#------------------------------------------------------------------------------ #$Date: 2015-02-27 07:51:47 +0200 (Fri, 27 Feb 2015) $ #$Revision: 132511 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/07/4030726.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_4030726 loop_ _publ_author_name 'Wang, Weiguo' 'Peng, Xianglong' 'Qin, Xiaoyu' 'Zhao, Xiangyun' 'Ma, Chen' 'Tung, Chen-Ho' 'Xu, Zhenghu' _publ_section_title ; Synthesis of Quinolinones with Palladium-Catalyzed Oxidative Annulation between Acrylamides and Arynes. ; _journal_name_full 'The Journal of organic chemistry' _journal_page_first 150225162816008 _journal_paper_doi 10.1021/jo5027673 _journal_year 2015 _chemical_formula_moiety 'C16 H13 N O2' _chemical_formula_sum 'C16 H13 N O2' _chemical_formula_weight 251.27 _chemical_name_systematic ; ? ; _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 _atom_sites_solution_primary iterative _audit_creation_date 2014-10-27 _audit_creation_method ; Olex2 1.2 (compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874) ; _cell_angle_alpha 90 _cell_angle_beta 90.917(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 8.3004(4) _cell_length_b 21.1079(9) _cell_length_c 14.7263(6) _cell_measurement_reflns_used 3874 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 62.897 _cell_measurement_theta_min 3.660 _cell_volume 2579.8(2) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution ; Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012) ; _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.882 _diffrn_measured_fraction_theta_max 0.967 _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0711 _diffrn_reflns_av_unetI/netI 0.0914 _diffrn_reflns_laue_measured_fraction_full 0.882 _diffrn_reflns_laue_measured_fraction_max 0.967 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 17775 _diffrn_reflns_point_group_measured_fraction_full 0.807 _diffrn_reflns_point_group_measured_fraction_max 0.886 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 63.685 _diffrn_reflns_theta_min 3.660 _exptl_absorpt_coefficient_mu 0.691 _exptl_crystal_density_diffrn 1.294 _exptl_crystal_description block _exptl_crystal_F_000 1056 _refine_diff_density_max 0.646 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.097 _refine_ls_abs_structure_details ; Flack x determined using 1799 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.6(4) _refine_ls_extinction_coef 0.0009(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 690 _refine_ls_number_reflns 7533 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.1285 _refine_ls_R_factor_gt 0.0976 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2486 _refine_ls_wR_factor_ref 0.2936 _reflns_Friedel_coverage 0.778 _reflns_friedel_fraction_full 0.727 _reflns_friedel_fraction_max 0.800 _reflns_number_gt 5161 _reflns_number_total 7533 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL CF solution in P21 New: P21 New: P21 CELL 1.54184 8.3004 21.1079 14.7263 90 90.917 90 ZERR 8 0.0004 0.0009 0.0006 0 0.003 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H N O UNIT 128 104 8 16 L.S. 5 PLAN -20 BOND $H CONF fmap 2 acta REM K:/Measurements%20of%20single%20crystal%20for%20SDU/2014/Xu%20Zheng-H REM u/6-G-2-16/test.hkl WGHT 0.200000 EXTI 0.000893 FVAR 0.31867 O1 4 -0.459669 0.035636 0.357520 11.00000 0.08970 0.07682 = 0.05434 0.01978 0.00018 0.02239 O2 4 -0.347136 0.151875 0.368293 11.00000 0.11248 0.08789 = 0.04009 -0.00094 0.00234 0.01512 N1 3 -0.443357 0.074503 0.278925 11.00000 0.06810 0.06840 = 0.04294 0.00889 0.00461 0.01221 C1 1 -0.600750 0.052161 0.407317 11.00000 0.11355 0.10193 = 0.09656 0.02297 0.04740 0.01115 AFIX 137 H1A 2 -0.689943 0.057965 0.365846 11.00000 -1.50000 H1B 2 -0.581462 0.090762 0.440206 11.00000 -1.50000 H1C 2 -0.625251 0.018814 0.449220 11.00000 -1.50000 AFIX 0 C2 1 -0.601229 -0.038935 0.107783 11.00000 0.08764 0.06459 = 0.08998 -0.00456 -0.00561 0.01224 AFIX 43 H2 2 -0.649344 -0.078662 0.104115 11.00000 -1.20000 AFIX 0 C3 1 -0.570433 -0.006470 0.029058 11.00000 0.09123 0.06937 = 0.06739 -0.00680 -0.00651 0.01784 AFIX 43 H3 2 -0.598623 -0.024106 -0.026845 11.00000 -1.20000 AFIX 0 C4 1 -0.496621 0.053163 0.032948 11.00000 0.07042 0.07770 = 0.05159 -0.01238 0.00091 0.00775 AFIX 43 H4 2 -0.476584 0.075242 -0.020343 11.00000 -1.20000 AFIX 0 C5 1 -0.452790 0.079666 0.117436 11.00000 0.06125 0.05736 = 0.04713 0.00224 0.00290 0.01269 C6 1 -0.486430 0.045414 0.197720 11.00000 0.06160 0.05515 = 0.04753 0.00523 0.00097 0.01822 C7 1 -0.562341 -0.013967 0.193006 11.00000 0.06863 0.06397 = 0.06671 0.00736 0.01144 0.01373 AFIX 43 H7 2 -0.586190 -0.036186 0.245642 11.00000 -1.20000 AFIX 0 C8 1 -0.382640 0.140174 0.124601 11.00000 0.06238 0.06421 = 0.05135 -0.00127 0.00414 0.01429 AFIX 43 H8 2 -0.360525 0.162331 0.071656 11.00000 -1.20000 AFIX 0 C9 1 -0.345478 0.167845 0.206926 11.00000 0.05578 0.05947 = 0.05108 0.00182 -0.00240 0.01248 C10 1 -0.375018 0.132597 0.290894 11.00000 0.05972 0.07092 = 0.04861 0.00083 -0.00005 0.01373 C11 1 -0.280019 0.232339 0.211420 11.00000 0.05698 0.07206 = 0.05203 -0.00540 -0.00303 0.01377 C12 1 -0.335281 0.278004 0.151436 11.00000 0.08879 0.05806 = 0.07291 -0.00154 -0.01582 0.00376 AFIX 43 H12 2 -0.418854 0.268098 0.111081 11.00000 -1.20000 AFIX 0 C13 1 -0.268566 0.338701 0.149983 11.00000 0.09602 0.06819 = 0.09284 -0.00634 -0.01706 0.01824 AFIX 43 H13 2 -0.300047 0.367405 0.105194 11.00000 -1.20000 AFIX 0 C14 1 -0.158394 0.355555 0.213705 11.00000 0.07514 0.07617 = 0.08987 -0.01839 0.00555 0.00812 AFIX 43 H14 2 -0.118889 0.396778 0.215236 11.00000 -1.20000 AFIX 0 C15 1 -0.104416 0.312055 0.276290 11.00000 0.05812 0.10439 = 0.05688 -0.02024 -0.00064 0.00145 AFIX 43 H15 2 -0.027854 0.323915 0.319846 11.00000 -1.20000 AFIX 0 C16 1 -0.161479 0.252123 0.275231 11.00000 0.05877 0.08588 = 0.05394 0.00012 -0.00531 0.01099 AFIX 43 H16 2 -0.121734 0.223155 0.317573 11.00000 -1.20000 AFIX 0 O5 4 -0.265249 0.288569 -0.141075 11.00000 0.08001 0.06389 = 0.05205 -0.01411 -0.01220 0.00713 O6 4 -0.366714 0.170639 -0.127538 11.00000 0.10451 0.06675 = 0.04226 -0.00313 0.01993 -0.00305 N3 3 -0.281816 0.250148 -0.218189 11.00000 0.05528 0.05620 = 0.05152 -0.00946 -0.00010 0.00435 C17 1 -0.109848 0.274132 -0.095208 11.00000 0.08284 0.10480 = 0.06865 -0.02289 -0.02696 0.01075 AFIX 137 H17A 2 -0.026239 0.272305 -0.139427 11.00000 -1.50000 H17B 2 -0.117220 0.234037 -0.064783 11.00000 -1.50000 H17C 2 -0.085160 0.306677 -0.051626 11.00000 -1.50000 AFIX 0 C18 1 -0.196567 0.340097 -0.307365 11.00000 0.07287 0.06400 = 0.06979 -0.01148 0.00632 -0.00466 AFIX 43 H18 2 -0.176634 0.363784 -0.255134 11.00000 -1.20000 AFIX 0 C19 1 -0.170095 0.365601 -0.392036 11.00000 0.11151 0.06989 = 0.07345 0.00195 0.01868 -0.02387 AFIX 43 H19 2 -0.134097 0.407187 -0.396562 11.00000 -1.20000 AFIX 0 C20 1 -0.196033 0.330522 -0.470672 11.00000 0.11056 0.08229 = 0.07182 0.00465 0.01371 -0.02440 AFIX 43 H20 2 -0.178169 0.348452 -0.527312 11.00000 -1.20000 AFIX 0 C21 1 -0.248542 0.268847 -0.463756 11.00000 0.08323 0.07515 = 0.05011 0.00087 0.00878 -0.01561 AFIX 43 H21 2 -0.265285 0.244807 -0.515983 11.00000 -1.20000 AFIX 0 C22 1 -0.276905 0.242108 -0.378187 11.00000 0.06456 0.05889 = 0.05180 0.00200 0.00499 0.00206 C23 1 -0.253089 0.278881 -0.301565 11.00000 0.04748 0.05641 = 0.05313 -0.00046 0.00310 0.00489 C24 1 -0.336205 0.178994 -0.368621 11.00000 0.06898 0.06310 = 0.04104 -0.00295 0.00319 0.00136 AFIX 43 H24 2 -0.355612 0.155185 -0.420796 11.00000 -1.20000 AFIX 0 C25 1 -0.365286 0.152413 -0.287291 11.00000 0.05190 0.06085 = 0.05086 -0.00284 0.00467 0.00312 C26 1 -0.342653 0.189689 -0.203905 11.00000 0.04725 0.06263 = 0.04891 -0.00240 0.00455 0.00473 C27 1 -0.421510 0.086259 -0.279418 11.00000 0.05309 0.07110 = 0.04367 -0.00541 0.00033 -0.00394 C28 1 -0.546116 0.067193 -0.222865 11.00000 0.05374 0.08189 = 0.05174 -0.00442 0.00484 0.00578 AFIX 43 H28 2 -0.597304 0.097076 -0.186976 11.00000 -1.20000 AFIX 0 C29 1 -0.594149 0.004925 -0.219497 11.00000 0.06275 0.08641 = 0.05698 0.00848 0.00411 -0.01276 AFIX 43 H29 2 -0.676968 -0.007153 -0.181386 11.00000 -1.20000 AFIX 0 C30 1 -0.520271 -0.038921 -0.272012 11.00000 0.07580 0.07535 = 0.08093 -0.00483 0.00994 -0.01217 AFIX 43 H30 2 -0.553231 -0.080994 -0.269788 11.00000 -1.20000 AFIX 0 C31 1 -0.398537 -0.021918 -0.327838 11.00000 0.10045 0.06538 = 0.07809 -0.02072 0.03149 -0.01008 AFIX 43 H31 2 -0.349465 -0.052272 -0.363872 11.00000 -1.20000 AFIX 0 C32 1 -0.348338 0.039627 -0.331028 11.00000 0.07671 0.06150 = 0.07551 -0.00903 0.03548 -0.00840 AFIX 43 H32 2 -0.263539 0.050542 -0.368466 11.00000 -1.20000 AFIX 0 O3 4 0.051394 0.026476 -0.097302 11.00000 0.07873 0.08790 = 0.06250 -0.02951 -0.00553 0.02205 O4 4 0.155971 0.144515 -0.113368 11.00000 0.08307 0.08468 = 0.05368 -0.00401 0.01279 0.00942 N2 3 0.064378 0.066311 -0.022035 11.00000 0.06764 0.06768 = 0.04647 -0.00967 0.00144 0.01398 C33 1 -0.085667 0.040918 -0.149751 11.00000 0.13661 0.10331 = 0.08097 -0.00124 -0.04710 -0.00727 AFIX 137 H33A 2 -0.086698 0.015557 -0.203871 11.00000 -1.50000 H33B 2 -0.083946 0.084960 -0.165974 11.00000 -1.50000 H33C 2 -0.180447 0.032151 -0.115412 11.00000 -1.50000 AFIX 0 C34 1 -0.037089 -0.022061 0.064768 11.00000 0.07475 0.07610 = 0.07382 -0.00841 -0.00388 0.00051 AFIX 43 H34 2 -0.052383 -0.046144 0.012454 11.00000 -1.20000 AFIX 0 C35 1 -0.075505 -0.046488 0.151288 11.00000 0.09178 0.06878 = 0.09140 0.00412 0.00694 -0.00227 AFIX 43 H35 2 -0.112293 -0.087967 0.155810 11.00000 -1.20000 AFIX 0 C36 1 -0.060012 -0.010782 0.228361 11.00000 0.09270 0.09276 = 0.06884 0.02806 0.01304 0.02238 AFIX 43 H36 2 -0.092603 -0.027114 0.283770 11.00000 -1.20000 AFIX 0 C37 1 0.005008 0.050486 0.223989 11.00000 0.08396 0.07798 = 0.05481 -0.00574 0.00265 0.00472 AFIX 43 H37 2 0.020461 0.074144 0.276687 11.00000 -1.20000 AFIX 0 C38 1 0.046452 0.075703 0.139461 11.00000 0.06169 0.07584 = 0.04934 -0.00458 0.00345 0.00807 C39 1 0.024358 0.039227 0.060618 11.00000 0.05907 0.05410 = 0.05592 -0.00338 -0.00008 0.00924 C40 1 0.110994 0.138882 0.129531 11.00000 0.06443 0.06405 = 0.05063 -0.00756 0.00769 0.00857 AFIX 43 H40 2 0.125783 0.163678 0.181197 11.00000 -1.20000 AFIX 0 C41 1 0.150681 0.163311 0.048050 11.00000 0.05406 0.06205 = 0.04888 -0.00271 0.00506 0.01311 C42 1 0.125760 0.125777 -0.034896 11.00000 0.06029 0.07582 = 0.04749 -0.00575 0.00206 0.01775 C43 1 0.210998 0.228891 0.039609 11.00000 0.05703 0.06956 = 0.05032 -0.00343 0.00519 0.00432 C44 1 0.150085 0.275450 0.096445 11.00000 0.07306 0.08088 = 0.07240 -0.00719 0.01980 -0.00446 AFIX 43 H44 2 0.071377 0.265262 0.138248 11.00000 -1.20000 AFIX 0 C45 1 0.207341 0.337527 0.090619 11.00000 0.08121 0.06885 = 0.10794 -0.00447 0.02058 0.00231 AFIX 43 H45 2 0.165607 0.368287 0.128858 11.00000 -1.20000 AFIX 0 C46 1 0.322834 0.354163 0.030310 11.00000 0.07175 0.08715 = 0.09340 0.01751 -0.01001 -0.01094 AFIX 43 H46 2 0.359086 0.395745 0.026340 11.00000 -1.20000 AFIX 0 C47 1 0.384746 0.307006 -0.025092 11.00000 0.06542 0.10188 = 0.06586 0.02336 0.00299 -0.00510 AFIX 43 H47 2 0.464784 0.317519 -0.065921 11.00000 -1.20000 AFIX 0 C48 1 0.332195 0.246008 -0.021591 11.00000 0.05212 0.08955 = 0.05080 0.00046 0.00086 0.00850 AFIX 43 H48 2 0.376287 0.215629 -0.059595 11.00000 -1.20000 AFIX 0 O7 4 0.128291 0.173871 -0.614658 11.00000 0.08202 0.07455 = 0.05267 0.00227 -0.00358 0.00120 O8 4 0.241069 0.290387 -0.602321 11.00000 0.09734 0.07195 = 0.05657 0.01512 -0.00621 0.00615 N4 3 0.224406 0.253149 -0.524592 11.00000 0.07013 0.06357 = 0.04372 0.01071 -0.00164 0.01123 C49 1 0.380425 0.275245 -0.650715 11.00000 0.08390 0.11432 = 0.07497 0.01866 0.01067 -0.00286 AFIX 137 H49A 2 0.388422 0.302668 -0.702454 11.00000 -1.50000 H49B 2 0.374491 0.232013 -0.670731 11.00000 -1.50000 H49C 2 0.473570 0.280711 -0.612024 11.00000 -1.50000 AFIX 0 C50 1 0.325866 0.342811 -0.439187 11.00000 0.06955 0.06575 = 0.07455 0.00404 -0.00730 0.00156 AFIX 43 H50 2 0.342665 0.365916 -0.491968 11.00000 -1.20000 AFIX 0 C51 1 0.363139 0.367882 -0.354352 11.00000 0.09425 0.06863 = 0.10016 -0.00835 -0.00133 -0.00343 AFIX 43 H51 2 0.404768 0.408717 -0.350521 11.00000 -1.20000 AFIX 0 C52 1 0.339952 0.333558 -0.274478 11.00000 0.09813 0.08789 = 0.06840 -0.02726 -0.00922 -0.00105 AFIX 43 H52 2 0.367938 0.351518 -0.218757 11.00000 -1.20000 AFIX 0 C53 1 0.276960 0.274251 -0.277489 11.00000 0.07439 0.08231 = 0.06624 -0.01708 0.00114 0.00497 AFIX 43 H53 2 0.259197 0.251654 -0.224368 11.00000 -1.20000 AFIX 0 C54 1 0.238740 0.247465 -0.363821 11.00000 0.06726 0.06361 = 0.05078 -0.00138 -0.00686 0.01146 C55 1 0.263127 0.282503 -0.442372 11.00000 0.05992 0.04979 = 0.06438 0.00310 0.00278 0.00951 C56 1 0.173444 0.184630 -0.372426 11.00000 0.06744 0.06836 = 0.04459 