#------------------------------------------------------------------------------ #$Date: 2021-10-03 22:51:47 +0300 (Sun, 03 Oct 2021) $ #$Revision: 269484 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/51/90/4519062.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_4519062 loop_ _publ_author_name 'Khake, Shrikant M.' 'Chatani, Naoto' _publ_section_title ; Rh(III)-Catalyzed [3 + 2] Annulation of Aniline Derivatives with Vinylsilanes via C--H Activation/Alkene Cyclization: Access to Highly Regioselective Indoline Derivatives ; _journal_issue 19 _journal_name_full 'ACS Catalysis' _journal_page_first 12375 _journal_page_last 12383 _journal_paper_doi 10.1021/acscatal.1c03603 _journal_volume 11 _journal_year 2021 _chemical_formula_sum 'C31 H27 N3 Si' _chemical_formula_weight 469.64 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2017/1 _cell_angle_alpha 109.919(6) _cell_angle_beta 90.438(4) _cell_angle_gamma 106.701(6) _cell_formula_units_Z 2 _cell_length_a 9.4517(5) _cell_length_b 10.5860(7) _cell_length_c 13.7057(7) _cell_measurement_reflns_used 3258 _cell_measurement_temperature 123(2) _cell_measurement_theta_max 67.99 _cell_measurement_theta_min 4.60 _cell_volume 1226.40(14) _computing_cell_refinement 'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.43a (Rigaku OD, 2019)' _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_structure_solution 'SIR92 (Altomare, et al., 1994)' _diffrn_ambient_temperature 123(2) _diffrn_detector_area_resol_mean 10.000 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'Rigaku XtaLAB P200' _diffrn_measurement_method \w _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.1078 _diffrn_reflns_av_unetI/netI 0.0946 _diffrn_reflns_Laue_measured_fraction_full 0.987 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 10259 _diffrn_reflns_point_group_measured_fraction_full 0.987 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_theta_full 67.000 _diffrn_reflns_theta_max 68.044 _diffrn_reflns_theta_min 3.454 _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_T_max 0.814 _exptl_absorpt_correction_T_min 0.356 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.43a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 496 _exptl_crystal_size_max 0.800 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.639 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.125 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 317 _refine_ls_number_reflns 4366 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.199 _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.0971 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.001 _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 0.2811 _refine_ls_wR_factor_ref 0.3174 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3121 _reflns_number_total 4366 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file cs1c03603_si_002.cif _cod_data_source_block shelx _cod_original_cell_volume 1226.39(13) _cod_database_code 4519062 _shelx_shelxl_version_number 2017/1 _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 0.494 _shelx_estimated_absorpt_t_max 0.821 _shelx_res_file ; TITL xcalibur shelx.res created by SHELXL-2017/1 at 14:34:05 on 27-Aug-2021 CELL 1.54184 9.4517 10.5860 13.7057 109.919 90.438 106.701 ZERR 2.00 0.0005 0.0007 0.0007 0.006 0.004 0.006 LATT 1 SFAC C H N SI UNIT 62 54 6 2 MERG 2 FMAP 2 PLAN 20 SIZE 0.200 0.300 0.800 ACTA 134.00 BOND $H LIST 4 WPDB -2 L.S. 5 TEMP -150.00 WGHT 0.200000 FVAR 2.71155 C1 1 0.397319 0.607057 0.920148 11.00000 0.03248 0.03754 = 0.03264 0.01123 0.01131 0.01747 C2 1 0.359740 0.491969 0.825939 11.00000 0.03165 0.03414 = 0.03454 0.00753 0.00730 0.01438 C3 1 0.469311 0.449984 0.769117 11.00000 0.04200 0.04473 = 0.03774 0.00163 0.01203 0.02040 AFIX 43 H3 2 0.443768 0.374502 0.703454 11.00000 -1.20000 AFIX 0 C4 1 0.616835 0.520138 0.809844 11.00000 0.03723 0.04607 = 0.04628 0.00758 0.01510 0.02046 AFIX 43 H4 2 0.693753 0.495824 0.770664 11.00000 -1.20000 AFIX 0 C5 1 0.652198 0.625871 0.907826 11.00000 0.03482 0.03908 = 0.04812 0.01233 0.00788 0.01415 AFIX 43 H5 2 0.753917 0.670020 0.935589 11.00000 -1.20000 AFIX 0 C6 1 0.543891 0.670356 0.967680 11.00000 0.03816 0.03836 = 0.03574 0.00803 0.00873 0.01488 C7 1 0.588957 0.772618 1.078292 11.00000 0.04002 0.04670 = 0.03595 0.00653 0.00103 0.01865 AFIX 137 H7A 2 0.604670 0.868914 1.079780 11.00000 -1.50000 H7B 2 0.681346 0.765820 1.105889 11.00000 -1.50000 H7C 2 0.510243 0.749807 1.121337 11.00000 -1.50000 AFIX 0 C8 1 0.241337 0.760091 1.002743 11.00000 0.03430 0.04035 = 0.02509 0.00647 0.00962 0.01277 C9 1 0.332019 1.000141 1.065834 11.00000 0.04526 0.04033 = 0.03726 0.00737 0.00921 0.01542 AFIX 43 H9 2 0.412665 1.084727 1.081733 11.00000 -1.20000 AFIX 0 C10 1 0.192873 1.010481 1.090511 11.00000 0.04568 0.03867 = 0.04880 0.00971 0.01927 0.02059 AFIX 43 H10 2 0.175858 1.098955 1.122311 11.00000 -1.20000 AFIX 0 C11 1 0.081647 0.885035 1.066107 11.00000 0.03797 0.04540 = 0.04035 0.00686 0.01458 0.01732 AFIX 43 H11 2 -0.015325 0.888693 1.081255 11.00000 -1.20000 AFIX 0 C12 1 0.135797 