 0.49 0.06 1 -3 13 0.52 0.09 -1 -3 -13 0.73 0.13 -1 3 -13 0.62 0.11 2 -3 13 1.99 0.13 -2 -3 -13 1.66 0.15 2 -3 13 1.94 0.09 -2 -4 13 0.38 0.07 -2 4 13 0.39 0.07 2 4 -13 0.38 0.09 1 -4 -13 6.26 0.27 -1 -4 13 6.69 0.26 -1 -4 13 6.15 0.22 1 4 -13 6.36 0.29 -1 4 13 6.18 0.24 0 -4 13 1.97 0.11 0 -4 13 1.74 0.15 0 -4 -13 1.80 0.18 0 4 -13 2.21 0.19 1 -4 13 6.15 0.26 -1 -4 -13 6.72 0.29 1 -4 13 6.37 0.23 -1 4 -13 6.26 0.28 2 -4 13 0.55 0.07 -2 -4 -13 0.43 0.09 2 -4 13 0.57 0.07 -2 -5 13 2.62 0.14 -2 5 13 2.24 0.12 2 5 -13 2.52 0.16 1 -5 -13 -0.02 0.10 -1 -5 13 0.05 0.07 -1 -5 13 0.06 0.05 0 -5 13 0.86 0.09 0 -5 13 0.91 0.12 0 -5 -13 0.93 0.16 0 5 -13 0.77 0.12 1 -5 13 0.10 0.08 1 -5 13 0.04 0.05 -1 -5 -13 0.02 0.10 -1 5 -13 0.06 0.09 2 -5 13 3.31 0.13 -2 -5 -13 3.17 0.18 2 -5 13 3.10 0.16 -1 -6 13 1.05 0.08 1 -6 -13 1.15 0.14 -1 -6 13 1.13 0.12 0 -6 13 0.49 0.08 0 -6 13 0.40 0.06 0 -6 -13 0.38 0.10 0 6 -13 0.55 0.11 1 -6 13 0.85 0.13 -1 -6 -13 1.12 0.15 1 -6 13 1.15 0.09 -1 6 -13 1.21 0.14 -1 -7 13 1.70 0.12 -1 -7 13 1.58 0.09 0 -7 -13 2.69 0.18 0 -7 13 2.92 0.17 0 -7 13 3.13 0.13 0 7 -13 2.78 0.19 1 -7 13 1.42 0.13 1 -7 13 1.33 0.09 -1 -7 -13 1.32 0.16 -1 7 -13 1.11 0.13 -1 -8 13 1.66 0.09 -1 -8 13 1.61 0.12 0 -8 13 1.64 0.13 0 -8 -13 1.67 0.14 0 -8 13 1.69 0.10 0 8 -13 1.63 0.15 1 -8 13 1.93 0.13 -1 -8 -13 1.85 0.16 1 -8 13 1.84 0.10 0 0 14 1.15 0.10 0 0 -14 1.12 0.14 0 -1 14 1.20 0.11 0 -1 -14 1.21 0.15 0 1 14 1.23 0.10 0 1 -14 1.21 0.14 0 -2 -14 2.80 0.17 0 -2 14 2.68 0.15 0 2 -14 2.74 0.17 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 5349 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp O1 O 0.9975(3) 0.57891(10) 0.61621(14) 0.0226(4) Uani 1 1 d . . O2 O 0.6922(3) 0.54851(9) 0.82723(16) 0.0233(4) Uani 1 1 d . . O3 O 1.0633(3) 0.47542(9) 0.69549(14) 0.0228(4) Uani 1 1 d . . O4 O 0.8210(3) 0.65929(10) 0.87146(15) 0.0272(4) Uani 1 1 d . . C1 C 1.1042(5) 0.51353(14) 0.5943(2) 0.0211(6) Uani 1 1 d . . C2 C 1.0203(5) 0.59275(14) 0.7341(2) 0.0221(6) Uani 1 1 d . . H2 H 1.1401 0.6286 0.7504 0.027 Uiso 1 1 calc R U C3 C 0.7836(5) 0.61049(14) 0.7847(2) 0.0219(6) Uani 1 1 d . . H3 H 0.6789 0.6298 0.7252 0.026 Uiso 1 1 calc R U C4 C 0.8826(5) 0.50859(15) 0.8706(2) 0.0239(6) Uani 1 1 d . . H4 H 0.8402 0.4589 0.8655 0.029 Uiso 1 1 calc R U