0.00693 0.00205 0.00766 AFIX 43 H56 2 0.156335 0.161354 -0.319835 11.00000 -1.20000 AFIX 0 C57 1 0.135639 0.157708 -0.453561 11.00000 0.05493 0.06269 = 0.04703 0.00884 -0.00710 0.00689 C58 1 0.159456 0.193523 -0.537345 11.00000 0.05616 0.05479 = 0.04975 0.00166 -0.00338 0.01073 C59 1 0.073091 0.091507 -0.460341 11.00000 0.05552 0.07652 = 0.03615 0.00051 0.00315 0.00524 C60 1 0.140222 0.044844 -0.405007 11.00000 0.07911 0.06004 = 0.06161 0.00516 -0.01759 0.00399 AFIX 43 H60 2 0.224904 0.055262 -0.365674 11.00000 -1.20000 AFIX 0 C61 1 0.084029 -0.016433 -0.407200 11.00000 0.08844 0.06171 = 0.07272 0.00456 -0.00096 0.00282 AFIX 43 H61 2 0.130919 -0.047039 -0.369826 11.00000 -1.20000 AFIX 0 C62 1 -0.040234 -0.032196 -0.464118 11.00000 0.06564 0.07082 = 0.07255 -0.01076 0.00402 -0.00442 AFIX 43 H62 2 -0.078236 -0.073642 -0.465156 11.00000 -1.20000 AFIX 0 C63 1 -0.110007 0.012179 -0.519867 11.00000 0.05437 0.09577 = 0.05855 -0.02686 0.00362 0.00195 AFIX 43 H63 2 -0.194720 0.000991 -0.558734 11.00000 -1.20000 AFIX 0 C64 1 -0.052742 0.074672 -0.517923 11.00000 0.05307 0.09092 = 0.04528 -0.00618 0.00055 0.01047 AFIX 43 H64 2 -0.099831 0.105005 -0.555680 11.00000 -1.20000 AFIX 0 HKLF 4 REM CF solution in P21 New: P21 New: P21 REM R1 = 0.0976 for 5161 Fo > 4sig(Fo) and 0.1285 for all 7533 data REM 690 parameters refined using 1 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.646, deepest hole -0.286, 1-sigma level 0.097 Q1 1 0.1558 0.2881 0.3346 11.00000 0.05 0.65 Q2 1 -0.0204 0.0700 -0.2445 11.00000 0.05 0.56 Q3 1 -0.5497 0.0441 0.5393 11.00000 0.05 0.56 Q4 1 0.0554 0.1757 0.3428 11.00000 0.05 0.56 Q5 1 -0.4905 0.0668 0.4602 11.00000 0.05 0.55 Q6 1 -0.4845 -0.0204 0.0722 11.00000 0.05 0.55 Q7 1 -0.4127 0.1894 -0.0596 11.00000 0.05 0.53 Q8 1 0.1385 0.2528 0.2572 11.00000 0.05 0.52 Q9 1 0.0708 0.1455 -0.1572 11.00000 0.05 0.52 Q10 1 -0.0380 0.0393 -0.1574 11.00000 0.05 0.52 Q11 1 -0.0626 0.0423 -0.3185 11.00000 0.05 0.52 Q12 1 -0.2548 0.2466 -0.5414 11.00000 0.05 0.51 Q13 1 -0.4197 0.1643 -0.4763 11.00000 0.05 0.51 Q14 1 0.0711 0.1898 0.2677 11.00000 0.05 0.50 Q15 1 -0.0427 0.0754 -0.4058 11.00000 0.05 0.48 Q16 1 0.0592 0.1300 -0.2274 11.00000 0.05 0.47 Q17 1 -0.5175 0.0344 0.3807 11.00000 0.05 0.46 Q18 1 -0.6667 0.0034 -0.0390 11.00000 0.05 0.46 Q19 1 -0.5221 0.0776 0.6139 11.00000 0.05 0.46 Q20 1 -0.1174 -0.0157 -0.3366 11.00000 0.05 0.46 REM The information below was added by Olex2. REM REM R1 = 0.0976 for 5161 Fo > 4sig(Fo) and 0.1285 for all 17793 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.65, deepest hole -0.29 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.1285 REM R1_gt = 0.0976 REM wR_ref = 0.2936 REM GOOF = 1.062 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 17793 REM Reflections_gt = 5161 REM Parameters = n/a REM Hole = -0.29 REM Peak = 0.65 REM Flack = 0.6(4) ; _[local]_cod_data_source_file jo5027673_si_002.cif _[local]_cod_data_source_block test _cod_database_code 4030726 _shelxl_version_number 2013-4 _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. ; _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.a Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C21(H21), C24(H24), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C56(H56), C60(H60), C61(H61), C62(H62), C63(H63), C64(H64) 2.b Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C17(H17A,H17B,H17C), C33(H33A,H33B,H33C), C49(H49A,H49B,H49C) ; _olex2_submission_special_instructions 'No special instructions were received' 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 O1 O -0.4597(9) 0.0356(3) 0.3575(4) 0.0736(19) Uani 1 1 d . O2 O -0.3471(10) 0.1519(4) 0.3683(4) 0.080(2) Uani 1 1 d . N1 N -0.4434(9) 0.0745(4) 0.2789(4) 0.0598(18) Uani 1 1 d . C1 C -0.6008(17) 0.0522(7) 0.4073(9) 0.104(4) Uani 1 1 d . H1A H -0.6899 0.0580 0.3658 0.155 Uiso 1 1 calc GR H1B H -0.5815 0.0908 0.4402 0.155 Uiso 1 1 calc GR H1C H -0.6253 0.0188 0.4492 0.155 Uiso 1 1 calc GR C2 C -0.6012(15) -0.0389(5) 0.1078(8) 0.081(3) Uani 1 1 d . H2 H -0.6493 -0.0787 0.1041 0.097 Uiso 1 1 calc R C3 C -0.5704(14) -0.0065(5) 0.0291(7) 0.076(3) Uani 1 1 d . H3 H -0.5986 -0.0241 -0.0268 0.091 Uiso 1 1 calc R C4 C -0.4966(12) 0.0532(5) 0.0329(6) 0.067(2) Uani 1 1 d . H4 H -0.4766 0.0752 -0.0203 0.080 Uiso 1 1 calc R C5 C -0.4528(11) 0.0797(4) 0.1174(5) 0.0552(19) Uani 1 1 d . C6 C -0.4864(11) 0.0454(4) 0.1977(5) 0.055(2) Uani 1 1 d . C7 C -0.5623(12) -0.0140(5) 0.1930(7) 0.066(2) Uani 1 1 d . H7 H -0.5862 -0.0362 0.2456 0.080 Uiso 1 1 calc R C8 C -0.3826(11) 0.1402(4) 0.1246(6) 0.059(2) Uani 1 1 d . H8 H -0.3605 0.1623 0.0717 0.071 Uiso 1 1 calc R C9 C -0.3455(10) 0.1678(4) 0.2069(5) 0.0555(19) Uani 1 1 d . C10 C -0.3750(11) 0.1326(5) 0.2909(5) 0.060(2) Uani 1 1 d . C11 C -0.2800(11) 0.2323(5) 0.2114(6) 0.060(2) Uani 1 1 d . C12 C -0.3353(14) 0.2780(5) 0.1514(7) 0.073(3) Uani 1 1 d . H12 H -0.4189 0.2681 0.1111 0.088 Uiso 1 1 calc R C13 C -0.2686(15) 0.3387(6) 0.1500(8) 0.086(3) Uani 1 1 d . H13 H -0.3000 0.3674 0.1052 0.103 Uiso 1 1 calc R C14 C -0.1584(14) 0.3556(6) 0.2137(8) 0.080(3) Uani 1 1 d . H14 H -0.1189 0.3968 0.2152 0.096 Uiso 1 1 calc R C15 C -0.1044(12) 0.3121(6) 0.2763(6) 0.073(3) Uani 1 1 d . H15 H -0.0279 0.3239 0.3198 0.088 Uiso 1 1 calc R C16 C -0.1615(11) 0.2521(5) 0.2752(6) 0.066(2) Uani 1 1 d . H16 H -0.1217 0.2232 0.3176 0.080 Uiso 1 1 calc R O5 O -0.2652(8) 0.2886(3) -0.1411(4) 0.0655(16) Uani 1 1 d . O6 O -0.3667(9) 0.1706(3) -0.1275(4) 0.0710(18) Uani 1 1 d . N3 N -0.2818(8) 0.2501(3) -0.2182(4) 0.0543(16) Uani 1 1 d . C17 C -0.1098(14) 0.2741(6) -0.0952(7) 0.086(3) Uani 1 1 d . H17A H -0.0262 0.2723 -0.1394 0.129 Uiso 1 1 calc GR H17B H -0.1172 0.2340 -0.0648 0.129 Uiso 1 1 calc GR H17C H -0.0852 0.3067 -0.0516 0.129 Uiso 1 1 calc GR C18 C -0.1966(12) 0.3401(5) -0.3074(7) 0.069(2) Uani 1 1 d . H18 H -0.1766 0.3638 -0.2551 0.083 Uiso 1 1 calc R C19 C -0.1701(16) 0.3656(6) -0.3920(7) 0.085(3) Uani 1 1 d . H19 H -0.1341 0.4072 -0.3966 0.102 Uiso 1 1 calc R C20 C -0.1960(16) 0.3305(6) -0.4707(8) 0.088(3) Uani 1 1 d . H20 H -0.1782 0.3485 -0.5273 0.106 Uiso 1 1 calc R C21 C -0.2485(13) 0.2688(5) -0.4638(6) 0.069(2) Uani 1 1 d . H21 H -0.2653 0.2448 -0.5160 0.083 Uiso 1 1 calc R C22 C -0.2769(11) 0.2421(4) -0.3782(6) 0.058(2) Uani 1 1 d . C23 C -0.2531(10) 0.2789(4) -0.3016(5) 0.0523(18) Uani 1 1 d . C24 C -0.3362(11) 