0.504137 0.904982 11.00000 0.03380 0.03892 = 0.03255 0.00231 0.00963 0.00936 AFIX 23 H12A 2 0.049153 0.531235 0.888525 11.00000 -1.20000 H12B 2 0.106546 0.444680 0.948206 11.00000 -1.20000 AFIX 0 C13 1 0.192055 0.424018 0.803195 11.00000 0.03599 0.03187 = 0.03239 0.00110 0.00859 0.01241 AFIX 13 H13 2 0.168571 0.322898 0.796533 11.00000 -1.20000 AFIX 0 C14 1 0.138359 0.619623 0.697082 11.00000 0.03893 0.03912 = 0.02604 0.00101 0.01024 0.01589 C15 1 0.282519 0.715148 0.717569 11.00000 0.03641 0.04474 = 0.04008 0.00694 0.00872 0.01821 AFIX 43 H15 2 0.365237 0.682771 0.722544 11.00000 -1.20000 AFIX 0 C16 1 0.306902 0.855670 0.730705 11.00000 0.04060 0.04422 = 0.03753 0.00485 0.00560 0.01257 AFIX 43 H16 2 0.405306 0.919161 0.745961 11.00000 -1.20000 AFIX 0 C17 1 0.187085 0.903245 0.721492 11.00000 0.06025 0.03817 = 0.04142 0.00301 0.00643 0.01972 AFIX 43 H17 2 0.203567 0.998907 0.728405 11.00000 -1.20000 AFIX 0 C18 1 0.043855 0.811923 0.702293 11.00000 0.04453 0.05040 = 0.04936 0.00573 0.00676 0.02330 AFIX 43 H18 2 -0.038194 0.845302 0.697624 11.00000 -1.20000 AFIX 0 C19 1 0.019827 0.672215 0.689885 11.00000 0.03829 0.04762 = 0.04068 0.00399 0.01020 0.01836 AFIX 43 H19 2 -0.079207 0.610201 0.676157 11.00000 -1.20000 AFIX 0 C20 1 -0.097341 0.326893 0.661487 11.00000 0.03657 0.03464 = 0.02813 -0.00099 0.00836 0.01691 C21 1 -0.162635 0.267618 0.733050 11.00000 0.04106 0.03888 = 0.02814 0.00271 0.00771 0.01767 AFIX 43 H21 2 -0.104121 0.282354 0.794926 11.00000 -1.20000 AFIX 0 C22 1 -0.312459 0.186947 0.715576 11.00000 0.04213 0.03688 = 0.03993 0.00396 0.02012 0.01381 AFIX 43 H22 2 -0.355009 0.147176 0.765154 11.00000 -1.20000 AFIX 0 C23 1 -0.398250 0.165302 0.626164 11.00000 0.03452 0.03714 = 0.04237 -0.00519 0.00771 0.01043 AFIX 43 H23 2 -0.500065 0.110210 0.613795 11.00000 -1.20000 AFIX 0 C24 1 -0.335584 0.224198 0.554118 11.00000 0.03872 0.04906 = 0.03537 0.00202 0.00061 0.02000 AFIX 43 H24 2 -0.395195 0.210334 0.492984 11.00000 -1.20000 AFIX 0 C25 1 -0.186610 0.303056 0.570931 11.00000 0.04323 0.04632 = 0.03188 0.00473 0.01037 0.01784 AFIX 43 H25 2 -0.144546 0.341371 0.520516 11.00000 -1.20000 AFIX 0 C26 1 0.193193 0.336015 0.566842 11.00000 0.03612 0.03993 = 0.02949 0.00395 0.00711 0.01688 C27 1 0.280784 0.401920 0.506283 11.00000 0.03712 0.04344 = 0.03569 0.00443 0.00879 0.01537 AFIX 43 H27 2 0.298513 0.500099 0.521739 11.00000 -1.20000 AFIX 0 C28 1 0.342919 0.326195 0.423315 11.00000 0.03885 0.05989 = 0.03431 0.00825 0.01135 0.01649 AFIX 43 H28 2 0.403598 0.372957 0.383244 11.00000 -1.20000 AFIX 0 C29 1 0.316147 0.182670 0.399303 11.00000 0.04371 0.05947 = 0.03508 -0.00114 0.01352 0.02351 AFIX 43 H29 2 0.357371 0.130686 0.342145 11.00000 -1.20000 AFIX 0 C30 1 0.228834 0.114558 0.458909 11.00000 0.04629 0.04409 = 0.04383 0.00202 0.00745 0.02293 AFIX 43 H30 2 0.211912 0.016520 0.443620 11.00000 -1.20000 AFIX 0 C31 1 0.167031 0.190726 0.540452 11.00000 0.04409 0.04744 = 0.03545 0.00571 0.01280 0.02030 AFIX 43 H31 2 0.105165 0.143278 0.579640 11.00000 -1.20000 AFIX 0 N1 3 0.262660 0.630477 0.959930 11.00000 0.03128 0.03828 = 0.02970 0.00188 0.00832 0.01083 N2 3 0.358131 0.876505 1.020627 11.00000 0.03474 0.03851 = 0.03501 0.00705 0.00873 0.01222 N3 3 0.099452 0.757520 1.022449 11.00000 0.03683 0.04281 = 0.03637 0.00652 0.01374 0.01647 SI1 4 0.105928 0.430144 0.681186 11.00000 0.03329 0.03683 = 0.02895 0.00211 0.00996 0.01435 HKLF 4 REM xcalibur REM R1 = 0.0971 for 3121 Fo > 4sig(Fo) and 0.1242 for all 4366 data REM 317 parameters refined using 0 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.639, deepest hole -0.661, 1-sigma level 0.125 Q1 1 0.0954 0.3942 0.7437 11.00000 0.05 0.64 Q2 1 0.1394 0.4646 0.6144 11.00000 0.05 0.54 Q3 1 0.1894 0.2851 0.5728 11.00000 0.05 0.50 Q4 1 0.2009 0.4633 0.7489 11.00000 0.05 0.49 Q5 1 0.1365 0.3195 0.6555 11.00000 0.05 0.48 Q6 1 0.1235 0.5361 0.7627 11.00000 0.05 0.48 Q7 1 0.0318 0.3355 0.7611 11.00000 0.05 0.44 Q8 1 0.2308 0.9955 0.7588 11.00000 0.05 0.42 Q9 1 -0.4052 0.1845 0.4198 11.00000 0.05 0.41 Q10 1 0.2729 0.6592 0.8991 11.00000 0.05 0.41 Q11 1 0.0977 0.7331 1.0805 11.00000 0.05 0.41 Q12 1 -0.3361 0.1655 0.7452 11.00000 0.05 0.40 Q13 1 0.3659 1.0734 0.7822 11.00000 0.05 0.40 Q14 1 0.2609 0.3739 0.6577 11.00000 0.05 0.40 Q15 1 0.3871 0.9024 0.9599 11.00000 0.05 0.39 Q16 1 0.4055 0.5602 0.5197 11.00000 0.05 0.39 Q17 1 0.3226 0.3846 0.6010 11.00000 0.05 0.39 Q18 1 0.0887 0.7983 0.8821 11.00000 0.05 0.38 Q19 1 0.1413 0.1182 0.6087 11.00000 0.05 0.37 Q20 1 0.3720 0.2798 0.3571 11.00000 0.05 0.37 ; _shelx_res_checksum 46882 _shelx_hkl_file ; 0 0 1 2204.01 93.81 0 0 2 4245.45 179.55 0 0 331878.20 1245.40 0 0 412159.30 502.09 0 0 511543.40 468.34 0 0 511661.20 462.69 0 0 6 2169.84 103.75 0 0 6 2403.28 134.92 0 0 -6 2006.64 118.22 0 0 7 1386.69 85.38 0 0 7 1590.38 109.16 0 0 -7 1378.45 96.04 0 0 812891.60 550.50 0 0 -811894.20 535.14 0 0 9 42.62 31.45 0 0 -9 2.37 26.95 0 0 10 1616.59 129.04 0 0 -10 1983.04 135.89 0 0 11 351.35 70.11 0 0 11 435.16 102.60 0 0 11 401.17 51.24 0 0 -11 404.50 69.78 0 0 12 183.27 76.06 0 0 12 265.34 