C5 C 1.0808(5) 0.52244(14) 0.7879(2) 0.0230(6) Uani 1 1 d . . H5 H 1.2369 0.5219 0.8249 0.028 Uiso 1 1 calc R U C6 C 1.3617(5) 0.52147(15) 0.5715(2) 0.0266(6) Uani 1 1 d . . H6A H 1.3851 0.5545 0.5101 0.040 Uiso 1 1 calc R U H6B H 1.4272 0.4770 0.5498 0.040 Uiso 1 1 calc R U H6C H 1.4393 0.5381 0.6401 0.040 Uiso 1 1 calc R U C7 C 0.9790(5) 0.47890(15) 0.4974(2) 0.0251(6) Uani 1 1 d . . H7A H 0.8117 0.4787 0.5124 0.038 Uiso 1 1 calc R U H7B H 1.0345 0.4316 0.4898 0.038 Uiso 1 1 calc R U H7C H 1.0095 0.5040 0.4271 0.038 Uiso 1 1 calc R U C8 C 0.6096(6) 0.67802(17) 0.9274(3) 0.0352(7) Uani 1 1 d . . H8A H 0.4963 0.6937 0.8712 0.053 Uiso 1 1 calc R U H8B H 0.6406 0.7150 0.9814 0.053 Uiso 1 1 calc R U H8C H 0.5474 0.6381 0.9677 0.053 Uiso 1 1 calc R U C9 C 0.9378(5) 0.52505(15) 0.9925(2) 0.0260(6) Uani 1 1 d . . H9 H 0.9949 0.5726 1.0082 0.031 Uiso 1 1 calc R U C10 C 1.0283(7) 0.46968(19) 1.0676(3) 0.0401(8) Uani 1 1 d . . H10A H 1.1404 0.4828 1.1273 0.048 Uiso 1 1 calc R U H10B H 1.0549 0.4239 1.0338 0.048 Uiso 1 1 calc R U C11 C 0.7790(6) 0.49377(15) 1.0805(3) 0.0339(7) Uani 1 1 d . . H11 H 0.6592 0.4615 1.0501 0.041 Uiso 1 1 calc R U C12 C 0.7062(6) 0.53394(17) 1.1765(3) 0.0339(7) Uani 1 1 d . . C13 C 0.6456(6) 0.56754(19) 1.2544(3) 0.0384(8) Uani 1 1 d . . H13 H 0.5970 0.5945 1.3169 0.046 Uiso 1 1 calc R U O5 O 0.4174(4) 0.35384(9) 0.43011(16) 0.0265(4) Uani 1 1 d . . O6 O 0.7986(3) 0.27806(10) 0.55303(16) 0.0243(4) Uani 1 1 d . . O7 O 0.4896(4) 0.25185(10) 0.34700(15) 0.0272(4) Uani 1 1 d . . O8 O 0.6613(3) 0.16900(10) 0.60083(15) 0.0267(4) Uani 1 1 d . . C21 C 0.3810(5) 0.31703(15) 0.3279(2) 0.0249(6) Uani 1 1 d . . C22 C 0.4654(5) 0.23632(14) 0.4645(2) 0.0222(6) Uani 1 1 d . . H22 H 0.3438 0.2008 0.4792 0.027 Uiso 1 1 calc R U C23 C 0.7010(5) 0.21651(14) 0.5126(2) 0.0241(6) Uani 1 1 d . . H23 H 0.8013 0.1958 0.4526 0.029 Uiso 1 1 calc R U C24 C 0.6138(5) 0.31930(14) 0.5993(2) 0.0233(6) Uani 1 1 d . . H24 H 0.6581 0.3688 0.5924 0.028 Uiso 1 1 calc R U C25 C 0.4096(5) 0.30558(14) 0.5210(2) 0.0227(6) Uani 1 1 d . . H25 H 0.2572 0.3055 0.5614 0.027 Uiso 1 1 calc R U C26 C 0.5063(6) 0.35353(17) 0.2338(3) 0.0337(7) Uani 1 1 d . . H26A H 0.6727 0.3551 0.2507 0.051 Uiso 1 1 calc R U H26B H 0.4464 0.4004 0.2269 0.051 Uiso 1 1 calc R U H26C H 