0.1790(4) -0.3686(5) 0.058(2) Uani 1 1 d . H24 H -0.3556 0.1552 -0.4208 0.069 Uiso 1 1 calc R C25 C -0.3653(10) 0.1524(4) -0.2873(5) 0.0545(19) Uani 1 1 d . C26 C -0.3427(10) 0.1897(4) -0.2039(5) 0.0529(19) Uani 1 1 d . C27 C -0.4215(11) 0.0863(4) -0.2794(5) 0.056(2) Uani 1 1 d . C28 C -0.5461(11) 0.0672(5) -0.2229(6) 0.062(2) Uani 1 1 d . H28 H -0.5973 0.0971 -0.1870 0.075 Uiso 1 1 calc R C29 C -0.5941(12) 0.0049(5) -0.2195(6) 0.069(2) Uani 1 1 d . H29 H -0.6770 -0.0072 -0.1814 0.082 Uiso 1 1 calc R C30 C -0.5203(14) -0.0389(6) -0.2720(7) 0.077(3) Uani 1 1 d . H30 H -0.5532 -0.0810 -0.2698 0.093 Uiso 1 1 calc R C31 C -0.3985(15) -0.0219(5) -0.3278(7) 0.081(3) Uani 1 1 d . H31 H -0.3495 -0.0523 -0.3639 0.097 Uiso 1 1 calc R C32 C -0.3483(12) 0.0396(5) -0.3310(7) 0.071(3) Uani 1 1 d . H32 H -0.2635 0.0505 -0.3685 0.085 Uiso 1 1 calc R O3 O 0.0514(9) 0.0265(4) -0.0973(4) 0.076(2) Uani 1 1 d . O4 O 0.1560(9) 0.1445(4) -0.1134(4) 0.0737(18) Uani 1 1 d . N2 N 0.0644(9) 0.0663(4) -0.0220(4) 0.0606(18) Uani 1 1 d . C33 C -0.0857(19) 0.0409(7) -0.1498(8) 0.107(5) Uani 1 1 d . H33A H -0.0867 0.0156 -0.2039 0.161 Uiso 1 1 calc GR H33B H -0.0839 0.0850 -0.1660 0.161 Uiso 1 1 calc GR H33C H -0.1804 0.0322 -0.1154 0.161 Uiso 1 1 calc GR C34 C -0.0371(13) -0.0221(5) 0.0648(7) 0.075(3) Uani 1 1 d . H34 H -0.0524 -0.0461 0.0125 0.090 Uiso 1 1 calc R C35 C -0.0755(15) -0.0465(6) 0.1513(8) 0.084(3) Uani 1 1 d . H35 H -0.1123 -0.0880 0.1558 0.101 Uiso 1 1 calc R C36 C -0.0600(15) -0.0108(6) 0.2284(8) 0.085(3) Uani 1 1 d . H36 H -0.0926 -0.0271 0.2838 0.102 Uiso 1 1 calc R C37 C 0.0050(13) 0.0505(5) 0.2240(6) 0.072(3) Uani 1 1 d . H37 H 0.0205 0.0741 0.2767 0.087 Uiso 1 1 calc R C38 C 0.0465(11) 0.0757(5) 0.1395(6) 0.062(2) Uani 1 1 d . C39 C 0.0244(11) 0.0392(4) 0.0606(6) 0.0564(19) Uani 1 1 d . C40 C 0.1110(11) 0.1389(4) 0.1295(6) 0.060(2) Uani 1 1 d . H40 H 0.1258 0.1637 0.1812 0.072 Uiso 1 1 calc R C41 C 0.1507(10) 0.1633(4) 0.0480(5) 0.055(2) Uani 1 1 d . C42 C 0.1258(11) 0.1258(5) -0.0349(5) 0.061(2) Uani 1 1 d . C43 C 0.2110(11) 0.2289(4) 0.0396(6) 0.059(2) Uani 1 1 d . C44 C 0.1501(13) 0.2754(5) 0.0964(7) 0.075(3) Uani 1 1 d . H44 H 0.0714 0.2653 0.1382 0.090 Uiso 1 1 calc R C45 C 0.2073(14) 0.3375(6) 0.0906(8) 0.086(3) Uani 1 1 d . H45 H 0.1656 0.3683 0.1289 0.103 Uiso 1 1 calc R C46 C 0.3228(14) 0.3542(6) 0.0303(8) 0.084(3) Uani 1 1 d . H46 H 0.3591 0.3957 0.0263 0.101 Uiso 1 1 calc R C47 C 0.3847(13) 0.3070(6) -0.0251(7) 0.078(3) Uani 1 1 d . H47 H 0.4648 0.3175 -0.0659 0.093 Uiso 1 1 calc R C48 C 0.3322(11) 0.2460(5) -0.0216(6) 0.064(2) Uani 1 1 d . H48 H 0.3763 0.2156 -0.0596 0.077 Uiso 1 1 calc R O7 O 0.1283(9) 0.1739(3) -0.6147(4) 0.0698(17) Uani 1 1 d . O8 O 0.2411(10) 0.2904(3) -0.6023(4) 0.075(2) Uani 1 1 d . N4 N 0.2244(9) 0.2531(4) -0.5246(4) 0.0592(18) Uani 1 1 d . C49 C 0.3804(15) 0.2752(7) -0.6507(7) 0.091(3) Uani 1 1 d . H49A H 0.3884 0.3027 -0.7025 0.136 Uiso 1 1 calc GR H49B H 0.3745 0.2320 -0.6707 0.136 Uiso 1 1 calc GR H49C H 0.4736 0.2807 -0.6120 0.136 Uiso 1 1 calc GR C50 C 0.3259(12) 0.3428(5) -0.4392(7) 0.070(2) Uani 1 1 d . H50 H 0.3427 0.3659 -0.4920 0.084 Uiso 1 1 calc R C51 C 0.3631(15) 0.3679(6) -0.3544(9) 0.088(3) Uani 1 1 d . H51 H 0.4048 0.4087 -0.3505 0.105 Uiso 1 1 calc R C52 C 0.3400(15) 0.3336(6) -0.2745(8) 0.085(3) Uani 1 1 d . H52 H 0.3679 0.3515 -0.2188 0.102 Uiso 1 1 calc R C53 C 0.2770(13) 0.2743(5) -0.2775(7) 0.074(3) Uani 1 1 d . H53 H 0.2592 0.2517 -0.2244 0.089 Uiso 1 1 calc R C54 C 0.2387(11) 0.2475(5) -0.3638(6) 0.061(2) Uani 1 1 d . C55 C 0.2631(11) 0.2825(4) -0.4424(6) 0.058(2) Uani 1 1 d . C56 C 0.1734(11) 0.1846(5) -0.3724(5) 0.060(2) Uani 1 1 d . H56 H 0.1563 0.1614 -0.3198 0.072 Uiso 1 1 calc R C57 C 0.1356(10) 0.1577(4) -0.4536(5) 0.0550(19) Uani 1 1 d . C58 C 0.1595(10) 0.1935(4) -0.5373(6) 0.0536(19) Uani 1 1 d . C59 C 0.0731(11) 0.0915(4) -0.4603(5) 0.056(2) Uani 1 1 d . C60 C 0.1402(13) 0.0448(5) -0.4050(6) 0.067(2) Uani 1 1 d . H60 H 0.2249 0.0553 -0.3657 0.081 Uiso 1 1 calc R C61 C 0.0840(14) -0.0164(5) -0.4072(7) 0.074(3) Uani 1 1 d . H61 H 0.1309 -0.0470 -0.3698 0.089 Uiso 1 1 calc R C62 C -0.0402(12) -0.0322(5) -0.4641(7) 0.070(2) Uani 1 1 d . H62 H -0.0782 -0.0736 -0.4652 0.084 Uiso 1 1 calc R C63 C -0.1100(12) 0.0122(5) -0.5199(6) 0.070(3) Uani 1 1 d . H63 H -0.1947 0.0010 -0.5587 0.083 Uiso 1 1 calc R C64 C -0.0527(11) 0.0747(5) -0.5179(5) 0.063(2) Uani 1 1 d . H64 H -0.0998 0.1050 -0.5557 0.076 Uiso 1 1 calc R 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 0.090(5) 0.077(5) 0.054(3) 0.020(3) 0.000(3) 0.022(3) O2 0.112(6) 0.088(5) 0.040(3) -0.001(3) 0.002(3) 0.015(4) N1 0.068(5) 0.068(5) 0.043(4) 0.009(3) 0.005(3) 0.012(4) C1 0.114(10) 0.102(10) 0.097(8) 0.023(7) 0.047(7) 0.011(7) C2 0.088(8) 0.065(6) 0.090(7) -0.005(5) -0.006(6) 0.012(5) C3 0.091(8) 0.069(6) 0.067(6) -0.007(5) -0.007(5) 0.018(5) C4 0.070(6) 0.078(7) 0.052(5) -0.012(4) 0.001(4) 0.008(5) C5 0.061(5) 0.057(5) 0.047(4) 0.002(4) 0.003(3) 0.013(4) C6 0.062(5) 0.055(5) 0.048(4) 0.005(4) 0.001(3) 0.018(4) C7 0.069(6) 0.064(6) 0.067(5) 0.007(4) 0.011(4) 0.014(4) C8 0.062(5) 0.064(6) 0.051(4) -0.001(4) 0.004(3) 0.014(4) C9 0.056(5) 0.059(5) 0.051(4) 0.002(4) -0.002(3) 0.012(4) C10 0.060(5) 0.071(6) 0.049(5) 0.001(4) 0.000(4) 0.014(4) C11 0.057(5) 0.072(6) 0.052(4) -0.005(4) -0.003(4) 0.014(4) C12 0.089(7) 0.058(6) 0.073(6) -0.002(5) -0.016(5) 0.004(5) C13 0.096(8) 0.068(7) 0.093(7) -0.006(6) -0.017(6) 0.018(6) C14 0.075(7) 0.076(7) 0.090(7) -0.018(6) 0.006(5) 0.008(5) C15 0.058(6) 0.104(8) 0.057(5) -0.020(5) -0.001(4) 0.001(5) C16 0.059(6) 0.086(7) 0.054(5) 0.000(4) -0.005(4) 0.011(4) O5 0.080(4) 0.064(4) 0.052(3) -0.014(3) -0.012(3) 0.007(3) O6 0.105(5) 0.067(4) 0.042(3) -0.003(3) 0.020(3) -0.003(3) N3 0.055(4) 0.056(4) 0.052(4) -0.009(3) 0.000(3) 0.004(3) C17 0.083(8) 0.105(9) 0.069(6) -0.023(6) -0.027(5) 0.011(6) C18 0.073(6) 0.064(6) 0.070(5) -0.011(5) 0.006(4) -0.005(4) C19 0.112(9) 0.070(7) 0.073(6) 0.002(5) 0.019(6) -0.024(6) C20 0.111(9) 0.082(8) 0.072(6) 0.005(5) 0.014(6) -0.024(6) C21 0.083(7) 0.075(6) 0.050(4) 0.001(4) 0.009(4) -0.016(5) C22 0.065(5) 0.059(5) 0.052(4) 0.002(4) 0.005(4) 0.002(4) C23 0.047(5) 0.056(5) 0.053(4) 0.000(4) 0.003(3) 0.005(3) C24 0.069(6) 0.063(5) 0.041(4) -0.003(4) 0.003(3) 0.001(4) C25 0.052(5) 0.061(5) 0.051(4) -0.003(4) 0.005(3) 0.003(3) C26 