45.05 0 0 13 83.67 29.76 0 0 13 68.29 24.18 0 0 13 24.36 61.84 0 0 13 -3.89 58.95 0 0 14 19.25 17.65 0 0 14 -19.11 42.33 0 0 14 13.49 21.99 0 0 15 26.08 13.23 0 0 -15 22.97 15.59 0 -1 15 581.48 47.47 0 -1 15 649.61 61.21 0 -1 14 128.80 75.80 0 -1 14 338.12 40.13 0 -1 13 48.40 22.77 0 -1 13 38.64 66.65 0 -1 13 24.30 21.91 0 -1 12 2242.02 136.72 0 -1 12 2281.50 133.60 0 -1 12 2346.75 222.82 0 1 -11 4438.27 272.14 0 -1 11 4749.58 234.16 0 1 -10 3087.36 195.85 0 1 -9 3797.03 213.61 0 -1 9 3863.66 218.64 0 1 -811779.10 511.18 0 -1 811623.60 516.84 0 -1 7 39.36 24.86 0 -1 611586.20 478.84 0 -1 610957.90 463.53 0 -1 5 403.51 35.44 0 -1 5 373.08 51.93 0 -1 4 7498.74 338.98 0 -1 3 332.17 20.03 0 -1 3 573.77 54.98 0 -1 216125.10 631.52 0 -1 217479.70 667.08 0 1 -1 -1.66 3.68 0 -1 014560.30 566.43 0 -1 -1 657.19 32.98 0 -1 -2 4146.52 165.10 0 1 3 8011.16 349.41 0 1 3 9236.22 343.43 0 -1 -3 8327.00 348.56 0 1 4 2409.53 118.79 0 -1 -4 2470.56 118.93 0 1 5 359.10 31.42 0 -1 -5 283.61 36.07 0 1 6 2825.03 151.82 0 1 6 2550.71 124.36 0 1 7 3552.51 172.54 0 1 7 3358.04 191.89 0 -1 -7 3262.50 181.10 0 1 8 290.72 54.87 0 1 8 258.66 40.07 0 -1 -8 259.21 47.82 0 1 9 155.49 45.05 0 -1 -9 142.03 42.81 0 1 10 166.92 37.50 0 1 10 156.61 47.70 0 1 11 83.99 76.02 0 1 11 314.33 50.60 0 1 12 9.67 25.90 0 1 12 43.76 68.19 0 1 13 81.98 24.54 0 1 13 81.09 30.01 0 1 13 53.22 67.73 0 1 14 678.66 52.60 0 1 14 858.68 68.12 0 -2 16 266.98 61.28 0 -2 15 386.00 40.30 0 -2 15 322.28 80.81 0 -2 15 423.39 48.79 0 -2 14 3181.15 250.46 0 -2 14 3271.12 167.68 0 -2 13 689.04 63.00 0 -2 13 581.74 119.35 0 -2 13 633.05 61.39 0 -2 12 111.84 75.59 0 -2 12 87.70 27.56 0 -2 12 72.95 25.53 0 2 -11 1559.38 135.06 0 -2 11 1658.91 103.59 0 -2 11 1735.27 105.31 0 -2 11 1391.45 126.35 0 2 -10 1161.52 105.37 0 -2 10 1051.01 100.95 0 -2 9 131.27 40.43 0 -2 8 3865.12 203.28 0 -2 8 3852.20 197.00 0 -2 712443.10 559.96 0 -2 714327.10 562.26 0 -2 6 2146.69 126.88 0 -2 6 2876.62 137.77 0 2 -5 9177.03 373.31 0 -2 5 9047.90 379.02 0 -2 5 8754.34 379.26 0 2 -433778.90 1302.06 0 -2 434396.80 1316.76 0 -2 435621.70 1307.50 0 -2 431857.90 1294.62 0 -2 432946.90 1363.04 0 -2 386153.60 3639.11 0 -2 389140.00 3680.97 0 -2 272842.60 2802.72 0 -2 013104.30 519.89 0 -2 -1 6365.99 218.86 0 -2 -1 4322.62 209.22 0 -2 -2 467.06 30.79 0 2 3 224.28 30.80 0 -2 -3 264.50 28.47 0 2 4 738.03 58.69 0 -2 -4 811.77 56.50 0 2 5 159.00 32.02 0 2 5 203.59 29.08 0 -2 -5 200.67 32.59 0 2 6 5943.15 255.36 0 2 6 5999.09 272.15 0 2 6 5296.16 253.97 0 -2 -6 5371.66 262.46 0 2 7 8424.44 383.24 0 2 7 8996.20 368.00 0 2 7 7816.70 366.27 0 -2 -7 8241.24 379.42 0 2 8 -6.41 26.31 0 2 8 3.29 19.51 0 2 8 6.41 42.91 0 2 9 93.47 37.55 0 2 9 47.44 58.21 0 2 10 1.93 23.75 0 2 10 -49.91 66.26 0 2 10 1.65 20.31 0 2 11 -8.85 65.75 0 2 12 113.28 80.37 0 2 13 2.26 15.34 0 2 13 -7.58 58.07 0 2 14 -3.90 11.22 0 -2 -14 4.37 15.30 0 -3 16 -3.05 46.15 0 -3 15 3.94 57.86 0 -3 14 1068.13 79.63 0 -3 13 375.53 151.90 0 -3 13 2250.39 116.92 0 -3 12 4336.00 277.01 0 -3 12 4885.15 179.99 0 -3 12 1660.84 240.68 0 -3 12 504.49 196.29 0 3 -11 1815.10 140.10 0 -3 11 1671.56 132.23 0 -3 11 2205.64 192.56 0 -3 11 2052.28 111.07 0 -3 10 2917.06 174.05 0 -3 9 1342.77 102.09 0 -3 9 1121.66 92.27 0 -3 8 923.26 79.12 0 -3 8 916.57 80.46 0 -3 7 875.63 68.47 0 -3 7 861.73 76.52 0 3 -6 5494.40 248.70 0 -3 6 5421.10 264.29 0 -3 6 5867.30 251.76 0 3 -5 2070.61 117.63 0 3 -5 2684.20 121.93 0 -3 5 2738.64 122.97 0 -3 5 2949.38 144.07 0 -3 5 2202.07 115.77 0 -3 5 2445.22 108.29 0 3 -4 154.64 21.42 0 -3 4 210.19 19.62 0 -3 4 174.97 24.18 0 -3 322851.50 964.34 0 -3 323350.40 945.50 0 -3 215957.40 756.46 0 -3 218867.30 725.92 0 -3 1 2165.69 113.17 0 -3 1 2198.75 146.49 0 -3 1 2475.43 107.70 0 3 0 1393.65 71.76 0 -3 0 1244.58 77.75 0 -3 0 1395.23 101.85 0 3 1 16.87 10.47 0 -3 -1 21.52 9.08 0 -3 -1 14.29 11.77 0 -3 -1 1.55 11.18 0 3 2 593.35 40.90 0 3 2 771.86 49.39 0 -3 -2 766.66 46.06 0 -3 -2 503.91 33.05 0 -3 -2 343.04 37.01 0 3 3 660.61 47.77 0 3 3 581.40 59.38 0 -3 -3 662.24 49.62 0 3 4 275.24 44.39 0 3 5 8575.28 377.31 0 3 5 8186.09 391.25 0 3 6 38.84 20.96 0 3 6 41.97 25.61 0 3 7 579.91 59.76 0 3 7 426.66 52.61 0 3 8 932.86 120.88 0 3 8 1002.83 87.28 0 3 9 79.31 32.34 0 3 9 96.38 33.82 0 3 9 42.02 33.40 0 3 10 280.43 48.66 0 3 10 315.97 47.68 0 3 11 584.71 63.90 0 3 11 573.06 61.59 0 3 12 477.17 53.57 0 3 12 144.91 75.64 0 3 13 94.71 23.97 0 3 13 70.30 19.42 0 -4 16 35.92 45.04 0 -4 15 -37.28 84.38 0 -4 15 -7.55 64.24 0 -4 14 89.12 97.18 0 -4 14 40.00 111.40 0 -4 13 133.92 68.24 0 -4 13 69.98 111.76 0 -4 13 194.72 35.19 0 -4 13 34.16 95.14 0 -4 12 47.58 89.61 0 -4 12 13.06 48.51 0 -4 12 6.95 18.03 0 4 -11 3838.01 227.49 0 -4 11 4832.25 201.47 0 -4 11 4544.81 281.22 0 -4 11 3956.43 220.63 0 4 -10 261.44 55.60 0 -4 10 392.44 64.52 0 -4 10 303.41 50.52 0 -4 9 184.19 38.34 0 -4 9 254.32 52.96 0 -4 8 29.13 23.67 0 -4 8 77.56 34.57 0 4 -7 3742.68 194.42 0 -4 7 4895.61 231.08 0 4 -6 818.50 60.35 0 4 -6 786.27 60.49 0 -4 6 816.68 79.43 0 -4 6 852.06 51.50 0 4 -5 5157.15 243.40 0 4 -5 5140.20 236.51 0 -4 4 