#------------------------------------------------------------------------------ #$Date: 2016-06-17 01:46:50 +0300 (Fri, 17 Jun 2016) $ #$Revision: 183572 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/12/50/4125093.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_4125093 loop_ _publ_author_name 'Transue, Wesley J.' 'Velian, Alexandra' 'Nava, Matthew' 'Martin-Drumel, Marie-Aline' 'Womack, Caroline C.' 'Jiang, Jun' 'Hou, Gao-Lei' 'Wang, Xue-Bin' 'McCarthy, Michael C.' 'Field, Robert W.' 'Cummins, Christopher C.' _publ_section_title ; A Molecular Precursor to Phosphaethyne and Its Application in Synthesis of the Aromatic 1,2,3,4-Phosphatriazolate Anion. ; _journal_issue 21 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 6731 _journal_page_last 6734 _journal_paper_doi 10.1021/jacs.6b03910 _journal_volume 138 _journal_year 2016 _chemical_formula_sum 'C7 H19 N6 P S' _chemical_formula_weight 250.31 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 90.002(2) _cell_angle_beta 89.996(2) _cell_angle_gamma 83.296(2) _cell_formula_units_Z 2 _cell_length_a 6.0072(5) _cell_length_b 10.1348(9) _cell_length_c 10.3082(9) _cell_measurement_reflns_used 9816 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 28.29 _cell_measurement_theta_min 2.83 _cell_volume 623.29(9) _computing_cell_refinement 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_data_collection 'APEX2 v2011.4.0 (Bruker-AXS, 2011)' _computing_data_reduction 'SAINT 7.46A (Bruker-AXS, 2011)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 8.3 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker Smart APEX2 CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_unetI/netI 0.0129 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 3070 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.318 _diffrn_reflns_theta_min 1.976 _diffrn_source 'I\mS micro-focus sealed tube, multilayer optics' _exptl_absorpt_coefficient_mu 0.370 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS (Sheldrick, 2009)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.334 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 268 _exptl_crystal_size_max 0.180 _exptl_crystal_size_mid 0.150 _exptl_crystal_size_min 0.070 _exptl_transmission_factor_max 0.745687 _exptl_transmission_factor_min 0.688383 _refine_diff_density_max 0.451 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.051 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 146 _refine_ls_number_reflns 3070 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0271 _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^)+(0.0416P)^2^+0.1288P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0722 _refine_ls_wR_factor_ref 0.0741 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2839 _reflns_number_total 3070 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja6b03910_si_004.cif _cod_data_source_block wt_6 _cod_depositor_comments 'Adding full bibliography for 4125091--4125093.cif.' _cod_database_code 4125093 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.936 _shelx_estimated_absorpt_t_max 0.975 _shelx_res_file ; wt_6.res created by SHELXL-2014/7 TITL wt_5.res in P-1 REM Old TITL wt in P-1 REM SHELXT solution in P-1 REM R1 0.096, Rweak 0.003, Alpha 0.027, Orientation as input REM Formula found by SHELXT: C13 P S CELL 0.71073 6.0072 10.1348 10.3082 90.002 89.996 83.296 ZERR 2.000 0.0005 0.0009 0.0009 0.002 0.002 0.002 LATT 1 SFAC C H N P S UNIT 14 38 12 2 2 TEMP -173.170 SIZE 0.070 0.150 0.180 L.S. 10 BOND $H LIST 4 FMAP 2 PLAN 20 omit 0 0 7 omit 0 0 5 omit 0 -3 9 acta dfix 0.95 c1 h1 rem Tris(dimethylamino)sulfonium cation WGHT 0.041600 0.128800 BASF 0.47707 FVAR 1.71569 S1 5 0.525814 0.675566 0.750026 11.00000 0.01328 0.01460 = 0.01513 -0.00003 -0.00013 -0.00105 N10 3 0.275347 0.614111 0.749964 11.00000 0.01581 0.01686 = 0.01663 0.00027 -0.00043 -0.00576 C11 1 0.247565 0.533847 0.868119 11.00000 0.02214 0.02004 = 0.02071 0.00312 0.00279 -0.00523 AFIX 137 H11A 2 0.101357 0.499964 0.865657 11.00000 -1.50000 H11B 2 0.256335 0.589503 0.945274 11.00000 -1.50000 H11C 2 0.366668 0.459099 0.871409 11.00000 -1.50000 AFIX 0 C12 1 0.247320 0.533810 0.631917 11.00000 0.02218 0.01964 = 0.02095 -0.00331 -0.00319 -0.00489 AFIX 137 H12A 2 0.366877 0.459329 0.628332 11.00000 -1.50000 H12B 2 0.255130 0.589546 0.554741 11.00000 -1.50000 H12C 2 0.101449 0.499539 0.634743 11.00000 -1.50000 AFIX 0 N20 3 0.499002 0.759295 0.615674 11.00000 0.01396 0.01845 = 0.01568 0.00192 0.00146 -0.00199 C21 1 0.711792 0.783051 