0.047(5) 0.063(5) 0.049(5) -0.002(4) 0.005(3) 0.005(3) C27 0.053(5) 0.071(6) 0.044(4) -0.005(4) 0.000(3) -0.004(4) C28 0.054(5) 0.082(7) 0.052(5) -0.004(4) 0.005(4) 0.006(4) C29 0.063(6) 0.086(7) 0.057(5) 0.008(5) 0.004(4) -0.013(5) C30 0.076(7) 0.075(7) 0.081(6) -0.005(5) 0.010(5) -0.012(5) C31 0.100(8) 0.065(6) 0.078(6) -0.021(5) 0.031(6) -0.010(5) C32 0.077(6) 0.062(6) 0.076(6) -0.009(5) 0.035(5) -0.008(5) O3 0.079(5) 0.088(5) 0.063(3) -0.030(3) -0.006(3) 0.022(3) O4 0.083(5) 0.085(5) 0.054(4) -0.004(3) 0.013(3) 0.009(3) N2 0.068(5) 0.068(5) 0.046(4) -0.010(3) 0.001(3) 0.014(4) C33 0.137(12) 0.103(10) 0.081(7) -0.001(7) -0.047(8) -0.007(8) C34 0.075(7) 0.076(7) 0.074(6) -0.008(5) -0.004(5) 0.001(5) C35 0.092(8) 0.069(7) 0.091(7) 0.004(6) 0.007(6) -0.002(5) C36 0.093(8) 0.093(8) 0.069(6) 0.028(6) 0.013(5) 0.022(6) C37 0.084(7) 0.078(7) 0.055(5) -0.006(5) 0.003(4) 0.005(5) C38 0.062(5) 0.076(6) 0.049(4) -0.005(4) 0.003(4) 0.008(4) C39 0.059(5) 0.054(5) 0.056(4) -0.003(4) 0.000(4) 0.009(4) C40 0.064(5) 0.064(6) 0.051(5) -0.008(4) 0.008(4) 0.009(4) C41 0.054(5) 0.062(5) 0.049(4) -0.003(4) 0.005(3) 0.013(4) C42 0.060(6) 0.076(6) 0.047(5) -0.006(4) 0.002(4) 0.018(4) C43 0.057(5) 0.070(6) 0.050(4) -0.003(4) 0.005(3) 0.004(4) C44 0.073(7) 0.081(7) 0.072(6) -0.007(5) 0.020(5) -0.004(5) C45 0.081(7) 0.069(7) 0.108(8) -0.004(6) 0.021(6) 0.002(5) C46 0.072(7) 0.087(8) 0.093(7) 0.018(6) -0.010(6) -0.011(5) C47 0.065(6) 0.102(9) 0.066(6) 0.023(6) 0.003(5) -0.005(5) C48 0.052(5) 0.090(7) 0.051(4) 0.000(4) 0.001(4) 0.008(4) O7 0.082(5) 0.075(4) 0.053(4) 0.002(3) -0.004(3) 0.001(3) O8 0.097(5) 0.072(5) 0.057(3) 0.015(3) -0.006(3) 0.006(4) N4 0.070(5) 0.064(5) 0.044(3) 0.011(3) -0.002(3) 0.011(3) C49 0.084(8) 0.114(10) 0.075(6) 0.019(7) 0.011(6) -0.003(6) C50 0.070(6) 0.066(6) 0.075(6) 0.004(5) -0.007(4) 0.002(4) C51 0.094(8) 0.069(7) 0.100(8) -0.008(6) -0.001(6) -0.003(5) C52 0.098(8) 0.088(8) 0.068(6) -0.027(6) -0.009(6) -0.001(6) C53 0.074(7) 0.082(7) 0.066(5) -0.017(5) 0.001(5) 0.005(5) C54 0.067(6) 0.064(6) 0.051(4) -0.001(4) -0.007(4) 0.011(4) C55 0.060(5) 0.050(5) 0.064(5) 0.003(4) 0.003(4) 0.010(4) C56 0.067(6) 0.068(6) 0.045(4) 0.007(4) 0.002(4) 0.008(4) C57 0.055(5) 0.063(5) 0.047(4) 0.009(3) -0.007(3) 0.007(4) C58 0.056(5) 0.055(5) 0.050(4) 0.002(3) -0.003(3) 0.011(3) C59 0.056(5) 0.077(6) 0.036(4) 0.001(4) 0.003(3) 0.005(4) C60 0.079(6) 0.060(6) 0.062(5) 0.005(4) -0.018(4) 0.004(4) C61 0.088(7) 0.062(6) 0.073(6) 0.005(5) -0.001(5) 0.003(5) C62 0.066(6) 0.071(6) 0.073(6) -0.011(5) 0.004(5) -0.004(5) C63 0.054(6) 0.096(8) 0.059(5) -0.027(5) 0.004(4) 0.002(5) C64 0.053(5) 0.091(7) 0.045(4) -0.006(4) 0.001(3) 0.010(4) 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 N1 O1 C1 111.3(7) C6 N1 O1 114.7(7) C10 N1 O1 117.2(7) C10 N1 C6 127.7(7) O1 C1 H1A 109.5 O1 C1 H1B 109.5 O1 C1 H1C 109.5 H1A C1 H1B 109.5 H1A C1 H1C 109.5 H1B C1 H1C 109.5 C3 C2 H2 119.1 C3 C2 C7 121.8(11) C7 C2 H2 119.1 C2 C3 H3 120.0 C2 C3 C4 120.1(10) C4 C3 H3 120.0 C3 C4 H4 120.0 C3 C4 C5 120.0(9) C5 C4 H4 120.0 C4 C5 C6 118.9(9) C8 C5 C4 121.9(8) C8 C5 C6 119.2(8) N1 C6 C5 116.2(8) N1 C6 C7 123.2(8) C7 C6 C5 120.6(8) C2 C7 C6 118.6(9) C2 C7 H7 120.7 C6 C7 H7 120.7 C5 C8 H8 118.7 C9 C8 C5 122.5(8) C9 C8 H8 118.7 C8 C9 C10 119.3(9) C8 C9 C11 120.7(8) C10 C9 C11 120.0(8) O2 C10 N1 119.4(8) O2 C10 C9 125.6(9) N1 C10 C9 115.0(7) C12 C11 C9 120.0(8) C12 C11 C16 116.1(9) C16 C11 C9 123.9(8) C11 C12 H12 119.2 C11 C12 C13 121.5(10) C13 C12 H12 119.2 C12 C13 H13 120.1 C14 C13 C12 119.8(11) C14 C13 H13 120.1 C13 C14 H14 119.9 C13 C14 C15 120.1(12) C15 C14 H14 119.9 C14 C15 H15 119.7 C16 C15 C14 120.6(10) C16 C15 H15 119.7 C11 C16 H16 119.2 C15 C16 C11 121.7(9) C15 C16 H16 119.2 N3 O5 C17 109.0(7) C23 N3 O5 116.5(7) C26 N3 O5 116.1(6) C26 N3 C23 126.9(7) O5 C17 H17A 109.5 O5 C17 H17B 109.5 O5 C17 H17C 109.5 H17A C17 H17B 109.5 H17A C17 H17C 109.5 H17B C17 H17C 109.5 C19 C18 H18 120.6 C23 C18 H18 120.6 C23 C18 C19 118.8(9) C18 C19 H19 119.3 C18 C19 C20 121.4(10) C20 C19 H19 119.3 C19 C20 H20 120.4 C21 C20 C19 119.2(10) C21 C20 H20 120.4 C20 C21 H21 119.9 C20 C21 C22 120.3(9) C22 C21 H21 119.9 C21 C22 C24 121.8(8) C23 C22 C21 118.9(8) C23 C22 C24 119.3(8) C18 C23 N3 121.7(8) C18 C23 C22 121.4(8) C22 C23 N3 116.8(8) C22 C24 H24 118.6 C25 C24 C22 122.9(8) C25 C24 H24 118.6 C24 C25 C26 119.9(8) C24 C25 C27 121.6(8) C26 C25 C27 118.5(7) O6 C26 N3 120.7(8) O6 C26 C25 125.2(8) N3 C26 C25 114.0(7) C28 C27 C25 123.8(8) C32 C27 C25 119.0(8) C32 C27 C28 117.1(9) C27 C28 H28 119.5 C29 C28 C27 121.0(9) C29 C28 H28 119.5 C28 C29 H29 120.1 C30 C29 C28 119.8(9) C30 C29 H29 120.1 C29 C30 H30 119.7 C29 C30 C31 120.7(11) C31 C30 H30 119.7 C30 C31 H31 119.9 C30 C31 C32 120.1(10) C32 C31 H31 119.9 C27 C32 H32 119.4 C31 C32 C27 121.3(9) C31 C32 H32 119.4 N2 O3 C33 111.1(8) C39 N2 O3 115.6(8) C42 N2 O3 117.9(7) C42 N2 C39 126.4(7) O3 C33 H33A 109.5 O3 C33 H33B 109.5 O3 C33 H33C 109.5 H33A C33 H33B 109.5 H33A C33 H33C 109.5 H33B C33 H33C 109.5 C35 C34 H34 121.1 C39 C34 H34 121.1 C39 C34 C35 117.8(10) C34 C35 H35 119.1 C36 C35 C34 121.8(11) C36 C35 H35 119.1 C35 C36 H36 120.0 C35 C36 C37 120.1(10) C37 C36 H36 120.0 C36 C37 H37 120.3 C38 C37 C36 119.4(10) C38 C37 H37 120.3 C37 C38 C39 119.7(9) C37 C38 C40 122.5(8) C39 C38 C40 117.8(8) N2 C39 C34 120.9(8) N2 C39 C38 118.0(8) C34 C39 C38 121.1(9) C38 C40 H40 118.7 C41 C40 C38 122.5(8) C41 C40 H40 118.7 C40 C41 C42 120.0(9) C40 C41 C43 121.3(8) C42 C41 C43 118.6(8) O4 C42 N2 119.9(8) O4 C42 C41 124.8(10) N2 C42 C41 115.3(7) C44 C43 C41 119.0(8) C44 C43 C48 118.3(9) C48 C43 C41 122.7(8) C43 C44 H44 120.1 C43 C44 C45 119.9(10) C45 C44 H44 120.1 C44 C45 H45 119.2 C46 C45 C44 121.7(11) C46 C45 H45 119.2 C45 C46 H46 121.0 C45 C46 C47 117.9(11) C47 C46 H46 121.0 C46 C47 H47 118.9 C48 C47 C46 122.2(10) C48 C47 H47 118.9 C43 C48 H48 120.0 C47 C48 C43 120.0(9) C47 C48 H48 120.0 N4 O8 C49 112.4(8) C55 N4 O8 115.9(7) C58 N4 O8 116.4(7) C58 N4 C55 127.4(7) O8 C49 H49A 109.5 O8 C49 H49B 109.5 O8 C49 H49C 109.5 H49A C49 H49B 109.5 H49A C49 H49C 109.5 H49B C49 H49C 109.5 C51 C50 H50 121.2 C55 C50 H50 121.2 C55 C50 C51 117.5(10) C50 C51 H51 119.0 C50 C51 C52 121.9(11) C52 C51 H51 119.0 C51 C52 H52 119.7 C53 C52 C51 120.6(10) C53 C52 H52 119.7 C52 C53 H53 120.8 C52 C53 C54 118.4(11) C54 C53 H53 120.8 C53 C54 C56 121.6(9) C55 C54 C53 119.9(10) C55 