0.4814 0.3289 0.1626 0.051 Uiso 1 1 calc R U C27 C 0.1252(5) 0.30876(17) 0.3045(2) 0.0305(7) Uani 1 1 d . . H27A H 0.1036 0.2799 0.2374 0.046 Uiso 1 1 calc R U H27B H 0.0557 0.3539 0.2911 0.046 Uiso 1 1 calc R U H27C H 0.0501 0.2871 0.3697 0.046 Uiso 1 1 calc R U C28 C 0.8718(6) 0.15020(16) 0.6577(3) 0.0341(7) Uani 1 1 d . . H28A H 0.9880 0.1361 0.6018 0.051 Uiso 1 1 calc R U H28B H 0.8409 0.1120 0.7095 0.051 Uiso 1 1 calc R U H28C H 0.9303 0.1896 0.7006 0.051 Uiso 1 1 calc R U C29 C 0.5679(5) 0.30363(14) 0.7223(2) 0.0241(6) Uani 1 1 d . . H29 H 0.5009 0.2575 0.7402 0.029 Uiso 1 1 calc R U C30 C 0.5017(6) 0.36185(16) 0.7988(3) 0.0322(7) Uani 1 1 d . . H30A H 0.3947 0.3518 0.8622 0.039 Uiso 1 1 calc R U H30B H 0.4827 0.4079 0.7645 0.039 Uiso 1 1 calc R U C31 C 0.7453(5) 0.33217(15) 0.8047(2) 0.0265(6) Uani 1 1 d . . H31 H 0.8696 0.3612 0.7702 0.032 Uiso 1 1 calc R U C32 C 0.8152(5) 0.29267(15) 0.9018(2) 0.0285(6) Uani 1 1 d . . C33 C 0.8753(6) 0.26041(17) 0.9812(3) 0.0359(7) Uani 1 1 d . . H33 H 0.9236 0.2345 1.0450 0.043 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0272(10) 0.0216(10) 0.0191(9) -0.0002(7) 0.0001(8) 0.0027(8) O2 0.0206(10) 0.0262(10) 0.0232(9) -0.0025(7) 0.0005(8) -0.0028(8) O3 0.0302(10) 0.0189(9) 0.0193(9) -0.0013(8) 0.0020(8) 0.0006(9) O4 0.0298(10) 0.0247(10) 0.0272(10) -0.0066(8) 0.0007(8) 0.0017(9) C1 0.0240(14) 0.0192(13) 0.0200(12) 0.0011(11) 0.0009(11) 0.0005(11) C2 0.0237(15) 0.0225(15) 0.0202(13) -0.0006(11) -0.0005(11) -0.0019(11) C3 0.0226(14) 0.0215(13) 0.0215(13) -0.0012(10) -0.0034(10) -0.0008(12) C4 0.0266(14) 0.0225(14) 0.0227(13) 0.0000(11) 0.0011(12) 0.0006(12) C5 0.0257(14) 0.0215(15) 0.0218(13) -0.0003(11) -0.0033(11) 0.0007(12) C6 0.0266(15) 0.0289(16) 0.0244(13) -0.0025(12) -0.0009(12) -0.0001(13) C7 0.0235(13) 0.0281(15) 0.0237(12) -0.0044(13) 0.0001(10) 0.0002(13) C8 0.0353(17) 0.0359(19) 0.0346(16) -0.0086(14) 0.0059(13) 0.0064(14) C9 0.0316(16) 0.0270(16) 0.0194(13) -0.0024(11) 0.0001(11) 0.0018(12) C10 0.056(2) 0.0410(19) 0.0236(15) -0.0016(15) -0.0008(14) 0.0184(17) C11 0.0505(19) 0.0290(17) 0.0223(15) -0.0010(11) 0.0049(14) -0.0053(15) C12 0.0361(16) 0.0378(17) 0.0278(15) 0.0005(14) 0.0006(13) -0.0071(15) C13 0.0371(19) 0.051(2) 0.0269(16) -0.0111(15) 0.0048(14) -0.0062(16) O5 0.0314(11) 