0.553865 11.00000 0.01637 0.02159 = 0.01993 -0.00064 0.00432 -0.00472 AFIX 137 H21A 2 0.691440 0.788608 0.459617 11.00000 -1.50000 H21B 2 0.827454 0.709734 0.574678 11.00000 -1.50000 H21C 2 0.758057 0.866617 0.586177 11.00000 -1.50000 AFIX 0 C22 1 0.310069 0.862248 0.590839 11.00000 0.01700 0.01960 = 0.01678 0.00195 -0.00147 -0.00015 AFIX 137 H22A 2 0.350371 0.948839 0.618625 11.00000 -1.50000 H22B 2 0.178399 0.841425 0.639471 11.00000 -1.50000 H22C 2 0.275627 0.865036 0.497885 11.00000 -1.50000 AFIX 0 N30 3 0.498904 0.759349 0.884214 11.00000 0.01397 0.01824 = 0.01591 -0.00223 -0.00168 -0.00152 C31 1 0.310039 0.862405 0.909136 11.00000 0.01690 0.01935 = 0.01651 -0.00166 0.00134 0.00022 AFIX 137 H31A 2 0.275689 0.865206 1.002104 11.00000 -1.50000 H31B 2 0.178286 0.841639 0.860558 11.00000 -1.50000 H31C 2 0.350419 0.948973 0.881335 11.00000 -1.50000 AFIX 0 C32 1 0.711713 0.783130 0.946257 11.00000 0.01668 0.02107 = 0.02016 0.00069 -0.00491 -0.00438 AFIX 137 H32A 2 0.757435 0.867054 0.914531 11.00000 -1.50000 H32B 2 0.827738 0.710174 0.924944 11.00000 -1.50000 H32C 2 0.691430 0.787970 1.040540 11.00000 -1.50000 AFIX 0 rem 1,2,3,4-Triazaphospholate anion P1 4 0.205244 0.697007 0.249993 11.00000 0.02186 0.01678 = 0.02284 -0.00001 -0.00022 -0.00372 C1 1 0.034302 0.845697 0.249913 11.00000 0.01738 0.02498 = 0.01558 -0.00006 -0.00008 -0.00102 H1 2 -0.122472 0.865848 0.249188 11.00000 -1.20000 N1 3 0.152140 0.950107 0.250021 11.00000 0.02688 0.01916 = 0.01752 -0.00010 -0.00057 -0.00162 N2 3 0.374340 0.911471 0.249960 11.00000 0.02564 0.02608 = 0.01698 0.00005 -0.00054 -0.01073 N3 3 0.431262 0.780865 0.250023 11.00000 0.01654 0.02782 = 0.01779 -0.00012 -0.00032 -0.00265 HKLF 5 REM wt_5.res in P-1 REM R1 = 0.0271 for 2839 Fo > 4sig(Fo) and 0.0293 for all 3070 data REM 146 parameters refined using 1 restraints END WGHT 0.0416 0.1288 REM Highest difference peak 0.451, deepest hole -0.311, 1-sigma level 0.051 Q1 1 0.5093 0.7352 0.6800 11.00000 0.05 0.45 Q2 1 0.0978 0.7803 0.2530 11.00000 0.05 0.40 Q3 1 0.5114 0.7340 0.8242 11.00000 0.05 0.36 Q4 1 0.4015 0.8441 0.2526 11.00000 0.05 0.28 Q5 1 0.2189 0.6159 0.2810 11.00000 0.05 0.28 Q6 1 0.2608 0.5835 0.8023 11.00000 0.05 0.28 Q7 1 0.2602 0.5849 0.7011 11.00000 0.05 0.28 Q8 1 0.4945 0.7026 0.9121 11.00000 0.05 0.27 Q9 1 0.4175 0.7998 0.6136 11.00000 0.05 0.24 Q10 1 0.0901 0.8882 0.2482 11.00000 0.05 0.24 Q11 1 0.4121 0.7926 0.8965 11.00000 0.05 0.24 Q12 1 0.6053 0.7715 0.5888 11.00000 0.05 0.24 Q13 1 0.5848 0.7726 0.8998 11.00000 0.05 0.24 Q14 1 0.1256 1.0226 0.2572 11.00000 0.05 0.23 Q15 1 0.3446 0.7357 0.2408 11.00000 0.05 0.23 Q16 1 0.6106 0.6089 0.7406 11.00000 0.05 0.22 Q17 1 0.4273 0.9912 0.2506 11.00000 0.05 0.21 Q18 1 0.2509 0.9350 0.2463 11.00000 0.05 0.21 Q19 1 0.2011 0.6781 0.7490 11.00000 0.05 0.21 Q20 1 0.0619 0.9216 0.7527 11.00000 0.05 0.20 ; _shelx_res_checksum 60273 _shelx_hkl_file ; 1 0 0 6539.30 28.9345 1 -1 0 3 4630.87 97.7675 -2 2 0 0 4630.87 97.7675 1 3 0 0 873.899 5.26004 1 4 0 0 2287.70 13.0918 1 5 0 0 306.066 4.25589 1 6 0 0 146.525 3.05415 1 7 0 0 37.9728 2.08215 1 -7 1 0 92.2795 2.90314 1 -6 1 0 198.881 3.89528 1 -5 1 0 23.8684 1.33616 1 -4 1 0 406.112 3.30460 1 -3 1 0 930.318 6.05954 1 -2 1 0 1.88910 0.21223 1 -1 1 0 1937.22 10.1538 1 0 1 0 0.08989 0.05714 1 1 1 0 3357.20 14.0132 1 2 1 0 394.999 2.47315 1 3 1 0 137.022 1.58002 1 4 1 0 1184.55 7.72797 1 5 1 0 22.6803 1.20767 1 6 1 0 999.483 9.07305 1 7 1 0 7.93496 1.05499 1 8 1 0 0.88033 1.03233 1 -7 2 0 53.1990 2.69563 1 -6 2 0 3.33182 0.77119 1 -5 2 0 161.987 3.02946 1 -4 2 0 1005.08 7.79557 1 -3 2 0 116.209 1.25310 1 -2 2 0 41.5346 0.66799 1 -1 2 0 3309.13 16.7034 1 0 2 0 5532.76 29.1215 1 1 2 0 2769.03 13.2863 1 2 2 0 3836.92 18.4726 1 3 2 0 6216.72 31.3140 1 4 2 0 912.089 6.12859 1 5 2 0 48.3770 1.66637 1 6 2 0 648.162 6.68907 1 -3 -1 11 585.287 7.25565 -2 7 2 0 585.287 7.25565 1 8 2 0 0.86588 0.96339 1 -7 3 0 136.796 3.65489 1 -6 3 0 452.471 6.61033 1 -5 3 0 38.6281 2.06259 1 -4 3 0 184.367 2.63520 1 -3 3 0 1044.53 6.39704 1 -2 3 0 1282.22 7.45900 1 -1 3 0 3795.76 20.4962 1 0 3 0 177.597 1.51063 1 1 3 0 1842.84 9.91095 1 2 3 0 3.71288 0.24631 1 3 3 0 4473.73 21.8505 1 4 3 0 938.299 6.84464 1 5 3 0 63.4829 1.65057 1 6 3 0 6.65412 0.85100 1 -3 -2 11 289.465 4.83290 -2 7 3 0 289.465 4.83290 1 -7 4 0 2.81937 1.07134 1 -6 4 0 316.740 5.09023 1 -5 4 0 462.145 6.44264 1 -4 4 0 58.8392 1.75411 1 -3 4 0 94.1034 1.51339 1 -2 4 0 9.11554 0.44525 1 -1 4 1 2676.43 23.5486 -2 -1 4 0 2676.43 23.5486 1 0 4 0 140.171 