C54 C56 118.5(8) C50 C55 N4 121.5(8) C50 C55 C54 121.6(9) C54 C55 N4 116.9(8) C54 C56 H56 118.4 C57 C56 C54 123.1(8) C57 C56 H56 118.4 C56 C57 C58 119.6(8) C56 C57 C59 121.8(7) C58 C57 C59 118.6(7) O7 C58 N4 120.5(8) O7 C58 C57 125.1(9) N4 C58 C57 114.5(7) C60 C59 C57 119.2(8) C64 C59 C57 122.7(8) C64 C59 C60 118.0(9) C59 C60 H60 119.3 C61 C60 C59 121.4(9) C61 C60 H60 119.3 C60 C61 H61 120.1 C62 C61 C60 119.9(10) C62 C61 H61 120.1 C61 C62 H62 119.6 C61 C62 C63 120.8(10) C63 C62 H62 119.6 C62 C63 H63 120.3 C62 C63 C64 119.5(9) C64 C63 H63 120.3 C59 C64 C63 120.5(9) C59 C64 H64 119.8 C63 C64 H64 119.8 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance O1 N1 1.427(9) O1 C1 1.435(14) O2 C10 1.229(11) N1 C6 1.386(11) N1 C10 1.361(13) C1 H1A 0.9600 C1 H1B 0.9600 C1 H1C 0.9600 C2 H2 0.9300 C2 C3 1.374(15) C2 C7 1.394(15) C3 H3 0.9300 C3 C4 1.401(16) C4 H4 0.9300 C4 C5 1.407(12) C5 C6 1.417(12) C5 C8 1.407(13) C6 C7 1.404(14) C7 H7 0.9300 C8 H8 0.9300 C8 C9 1.376(12) C9 C10 1.467(12) C9 C11 1.467(14) C11 C12 1.381(13) C11 C16 1.413(13) C12 H12 0.9300 C12 C13 1.396(17) C13 H13 0.9300 C13 C14 1.348(15) C14 H14 0.9300 C14 C15 1.371(16) C15 H15 0.9300 C15 C16 1.351(15) C16 H16 0.9300 O5 N3 1.400(9) O5 C17 1.478(12) O6 C26 1.214(10) N3 C23 1.393(11) N3 C26 1.390(11) C17 H17A 0.9600 C17 H17B 0.9600 C17 H17C 0.9600 C18 H18 0.9300 C18 C19 1.379(14) C18 C23 1.378(13) C19 H19 0.9300 C19 C20 1.388(16) C20 H20 0.9300 C20 C21 1.377(15) C21 H21 0.9300 C21 C22 1.404(12) C22 C23 1.381(12) C22 C24 1.428(13) C24 H24 0.9300 C24 C25 1.348(11) C25 C26 1.468(11) C25 C27 1.477(12) C27 C28 1.397(13) C27 C32 1.389(13) C28 H28 0.9300 C28 C29 1.375(15) C29 H29 0.9300 C29 C30 1.359(16) C30 H30 0.9300 C30 C31 1.361(15) C31 H31 0.9300 C31 C32 1.365(14) C32 H32 0.9300 O3 N2 1.394(9) O3 C33 1.398(14) O4 C42 1.251(11) N2 C39 1.390(11) N2 C42 1.369(13) C33 H33A 0.9600 C33 H33B 0.9600 C33 H33C 0.9600 C34 H34 0.9300 C34 C35 1.416(16) C34 C39 1.392(14) C35 H35 0.9300 C35 C36 1.367(16) C36 H36 0.9300 C36 C37 1.403(17) C37 H37 0.9300 C37 C38 1.402(13) C38 C39 1.403(12) C38 C40 1.445(14) C40 H40 0.9300 C40 C41 1.352(12) C41 C42 1.468(12) C41 C43 1.478(13) C43 C44 1.391(13) C43 C48 1.408(13) C44 H44 0.9300 C44 C45 1.397(16) C45 H45 0.9300 C45 C46 1.363(16) C46 H46 0.9300 C46 C47 1.391(17) C47 H47 0.9300 C47 C48 1.361(15) C48 H48 0.9300 O7 C58 1.235(10) O8 N4 1.397(9) O8 C49 1.405(14) N4 C55 1.393(12) N4 C58 1.381(12) C49 H49A 0.9600 C49 H49B 0.9600 C49 H49C 0.9600 C50 H50 0.9300 C50 C51 1.387(15) C50 C55 1.376(14) C51 H51 0.9300 C51 C52 1.397(16) C52 H52 0.9300 C52 C53 1.357(16) C53 H53 0.9300 C53 C54 1.423(13) C54 C55 1.391(13) C54 C56 1.438(14) C56 H56 0.9300 C56 C57 1.355(12) C57 C58 1.463(11) C57 C59 1.493(13) C59 C60 1.389(12) C59 C64 1.381(12) C60 H60 0.9300 C60 C61 1.375(14) C61 H61 0.9300 C61 C62 1.360(15) C62 H62 0.9300 C62 C63 1.368(15) C63 H63 0.9300 C63 C64 1.402(15) C64 H64 0.9300 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 O1 N1 C6 C5 -172.3(7) O1 N1 C6 C7 9.0(12) O1 N1 C10 O2 -8.0(12) O1 N1 C10 C9 173.8(7) N1 C6 C7 C2 179.7(9) C1 O1 N1 C6 -103.3(10) C1 O1 N1 C10 82.4(11) C2 C3 C4 C5 0.5(15) C3 C2 C7 C6 -1.4(16) C3 C4 C5 C6 -0.8(14) C3 C4 C5 C8 -178.1(9) C4 C5 C6 N1 -178.8(8) C4 C5 C6 C7 0.0(13) C4 C5 C8 C9 177.1(8) C5 C6 C7 C2 1.1(13) C5 C8 C9 C10 1.9(13) C5 C8 C9 C11 -176.9(8) C6 N1 C10 O2 178.6(8) C6 N1 C10 C9 0.4(13) C6 C5 C8 C9 -0.2(12) C7 C2 C3 C4 0.6(17) C8 C5 C6 N1 -1.3(12) C8 C5 C6 C7 177.4(8) C8 C9 C10 O2 180.0(9) C8 C9 C10 N1 -1.9(12) C8 C9 C11 C12 37.5(13) C8 C9 C11 C16 -143.1(9) C9 C11 C12 C13 -175.9(10) C9 C11 C16 C15 179.7(9) C10 N1 C6 C5 1.2(13) C10 N1 C6 C7 -177.4(8) C10 C9 C11 C12 -141.3(9) C10 C9 C11 C16 38.2(12) C11 C9 C10 O2 -1.3(14) C11 C9 C10 N1 176.8(8) C11 C12 C13 C14 -6.4(18) C12 C11 C16 C15 -0.9(13) C12 C13 C14 C15 4.1(18) C13 C14 C15 C16 -0.4(16) C14 C15 C16 C11 -1.2(15) C16 C11 C12 C13 4.6(15) O5 N3 C23 C18 6.0(12) O5 N3 C23 C22 -176.9(7) O5 N3 C26 O6 -5.7(11) O5 N3 C26 C25 177.1(7) C17 O5 N3 C23 -102.8(9) C17 O5 N3 C26 84.3(9) C18 C19 C20 C21 0(2) C19 C18 C23 N3 179.7(9) C19 C18 C23 C22 2.8(15) C19 C20 C21 C22 0.6(19) C20 C21 C22 C23 0.8(16) C20 C21 C22 C24 178.0(10) C21 C22 C23 N3 -179.6(8) C21 C22 C23 C18 -2.5(14) C21 C22 C24 C25 -179.6(9) C22 C24 C25 C26 2.7(13) C22 C24 C25 C27 -177.9(8) C23 N3 C26 O6 -177.9(8) C23 N3 C26 C25 5.0(12) C23 C18 C19 C20 -1.3(18) C23 C22 C24 C25 -2.4(13) C24 C22 C23 N3 3.1(12) C24 C22 C23 C18 -179.8(9) C24 C25 C26 O6 179.3(8) C24 C25 C26 N3 -3.7(11) C24 C25 C27 C28 -135.2(9) C24 C25 C27 C32 44.4(13) C25 C27 C28 C29 179.2(8) C25 C27 C32 C31 -178.4(10) C26 N3 C23 C18 178.1(8) C26 N3 C23 C22 -4.8(12) C26 C25 C27 C28 44.1(12) C26 C25 C27 C32 -136.2(9) C27 C25 C26 O6 -0.1(13) C27 C25 C26 N3 176.9(7) C27 C28 C29 C30 -0.2(15) C28 C27 C32 C31 1.3(16) C28 C29 C30 C31 0.2(17) C29 C30 C31 C32 1(2) C30 C31 C32 C27 -1.3(19) C32 C27 C28 C29 -0.5(14) O3 N2 C39 C34 -5.1(12) O3 N2 C39 C38 175.4(7) O3 N2 C42 O4 5.7(12) O3 N2 C42 C41 -174.5(7) C33 O3 N2 C39 104.8(11) C33 O3 N2 C42 -80.0(11) C34 C35 C36 C37 -4.1(19) C35 C34 C39 N2 -179.9(9) C35 C34 C39 C38 -0.4(15) C35 C36 C37 C38 3.1(17) C36 C37 C38 C39 -0.8(15) C36 C37 C38 C40 178.8(9) C37 C38 C39 N2 178.9(8) C37 C38 C39 C34 -0.5(14) C37 C38 C40 C41 -179.9(9) C38 C40 C41 C42 1.2(13) C38 C40 C41 C43 177.8(8) C39 N2 C42 O4 -179.7(8) C39 N2 C42 C41 0.2(12) C39 C34 C35 C36 2.8(17) C39 C38 C40 C41 -0.3(13) C40 C38 C39 N2 -0.6(12) C40 C38 C39 C34 179.9(9) C40 C41 C42 O4 178.7(8) C40 C41 C42 N2 -1.1(12) C40 C41 C43 C44 -35.0(13) C40 C41 C43 C48 142.7(9) C41 C43 C44 C45 179.0(10) C41 C43 C48 C47 -178.8(8) C42 N2 C39 C34 -179.9(9) C42 N2 C39 C38 0.7(13) C42 C41 C43 C44 141.6(9) C42 C41 C43 C48 -40.7(12) C43 C41 C42 O4 2.0(13) C43 C41 C42 N2 -177.8(7) C43 C44 C45 C46 -0.1(19) C44 C43 C48 C47 -1.1(14) C44 C45 C46 C47 -0.9(18) C45 C46 C47 C48 1.0(16) C46 C47 C48 C43 0.1(15) C48 C43 C44 C45 1.2(15) O8 N4 C55 C50 -4.9(13) O8 N4 C55 C54 176.5(7) O8 N4 C58 O7 4.4(12) O8 N4 C58 C57 -176.6(7) C49 O8 N4 C55 103.6(10) C49 O8 N4 C58 -81.5(10) C50 C51 C52 C53 -1.1(19) C51 C50 C55 N4 -179.0(9) C51 C50 C55 C54 -0.5(15) C51 C52 C53 C54 1.4(17) C52 C53 C54 C55 -1.3(15) C52 C53 C54 C56 179.3(10) C53 C54 C55 N4 179.5(8) C53 C54 C55 C50 0.9(14) C53 C54 C56 C57 180.0(9) C54 C56 C57 C58 -0.7(14) C54 C56 C57 C59 177.9(8) C55 N4 C58 O7 178.7(8) C55 N4 C58 