0.0226(10) 0.0255(10) 0.0019(8) -0.0053(9) 0.0022(9) O6 0.0234(10) 0.0239(10) 0.0256(10) 0.0014(7) -0.0002(8) 0.0007(9) O7 0.0362(11) 0.0258(10) 0.0197(8) 0.0009(8) 0.0000(8) 0.0048(9) O8 0.0348(11) 0.0221(10) 0.0233(9) 0.0040(8) -0.0017(8) 0.0026(9) C21 0.0255(14) 0.0263(14) 0.0230(12) 0.0027(11) -0.0019(11) 0.0020(12) C22 0.0231(13) 0.0234(15) 0.0201(13) 0.0020(11) 0.0006(10) -0.0028(11) C23 0.0280(15) 0.0218(14) 0.0225(13) 0.0001(11) 0.0008(12) 0.0012(12) C24 0.0242(13) 0.0185(14) 0.0272(13) 0.0019(11) -0.0018(12) -0.0007(12) C25 0.0190(13) 0.0276(16) 0.0216(12) 0.0037(11) 0.0010(11) 0.0008(11) C26 0.0246(15) 0.0444(19) 0.0321(15) 0.0105(14) -0.0016(13) 0.0038(14) C27 0.0262(15) 0.0412(18) 0.0242(13) -0.0001(13) -0.0016(12) -0.0014(14) C28 0.0441(18) 0.0272(16) 0.0309(16) 0.0059(13) -0.0053(14) 0.0074(14) C29 0.0250(15) 0.0218(14) 0.0254(13) -0.0006(11) -0.0024(11) 0.0014(12) C30 0.0381(17) 0.0327(17) 0.0257(15) -0.0050(13) -0.0046(13) 0.0096(14) C31 0.0305(16) 0.0252(15) 0.0238(14) -0.0023(11) -0.0061(11) 0.0012(12) C32 0.0309(16) 0.0291(15) 0.0255(13) -0.0037(13) -0.0010(13) -0.0001(13) C33 0.0338(16) 0.0448(19) 0.0293(15) 0.0088(14) -0.0049(13) 0.0016(15) 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' 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 C2 O1 C1 107.74(19) C3 O2 C4 107.8(2) C1 O3 C5 107.19(19) C3 O4 C8 112.1(2) O3 C1 O1 103.8(2) O3 C1 C7 108.9(2) O1 C1 C7 109.1(2) O3 C1 C6 111.3(2) O1 C1 C6 111.1(2) C7 C1 C6 112.2(2) O1 C2 C3 110.1(2) O1 C2 C5 104.7(2) C3 C2 C5 103.9(2) O1 C2 H2 112.5 C3 C2 H2 112.5 C5 C2 H2 112.5 O2 C3 O4 111.9(2) O2 C3 C2 106.2(2) O4 C3 C2 107.4(2) O2 C3 H3 110.4 O4 C3 H3 110.4 C2 C3 H3 110.4 O2 C4 C9 112.7(2) O2 C4 C5 104.2(2) C9 C4 C5 114.6(2) O2 C4 H4 108.4 C9 C4 H4 108.4 C5 C4 H4 108.4 O3 C5 C4 108.9(2) O3 C5 C2 103.72(19) C4 C5 C2 104.5(2) O3 C5 H5 113.0 C4 C5 H5 113.0 C2 C5 H5 113.0 C1 C6 H6A 109.5 C1 C6 H6B 109.5 H6A C6 H6B 109.5 C1 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C1 C7 H7A 109.5 C1 C7 H7B 109.5 H7A C7 H7B 109.5 C1 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 O4 C8 H8A 109.5 O4 C8 H8B 109.5 H8A C8 H8B 109.5 O4 C8 H8C 109.5 H8A C8 H8C 109.5 H8B C8 H8C 109.5 C10 C9 C4 119.2(3) C10 C9 C11 60.7(2) C4 C9 C11 116.3(3) C10 C9 H9 116.3 C4 C9 H9 116.3 C11 C9 