1.44075 1 1 4 0 32.6177 0.65357 1 2 4 0 629.700 3.76826 1 3 4 0 1969.08 10.8775 1 4 4 0 75.9123 1.49193 1 5 4 0 504.813 5.36296 1 6 4 0 293.253 4.54950 1 7 4 0 99.2901 2.81159 1 -7 5 0 288.073 6.05996 1 -6 5 0 7.08156 1.20219 1 -5 5 0 266.227 4.52390 1 -4 5 0 270.520 3.92250 1 -2 5 4 117.998 2.07288 -2 -3 5 0 117.998 2.07288 1 -2 5 0 1.30510 0.30338 1 -1 5 1 1212.40 7.60866 -2 -1 5 0 1212.40 7.60866 1 0 5 0 690.303 5.03467 1 1 5 0 0.30635 0.21511 1 2 5 0 57.0834 0.91126 1 3 5 0 1315.38 7.40311 1 4 5 0 903.271 7.18752 1 5 5 0 39.3398 1.72849 1 6 5 0 152.030 3.21060 1 7 5 0 256.261 4.56072 1 -6 6 0 107.432 3.68596 1 -3 6 7 33.9309 4.56800 -2 -5 6 0 33.9309 4.56800 1 -4 6 0 344.090 4.74637 1 -2 6 4 2381.52 20.0495 -2 -3 6 0 2381.52 20.0495 1 -2 6 0 4.82460 0.53211 1 -1 6 0 1239.22 7.95428 1 0 6 0 110.130 1.44969 1 1 6 0 395.178 3.09858 1 2 6 0 1.80030 0.29662 1 3 6 0 418.964 3.50065 1 4 6 0 7.21520 0.75162 1 5 6 0 2.30768 0.64236 1 -2 -5 10 152.073 4.78302 -2 6 6 0 152.073 4.78302 1 7 6 0 11.6942 1.42106 1 -6 7 0 133.697 4.17755 1 -5 7 0 170.722 4.09304 1 -4 7 0 17.4479 1.42690 1 -3 7 0 292.394 4.21322 1 -2 7 0 1149.93 8.75449 1 -1 7 0 47.7726 1.26838 1 0 7 0 14.7714 0.74666 1 1 7 0 979.304 6.81927 1 2 7 0 88.0669 1.35857 1 3 7 0 338.539 3.39127 1 -1 -6 7 129.067 8.57830 -2 4 7 0 129.067 8.57830 1 5 7 0 41.2093 1.99700 1 -2 -6 10 525.045 7.36679 -2 6 7 0 525.045 7.36679 1 7 7 0 227.635 4.72094 1 -5 8 0 176.525 4.37721 1 -4 8 0 35.2509 2.07878 1 -3 8 0 562.884 7.55437 1 -2 8 0 1.02881 0.48522 1 -1 8 0 220.099 3.01596 1 0 8 0 192.439 2.45132 1 1 8 0 168.271 2.30226 1 2 8 0 16.4925 0.86837 1 3 8 0 192.503 2.62579 1 -1 -7 7 77.6269 2.61390 -2 4 8 0 77.6269 2.61390 1 5 8 0 119.925 2.94762 1 -2 -7 10 272.956 6.09411 -2 6 8 0 272.956 6.09411 1 -5 9 0 275.998 5.76804 1 -3 9 5 5.24003 1.91302 -2 -4 9 0 5.24003 1.91302 1 -3 9 0 85.4641 3.14042 1 -2 9 2 903.162 8.64777 -2 -2 9 0 903.162 8.64777 1 -1 9 0 761.465 7.00031 1 0 9 0 298.595 3.56136 1 1 9 0 678.370 6.36980 1 2 9 0 40.8620 1.53583 1 3 9 0 72.8360 1.88966 1 4 9 0 727.001 7.14325 1 5 9 0 14.6444 1.54075 1 6 9 0 209.029 4.62902 1 -3 10 5 13.2707 1.80109 -2 -4 10 0 13.2707 1.80109 1 -3 10 0 9.73191 1.35452 1 -2 10 2 442.100 18.3889 -2 -2 10 0 442.100 18.3889 1 -1 10 0 106.115 2.32812 1 0 10 0 1.83196 0.57624 1 1 10 0 48.5423 2.07713 1 2 10 0 63.9180 1.95812 1 3 10 0 0.17430 0.57704 1 4 10 0 0.05112 0.62915 1 5 10 0 0.27755 0.94656 1 6 10 0 5.62765 1.34041 1 -3 11 0 274.565 5.71864 1 -2 11 0 59.7903 2.39179 1 -1 11 0 5.85928 0.92387 1 0 11 0 848.031 8.86808 1 1 11 0 630.058 7.56048 1 2 11 0 15.4378 1.40067 1 0 -10 6 55.0059 4.28095 -2 3 11 0 55.0059 4.28095 1 4 11 0 673.933 8.49788 1 -1 -10 9 425.795 7.91610 -2 5 11 0 425.795 7.91610 1 -2 12 0 945.971 10.7849 1 -1 12 0 0.76182 0.81835 1 0 12 0 32.9502 2.03458 1 1 12 0 649.367 8.05476 1 2 12 0 525.998 6.67038 1 0 -11 6 493.816 7.26727 -2 3 12 0 493.816 7.26727 1 4 12 0 1.33574 0.97737 1 -1 13 0 0.17434 0.99820 1 0 13 0 598.220 8.04397 1 1 -12 3 162.633 4.73557 -2 1 13 0 162.633 4.73557 1 2 13 0 52.6824 2.80327 1 0 -12 6 85.2054 3.43897 -2 3 13 0 85.2054 3.43897 1 -3 -13 1 208.645 5.34954 1 -2 -13 1 124.200 3.80136 1 -1 -13 1 25.9132 1.91076 1 1 -13 1 315.797 7.13630 -2 0 -13 1 315.797 7.13630 1 1 -13 1 129.738 3.90677 1 -1 -11 7 29.1936 3.48971 -2 -4 -12 1 29.1936 3.48971 1 -3 -12 1 4.82624 0.99694 1 -2 -12 1 252.418 4.64120 1 -1 -12 1 171.038 3.97677 1 0 -12 1 20.3298 1.68247 1 1 -12 1 179.776 3.83994 1 2 -12 1 3.81513 1.03720 1 -5 -11 1 220.219 5.34299 1 -4 -11 1 99.8653 3.29263 1 -3 -11 1 275.642 4.35283 1 -2 -11 1 92.9500 2.44445 1 -1 -11 1 1.72355 0.66990 1 0 -11 1 72.5381 2.68581 1 1 -11 1 286.158 4.62423 1 2 -11 1 0.91474 0.83462 1 3 -11 1 225.831 4.82153 1 -6 -10 1 393.885 6.74815 1 -5 -10 1 99.0398 3.26052 1 -4 -10 1 14.7847 1.67355 1 -3 -10 1 228.894 3.58342 1 -2 -10 1 268.453 3.93162 1 -1 -10 1 3.38244 0.68827 1 0 -10 1 118.909 2.41847 1 -1 10 1 1519.55 14.3215 -2 1 -10 1 1519.55 14.3215 1 2 -10 1 325.905 4.65796 1 -2 10 4 246.021 4.36563 -2 3 -10 1 246.021 4.36563 1 4 -10 1 147.252 3.93482 1 -6 -9 1 201.958 4.45922 1 -5 -9 1 391.942 6.26076 1 -4 -9 1 0.64793 0.70339 1 -3 -9 1 3.75889 0.69186 1 -2 -9 1 1297.19 10.2778 1 0 -9 2 6.55188 2.81264 -2 -1 -9 1 6.55188 2.81264 1 0 -9 1 360.800 4.17890 1 -1 9 1 16.6201 1.15650 -2 1 -9 1 16.6201 1.15650 1 2 -9 1 41.5135 1.74942 1 -2 9 4 253.173 4.36424 -2 3 -9 1 253.173 4.36424 1 4 -9 1 57.8894 2.87112 1 5 -9 1 8.71618 1.54048 1 -6 -8 1 2.45894 0.91571 1 -5 -8 1 15.8536 1.46682 1 -4 -8 1 20.2268 1.63311 1 -3 -8 1 485.125 4.87934 1 -2 -8 1 27.9496 1.08164 1 0 -8 2 1560.96 11.1820 -2 -1 -8 1 1560.96 11.1820 1 0 -8 1 325.643 3.63806 1 -1 8 1 923.849 8.49819 -2 1 -8 1 923.849 8.49819 1 2 -8 1 1.12280 0.54072 1 3 -8 1 112.009 2.38288 1 4 -8 1 698.194 8.62088 1 5 -8 1 50.5996 2.95685 1 -3 -6 11 26.2054 2.18246 -2 -7 -7 1 26.2054 2.18246 1 -6 -7 1 105.415 2.85569 1 -5 -7 1 12.0278 1.19211 1 -4 -7 1 7.47563 0.92086 1 -3 -7 1 128.241 1.89464 1 -2 -7 1 1278.85 8.53179 1 -1 -7 1 392.527 3.51176 1 0 -7 1 4.35294 0.47263 1 1 -7 1 357.631 3.61546 1 2 -7 1 15.3824 0.99836 1 3 -7 1 50.6648 1.67169 1 4 -7 1 60.1617 2.62976 1 5 -7 1 100.161 3.46992 1 6 -7 1 137.341 4.41412 1 -3 -5 11 277.782 5.53668 -2 -7 -6 1 277.782 5.53668 1 -6 -6 1 13.4006 1.25578 1 -5 -6 1 644.597 7.30098 1 -4 -6 1 26.8916 1.37306 1 -3 -6 1 3.10568 0.41258 1 -2 -6 1 72.1861 1.12406 1 -1 -6 1 85.7628 1.25702 1 0 -6 1 4.08726 0.41011 1 1 -6 1 72.8378 1.29952 1 2 -6 1 260.031 2.93086 1 3 -6 1 0.56338 0.43034 1 4 -6 1 186.954 3.45105 1 5 -6 1 17.7384 1.80292 1 -3 7 9 44.3758 4.89083 -2 6 -6 1 44.3758 4.89083 1 -7 -5 1 144.774 3.25506 1 -6 -5 1 125.800 2.82431 1 -5 -5 1 0.31262 0.51742 1 -4 -5 1 788.484 7.19748 1 -3 -5 1 176.277 1.86410 1 -2 -5 1 18.3639 0.61392 1 -1 -5 1 50.7397 0.93493 1 0 5 0 848.527 9.37177 -2 0 -5 1 848.527 9.37177 1 1 -5 1 1314.31 8.19623 1 2 -5 1 2.72716 0.39848 1 3 -5 1 0.39786 0.36116 1 -2 6 6 212.193 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3 8 429.412 5.11278 1 -2 3 8 1.46912 0.48424 1 -1 3 8 131.101 2.25106 1 0 3 8 469.441 4.72744 1 1 3 8 169.505 2.35603 1 2 3 8 12.6646 0.94117 1 3 0 8 1072.79 23.5637 -2 3 3 8 1072.79 23.5637 1 4 3 8 162.359 3.25952 1 5 3 8 57.2770 2.49639 1 6 3 8 73.3876 3.38518 1 -5 4 8 319.601 12.8747 1 -4 4 8 34.5281 1.82800 1 -3 4 8 24.6743 1.20096 1 -2 4 8 124.229 2.22810 1 -1 4 8 57.1599 1.68254 1 0 4 8 1.91112 0.54669 1 1 4 8 2.44095 0.55539 1 2 4 8 243.252 3.38375 1 3 4 8 357.922 4.31613 1 4 4 8 11.7561 1.21821 1 5 4 8 232.928 3.96636 1 6 4 8 361.374 6.10857 1 -5 5 8 32.1662 3.06015 1 -4 5 8 3.20995 0.88106 1 -3 5 8 65.6351 1.87631 1 -2 5 8 165.624 2.75591 1 -1 5 8 33.1227 1.49952 1 0 5 8 652.040 6.40204 1 1 5 8 266.788 3.45930 1 2 5 8 12.2750 1.00021 1 3 5 8 134.556 2.88104 1 4 5 8 269.171 4.53780 1 5 5 8 3.34340 0.95613 1 6 5 8 175.106 4.37440 1 -5 6 8 0.44917 0.85450 1 -4 6 8 15.3007 1.70137 1 -3 6 8 225.858 3.65981 1 -2 6 8 145.333 2.81573 1 -1 6 8 6.61828 0.85988 1 0 6 8 122.612 2.69708 1 1 6 8 5.30520 0.70099 1 4 -3 7 315.111 16.0294 -2 2 6 8 315.111 16.0294 1 3 6 8 1.66953 0.67517 1 4 6 8 325.571 5.07418 1 5 6 8 0.88183 0.85798 1 -4 7 8 20.5229 1.76888 1 -3 7 8 170.801 3.53566 1 -2 7 8 553.334 6.44850 1 -1 7 8 12.7118 1.15416 1 0 7 8 1.67016 0.68917 1 1 7 8 337.244 4.25599 1 4 -4 7 59.7828 3.29916 -2 2 7 8 59.7828 3.29916 1 3 7 8 92.4487 2.74296 1 4 7 8 17.8490 1.55045 1 5 7 8 1.32585 0.93536 1 -3 8 8 44.2698 2.31953 1 -2 8 8 39.6177 2.15280 1 -1 8 8 26.1082 1.65835 1 0 8 8 207.918 3.80118 1 1 8 8 2.77530 0.66262 1 2 8 8 114.994 2.49282 1 3 8 8 257.453 4.25510 1 4 8 8 75.4798 2.93350 1 -3 9 8 192.543 4.49270 1 -2 9 8 299.591 5.35019 1 -1 9 8 107.043 2.96154 1 0 9 8 21.0982 1.57719 1 1 9 8 500.082 5.71355 1 2 9 8 259.306 4.22935 1 3 9 8 73.3203 2.79539 1 4 9 8 63.4834 2.78927 1 -2 10 8 91.4152 5.53491 1 -1 10 8 7.37006 1.18969 1 0 10 8 0.33868 0.82456 1 1 10 8 5.55827 1.08087 1 2 10 8 26.0400 1.77624 1 3 10 8 6.51780 1.12574 1 -1 -10 9 15.0125 1.93315 1 0 -10 9 4.11146 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5 -2 9 676.312 8.41488 1 -6 -1 9 6.92221 3.61650 1 -5 -1 9 330.595 13.4461 1 -4 -1 9 373.766 13.7571 1 -3 -1 9 149.170 2.71135 1 -2 -1 9 243.485 3.46533 1 -1 -1 9 2.04093 0.64010 1 0 -1 9 79.5738 2.35540 1 4 4 5 1109.15 22.8517 -2 1 -1 9 1109.15 22.8517 1 2 -1 9 458.833 5.18389 1 3 4 8 360.590 18.1764 -2 3 -1 9 360.590 18.1764 1 4 -1 9 0.38548 0.75707 1 5 -1 9 224.811 4.43775 1 -6 0 9 1.42076 3.48002 1 -5 0 9 3.71046 2.68229 1 -4 0 9 166.144 13.4014 1 -3 0 9 179.925 3.26194 1 -2 0 9 16.1401 1.01403 1 -1 0 9 285.413 3.76243 1 0 0 9 0.63095 0.60542 1 1 0 9 285.470 3.34873 1 2 0 9 15.0892 1.13942 1 3 0 9 184.627 3.26425 1 4 0 9 196.625 3.74355 1 5 0 9 3.94483 0.95367 1 6 0 9 1.62974 1.14578 1 -5 1 9 218.748 16.2358 1 -4 1 9 -0.9954 2.88254 1 -3 1 9 17.9817 1.27196 1 -2 1 9 482.495 4.90758 1 -1 1 9 869.299 7.78179 1 0 1 9 78.7512 2.28430 1 1 1 9 2.48649 0.56704 1 2 1 9 241.761 3.25501 1 3 1 9 151.441 2.91182 1 4 1 9 370.020 5.60115 1 5 1 9 356.744 5.67863 1 6 1 9 