1858.71 107.02 0 -4 4 2011.96 70.54 0 -4 311047.50 234.50 0 -4 312171.60 149.44 0 -4 2 806.18 101.61 0 -4 2 1182.30 84.32 0 4 -120052.50 236.00 0 -4 121538.90 411.81 0 4 0 2688.89 113.83 0 -4 0 2765.05 111.74 0 4 1 639.71 53.25 0 4 1 563.21 42.94 0 -4 -1 525.83 38.83 0 4 2 7.96 13.63 0 -4 -2 1.84 9.13 0 4 3 1216.72 91.39 0 4 3 856.47 64.01 0 4 4 1829.86 110.35 0 4 4 2132.32 137.42 0 4 5 132.74 43.31 0 4 6 13.02 32.96 0 4 6 52.54 25.47 0 4 6 2.66 46.30 0 4 6 27.76 23.67 0 4 7 1297.34 105.93 0 4 7 2010.84 155.74 0 4 7 1417.93 101.79 0 4 7 1917.27 127.16 0 4 8 302.09 56.82 0 4 8 370.41 49.47 0 4 8 246.32 77.87 0 4 9 178.57 37.35 0 4 9 141.87 72.35 0 4 9 157.89 36.24 0 4 9 194.57 46.47 0 4 10 8.47 23.54 0 4 10 7.89 18.91 0 4 10 19.93 26.28 0 4 10 3.64 60.48 0 4 11 23.43 59.67 0 4 11 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2304.59 137.58 -9 6 -2 748.97 120.99 -9 6 -2 1.54 26.26 9 -6 3 220.07 72.93 -9 6 -3 317.46 45.07 9 -6 4 157.00 70.91 -9 6 -4 305.15 100.70 -9 6 -4 243.68 36.90 9 -6 5 795.83 126.33 -9 6 -5 874.82 67.75 -9 6 -5 625.03 122.11 9 -6 6 290.79 94.06 -9 6 -6 283.73 37.15 -9 6 -7 25.62 16.18 9 -6 8 -7.39 65.73 9 -6 8 1249.91 107.03 9 -6 9 -1.71 44.48 -9 5 8 1489.44 83.92 -9 5 7 2523.77 129.82 -9 5 6 9.54 15.84 -9 5 6 11.60 20.20 -9 5 5 -45.68 47.12 -9 5 5 1.46 21.14 -9 5 4 173.52 54.85 -9 5 4 42.16 24.03 -9 5 3 1164.46 137.53 -9 5 3 1060.17 103.01 -9 5 3 1007.76 82.59 -9 5 2 792.13 121.42 -9 5 2 621.24 63.93 -9 5 1 366.79 102.31 -9 5 1 456.54 55.09 -9 5 0 -1.71 23.31 -9 5 0 51.31 78.90 9 -5 1 368.93 78.09 -9 5 -1 125.54 86.96 -9 5 -1 525.76 56.89 -9 5 -1 29.98 81.63 9 -5 2 575.02 95.65 -9 5 -2 159.23 92.41 -9 5 -2 52.27 75.83 -9 5 -2 583.68 58.37 9 -5 3 95.24 62.45 -9 5 -3 3.44 79.16 -9 5 -3 124.97 30.91 9 -5 4 75.29 65.21 -9 5 -4 41.16 23.90 9 -5 5 579.66 117.56 -9 5 -5 603.41 106.87 -9 5 -5 442.92 50.17 -9 5 -6 1.26 14.77 9 -5 7 102.34 80.44 -9 5 -7 7.88 15.43 9 -5 8 204.24 81.96 9 -5 8 206.98 109.68 -9 5 -8 171.07 28.10 9 -5 9 266.19 108.88 -9 5 -9 422.68 37.85 -9 4 8 32.93 17.24 -9 4 7 955.83 65.99 -9 4 7 744.95 62.84 -9 4 6 912.61 96.66 -9 4 6 962.64 69.53 -9 4 6 816.43 68.63 -9 4 5 278.10 67.49 -9 4 5 -9.93 19.28 -9 4 4 160.71 58.43 -9 4 4 189.74 36.26 -9 4 3 -47.16 55.83 -9 4 3 64.15 89.84 -9 4 3 75.96 25.51 -9 4 2 169.49 98.85 -9 4 2 1831.11 195.52 -9 4 1 329.91 94.43 -9 4 1 79.77 88.65 -9 4 0 147.40 39.11 -9 4 -1 1353.84 121.11 -9 4 -1 1685.60 104.44 -9 4 -2 536.22 104.81 -9 4 -2 -6.95 66.88 9 -4 3 163.80 72.03 -9 4 -3 129.83 33.94 9 -4 4 -29.58 58.30 -9 4 -4 -1.58 21.31 -9 4 -5 231.62 37.04 9 -4 6 21.43 70.88 -9 4 -6 74.58 25.98 9 -4 7 91.58 74.73 -9 4 -7 27.33 18.95 9 -4 8 -26.41 41.94 -9 4 -8 11.92 14.79 9 -4 9 223.02 96.63 -9 4 -9 275.68 31.83 -9 3 8 42.58 18.65 -9 3 7 1008.99 109.09 -9 3 7 1234.30 78.52 -9 3 7 1093.91 76.54 -9 3 6 421.05 43.53 -9 3 6 290.78 39.79 -9 3 5 -15.29 57.12 -9 3 5 -5.77 88.35 -9 3 5 45.12 21.41 -9 3 4 -62.73 64.58 -9 3 4 10.68 53.23 -9 3 4 -46.92 92.41 -9 3 4 12.14 17.21 -9 3 3 42.92 49.38 -9 3 3 -46.61 89.74 -9 3 2 -25.11 50.82 -9 3 2 -107.49 88.15 -9 3 2 -30.51 66.47 -9 3 2 -8.17 24.96 -9 3 1 497.33 99.05 -9 3 1 1328.71 169.50 -9 3 1 521.34 119.25 -9 3 1 1138.82 117.20 -9 3 1 1188.17 92.65 -9 3 0 6.34 51.34 -9 3 0 13.06 62.31 -9 3 0 62.66 41.34 -9 3 0 60.10 31.09 -9 3 -1 -6.47 58.69 -9 3 -1 72.60 68.53 -9 3 -1 113.13 45.80 -9 3 -1 94.86 34.94 -9 3 -2 -23.43 57.77 -9 3 -2 -6.55 58.59 -9 3 -2 -2.95 33.59 -9 3 -2 17.96 25.32 -9 3 -3 44.66 56.22 -9 3 -3 53.26 37.01 9 -3 4 295.17 67.88 -9 3 -4 164.50 46.38 9 -3 5 -40.08 68.85 9 -3 5 39.02 42.89 9 -3 6 293.42 89.01 -9 3 -6 286.12 43.92 9 -3 7 19.04 59.20 9 -3 7 9.03 45.06 -9 3 -7 75.44 25.25 9 -3 8 55.35 53.47 9 -3 8 9.32 38.55 -9 3 -8 3.53 15.98 9 -3 9 77.18 76.43 -9 3 -9 104.61 22.37 -9 2 9 207.29 27.22 -9 2 8 1.04 13.82 -9 2 8 -1.02 14.87 -9 2 7 186.20 75.07 -9 2 7 7.76 15.96 -9 2 6 16.34 17.24 -9 2 5 1945.31 154.34 -9 2 5 2308.57 229.57 -9 2 4 -17.29 46.41 -9 2 4 -41.17 98.17 -9 2 3 3.01 51.41 -9 2 3 -46.91 90.85 -9 2 2 1058.70 136.75 -9 2 2 1622.38 199.58 -9 2 2 2606.15 237.21 -9 2 2 2708.42 190.25 -9 2 2 2335.06 140.03 -9 2 1 1256.07 167.82 -9 2 1 1261.55 131.75 -9 2 1 1376.51 107.20 -9 2 0 24.74 67.68 -9 2 0 126.73 80.92 -9 2 0 484.73 77.58 -9 2 0 472.99 60.64 -9 2 -1 -12.75 58.00 -9 2 -1 6.68 41.16 -9 2 -1 7.49 23.49 9 -2 2 629.27 89.89 -9 2 -2 571.77 85.76 -9 2 -2 657.59 67.33 9 -2 3 1305.19 125.86 -9 2 -3 1106.91 85.57 9 -2 4 388.76 75.69 -9 2 -4 367.47 51.69 -9 2 -4 298.34 61.75 9 -2 5 1187.22 136.60 -9 2 -5 1404.25 102.96 -9 2 -5 1126.88 114.94 9 -2 6 -52.10 65.98 9 -2 6 -3.18 38.75 9 -2 6 7.37 48.98 -9 2 -6 4.80 30.39 -9 2 -6 8.23 22.04 9 -2 7 -10.06 54.80 9 -2 7 38.52 46.64 -9 2 -7 37.59 22.81 -9 1 9 224.46 29.72 -9 1 8 688.29 103.67 -9 1 8 750.53 58.95 -9 1 7 41.61 18.70 -9 1 7 39.44 17.83 -9 1 6 891.80 119.90 -9 1 6 1337.99 80.63 -9 1 5 -32.48 51.67 -9 1 5 -52.83 101.32 -9 1 4 308.81 73.60 -9 1 4 1148.35 174.60 -9 1 3 3815.88 306.73 -9 1 2 249.55 95.81 -9 1 2 289.13 47.76 -9 1 2 315.64 77.58 -9 1 1 353.84 99.81 -9 1 1 360.09 52.61 -9 1 1 284.91 