C57 -2.3(13) C55 C50 C51 C52 0.6(17) C55 C54 C56 C57 0.5(14) C56 C54 C55 N4 -1.1(13) C56 C54 C55 C50 -179.7(9) C56 C57 C58 O7 -179.5(9) C56 C57 C58 N4 1.5(12) C56 C57 C59 C60 -40.7(13) C56 C57 C59 C64 137.4(9) C57 C59 C60 C61 178.4(9) C57 C59 C64 C63 -178.2(8) C58 N4 C55 C50 -179.2(8) C58 N4 C55 C54 2.2(14) C58 C57 C59 C60 137.9(9) C58 C57 C59 C64 -43.9(12) C59 C57 C58 O7 1.8(13) C59 C57 C58 N4 -177.2(7) C59 C60 C61 C62 -0.3(16) C60 C59 C64 C63 0.0(12) C60 C61 C62 C63 0.3(16) C61 C62 C63 C64 -0.2(15) C62 C63 C64 C59 0.0(13) C64 C59 C60 C61 0.1(14) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code -1 0 0 0.35744 0.29282 8 -2 0 0 66.7044 6.89558 8 2 0 0 77.6002 6.00304 3 3 0 0 14.4069 1.39529 3 4 0 0 350.13 25.8602 7 4 0 0 347.3 31.2553 5 4 0 0 291.176 26.5935 3 5 0 0 6.94998 1.39632 7 5 0 0 7.07478 1.67904 5 6 0 0 0.88599 1.13632 7 7 0 0 2.30714 2.21345 7 0 -1 0 -0.2653 0.33433 8 0 1 0 -0.1522 0.32847 8 1 -1 0 -4.8547 0.90613 8 -1 -1 0 -6.6664 0.85284 8 -1 1 0 -4.9997 0.89783 8 -2 -1 0 2021.63 179.526 8 2 -1 0 2154.37 159.417 3 2 -1 0 1898.84 179.512 8 2 1 0 1851.46 159.371 3 3 -1 0 11.0415 1.1891 3 3 1 0 11.4209 1.12824 3 4 -1 0 105.858 8.78694 7 4 -1 0 98.0422 8.98419 3 4 1 0 112.95 10.7124 5 4 1 0 128.132 8.85326 7 4 1 0 103.24 8.96252 3 5 -1 0 8.31289 1.4228 7 5 -1 0 5.49662 1.16541 3 5 1 0 7.53364 1.46552 7 5 1 0 6.20022 1.6609 5 6 -1 0 10.8719 1.81378 7 6 1 0 13.3607 1.95449 7 7 -1 0 1.35767 1.70383 7 0 -2 0 1541.49 152.544 8 0 2 0 1817.79 152.559 8 1 -2 0 4.70341 0.72118 8 -1 -2 0 2.49209 0.58726 8 1 -2 0 5.10892 0.55766 3 -1 2 0 4.24886 0.69135 8 2 -2 0 8934.64 708.65 3 -2 -2 0 8740.7 797.369 8 2 -2 0 9999.99 797.476 8 2 2 0 7576.54 708.434 3 3 -2 0 6.65161 0.81434 3 -3 -2 0 4.60002 0.91267 8 3 2 0 2.77558 0.56293 3 4 -2 0 269.547 18.6274 7 4 -2 0 251.757 19.178 3 4 2 0 198.994 22.4124 5 4 2 0 219.298 18.5884 7 5 -2 0 7.82761 1.32703 7 5 -2 0 6.92746 1.28265 3 5 2 0 6.35764 1.71105 5 5 2 0 5.6874 1.31933 7 6 -2 0 21.755 2.39494 10 6 -2 0 25.1136 2.68049 7 6 -2 0 20.2428 2.58339 11 6 2 0 17.2815 3.13032 5 7 -2 0 2.32481 0.77074 10 7 -2 0 2.01138 1.61946 7 0 -3 0 0.16173 0.491 8 0 3 0 -0.324 0.43648 8 1 -3 0 2.3392 0.43531 3 -1 -3 0 2.96326 0.59121 8 1 -3 0 1.68944 0.59721 8 -1 3 0 2.49231 0.6093 8 2 -3 0 5950.27 545.733 8 -2 -3 0 5695.16 545.633 8 2 -3 0 6440.43 484.807 3 3 -3 0 25.9681 2.1442 3 3 -3 0 21.5592 2.57029 8 -3 -3 0 19.0944 2.407 8 4 -3 0 519.724 38.4298 7 4 -3 0 517.959 39.6919 3 4 3 0 431.07 46.2914 5 5 -3 0 3.03673 1.02886 7 5 -3 0 3.97286 1.09475 3 5 3 0 3.6758 1.44999 5 6 -3 0 76.936 6.20489 7 6 -3 0 70.6778 7.06646 10 6 -3 0 66.6656 6.28553 3 6 3 0 68.8685 7.59609 5 7 -3 0 1.23468 1.62811 11 7 -3 0 2.15471 1.60569 7 7 -3 0 0.46621 0.6147 10 8 -3 0 5.75862 1.00422 10 0 -4 0 3476.69 329.063 8 0 4 0 3792.02 329.06 8 1 -4 0 4.92152 1.00505 8 1 -4 0 4.88194 0.7067 3 -1 -4 0 6.03661 0.95882 8 1 4 0 5.23738 0.98565 8 2 -4 0 76.0205 5.88965 3 -2 -4 0 65.0975 6.66138 8 2 -4 0 69.746 6.80402 8 3 -4 0 20.8191 2.02914 3 3 -4 0 16.5617 2.46163 8 -3 -4 0 24.2252 2.38487 8 4 -4 0 900.103 65.2292 3 4 -4 0 776.907 63.0667 7 4 4 0 743.948 75.9962 5 5 -4 0 13.6811 1.90293 3 5 -4 0 14.3536 1.78424 7 5 4 0 13.1367 2.36603 5 6 -4 0 83.1546 7.50626 3 6 -4 0 96.0796 7.28198 7 6 -4 0 89.4255 8.49571 10 6 -4 0 70.5267 8.89337 6 6 4 0 96.5338 8.99189 5 7 -4 0 4.06694 1.69452 7 7 -4 0 3.24448 1.54002 11 7 -4 0 2.20739 0.78831 10 7 -4 0 1.23486 0.85273 6 8 -4 0 0.74844 0.72547 10 0 -5 0 -0.6366 0.89932 8 1 -5 0 1.77858 0.43216 3 1 -5 0 1.36852 0.72284 8 -1 -5 0 1.71753 0.70153 8 -2 -5 0 43.7577 3.99345 8 2 -5 0 36.3299 3.43424 3 2 -5 0 40.1413 4.12689 8 3 -5 0 8.36598 1.17976 3 3 -5 0 6.99879 1.56062 8 4 -5 0 109.014 12.1187 8 4 -5 0 141.946 10.1162 7 4 5 0 120.583 12.3122 5 5 -5 0 14.85 1.87878 7 5 -5 0 14.6063 2.02325 3 5 5 0 13.8074 2.54084 5 6 -5 0 190.374 14.5602 7 6 -5 0 182.542 17.66 10 6 -5 0 179.094 15.1134 3 6 -5 0 170.177 18.4418 6 6 5 0 179.277 17.7054 5 7 -5 0 -0.2714 1.41566 11 7 -5 0 0.03533 0.65812 10 7 -5 0 0.12682 0.83229 6 7 5 0 -0.1678 2.31827 5 7 5 0 0.69941 1.03933 4 8 -5 0 3.51069 0.97417 10 9 -5 0 1.55577 0.68528 10 0 -6 0 612.17 47.5666 3 0 -6 0 566.434 53.8402 8 -1 -6 0 2.82913 0.93133 8 1 -6 0 2.22131 0.50914 3 1 -6 0 1.6004 0.88094 8 2 -6 0 77.5225 7.70688 8 2 -6 0 75.6524 6.57222 3 -2 -6 0 83.0916 7.5399 8 3 -6 0 20.875 1.95571 3 3 -6 0 17.3126 2.43366 8 3 -6 0 17.1638 1.77425 7 3 6 0 17.1312 2.49146 5 4 -6 0 502.745 41.1753 3 4 -6 0 477.173 39.7699 7 4 6 0 544.778 48.1246 5 5 -6 0 10.2673 1.63053 7 5 -6 0 12.1752 2.0068 3 5 6 0 13.3411 2.41336 5 6 -6 0 131.51 10.2589 3 6 -6 0 118.414 11.5113 10 6 -6 0 127.806 9.67308 7 6 -6 0 116.063 12.0232 6 6 6 0 120.167 11.9877 5 6 6 0 96.8682 10.7384 1 7 -6 0 3.20312 1.82313 11 7 -6 0 3.45229 0.87644 10 7 -6 0 5.82949 1.12498 6 7 6 0 3.29926 2.65986 5 7 6 0 2.15628 1.24947 4 8 -6 0 15.9884 1.91318 10 8 -6 0 13.2761 1.94671 6 9 -6 0 1.40677 0.68281 10 0 -7 0 0.13812 0.27472 3 0 -7 0 0.88554 0.79279 8 -1 -7 0 0.54702 0.69321 8 1 -7 0 -0.6316 0.64519 8 1 -7 0 0.4265 0.34075 3 2 -7 0 560.07 50.3212 8 2 -7 0 554.267 44.3641 3 -2 -7 0 531.955 50.0684 8 3 -7 0 1.70874 1.15619 8 3 -7 0 1.52217 0.65879 7 3 -7 0 1.6924 0.76284 3 3 -7 0 2.04035 1.10906 12 3 7 0 2.51794 1.18622 5 4 -7 0 125.842 11.1213 3 4 -7 0 125.278 10.6706 7 4 7 0 150.569 13.1824 5 5 -7 0 14.7173 1.84505 7 5 -7 0 13.3904 2.17376 3 5 7 0 9.99736 2.37424 5 6 -7 0 42.3682 4.37995 6 6 -7 0 40.6016 4.21679 10 6 7 0 36.9948 3.87638 1 6 7 0 43.4985 5.35153 5 7 -7 0 1.21969 0.85213 6 7 -7 0 0.70846 0.72394 10 7 -7 0 1.36059 1.62069 11 7 7 0 0.46279 0.97312 4 7 7 0 2.06842 2.69769 5 7 7 0 2.93598 0.84383 1 8 -7 0 47.3187 5.19865 6 8 -7 0 53.6624 5.01952 10 8 7 0 44.6904 6.27066 4 9 -7 0 0.36989 0.73114 10 0 -8 0 339.44 30.53 8 0 -8 0 322.827 26.721 3 -1 -8 0 2.21093 0.94011 8 1 -8 0 3.32562 1.13833 8 1 -8 0 3.85484 0.66442 3 2 -8 0 399.384 38.1972 8 -2 -8 0 402.81 37.9529 8 2 -8 0 419.112 33.5486 3 2 8 0 431.767 39.2143 5 3 -8 0 3.34091 1.16992 12 3 -8 0 2.51845 0.85783 3 3 -8 0 3.30958 0.78764 7 3 8 0 4.01088 1.33297 5 4 -8 0 31.385 3.00226 7 4 -8 0 37.772 3.33916 3 4 8 0 29.964 4.04071 5 5 -8 0 18.003 2.11955 7 5 -8 0 16.6489 1.93087 10 5 -8 0 12.4016 2.31323 3 5 8 0 19.1058 3.12215 5 6 -8 0 18.9397 2.1741 10 6 -8 0 18.4234 2.30591 6 6 8 0 20.2527 2.83672 4 6 8 0 17.6418 1.98976 