8.41176 1.73294 1 -4 2 9 260.568 16.6672 1 -3 2 9 64.4796 1.81628 1 -2 2 9 135.377 2.24896 1 -1 2 9 984.851 8.53995 1 0 2 9 759.583 7.61464 1 1 2 9 -0.3632 0.42383 1 2 2 9 57.7923 1.89591 1 3 2 9 0.34411 0.59090 1 4 2 9 7.97846 1.13767 1 5 2 9 0.83467 0.89913 1 6 2 9 6.82082 1.60563 1 -4 3 9 675.635 13.2053 1 -3 3 9 1.22536 0.59523 1 -2 3 9 311.223 3.65149 1 -1 3 9 39.5289 1.66965 1 5 0 4 216.149 3.65276 -2 0 3 9 216.149 3.65276 1 1 3 9 205.003 2.85337 1 2 3 9 4.74052 0.74538 1 3 3 9 54.6845 2.12002 1 4 3 9 178.078 3.73703 1 5 3 9 214.819 4.30266 1 -4 4 9 116.770 4.64330 1 -3 4 9 2.37722 0.61525 1 -2 4 9 491.704 5.23898 1 -1 4 9 168.711 3.03830 1 5 -1 4 127.541 8.70493 -2 0 4 9 127.541 8.70493 1 1 4 9 389.078 4.75248 1 2 4 9 1154.94 9.57499 1 3 4 9 -0.0835 0.63165 1 4 4 9 0.08549 0.71644 1 5 4 9 220.173 4.16885 1 -4 5 9 19.4989 1.73178 1 -3 5 9 77.1096 2.18319 1 -2 5 9 126.988 2.61899 1 -1 5 9 548.000 6.17514 1 0 5 9 5.47392 0.86197 1 1 5 9 19.4860 1.19232 1 2 5 9 109.610 2.35774 1 3 5 9 282.954 4.40773 1 4 5 9 110.832 3.08950 1 5 5 9 0.88731 0.93734 1 -4 6 9 13.4955 1.71473 1 -3 6 9 29.4814 1.61457 1 -2 6 9 105.131 2.64713 1 -1 6 9 0.54950 0.62740 1 0 6 9 48.3414 2.31166 1 1 6 9 84.3687 1.98944 1 2 6 9 133.856 2.71654 1 3 6 9 45.3864 2.14116 1 4 6 9 3.00259 0.91297 1 3 -2 12 114.725 4.52441 -2 5 6 9 114.725 4.52441 1 -3 7 9 33.8086 1.97815 1 -2 7 9 66.0239 2.55067 1 6 -4 3 577.895 8.61249 -2 -1 7 9 577.895 8.61249 1 0 7 9 28.5967 1.74084 1 1 7 9 58.3202 2.39526 1 2 7 9 274.119 4.14410 1 3 7 9 155.717 3.31936 1 4 7 9 75.7021 3.02631 1 -7 5 0 281.482 7.16756 -2 -3 8 9 281.482 7.16756 1 -2 8 9 20.4235 1.83013 1 6 -5 3 116.245 3.71400 -2 -1 8 9 116.245 3.71400 1 0 8 9 264.833 4.49901 1 1 8 9 103.086 2.82126 1 2 8 9 7.99047 1.03443 1 3 8 9 62.8672 2.72936 1 4 8 9 1.03412 0.90573 1 -2 9 9 4.05171 1.10313 1 -1 9 9 3.75510 1.00951 1 0 9 9 17.6563 1.54264 1 1 9 9 28.3696 1.81703 1 2 9 9 471.051 6.37908 1 3 9 9 -1.0289 0.78441 1 0 10 9 2.60494 1.05540 1 1 10 9 13.6912 1.48830 1 -1 -9 10 354.440 6.77842 1 0 -9 10 32.8641 2.71481 1 -3 -8 10 103.623 3.53706 1 -2 -8 10 1.95191 1.02603 1 -1 -8 10 195.184 4.78348 1 0 -8 10 444.852 8.01732 1 1 -8 10 14.9752 1.61000 1 2 -8 10 56.5012 3.50237 1 -4 -7 10 7.28080 1.40100 1 -3 -7 10 268.384 4.84866 1 -2 -7 10 178.644 3.79441 1 -1 -7 10 191.292 4.06175 1 0 -7 10 52.4671 3.19855 1 4 10 5 13.2506 4.46570 -2 1 -7 10 13.2506 4.46570 1 2 -7 10 40.7999 2.67803 1 3 10 8 19.7292 9.47326 -2 3 -7 10 19.7292 9.47326 1 -4 -6 10 250.038 5.02557 1 -3 -6 10 54.4642 2.54131 1 -2 -6 10 69.0565 2.77144 1 -1 -6 10 125.535 3.38404 1 0 -6 10 132.132 3.70281 1 4 9 5 109.981 3.03770 -2 1 -6 10 109.981 3.03770 1 2 -6 10 388.617 6.44433 1 3 9 8 616.307 9.35877 -2 3 -6 10 616.307 9.35877 1 -4 -5 10 122.286 4.13392 1 -3 -5 10 483.288 6.30966 1 -2 -5 10 91.1347 2.74157 1 5 8 2 79.5319 5.90708 -2 -1 -5 10 79.5319 5.90708 1 0 -5 10 127.422 3.41522 1 4 8 5 32.7013 2.49415 -2 1 -5 10 32.7013 2.49415 1 2 -5 10 0.67100 0.88991 1 3 -5 10 146.812 3.97393 1 4 -5 10 1.52452 1.10723 1 -5 -4 10 97.7897 3.60557 1 -4 -4 10 0.18687 0.82355 1 -3 -4 10 53.2144 2.30556 1 -2 -4 10 60.6570 2.43325 1 -1 -4 10 294.092 4.86099 1 0 -4 10 0.30009 0.78206 1 1 -4 10 80.6369 2.44005 1 2 -4 10 438.245 6.02541 1 3 -4 10 283.423 5.09672 1 4 -4 10 32.7688 2.34059 1 -5 -3 10 18.2792 2.51976 1 -4 -3 10 191.608 3.99578 1 -3 -3 10 283.254 4.32050 1 -2 -3 10 6.14495 0.96596 1 -1 -3 10 61.7582 2.57022 1 0 -3 10 402.388 5.49781 1 1 -3 10 246.779 3.73107 1 2 -3 10 10.9783 1.15474 1 3 -3 10 249.943 4.68238 1 4 -3 10 6.22636 1.35262 1 -5 -2 10 0.51502 2.49322 1 -4 -2 10 239.683 5.22616 1 -3 -2 10 590.295 6.66888 1 -2 -2 10 1.29525 0.67285 1 -1 -2 10 39.9859 2.07912 1 5 5 4 372.879 7.23611 -2 0 -2 10 372.879 7.23611 1 1 -2 10 241.669 3.49458 1 2 -2 10 7.45257 0.94741 1 3 -2 10 228.967 4.16769 1 4 -2 10 1.22884 0.92311 1 5 -2 10 20.6733 1.98375 1 -5 -1 10 6.37537 3.08884 1 -4 -1 10 385.350 8.76388 1 -3 -1 10 2.30118 0.81452 1 6 4 1 249.670 3.84357 -2 -2 -1 10 249.670 3.84357 1 -1 -1 10 178.361 3.21547 1 5 4 4 84.3936 2.77160 -2 0 -1 10 84.3936 2.77160 1 1 -1 10 2.48249 0.60451 1 2 -1 10 53.0018 1.99897 1 3 -1 10 52.4744 2.41539 1 4 -1 10 8.76252 1.30887 1 5 -1 10 64.6473 2.92921 1 -5 0 10 15.0108 6.32045 1 -4 0 10 116.197 6.51416 1 -3 0 10 170.444 3.60151 1 6 3 1 251.202 5.13520 -2 -2 0 10 251.202 5.13520 1 -1 0 10 38.0317 1.85888 1 0 0 10 1791.76 14.8806 1 1 0 10 38.1184 1.39046 1 2 0 10 11.1343 1.01016 1 3 0 10 170.818 3.52960 1 4 0 10 141.768 3.52045 1 5 0 10 