77.85 -9 1 0 69.91 68.10 -9 1 0 107.23 55.36 -9 1 0 79.14 31.07 -9 1 -1 -21.75 48.69 -9 1 -1 -3.70 42.10 -9 1 -1 -3.59 22.53 9 -1 2 124.93 51.99 -9 1 -2 3.13 43.07 -9 1 -2 190.61 61.34 -9 1 -2 163.09 36.38 9 -1 3 13.17 34.58 9 -1 3 -52.10 49.71 -9 1 -3 -57.06 48.11 -9 1 -3 39.13 47.27 -9 1 -3 14.64 22.94 9 -1 4 243.69 64.00 9 -1 4 80.49 57.07 -9 1 -4 134.85 54.08 -9 1 -4 197.58 41.66 9 -1 5 211.06 57.61 9 -1 5 90.54 55.40 9 -1 5 39.99 55.42 -9 1 -5 206.21 39.47 -9 1 -5 178.16 54.06 9 -1 6 70.64 52.39 9 -1 6 191.32 52.57 -9 1 -6 224.06 38.72 -9 1 -6 162.99 48.25 -9 1 -7 499.89 65.37 -9 1 -7 672.22 57.55 -9 0 9 1243.39 75.99 -9 0 8 586.84 90.56 -9 0 8 492.93 122.66 -9 0 8 472.04 45.23 -9 0 7 268.16 109.33 -9 0 7 269.95 82.52 -9 0 7 274.11 106.27 -9 0 7 258.28 34.84 -9 0 6 37.34 43.64 -9 0 6 29.15 72.15 -9 0 6 104.15 97.65 -9 0 6 212.41 32.60 -9 0 5 72.36 91.45 -9 0 4 439.01 129.22 -9 0 4 523.35 128.07 -9 0 3 729.18 150.09 -9 0 3 542.24 128.95 -9 0 3 809.46 110.16 -9 0 2 -56.09 78.83 -9 0 2 11.48 53.18 -9 0 1 60.14 70.67 -9 0 0 233.38 90.87 -9 0 0 302.74 44.13 9 0 1 23.02 43.29 -9 0 -1 -21.16 61.53 -9 0 -1 86.81 61.50 -9 0 -1 52.34 24.31 9 0 2 -12.62 38.86 9 0 2 -14.59 44.98 -9 0 -2 17.63 43.66 -9 0 -2 27.68 50.44 -9 0 -2 -7.74 18.72 9 0 3 912.22 106.08 9 0 3 692.79 95.66 -9 0 -3 878.91 119.40 -9 0 -3 1092.82 82.38 9 0 4 -2.84 34.07 9 0 4 -14.64 47.61 -9 0 -4 36.41 50.60 -9 0 -4 7.50 18.82 9 0 5 56.86 51.16 -9 0 -5 196.66 34.08 -9 0 -5 149.55 55.38 9 0 6 283.98 54.73 -9 0 -6 342.42 40.72 -9 0 -6 300.47 60.70 -9 -1 9 479.96 106.94 -9 -1 8 179.88 95.77 -9 -1 8 275.91 63.99 -9 -1 7 215.08 66.06 -9 -1 7 200.17 101.98 -9 -1 6 -6.62 88.02 -9 -1 5 704.68 153.16 -9 -1 5 594.07 135.47 -9 -1 4 20.76 86.06 -9 -1 4 103.42 93.62 -9 -1 3 450.90 125.80 -9 -1 3 329.91 116.52 -9 -1 3 431.84 82.35 -9 -1 2 442.07 123.73 -9 -1 2 454.95 90.01 -9 -1 1 -6.44 80.80 -9 -1 1 43.99 52.74 -9 -1 0 -86.04 81.02 -9 -1 0 3.74 46.03 -9 -1 -1 142.37 79.68 -9 -1 -1 344.88 79.67 9 1 2 458.78 78.22 9 1 2 589.09 78.00 9 1 3 398.67 70.01 9 1 4 724.33 88.32 9 1 4 1057.45 100.12 -9 -1 -4 963.65 111.52 9 1 5 4.26 28.77 -9 -1 -5 45.99 44.02 -9 -1 -6 2.21 30.64 -9 -2 9 -71.30 87.95 -9 -2 8 -103.29 82.84 -9 -2 7 421.07 129.03 -9 -2 7 248.29 99.00 -9 -2 6 27.07 94.05 -9 -2 6 -50.83 50.43 -9 -2 5 769.58 158.75 -9 -2 5 751.77 143.58 -9 -2 4 46.96 88.46 -9 -2 3 114.21 97.92 -9 -2 3 14.70 38.16 -9 -2 2 826.68 160.54 -9 -2 2 856.02 101.46 -9 -2 1 277.25 113.21 -9 -2 1 213.22 58.99 -9 -2 0 58.04 85.69 -9 -2 0 9.25 41.30 -9 -2 -1 94.51 82.82 -9 -2 -1 147.97 55.61 9 2 2 680.47 87.87 -9 -2 -2 550.15 114.52 9 2 3 139.27 42.36 -9 -2 -3 137.20 51.85 9 2 4 508.79 65.81 -9 -2 -4 586.54 77.77 -9 -3 8 20.93 77.75 -9 -3 7 329.91 111.96 -9 -3 7 199.46 83.34 -9 -3 6 252.83 123.55 -9 -3 6 385.74 107.73 -9 -3 5 247.74 105.37 -9 -3 5 331.94 102.38 -9 -3 4 830.43 146.88 -9 -3 3 289.66 52.90 -9 -3 2 51.27 93.45 -9 -3 2 75.46 36.80 -9 -3 1 146.57 99.47 -9 -3 1 156.32 43.23 -9 -3 0 36.05 81.68 -9 -3 0 6.44 30.69 9 3 1 79.61 35.70 -9 -3 -1 47.63 74.65 -9 -3 -1 93.24 36.72 9 3 2 36.13 34.25 -9 -3 -2 42.20 58.69 -9 -3 -2 103.36 36.61 -9 -4 6 -20.42 57.66 -9 -4 5 -8.00 57.89 -9 -4 4 388.27 96.08 -9 -4 2 29.57 74.14 -9 -4 1 259.19 89.68 -9 -4 0 -8.67 60.70 10 -9 2 -98.97 102.54 10 -8 -1 653.92 78.45 10 -8 -1 628.38 118.09 10 -8 0 881.61 152.25 -10 8 0 395.30 41.08 10 -8 1 1003.57 172.34 10 -8 2 932.73 179.66 10 -8 3 1047.67 190.85 10 -8 4 907.72 188.87 10 -8 5 367.81 165.61 10 -8 5 555.08 64.99 -10 7 3 23.91 16.82 10 -7 -2 178.26 103.36 -10 7 2 111.75 25.81 -10 7 1 68.06 22.63 -10 7 0 51.02 69.22 10 -7 3 4.55 181.87 -10 7 -3 -23.30 64.92 10 -7 4 396.64 69.84 -10 7 -4 124.66 74.59 10 -7 5 35.42 43.98 10 -7 5 1281.31 226.24 10 -7 7 396.31 64.47 -10 6 5 1830.70 97.87 -10 6 4 -1.02 16.14 -10 6 3 392.08 43.13 -10 6 2 -4.52 63.21 -10 6 2 9.88 54.43 -10 6 2 1.23 16.99 -10 6 1 174.67 76.74 -10 6 0 1331.61 126.40 -10 6 0 194.99 101.49 -10 6 -2 331.86 87.52 -10 6 -2 12.94 63.70 10 -6 3 -42.42 46.97 -10 6 -3 9.70 17.08 10 -6 4 415.41 82.36 -10 6 -4 342.20 88.88 -10 6 -4 503.19 47.23 10 -6 5 334.26 81.44 10 -6 5 499.19 231.68 -10 6 -5 271.02 33.49 10 -6 6 282.15 77.19 -10 6 -6 207.36 27.91 -10 6 -7 31.45 13.22 -10 5 6 464.23 40.67 -10 5 5 466.24 43.84 -10 5 4 9.54 35.23 -10 5 4 5.47 15.75 -10 5 3 453.93 87.38 -10 5 3 613.17 68.48 -10 5 3 495.16 48.65 -10 5 2 564.92 97.35 -10 5 1 254.70 83.59 -10 5 1 -5.90 61.27 -10 5 0 281.51 85.64 10 -5 1 -13.28 37.17 -10 5 -1 64.46 73.17 -10 5 -1 8.93 19.94 10 -5 2 302.23 70.28 -10 5 -2 463.80 97.51 -10 5 -2 359.38 44.65 10 -5 3 62.29 53.57 -10 5 -3 11.66 58.15 -10 5 -3 57.27 23.25 -10 5 -4 533.43 95.68 -10 5 -4 205.44 34.86 10 -5 5 376.97 87.55 -10 5 -5 348.08 39.20 -10 5 -6 -6.70 13.96 10 -5 7 91.38 57.46 -10 5 -7 85.19 18.84 -10 4 6 69.32 19.41 -10 4 5 440.36 64.06 -10 4 5 431.91 42.04 -10 4 4 366.76 77.93 -10 4 4 289.23 60.83 -10 4 3 -75.19 70.37 -10 4 3 -5.92 44.80 -10 4 2 21.87 44.46 -10 4 2 91.35 69.23 10 -4 0 88.42 41.67 10 -4 1 634.35 84.18 -10 4 -1 83.68 75.54 10 -4 2 65.80 46.93 10 -4 3 549.24 93.65 -10 4 -3 88.20 73.14 -10 4 -3 16.45 57.30 -10 4 -3 626.04 57.47 -10 4 -4 840.97 118.07 -10 4 -4 1386.00 90.72 -10 4 -5 55.52 21.60 10 -4 6 206.84 74.66 -10 4 -6 186.26 28.86 10 -4 7 93.19 55.88 -10 4 -7 15.17 13.78 -10 3 7 694.29 48.91 -10 3 6 88.53 48.77 -10 3 6 132.26 22.24 -10 3 5 562.96 80.00 -10 3 4 89.15 53.72 -10 3 4 315.52 104.48 -10 3 2 -7.84 56.94 -10 3 2 185.35 88.86 -10 3 1 36.93 47.81 -10 3 0 -2.66 47.00 -10 3 0 -20.71 23.12 -10 3 -1 32.45 51.63 -10 3 -1 146.77 46.72 -10 3 -1 154.70 35.97 -10 3 -2 239.94 40.01 -10 3 -2 168.77 45.76 10 -3 3 -6.39 55.68 -10 3 -3 -9.29 20.73 -10 3 -3 8.91 28.17 10 -3 4 502.95 69.71 -10 3 -4 350.52 44.58 10 -3 5 -61.37 62.43 10 -3 5 -2.02 41.16 10 -3 6 76.25 58.98 -10 2 7 1023.11 96.49 -10 2 6 1791.62 179.96 -10 2 5 -40.24 54.34 -10 2 5 -23.36 85.36 -10 2 4 51.53 40.63 -10 2 4 -57.32 79.74 -10 2 3 140.80 52.72 -10 2 3 252.06 93.01 -10 2 2 116.17 52.02 -10 2 2 345.53 98.50 -10 2 1 511.62 110.26 -10 2 1 759.36 71.27 -10 2 0 39.43 48.50 -10 2 0 161.13 56.54 -10 2 0 187.96 38.78 10 -2 1 25.57 37.96 -10 2 -1 47.47 47.19 -10 2 -1 251.26 41.44 -10 2 -1 186.74 55.22 10 -2 2 345.04 58.81 10 -2 2 72.15 44.22 -10 2 -2 97.60 49.93 -10 2 -2 296.73 43.91 -10 2 -2 214.28 54.01 10 -2 3 65.95 38.66 10 -2 3 -2.09 44.01 10 -2 3 30.08 53.13 -10 2 -3 57.33 27.18 -10 2 -3 69.78 39.31 10 -2 4 141.41 61.60 10 -2 4 301.44 58.57 -10 2 -4 243.84 38.53 -10 2 -4 210.74 46.55 10 -2 5 -61.68 59.61 10 -2 5 -3.77 40.14 -10 2 -5 -22.69 28.62 -10 2 -5 -5.21 18.75 -10 2 -6 -20.89 20.59 -10 1 7 561.49 77.75 -10 1 7 1272.74 148.84 -10 1 6 2073.51 149.10 -10 1 5 -4.34 37.13 -10 1 4 4.75 41.22 -10 1 4 -30.68 60.35 -10 1 4 29.07 78.02 -10 1 3 99.70 51.68 -10 1 3 97.36 82.54 -10 1 2 2.54 41.68 -10 1 2 4.72 79.97 -10 1 1 1278.93 154.05 -10 1 1 1705.32 143.88 -10 1 1 1450.99 93.91 10 -1 0 -16.19 34.78 -10 1 0 -5.12 44.40 -10 1 0 -25.40 51.41 -10 1 0 -5.84 23.51 10 -1 1 -4.89 28.14 -10 1 -1 -17.66 41.27 -10 1 -1 12.39 40.83 -10 1 -1 7.22 19.48 10 -1 2 797.15 87.69 10 -1 2 332.82 59.51 -10 1 -2 201.17 56.78 -10 1 -2 652.30 86.93 -10 1 -2 691.02 60.35 10 -1 3 337.64 60.92 10 -1 3 151.57 49.24 -10 1 -3 341.62 42.74 -10 1 -3 242.41 58.32 10 -1 4 911.99 90.47 10 -1 4 383.99 64.12 10 -1 4 590.18 85.65 -10 1 -4 817.77 62.91 -10 1 -4 611.30 78.41 -10 1 -5 164.55 28.06 -10 1 -5 131.93 38.88 -10 0 7 256.57 55.22 -10 0 7 281.33 89.87 -10 0 6 37.25 49.17 -10 0 6 -4.43 76.07 -10 0 5 -15.34 38.87 -10 0 4 603.92 84.07 -10 0 4 1545.72 173.61 -10 0 3 136.22 53.10 -10 0 3 328.94 103.94 -10 0 2 431.77 110.01 -10 0 2 673.05 92.57 -10 0 1 349.79 89.37 -10 0 1 451.91 81.82 10 0 0 232.11 55.55 -10 0 0 76.49 47.31 -10 0 0 241.69 75.43 10 0 1 207.30 51.47 -10 0 -1 37.53 41.71 -10 0 -1 216.29 61.99 10 0 2 402.31 61.98 -10 0 -2 307.11 66.72 10 0 3 69.06 36.07 10 0 3 -30.57 47.43 -10 0 -3 27.01 40.13 10 0 4 97.81 36.33 -10 0 -4 81.08 39.77 -10 -1 7 -7.23 61.56 -10 -1 6 622.49 67.45 -10 -1 6 634.34 114.50 -10 -1 5 -17.25 38.57 -10 -1 4 -4.71 42.15 -10 -1 3 424.26 74.00 -10 -1 3 759.10 133.32 -10 -1 2 2.47 43.95 -10 -1 2 4.95 65.82 -10 -1 2 26.47 40.29 -10 -1 1 -43.38 43.31 -10 -1 1 -4.75 64.61 -10 -1 1 -26.83 39.62 10 1 0 29.92 34.63 -10 -1 0 6.79 37.79 -10 -1 0 52.11 58.16 -10 -1 0 37.60 41.38 10 1 1 158.41 43.92 -10 -1 -1 188.95 52.54 10 1 2 2.04 26.03 -10 -1 -2 22.13 36.75 -10 -2 5 -17.96 36.62 -10 -2 5 -31.71 71.53 -10 -2 4 6.65 40.81 -10 -2 3 59.52 71.38 -10 -2 2 -49.73 45.22 -10 -2 2 101.51 73.51 10 2 -1 128.83 38.96 -10 -2 1 -39.82 41.71 -10 -2 1 122.91 75.11 -10 -2 1 123.47 38.85 10 2 0 -3.86 25.85 -11 6 0 146.19 54.31 11 -6 2 -58.68 132.99 -11 6 -2 408.15 67.62 -11 5 2 101.38 51.70 -11 5 1 308.68 64.17 -11 5 -1 229.63 63.12 11 -5 2 3.67 34.09 -11 5 -2 217.66 61.25 11 -5 3 58.17 40.41 -11 5 -3 50.20 50.42 -11 4 2 342.94 64.52 -11 4 2 128.90 38.99 -11 4 1 293.53 64.81 -11 4 1 -36.56 33.74 -11 4 0 366.31 49.63 -11 4 -1 186.11 64.86 11 -4 2 85.24 40.85 -11 4 -2 321.74 66.71 11 -4 3 850.27 89.52 -11 3 4 391.89 56.58 -11 3 3 94.18 53.61 -11 3 3 124.25 42.27 -11 3 1 -51.21 40.77 11 -3 0 1245.49 95.47 -11 3 0 513.54 84.41 11 -3 1 373.10 59.63 -11 3 -1 12.87 52.95 11 -3 2 -21.07 43.57 -11 3 -2 55.98 51.87 -11 3 -2 15.62 19.55 11 -3 3 557.29 77.44 -11 3 -3 604.29 53.23 -11 2 4 648.92 72.19 -11 2 3 37.84 51.86 -11 2 2 20.08 41.06 -11 2 2 92.97 56.38 11 -2 -1 -5.32 29.46 11 -2 0 -28.74 36.85 11 -2 1 345.93 62.72 11 -2 2 41.34 48.33 -11 1 2 -1.83 43.58 -11 1 1 427.49 64.77 -11 1 0 -62.74 54.63 ; _shelx_hkl_checksum 84416 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -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 _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3973(4) 0.6071(4) 0.9201(3) 0.0330(9) Uani 1 1 d . . . . . C2 C 0.3597(4) 0.4920(4) 0.8259(3) 0.0338(9) Uani 1 1 d . . . . . C3 C 0.4693(5) 0.4500(5) 0.7691(3) 0.0434(11) Uani 1 1 d . . . . . H3 H 0.443768 0.374502 0.703454 0.052 Uiso 1 1 calc R U . . . C4 C 0.6168(5) 0.5201(5) 0.8098(3) 0.0439(11) Uani 1 1 d . . . . . H4 H 0.693753 0.495824 0.770664 0.053 Uiso 1 1 calc R U . . . C5 C 0.6522(5) 0.6259(4) 0.9078(3) 