H9 116.3 C9 C10 C11 60.4(2) C9 C10 H10A 117.7 C11 C10 H10A 117.7 C9 C10 H10B 117.7 C11 C10 H10B 117.7 H10A C10 H10B 114.9 C12 C11 C9 119.9(3) C12 C11 C10 121.5(3) C9 C11 C10 58.9(2) C12 C11 H11 115.0 C9 C11 H11 115.0 C10 C11 H11 115.0 C13 C12 C11 179.2(4) C12 C13 H13 180.0 C21 O5 C25 107.6(2) C23 O6 C24 107.9(2) C22 O7 C21 107.4(2) C23 O8 C28 112.1(2) O5 C21 O7 104.4(2) O5 C21 C26 108.6(2) O7 C21 C26 109.0(2) O5 C21 C27 110.7(2) O7 C21 C27 111.2(3) C26 C21 C27 112.6(2) O7 C22 C23 109.2(2) O7 C22 C25 104.9(2) C23 C22 C25 104.3(2) O7 C22 H22 112.6 C23 C22 H22 112.6 C25 C22 H22 112.6 O6 C23 O8 111.8(2) O6 C23 C22 105.5(2) O8 C23 C22 107.3(2) O6 C23 H23 110.7 O8 C23 H23 110.7 C22 C23 H23 110.7 O6 C24 C29 112.5(2) O6 C24 C25 104.1(2) C29 C24 C25 114.5(2) O6 C24 H24 108.5 C29 C24 H24 108.5 C25 C24 H24 108.5 O5 C25 C24 108.5(2) O5 C25 C22 104.1(2) C24 C25 C22 104.8(2) O5 C25 H25 112.9 C24 C25 H25 112.9 C22 C25 H25 112.9 C21 C26 H26A 109.5 C21 C26 H26B 109.5 H26A C26 H26B 109.5 C21 C26 H26C 109.5 H26A C26 H26C 109.5 H26B C26 H26C 109.5 C21 C27 H27A 109.5 C21 C27 H27B 109.5 H27A C27 H27B 109.5 C21 C27 H27C 109.5 H27A C27 H27C 109.5 H27B C27 H27C 109.5 O8 C28 H28A 109.5 O8 C28 H28B 109.5 H28A C28 H28B 109.5 O8 C28 H28C 109.5 H28A C28 H28C 109.5 H28B C28 H28C 109.5 C30 C29 C24 118.2(2) C30 C29 C31 60.49(19) C24 C29 C31 115.2(2) C30 C29 H29 117.0 C24 C29 H29 117.0 C31 C29 H29 117.0 C29 C30 C31 60.32(19) C29 C30 H30A 117.7 C31 C30 H30A 117.7 C29 C30 H30B 117.7 C31 C30 H30B 117.7 H30A C30 H30B 114.9 C32 C31 C29 120.3(3) C32 C31 C30 119.9(3) C29 C31 C30 59.20(19) C32 C31 H31 115.3 C29 C31 H31 115.3 C30 C31 H31 115.3 C33 C32 C31 179.2(4) C32 C33 H33 180.0 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 C2 1.426(3) O1 C1 1.438(3) O2 C3 1.410(3) O2 C4 1.439(3) O3 C1 1.428(3) O3 C5 1.429(3) O4 C3 1.415(3) O4 C8 1.433(4) C1 C7 1.512(4) C1 C6 1.516(4) C2 C3 1.529(4) C2 C5 1.550(4) C2 H2 1.0000 C3 H3 1.0000 C4 C9 1.509(4) C4 C5 1.528(4) C4 H4 1.0000 C5 H5 1.0000 C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C8 H8A 0.9800 C8 H8B 0.9800 C8 H8C 0.9800 C9 C10 1.492(4) C9 C11 1.514(4) C9 H9 1.0000 C10 C11 1.519(5) C10 H10A 0.9900 C10 H10B 0.9900 C11 C12 1.441(5) C11 H11 1.0000 C12 C13 1.182(5) C13 H13 0.9500 O5 C21 1.421(3) O5 C25 1.428(3) O6 C23 