23.7894 1.90364 1 -5 1 10 44.9206 9.53076 1 -4 1 10 5.74304 4.71100 1 -3 1 10 49.1965 2.10633 1 -2 1 10 53.8551 1.83102 1 -1 1 10 2.34055 0.68959 1 0 1 10 81.1240 2.54349 1 1 1 10 177.251 3.26801 1 2 1 10 252.158 3.76518 1 3 1 10 2.29868 0.76614 1 4 1 10 398.808 6.07810 1 3 3 12 146.532 4.27710 -2 5 1 10 146.532 4.27710 1 -4 2 10 -1.1792 0.86762 1 -3 2 10 221.201 4.15528 1 -2 2 10 6.53583 0.75144 1 -1 2 10 239.811 3.72687 1 0 2 10 190.775 3.45807 1 1 2 10 40.5791 1.89028 1 2 2 10 1.69397 0.65581 1 3 2 10 588.874 6.71107 1 4 2 10 248.912 4.65489 1 3 2 12 199.367 4.52271 -2 5 2 10 199.367 4.52271 1 -4 3 10 6.27658 1.30402 1 7 0 0 289.508 5.37855 -2 -3 3 10 289.508 5.37855 1 -2 3 10 12.7158 1.02897 1 6 0 3 250.556 11.6411 -2 -1 3 10 250.556 11.6411 1 0 3 10 412.795 5.36048 1 1 3 10 57.6183 2.51157 1 2 3 10 6.58501 0.87415 1 3 3 10 300.605 4.32465 1 4 3 10 197.557 3.93309 1 3 1 12 17.9525 3.22201 -2 5 3 10 17.9525 3.22201 1 -4 4 10 28.2341 2.91627 1 -7 1 0 349.657 6.37275 -2 -3 4 10 349.657 6.37275 1 -2 4 10 436.781 5.24191 1 6 -1 3 81.7299 7.22565 -2 -1 4 10 81.7299 7.22565 1 0 4 10 0.18523 0.70400 1 1 4 10 290.266 5.11473 1 2 4 10 53.6936 2.06860 1 3 4 10 53.2391 2.38237 1 4 4 10 0.92557 0.82762 1 5 4 10 104.626 3.35010 1 -4 5 10 0.80447 0.89353 1 -3 5 10 141.814 3.29917 1 -2 5 10 2.03349 0.73067 1 -1 5 10 0.52176 0.70030 1 0 5 10 121.588 2.96775 1 1 5 10 93.6866 3.07247 1 2 5 10 93.5520 2.68443 1 3 5 10 496.948 6.73725 1 4 5 10 122.651 3.30730 1 -3 6 10 516.918 7.44095 1 -2 6 10 381.886 5.54392 1 -1 6 10 5.29820 0.99878 1 0 6 10 131.915 3.33437 1 1 6 10 129.947 3.24406 1 5 -2 8 85.4949 4.96479 -2 2 6 10 85.4949 4.96479 1 3 6 10 51.4280 2.51501 1 4 -2 11 350.092 5.77276 -2 4 6 10 350.092 5.77276 1 -3 7 10 0.35407 0.86692 1 -2 7 10 45.5966 2.44694 1 -1 7 10 12.1191 1.33769 1 0 7 10 50.9882 2.54260 1 1 7 10 192.603 4.30142 1 5 -3 8 214.635 4.54929 -2 2 7 10 214.635 4.54929 1 3 7 10 281.125 4.95762 1 4 -3 11 398.070 6.72196 -2 4 7 10 398.070 6.72196 1 -2 8 10 50.7985 2.64287 1 -1 8 10 15.1612 1.53313 1 0 8 10 445.196 6.73215 1 1 8 10 196.008 4.43113 1 5 -4 8 306.953 12.9004 -2 2 8 10 306.953 12.9004 1 3 8 10 102.827 3.68833 1 0 9 10 32.1274 2.21429 1 1 9 10 374.549 6.39187 1 -1 -8 11 209.212 5.17302 1 0 -8 11 27.4938 2.48475 1 -2 -7 11 769.305 9.01113 1 -1 -7 11 293.035 5.53650 1 0 -7 11 18.8371 2.09043 1 1 -7 11 336.095 6.54836 1 -3 -6 11 31.4103 2.08710 1 6 9 1 383.774 6.09977 -2 -2 -6 11 383.774 6.09977 1 -1 -6 11 100.628 3.72586 1 5 9 4 23.9192 4.53206 -2 0 -6 11 23.9192 4.53206 1 1 -6 11 23.1090 2.11946 1 2 -6 11 260.890 5.58770 1 -4 -5 11 5.85619 1.34278 1 -3 -5 11 271.908 4.70471 1 6 8 1 92.0057 2.89327 -2 -2 -5 11 92.0057 2.89327 1 -1 -5 11 17.2075 1.69300 1 5 8 4 449.776 12.0373 -2 0 -5 11 449.776 12.0373 1 1 -5 11 702.782 9.51438 1 2 -5 11 69.8185 3.17005 1 3 -5 11 107.006 4.06520 1 -7 -7 2 102.048 6.52345 -2 -4 -4 11 102.048 6.52345 1 -3 -4 11 115.822 3.18328 1 6 7 1 682.858 12.2113 -2 -2 -4 11 682.858 12.2113 1 -1 -4 11 49.2075 2.53005 1 0 -4 11 -0.4936 0.83283 1 1 -4 11 425.562 6.52560 1 2 -4 11 474.919 6.74227 1 3 -4 11 4.82775 1.33008 1 -4 -3 11 33.6795 2.12952 1 -3 -3 11 42.3043 2.46464 1 -2 -3 11 36.2512 2.03438 1 -1 -3 11 -0.9998 0.73201 1 0 -3 11 17.4555 1.66085 1 1 -3 11 89.4060 3.46319 1 2 -3 11 -0.3711 0.74455 1 3 -3 11 81.9408 3.19884 1 4 -3 11 409.802 6.94840 1 -4 -2 11 14.8145 1.88009 1 -3 -2 11 7.38246 1.13094 1 -2 -2 11 172.721 3.48598 1 -1 -2 11 6.88960 1.07300 1 0 -2 11 205.362 3.91083 1 1 -2 11 391.345 5.76895 1 2 -2 11 287.042 4.66675 1 4 6 9 3.18095 1.99746 -2 3 -2 11 3.18095 1.99746 1 4 -2 11 129.100 3.86651 1 -4 -1 11 52.5638 2.86094 1 7 4 0 114.429 3.50607 -2 -3 -1 11 114.429 3.50607 1 -2 -1 11 7.71058 1.01545 1 -1 -1 11 14.7997 1.39404 1 0 -1 11 60.4578 2.53201 1 1 -1 11 82.0730 3.04994 1 2 -1 11 15.0220 1.32502 1 3 -1 11 3.87670 1.02246 1 4 -1 11 8.40245 1.35857 1 -4 0 11 191.675 6.11638 1 7 3 0 232.044 5.02535 -2 -3 0 11 232.044 5.02535 1 -2 0 11 0.36080 0.64681 1 -1 0 11 385.720 5.18609 1 0 0 11 6.70787 0.98167 1 1 0 11 377.277 5.54016 1 2 0 11 -0.0522 0.63335 1 3 0 11 23.9125 1.84763 1 4 0 11 198.245 4.33794 1 -4 1 11 4.02902 1.45796 1 -3 1 11 3.94511 0.96248 1 -2 1 11 16.5805 1.29331 1 -1 1 11 84.1351 2.45946 1 0 1 11 67.1806 2.71444 1 1 1 11 17.1405 1.42350 1 2 1 11 7.33171 0.98824 1 3 1 11 30.1201 1.94506 1 4 3 11 92.6357 3.35881 -2 4 1 11 92.6357 3.35881 1 -4 2 11 114.308 3.76998 1 -3 2 11 1.88604 0.87518 1 -2 2 11 278.907 4.29257 1 -1 2 11 389.073 5.19419 1 0 2 11 204.262 3.76838 1 