0.0409(10) Uani 1 1 d . . . . . H5 H 0.753917 0.670020 0.935589 0.049 Uiso 1 1 calc R U . . . C6 C 0.5439(4) 0.6704(4) 0.9677(3) 0.0381(9) Uani 1 1 d . . . . . C7 C 0.5890(5) 0.7726(5) 1.0783(3) 0.0420(10) Uani 1 1 d . . . . . H7A H 0.604670 0.868914 1.079780 0.063 Uiso 1 1 calc R U . . . H7B H 0.681346 0.765820 1.105889 0.063 Uiso 1 1 calc R U . . . H7C H 0.510243 0.749807 1.121337 0.063 Uiso 1 1 calc R U . . . C8 C 0.2413(4) 0.7601(4) 1.0027(3) 0.0344(9) Uani 1 1 d . . . . . C9 C 0.3320(5) 1.0001(4) 1.0658(3) 0.0422(10) Uani 1 1 d . . . . . H9 H 0.412665 1.084727 1.081733 0.051 Uiso 1 1 calc R U . . . C10 C 0.1929(5) 1.0105(4) 1.0905(3) 0.0442(11) Uani 1 1 d . . . . . H10 H 0.175858 1.098955 1.122311 0.053 Uiso 1 1 calc R U . . . C11 C 0.0816(5) 0.8850(4) 1.0661(3) 0.0425(10) Uani 1 1 d . . . . . H11 H -0.015325 0.888693 1.081255 0.051 Uiso 1 1 calc R U . . . C12 C 0.1358(4) 0.5041(4) 0.9050(3) 0.0383(10) Uani 1 1 d . . . . . H12A H 0.049153 0.531235 0.888525 0.046 Uiso 1 1 calc R U . . . H12B H 0.106546 0.444680 0.948206 0.046 Uiso 1 1 calc R U . . . C13 C 0.1921(4) 0.4240(4) 0.8032(3) 0.0358(9) Uani 1 1 d . . . . . H13 H 0.168571 0.322898 0.796533 0.043 Uiso 1 1 calc R U . . . C14 C 0.1384(4) 0.6196(4) 0.6971(3) 0.0367(9) Uani 1 1 d . . . . . C15 C 0.2825(4) 0.7151(4) 0.7176(3) 0.0413(10) Uani 1 1 d . . . . . H15 H 0.365237 0.682771 0.722544 0.050 Uiso 1 1 calc R U . . . C16 C 0.3069(5) 0.8557(5) 0.7307(3) 0.0436(10) Uani 1 1 d . . . . . H16 H 0.405306 0.919161 0.745961 0.052 Uiso 1 1 calc R U . . . C17 C 0.1871(5) 0.9032(5) 0.7215(3) 0.0486(11) Uani 1 1 d . . . . . H17 H 0.203567 0.998907 0.728405 0.058 Uiso 1 1 calc R U . . . C18 C 0.0439(5) 0.8119(5) 0.7023(3) 0.0494(11) Uani 1 1 d . . . . . H18 H -0.038194 0.845302 0.697624 0.059 Uiso 1 1 calc R U . . . C19 C 0.0198(5) 0.6722(5) 0.6899(3) 0.0442(11) Uani 1 1 d . . . . . H19 H -0.079207 0.610201 0.676157 0.053 Uiso 1 1 calc R U . . . C20 C -0.0973(4) 0.3269(4) 0.6615(3) 0.0351(9) Uani 1 1 d . . . . . C21 C -0.1626(4) 0.2676(4) 0.7331(3) 0.0373(9) Uani 1 1 d . . . . . H21 H -0.104121 0.282354 0.794926 0.045 Uiso 1 1 calc R U . . . C22 C -0.3125(5) 0.1869(4) 0.7156(3) 0.0419(10) Uani 1 1 d . . . . . H22 H -0.355009 0.147176 0.765154 0.050 Uiso 1 1 calc R U . . . C23 C -0.3983(4) 0.1653(4) 0.6262(3) 0.0434(11) Uani 1 1 d . . . . . H23 H -0.500065 0.110210 0.613795 0.052 Uiso 1 1 calc R U . . . C24 C -0.3356(5) 0.2242(5) 0.5541(3) 0.0432(10) Uani 1 1 d . . . . . H24 H -0.395195 0.210334 0.492984 0.052 Uiso 1 1 calc R U . . . C25 C -0.1866(5) 0.3031(4) 0.5709(3) 0.0421(10) Uani 1 1 d . . . . . H25 H -0.144546 0.341371 0.520516 0.050 Uiso 1 1 calc R U . . . C26 C 0.1932(4) 0.3360(4) 0.5668(3) 0.0363(9) Uani 1 1 d . . . . . C27 C 0.2808(4) 0.4019(5) 0.5063(3) 0.0407(10) Uani 1 1 d . . . . . H27 H 0.298513 0.500099 0.521739 0.049 Uiso 1 1 calc R U . . . C28 C 0.3429(5) 0.3262(5) 0.4233(3) 0.0464(11) Uani 1 1 d . . . . . H28 H 0.403598 0.372957 0.383244 0.056 Uiso 1 1 calc R U . . . C29 C 0.3161(5) 0.1827(5) 0.3993(3) 0.0492(12) Uani 1 1 d . . . . . H29 H 0.357371 0.130686 0.342145 0.059 Uiso 1 1 calc R U . . . C30 C 0.2288(5) 0.1146(5) 0.4589(3) 0.0464(11) Uani 1 1 d . . . . . H30 H 0.211912 0.016520 0.443620 0.056 Uiso 1 1 calc R U . . . C31 C 0.1670(5) 0.1907(5) 0.5405(3) 0.0434(10) Uani 1 1 d . . . . . H31 H 0.105165 0.143278 0.579640 0.052 Uiso 1 1 calc R U . . . N1 N 0.2627(3) 0.6305(3) 0.9599(2) 0.0358(8) Uani 1 1 d . . . . . N2 N 0.3581(4) 0.8765(3) 1.0206(2) 0.0375(8) Uani 1 1 d . . . . . N3 N 0.0995(4) 0.7575(4) 1.0224(2) 0.0398(8) Uani 1 1 d . . . . . Si1 Si 0.10593(11) 0.43014(11) 0.68119(7) 0.0348(4) Uani 1 1 d . . . . . 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 C1 0.032(2) 0.038(2) 0.0326(19) 0.0112(16) 0.0113(15) 0.0175(17) C2 0.032(2) 0.0341(19) 0.035(2) 0.0075(15) 0.0073(15) 0.0144(16) C3 0.042(2) 0.045(2) 0.038(2) 0.0016(18) 0.0120(18) 0.0204(19) C4 0.037(2) 0.046(2) 0.046(2) 0.0076(18) 0.0151(17) 0.0205(19) C5 0.035(2) 0.039(2) 0.048(2) 0.0123(18) 0.0079(17) 0.0141(17) C6 0.038(2) 0.038(2) 0.036(2) 0.0080(17) 0.0087(16) 0.0149(18) C7 0.040(2) 0.047(2) 0.036(2) 0.0065(18) 0.0010(17) 0.0186(19) C8 0.034(2) 0.040(2) 0.0251(18) 0.0065(15) 0.0096(14) 0.0128(17) C9 0.045(2) 0.040(2) 0.037(2) 0.0074(17) 0.0092(18) 0.0154(19) C10 0.046(2) 0.039(2) 0.049(2) 0.0097(18) 0.0193(19) 0.0206(19) C11 0.038(2) 0.045(2) 0.040(2) 0.0069(18) 0.0146(17) 0.0173(19) C12 0.034(2) 0.039(2) 0.033(2) 0.0023(16) 0.0096(15) 0.0094(17) C13 0.036(2) 0.0319(19) 0.0324(19) 0.0011(15) 0.0086(15) 0.0124(16) C14 0.039(2) 0.039(2) 0.0260(18) 0.0010(15) 0.0102(15) 0.0159(17) C15 0.036(2) 0.045(2) 0.040(2) 0.0069(18) 0.0087(17) 0.0182(19) C16 0.041(2) 0.044(2) 0.038(2) 0.0048(18) 0.0056(17) 0.0126(19) C17 0.060(3) 0.038(2) 0.041(2) 0.0030(18) 0.006(2) 0.020(2) C18 0.045(3) 0.050(3) 0.049(3) 0.006(2) 0.0068(19) 0.023(2) C19 0.038(2) 0.048(2) 0.041(2) 0.0040(18) 0.0102(17) 0.0184(19) C20 0.037(2) 0.0346(19) 0.0281(18) -0.0010(15) 0.0084(15) 0.0169(17) C21 0.041(2) 0.039(2) 0.0281(19) 0.0027(16) 0.0077(16) 0.0177(18) C22 