1.408(3) O6 C24 1.442(3) O7 C22 1.428(3) O7 C21 1.434(4) O8 C23 1.413(3) O8 C28 1.434(4) C21 C26 1.505(4) C21 C27 1.508(4) C22 C23 1.521(4) C22 C25 1.540(4) C22 H22 1.0000 C23 H23 1.0000 C24 C29 1.510(4) C24 C25 1.520(4) C24 H24 1.0000 C25 H25 1.0000 C26 H26A 0.9800 C26 H26B 0.9800 C26 H26C 0.9800 C27 H27A 0.9800 C27 H27B 0.9800 C27 H27C 0.9800 C28 H28A 0.9800 C28 H28B 0.9800 C28 H28C 0.9800 C29 C30 1.500(4) C29 C31 1.517(4) C29 H29 1.0000 C30 C31 1.520(4) C30 H30A 0.9900 C30 H30B 0.9900 C31 C32 1.439(4) C31 H31 1.0000 C32 C33 1.181(4) C33 H33 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 C5 O3 C1 O1 -36.5(3) C5 O3 C1 C7 -152.6(2) C5 O3 C1 C6 83.1(3) C2 O1 C1 O3 32.7(3) C2 O1 C1 C7 148.7(2) C2 O1 C1 C6 -87.1(3) C1 O1 C2 C3 -127.7(2) C1 O1 C2 C5 -16.6(3) C4 O2 C3 O4 -81.8(2) C4 O2 C3 C2 35.1(3) C8 O4 C3 O2 -61.9(3) C8 O4 C3 C2 -178.2(2) O1 C2 C3 O2 93.6(2) C5 C2 C3 O2 -18.1(3) O1 C2 C3 O4 -146.4(2) C5 C2 C3 O4 101.9(2) C3 O2 C4 C9 87.5(3) C3 O2 C4 C5 -37.3(3) C1 O3 C5 C4 136.6(2) C1 O3 C5 C2 25.7(3) O2 C4 C5 O3 -86.3(2) C9 C4 C5 O3 150.1(2) O2 C4 C5 C2 24.0(3) C9 C4 C5 C2 -99.6(3) O1 C2 C5 O3 -5.4(3) C3 C2 C5 O3 110.1(2) O1 C2 C5 C4 -119.4(2) C3 C2 C5 C4 -3.9(3) O2 C4 C9 C10 147.8(3) C5 C4 C9 C10 -93.2(3) O2 C4 C9 C11 78.2(3) C5 C4 C9 C11 -162.8(3) C4 C9 C10 C11 -105.6(3) C10 C9 C11 C12 110.9(4) C4 C9 C11 C12 -138.8(3) C4 C9 C11 C10 110.3(3) C9 C10 C11 C12 -108.3(3) C25 O5 C21 O7 -34.3(3) C25 O5 C21 C26 -150.4(2) C25 O5 C21 C27 85.5(3) C22 O7 C21 O5 32.5(3) C22 O7 C21 C26 148.4(2) C22 O7 C21 C27 -86.9(3) C21 O7 C22 C23 -129.6(2) C21 O7 C22 C25 -18.4(3) C24 O6 C23 O8 -80.3(2) C24 O6 C23 C22 36.1(3) C28 O8 C23 O6 -60.8(3) C28 O8 C23 C22 -176.1(2) O7 C22 C23 O6 91.4(2) C25 C22 C23 O6 -20.3(3) O7 C22 C23 O8 -149.2(2) C25 C22 C23 O8 99.1(2) C23 O6 C24 C29 87.8(3) C23 O6 C24 C25 -36.7(3) C21 O5 C25 C24 133.7(2) C21 O5 C25 C22 22.4(3) O6 C24 C25 O5 -88.8(2) C29 C24 C25 O5 148.0(2) O6 C24 C25 C22 22.0(3) C29 C24 C25 C22 -101.2(2) O7 C22 C25 O5 -2.3(3) C23 C22 C25 O5 112.5(2) O7 C22 C25 C24 -116.2(2) C23 C22 C25 C24 -1.4(3) O6 C24 C29 C30 143.8(3) C25 C24 C29 C30 -97.7(3) O6 C24 C29 C31 75.2(3) C25 C24 C29 C31 -166.2(2) C24 C29 C30 C31 -104.6(3) C30 C29 C31 C32 108.9(3) C24 C29 C31 C32 -141.6(3) C24 C29 C31 C30 109.5(3) C29 C30 C31 C32 -109.5(3)