1 2 11 8.48753 1.21003 1 5 2 8 187.834 3.75141 -2 2 2 11 187.834 3.75141 1 3 2 11 7.76848 1.15781 1 4 2 11 30.1182 2.15014 -2 4 2 11 30.1182 2.15014 1 -4 3 11 388.735 8.86355 1 -3 3 11 75.8685 2.78985 1 -2 3 11 0.45437 0.63437 1 -1 3 11 80.5191 2.50742 1 0 3 11 17.0561 1.48978 1 1 3 11 -0.1663 0.73280 1 5 1 8 75.7056 2.49935 -2 2 3 11 75.7056 2.49935 1 3 3 11 42.6915 2.21152 1 4 1 11 85.8144 3.43261 -2 4 3 11 85.8144 3.43261 1 -3 4 11 3.56229 0.91620 1 -2 4 11 475.400 5.72101 1 -1 4 11 397.348 5.89018 1 0 4 11 1.75947 0.85939 1 1 4 11 42.4189 2.47836 1 5 0 8 582.189 13.1923 -2 2 4 11 582.189 13.1923 1 3 4 11 116.345 3.43322 1 4 4 11 67.8124 3.21091 1 -3 5 11 102.264 2.87107 1 -2 5 11 70.1116 2.60527 1 -1 5 11 665.732 8.19616 1 0 5 11 254.929 4.55188 1 1 5 11 19.1336 1.75978 1 2 5 11 100.520 2.78578 1 3 5 11 283.759 5.30502 1 4 5 11 1.15621 0.98927 1 -2 6 11 256.411 4.56223 1 -1 6 11 23.4614 1.79752 1 0 6 11 22.3515 1.85608 1 6 -2 7 104.826 4.22825 -2 1 6 11 104.826 4.22825 1 2 6 11 194.219 4.05887 1 5 -2 10 53.1874 2.82318 -2 3 6 11 53.1874 2.82318 1 7 -3 4 453.148 13.3395 -2 -1 7 11 453.148 13.3395 1 0 7 11 21.6643 1.83166 1 6 -3 7 321.330 6.04179 -2 1 7 11 321.330 6.04179 1 2 7 11 778.167 10.0663 1 0 8 11 26.8115 2.08236 1 6 -4 7 240.754 5.40712 -2 1 8 11 240.754 5.40712 1 -2 -6 12 43.8439 2.61595 1 -1 -6 12 44.8397 2.60255 1 0 -6 12 183.745 4.91441 1 1 -6 12 92.6900 4.64472 1 -2 -5 12 2.38650 0.97781 1 -1 -5 12 12.8369 1.61176 1 0 -5 12 234.051 5.41301 1 1 -5 12 102.090 4.49172 1 2 -5 12 0.56814 0.98368 1 7 7 0 368.411 24.0453 -2 -3 -4 12 368.411 24.0453 1 -2 -4 12 98.0185 3.26730 1 -1 -4 12 205.364 4.44118 1 0 -4 12 253.796 5.12723 1 1 -4 12 1.15331 1.10040 1 2 -4 12 90.3461 3.15214 1 -3 -3 12 156.582 4.07309 1 -2 -3 12 15.5265 1.53849 1 -1 -3 12 90.2367 3.41683 1 0 -3 12 325.494 5.72238 1 1 -3 12 46.5830 2.70492 1 5 7 8 -2.0984 2.69739 -2 2 -3 12 -2.0984 2.69739 1 3 -3 12 431.115 7.11811 1 -3 -2 12 195.661 5.59603 1 -2 -2 12 39.3958 2.21132 1 -1 -2 12 28.7138 2.03219 1 6 6 5 205.740 14.0403 -2 0 -2 12 205.740 14.0403 1 1 -2 12 3.87552 1.16712 1 5 6 8 88.8565 3.05961 -2 2 -2 12 88.8565 3.05961 1 3 -2 12 5.16694 1.29277 1 -3 -1 12 -1.0707 0.97898 1 -2 -1 12 17.9991 1.53209 1 -1 -1 12 389.139 5.92568 1 6 5 5 125.958 3.58772 -2 0 -1 12 125.958 3.58772 1 1 -1 12 113.921 3.78523 1 5 5 8 37.2175 2.36587 -2 2 -1 12 37.2175 2.36587 1 3 -1 12 209.680 4.64271 1 -3 0 12 40.7223 2.88529 1 -2 0 12 5.68447 0.98937 1 -1 0 12 28.5218 1.91585 1 6 4 5 756.459 18.7868 -2 0 0 12 756.459 18.7868 1 1 0 12 28.4359 1.94161 1 2 0 12 4.05849 1.14403 1 3 0 12 42.4227 2.59851 1 -3 1 12 189.925 5.11339 1 -2 1 12 31.5002 1.88617 1 -1 1 12 103.782 2.96940 1 0 1 12 6.57163 1.06310 1 1 1 12 404.618 6.05915 1 2 1 12 15.2681 1.63289 1 3 1 12 -0.5402 0.85395 1 -3 2 12 7.28458 1.47946 1 -2 2 12 95.5145 2.70817 1 -1 2 12 4.41706 0.90439 1 0 2 12 102.347 2.99154 1 6 2 7 39.0166 2.70069 -2 1 2 12 39.0166 2.70069 1 2 2 12 37.5243 2.37633 1 5 2 10 212.331 4.87920 -2 3 2 12 212.331 4.87920 1 -3 3 12 420.756 9.34021 1 -2 3 12 2.38020 0.80406 1 7 1 4 57.3394 2.53077 -2 -1 3 12 57.3394 2.53077 1 0 3 12 324.529 5.31144 1 6 1 7 300.527 5.75587 -2 1 3 12 300.527 5.75587 1 2 3 12 16.5038 1.70808 1 5 1 10 158.721 13.5032 -2 3 3 12 158.721 13.5032 1 -2 4 12 88.8821 2.83222 1 7 0 4 1.80937 1.77727 -2 -1 4 12 1.80937 1.77727 1 0 4 12 250.028 4.95132 1 6 0 7 288.528 5.75371 -2 1 4 12 288.528 5.75371 1 2 4 12 87.4972 3.41183 1 3 4 12 166.519 4.06393 1 -2 5 12 0.39869 0.79314 1 -1 5 12 99.4784 3.33237 1 0 5 12 220.587 4.40325 1 1 5 12 10.4219 1.52231 1 2 5 12 2.26052 1.04331 1 -1 6 12 80.7828 3.30755 1 0 6 12 183.050 4.29484 1 1 6 12 45.8473 2.55817 1 2 6 12 42.3447 2.68539 1 -1 -4 13 14.5009 1.67785 1 6 8 5 54.4973 4.77596 -2 0 -4 13 54.4973 4.77596 1 -2 -3 13 63.4733 2.93620 1 -1 -3 13 45.1541 2.67621 1 0 -3 13 14.8233 1.70414 1 1 -3 13 66.6132 3.58913 1 -2 -2 13 183.236 4.02563 1 7 6 4 278.207 5.72684 -2 -1 -2 13 278.207 5.72684 1 0 -2 13 73.2753 3.36383 1 6 6 7 49.7512 3.13432 -2 1 -2 13 49.7512 3.13432 1 2 -2 13 140.988 4.24164 1 -2 -1 13 143.864 3.48085 1 7 5 4 958.918 10.6980 -2 -1 -1 13 958.918 10.6980 1 0 -1 13 14.7675 1.67024 1 6 5 7 34.7735 2.69820 -2 1 -1 13 34.7735 2.69820 1 2 -1 13 77.4528 3.40446 1 -2 0 13 24.5924 1.77576 1 7 4 4 53.0128 2.64202 -2 -1 0 13 53.0128 2.64202 1 0 0 13 5.57380 1.21269 1 1 0 13 52.5102 2.88796 1 2 0 13 23.6837 2.24762 1 -2 1 13 70.7089 2.83177 1 -1 1 13 27.4500 1.92188 1 0 1 13 13.7899 1.47550 1 1 1 13 201.733 4.82184 1 2 1 13 