0.042(2) 0.037(2) 0.040(2) 0.0040(17) 0.0201(18) 0.0138(18) C23 0.035(2) 0.037(2) 0.042(2) -0.0052(17) 0.0077(17) 0.0104(18) C24 0.039(2) 0.049(2) 0.035(2) 0.0020(18) 0.0006(17) 0.0200(19) C25 0.043(2) 0.046(2) 0.032(2) 0.0047(17) 0.0104(17) 0.0178(19) C26 0.036(2) 0.040(2) 0.0295(18) 0.0040(16) 0.0071(16) 0.0169(17) C27 0.037(2) 0.043(2) 0.036(2) 0.0044(17) 0.0088(17) 0.0154(18) C28 0.039(2) 0.060(3) 0.034(2) 0.0082(19) 0.0114(17) 0.016(2) C29 0.044(2) 0.059(3) 0.035(2) -0.0011(19) 0.0135(18) 0.024(2) C30 0.046(2) 0.044(2) 0.044(2) 0.0020(19) 0.0074(19) 0.023(2) C31 0.044(2) 0.047(2) 0.035(2) 0.0057(17) 0.0128(17) 0.020(2) N1 0.0313(17) 0.0383(18) 0.0297(16) 0.0019(13) 0.0083(13) 0.0108(14) N2 0.0347(18) 0.0385(18) 0.0350(17) 0.0071(14) 0.0087(14) 0.0122(15) N3 0.0368(18) 0.0428(19) 0.0364(18) 0.0065(14) 0.0137(14) 0.0165(15) Si1 0.0333(6) 0.0368(6) 0.0290(6) 0.0021(4) 0.0100(4) 0.0143(5) 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' Si Si 0.2541 0.3302 '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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 121.4(3) . . ? C6 C1 N1 129.3(3) . . ? C2 C1 N1 108.8(3) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 C13 128.6(3) . . ? C1 C2 C13 110.7(3) . . ? C2 C3 C4 118.7(3) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C5 120.0(3) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 122.7(4) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C1 C6 C5 115.8(3) . . ? C1 C6 C7 124.4(3) . . ? C5 C6 C7 119.6(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 N3 125.9(4) . . ? N2 C8 N1 118.6(3) . . ? N3 C8 N1 115.5(4) . . ? N2 C9 C10 123.1(4) . . ? N2 C9 H9 118.5 . . ? C10 C9 H9 118.5 . . ? C11 C10 C9 115.6(4) . . ? C11 C10 H10 122.2 . . ? C9 C10 H10 122.2 . . ? N3 C11 C10 124.8(4) . . ? N3 C11 H11 117.6 . . ? C10 C11 H11 117.6 . . ? N1 C12 C13 105.1(3) . . ? N1 C12 H12A 110.7 . . ? C13 C12 H12A 110.7 . . ? N1 C12 H12B 110.7 . . ? C13 C12 H12B 110.7 . . ? H12A C12 H12B 108.8 . . ? C2 C13 C12 102.8(3) . . ? C2 C13 Si1 114.8(3) . . ? C12 C13 Si1 113.8(3) . . ? C2 C13 H13 108.4 . . ? C12 C13 H13 108.4 . . ? Si1 C13 H13 108.4 . . ? C15 C14 C19 117.2(4) . . ? C15 C14 Si1 121.2(3) . . ? C19 C14 Si1 121.6(3) . . ? C16 C15 C14 121.4(4) . . ? C16 C15 H15 119.3 . . ? C14 C15 H15 119.3 . . ? C15 C16 C17 119.7(4) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C19 C18 C17 120.0(4) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C18 C19 C14 121.5(4) . . ? C18 C19 H19 119.3 . . ? C14 C19 H19 119.3 . . ? C21 C20 C25 118.0(4) . . ? C21 C20 Si1 121.9(3) . . ? C25 C20 Si1 120.1(3) . . ? C20 C21 C22 121.3(4) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 119.7(4) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C24 119.9(4) . . ? C22 C23 H23 120.1 . . ? C24 C23 H23 120.1 . . ? C25 C24 C23 120.4(4) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 C20 120.7(4) . . ? C24 C25 H25 119.6 . . ? C20 C25 H25 119.6 . . ? C27 C26 C31 117.9(3) . . ? C27 C26 Si1 124.0(3) . . ? C31 C26 Si1 118.1(3) . . ? C26 C27 C28 121.0(4) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C29 C28 C27 119.9(4) . . ? C29 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? C28 C29 C30 120.0(4) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C31 C30 C29 119.4(4) . . ? C31 C30 H30 120.3 . . ? C29 C30 H30 120.3 . . ? C30 C31 C26 121.7(4) . . ? C30 C31 H31 119.2 . . ? C26 C31 H31 119.2 . . ? C8 N1 C1 125.0(3) . . ? C8 N1 C12 120.2(3) . . ? C1 N1 C12 108.9(3) . . ? C9 N2 C8 116.1(3) . . ? C11 N3 C8 114.5(4) . . ? C14 Si1 C20 112.80(18) . . ? C14 Si1 C13 108.55(17) . . ? C20 Si1 C13 107.77(18) . . ? C14 Si1 C26 112.06(18) . . ? C20 Si1 C26 107.37(16) . . ? C13 Si1 C26 108.11(17) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C6 1.396(6) . ? C1 C2 1.396(5) . ? C1 N1 1.442(5) . ? C2 C3 1.385(5) . ? C2 C13 1.520(5) . ? C3 C4 1.385(6) . ? C3 H3 0.9500 . ? C4 C5 1.386(6) . ? C4 H4 0.9500 . ? C5 C6 1.403(5) . ? C5 H5 0.9500 . ? C6 C7 1.503(5) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 N2 1.344(5) . ? C8 N3 1.364(5) . ? C8 N1 1.371(5) . ? C9 N2 1.339(5) . ? C9 C10 1.386(6) . ? C9 H9 0.9500 . ? C10 C11 1.368(6) . ? C10 H10 0.9500 . ? C11 N3 1.338(5) . ? C11 H11 0.9500 . ? C12 N1 1.474(5) . ? C12 C13 1.553(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 Si1 1.883(4) . ? C13 H13 1.0000 . ? C14 C15 1.402(6) . ? C14 C19 1.403(6) . ? C14 Si1 1.874(4) . ? C15 C16 1.385(6) . ? C15 H15 0.9500 . ? C16 C17 1.386(6) . ? C16 H16 0.9500 . ? C17 C18 1.380(6) . ? C17 H17 0.9500 . ? C18 C19 1.379(6) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C20 C21 1.394(6) . ? C20 C25 1.402(6) . ? C20 Si1 1.882(4) . ? C21 C22 1.397(6) . ? C21 H21 0.9500 . ? C22 C23 1.378(6) . ? C22 H22 0.9500 . ? C23 C24 1.390(6) . ? C23 H23 0.9500 . ? C24 C25 1.386(6) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.391(6) . ? C26 C31 1.399(6) . ? C26 Si1 1.886(4) . ? C27 C28 1.393(5) . ? C27 H27 0.9500 . ? C28 C29 1.385(7) . ? C28 H28 0.9500 . ? C29 C30 1.392(7) . ? C29 H29 0.9500 . ? C30 C31 1.381(5) . ? C30 H30 0.9500 . ? C31 H31 0.9500 . ?