1 6 8 0 13.5221 3.22491 5 7 -8 0 3.96104 1.82504 11 7 -8 0 4.86706 1.04452 10 7 -8 0 5.421 1.14259 6 7 8 0 5.6878 2.86777 5 7 8 0 6.77006 1.04986 1 7 8 0 5.84078 1.48029 4 8 -8 0 34.0111 3.47385 6 8 -8 0 33.3539 3.35169 10 8 8 0 25.4948 4.15429 4 0 -9 0 1.76896 1.03732 8 1 -9 0 8.06667 1.78042 8 -1 -9 0 6.44867 1.55818 8 1 -9 0 10.3419 1.0857 3 2 -9 0 525.499 40.2741 3 -2 -9 0 444.215 45.5202 8 2 9 0 519.308 47.0603 5 3 -9 0 7.59092 1.72436 12 3 -9 0 11.775 1.46389 3 3 9 0 4.0865 1.58491 5 4 9 0 31.1819 3.05936 13 4 9 0 32.3188 4.06506 5 5 -9 0 2.48899 0.67315 10 5 -9 0 0.83558 1.31852 3 5 -9 0 1.28581 0.69442 6 5 9 0 1.47763 1.84328 5 6 -9 0 3.88784 0.82875 10 6 -9 0 3.87663 0.95097 6 6 -9 0 4.4828 1.65009 11 6 9 0 3.38476 1.2024 4 6 9 0 3.89192 0.80353 1 6 9 0 3.01277 2.42733 5 6 9 0 3.35149 1.08467 9 7 -9 0 2.59062 0.79439 10 7 -9 0 3.07295 1.75337 11 7 -9 0 3.9159 0.97426 6 7 9 0 0.90673 1.10691 4 7 9 0 2.54449 0.7657 1 7 9 0 3.3748 2.89571 5 8 -9 0 19.7865 2.31876 6 8 -9 0 22.5747 2.29567 10 8 9 0 17.6158 2.05836 1 8 9 0 17.6375 2.79627 4 0 -10 0 2706.62 245.624 8 -1 -10 0 12.888 2.31888 8 1 -10 0 17.9347 1.60234 3 1 10 0 10.9876 2.02291 5 2 -10 0 55.7389 5.11487 3 2 10 0 63.8576 6.19859 5 3 -10 0 5.23367 1.13644 3 3 -10 0 4.45115 1.50067 12 3 10 0 6.04049 1.68768 5 4 -10 0 1.69779 1.23601 3 4 10 0 1.0619 1.60211 5 4 10 0 2.46431 0.82197 13 5 -10 0 0.93332 1.56818 3 5 -10 0 1.57841 0.59433 10 5 -10 0 0.10679 0.61503 6 5 10 0 1.42278 1.99954 5 5 10 0 1.12922 0.60367 1 5 10 0 0.85872 0.85858 13 6 -10 0 26.3337 3.46111 6 6 -10 0 30.2693 3.29793 10 6 -10 0 33.7715 3.72464 11 6 10 0 33.9136 3.09059 1 6 10 0 35.5891 4.76643 5 6 10 0 32.4691 4.19472 4 6 10 0 30.1571 3.387 9 7 -10 0 3.00589 0.92098 6 7 -10 0 2.33027 1.85618 11 7 -10 0 3.17262 0.85613 10 7 10 0 3.4212 1.23586 4 7 10 0 3.7757 2.9224 5 7 10 0 3.04597 0.80861 1 8 -10 0 4.05894 0.87111 10 8 -10 0 3.26618 0.80425 6 8 10 0 4.10395 0.77746 1 8 10 0 3.30849 1.10692 4 0 11 0 1.34371 0.95551 5 -1 11 0 4.82791 1.29336 5 1 11 0 3.98725 1.20916 5 2 -11 0 50.462 4.05674 3 2 11 0 38.0657 4.8832 5 3 -11 0 1.52934 0.89507 3 3 -11 0 2.56147 1.37932 12 3 11 0 1.69248 0.73076 13 3 11 0 0.78524 1.35914 5 4 -11 0 1.27123 1.17294 3 4 11 0 2.92555 1.80043 5 4 11 0 2.43469 0.82762 13 5 -11 0 1.95059 0.79075 6 5 -11 0 1.94582 0.64969 10 5 11 0 1.76352 0.67408 1 5 11 0 1.87866 0.82337 9 5 11 0 2.99177 1.26228 4 5 11 0 2.15109 2.13463 5 5 11 0 2.08475 0.9657 13 6 -11 0 6.85806 1.95096 11 6 -11 0 6.35194 1.13006 6 6 -11 0 7.38615 1.05037 10 6 11 0 3.69828 2.94978 5 6 11 0 3.65463 1.11856 9 6 11 0 4.75472 1.41772 4 6 11 0 5.03952 0.92217 1 7 -11 0 0.36681 0.66465 10 7 -11 0 0.83623 0.77847 6 7 11 0 1.04423 0.68494 1 7 11 0 -0.1842 1.09781 4 8 -11 0 3.90629 0.80606 10 8 11 0 3.45968 0.74293 1 8 11 0 4.73411 1.11538 4 0 12 0 84.4037 8.47064 5 1 12 0 7.35687 1.57931 5 2 12 0 240.648 20.199 13 2 12 0 221.505 22.3824 5 3 -12 0 0.22759 1.36543 12 3 -12 0 0.91087 0.91838 3 3 12 0 0.50203 1.4653 5 3 12 0 0.19514 0.72737 13 4 -12 0 5.57116 0.96422 6 4 -12 0 4.86979 1.45947 3 4 -12 0 4.27109 0.85917 10 4 12 0 4.55488 1.98689 5 4 12 0 4.46957 0.97718 13 5 -12 0 1.24307 0.6904 10 5 -12 0 2.50599 0.77919 6 5 12 0 0.70073 2.36097 5 5 12 0 2.83997 0.73127 1 5 12 0 3.7054 0.97636 9 5 12 0 2.95266 1.16662 4 5 12 0 2.33479 0.96284 13 6 -12 0 3.02347 0.82696 10 6 -12 0 2.20203 0.86411 6 6 -12 0 2.80784 1.73846 11 6 12 0 3.46744 1.23184 4 6 12 0 4.64477 2.98199 5 6 12 0 5.02794 0.84701 1 6 12 0 4.89267 1.098 9 7 -12 0 0.61039 0.72538 6 7 -12 0 -0.5405 0.59597 10 7 12 0 -0.388 0.98037 4 7 12 0 0.15669 0.81415 9 7 12 0 0.46239 0.61197 1 8 -12 0 3.61105 0.74535 10 8 -12 0 4.20579 0.77569 6 8 12 0 3.90374 0.69974 1 8 12 0 3.88309 1.00785 4 0 13 0 -0.2054 0.97821 5 1 13 0 8.74256 1.79503 5 1 13 0 10.1474 1.22291 13 2 -13 0 23.6934 3.59437 12 2 13 0 26.3822 3.36021 5 2 13 0 25.8345 2.49471 13 3 -13 0 1.85949 1.09026 3 3 -13 0 0.30776 1.59198 12 3 13 0 1.64422 1.55612 5 3 13 0 0.95525 0.72995 13 4 -13 0 0.23899 0.64569 6 4 13 0 1.10399 0.76441 13 4 13 0 0.24519 0.60045 1 4 13 0 1.8511 1.89299 5 4 13 0 0.57336 0.66533 9 5 -13 0 1.09218 0.62839 10 5 -13 0 0.48387 1.49567 11 5 -13 0 0.63447 0.70739 6 5 13 0 1.89693 1.01669 4 5 13 0 1.94324 0.73971 1 5 13 0 1.65128 0.8034 9 5 13 0 1.51016 0.91878 13 5 13 0 0.85766 2.46128 5 6 -13 0 3.6039 1.85217 11 6 -13 0 4.08574 0.95633 6 6 -13 0 3.21802 0.88758 10 6 13 0 6.78671 0.97609 1 6 13 0 5.61704 1.30315 4 6 13 0 3.56008 3.00623 5 6 13 0 5.83001 1.07988 9 7 -13 0 0.09525 0.671 6 7 -13 0 -0.0601 0.57728 10 7 13 0 -0.9611 0.8698 4 7 13 0 -0.3299 0.72178 9 7 13 0 -0.1016 0.59141 1 8 -13 0 0.42783 0.53273 6 8 13 0 -0.1946 0.72595 4 8 13 0 0.43346 0.46731 1 0 14 0 48.312 5.53636 5 0 14 0 52.7926 4.65756 13 1 14 0 3.76398 0.77924 13 1 14 0 2.76861 1.39271 5 2 -14 0 2.42394 1.5615 12 2 14 0 1.12151 0.6929 13 2 14 0 2.68363 1.56294 5 3 -14 0 2.11932 2.0492 12 3 14 0 1.80958 1.73626 5 3 14 0 4.34608 0.90505 13 4 -14 0 5.33683 0.96964 6 4 14 0 4.30629 0.98663 13 4 14 0 3.79283 1.0826 2 4 14 0 4.44551 0.86251 1 4 14 0 3.9917 0.94663 9 4 14 0 2.27679 2.07611 5 4 14 0 6.54571 1.39831 4 5 -14 0 1.52823 1.77317 11 5 -14 0 -0.0194 0.65056 6 5 -14 0 -0.0498 0.58689 10 5 14 0 -1.9212 2.14974 5 5 14 0 0.50357 0.6346 1 5 14 0 0.50261 0.90402 13 5 14 0 0.65303 0.96794 4 5 14 0 0.50832 0.78981 9 5 14 0 0.58022 1.07166 2 6 -14 0 3.83183 0.86832 10 6 -14 0 5.76958 1.06069 6 6 14 0 5.81911 1.09131 9 6 14 0 4.11747 0.89947 1 6 14 0 3.84741 1.1982 4 7 -14 0 1.22467 0.58612 10 7 -14 0 1.04077 0.65403 6 7 14 0 0.58844 0.65255 9 7 14 0 -0.0224 0.92291 4 7 14 0 1.05789 0.62697 1 0 15 0 -0.7849 1.37495 5 0 15 0 -0.0115 0.61189 13 1 15 0 3.33489 0.79686 13 1 15 0 3.87131 1.54968 5 2 -15 0 1.41343 1.634 12 2 15 0 4.87862 1.71487 5 2 15 0 4.47356 0.88195 13 3 -15 0 3.07336 2.06506 12 3 15 0 3.76261 2.08208 5 3 15 0 3.36474 0.88076 1 3 15 0 5.50203 1.64366 4 3 15 0 4.90166 0.95669 13 3 15 0 3.65131 0.89523 9 4 15 0 12.6421 1.93151 4 4 15 0 7.81362 2.62431 5 4 15 0 12.1697 1.70976 2 4 15 0 9.13947 1.37245 1 4 15 0 10.5218 1.46109 9 4 15 0 11.9408 1.50356 13 5 -15 0 0.45408 0.76987 6 5 -15 0 -0.8309 1.58428 11 5 15 0 0.17996 0.75804 9 5 15 0 1.05828 0.71742 1 5 15 0 0.12583 0.89262 2 5 15 0 1.64286 2.43033 5 5 15 0 -0.6949 0.90505 4 5 15 0 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