148.209 4.34354 1 -2 2 13 135.989 3.67885 1 -1 2 13 24.4526 1.86888 1 0 2 13 61.9848 2.93374 1 1 2 13 96.3281 4.02028 1 2 2 13 187.478 4.84131 1 -1 3 13 73.6147 3.03768 1 7 1 6 21.5607 2.98294 -2 0 3 13 21.5607 2.98294 1 1 3 13 45.3306 2.79270 1 2 3 13 64.5371 3.53640 1 0 4 13 28.1077 2.21277 1 1 4 13 11.9880 1.64282 1 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 17422 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 S1 S 0.52581(4) 0.67557(2) 0.75003(2) 0.01438(8) Uani 1 1 d . . N10 N 0.27535(16) 0.61411(9) 0.74996(9) 0.01613(19) Uani 1 1 d . . C11 C 0.2476(2) 0.53385(12) 0.86812(11) 0.0207(2) Uani 1 1 d . . H11A H 0.1014 0.5000 0.8657 0.031 Uiso 1 1 calc R U H11B H 0.2563 0.5895 0.9453 0.031 Uiso 1 1 calc R U H11C H 0.3667 0.4591 0.8714 0.031 Uiso 1 1 calc R U C12 C 0.2473(2) 0.53381(12) 0.63192(11) 0.0207(2) Uani 1 1 d . . H12A H 0.3669 0.4593 0.6283 0.031 Uiso 1 1 calc R U H12B H 0.2551 0.5895 0.5547 0.031 Uiso 1 1 calc R U H12C H 0.1014 0.4995 0.6347 0.031 Uiso 1 1 calc R U N20 N 0.49900(16) 0.75930(9) 0.61567(9) 0.01603(19) Uani 1 1 d . . C21 C 0.71179(19) 0.78305(12) 0.55386(11) 0.0191(2) Uani 1 1 d . . H21A H 0.6914 0.7886 0.4596 0.029 Uiso 1 1 calc R U H21B H 0.8275 0.7097 0.5747 0.029 Uiso 1 1 calc R U H21C H 0.7581 0.8666 0.5862 0.029 Uiso 1 1 calc R U C22 C 0.31007(19) 0.86225(11) 0.59084(11) 0.0180(2) Uani 1 1 d . . H22A H 0.3504 0.9488 0.6186 0.027 Uiso 1 1 calc R U H22B H 0.1784 0.8414 0.6395 0.027 Uiso 1 1 calc R U H22C H 0.2756 0.8650 0.4979 0.027 Uiso 1 1 calc R U N30 N 0.49890(16) 0.75935(9) 0.88421(9) 0.01607(19) Uani 1 1 d . . C31 C 0.31004(19) 0.86241(11) 0.90914(11) 0.0178(2) Uani 1 1 d . . H31A H 0.2757 0.8652 1.0021 0.027 Uiso 1 1 calc R U H31B H 0.1783 0.8416 0.8606 0.027 Uiso 1 1 calc R U H31C H 0.3504 0.9490 0.8813 0.027 Uiso 1 1 calc R U C32 C 0.71171(19) 0.78313(12) 0.94626(11) 0.0191(2) Uani 1 1 d . . H32A H 0.7574 0.8671 0.9145 0.029 Uiso 1 1 calc R U H32B H 0.8277 0.7102 0.9249 0.029 Uiso 1 1 calc R U H32C H 0.6914 0.7880 1.0405 0.029 Uiso 1 1 calc R U P1 P 0.20524(5) 0.69701(3) 0.24999(3) 0.02038(9) Uani 1 1 d . . C1 C 0.0343(2) 0.84570(12) 0.24991(11) 0.0194(2) Uani 1 1 d D . H1 H -0.122(2) 0.8658(15) 0.2492(15) 0.023 Uiso 1 1 d D U N1 N 0.15214(18) 0.95011(10) 0.25002(10) 0.0213(2) Uani 1 1 d . . N2 N 0.37434(19) 0.91147(10) 0.24996(10) 0.0223(2) Uani 1 1 d . . N3 N 0.43126(17) 0.78086(10) 0.25002(10) 0.0207(2) 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 S1 0.01328(14) 0.01460(13) 0.01513(13) -0.00003(9) -0.00013(9) -0.00105(9) N10 0.0158(4) 0.0169(4) 0.0166(4) 0.0003(3) -0.0004(3) -0.0058(3) C11 0.0221(6) 0.0200(5) 0.0207(5) 0.0031(4) 0.0028(4) -0.0052(4) C12 0.0222(6) 0.0196(5) 0.0209(5) -0.0033(4) -0.0032(4) -0.0049(4) N20 0.0140(4) 0.0185(4) 0.0157(4) 0.0019(3) 0.0015(3) -0.0020(3) C21 0.0164(5) 0.0216(5) 0.0199(5) -0.0006(4) 0.0043(4) -0.0047(4) C22 0.0170(5) 0.0196(5) 0.0168(5) 0.0020(4) -0.0015(4) -0.0002(4) N30 0.0140(4) 0.0182(4) 0.0159(4) -0.0022(3) -0.0017(3) -0.0015(3) C31 0.0169(5) 0.0193(5) 0.0165(5) -0.0017(4) 0.0013(4) 0.0002(4) C32 0.0167(5) 0.0211(5) 0.0202(5) 0.0007(4) -0.0049(4) -0.0044(4) P1 0.02186(17) 0.01678(15) 0.02284(16) -0.00001(11) -0.00022(12) -0.00372(11) C1 0.0174(5) 0.0250(6) 0.0156(5) -0.0001(4) -0.0001(4) -0.0010(4) N1 0.0269(5) 0.0192(5) 0.0175(5) -0.0001(3) -0.0006(4) -0.0016(4) N2 0.0256(5) 0.0261(5) 0.0170(5) 0.0001(4) -0.0005(4) -0.0107(4) N3 0.0165(5) 0.0278(5) 0.0178(5) -0.0001(4) -0.0003(4) -0.0027(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 N30 S1 N20 117.17(5) N30 S1 N10 98.88(5) N20 S1 N10 98.84(5) C12 N10 C11 110.17(9) C12 N10 S1 111.37(8) C11 N10 S1 111.25(7) N10 C11 H11A 109.5 N10 C11 H11B 109.5 H11A C11 H11B 109.5 N10 C11 H11C 109.5 H11A C11 H11C 109.5 H11B C11 H11C 109.5 N10 C12 H12A 109.5 N10 C12 H12B 109.5 H12A C12 H12B 109.5 N10 C12 H12C 109.5 H12A C12 H12C 109.5 H12B C12 H12C 109.5 C22 N20 C21 114.90(9) C22 N20 S1 122.73(8) C21 N20 S1 114.81(8) N20 C21 H21A 109.5 N20 C21 H21B 109.5 H21A C21 H21B 109.5 N20 C21 H21C 109.5 H21A C21 H21C 109.5 H21B C21 H21C 109.5 N20 C22 H22A 109.5 N20 C22 H22B 109.5 H22A C22 H22B 109.5 N20 C22 H22C 109.5 H22A C22 H22C 109.5 H22B C22 H22C 109.5 C31 N30 C32 114.80(9) C31 N30 S1 122.81(8) C32 N30 S1 114.86(8) N30 C31 H31A 109.5 N30 C31 H31B 109.5 H31A C31 H31B 109.5 N30 C31 H31C 109.5 H31A C31 H31C 109.5 H31B C31 H31C 109.5 N30 C32 H32A 109.5 N30 C32 H32B 109.5 H32A C32 H32B 109.5 N30 C32 H32C 109.5 H32A C32 H32C 109.5 H32B C32 H32C 109.5 N3 P1 C1 89.54(6) N1 C1 P1 112.03(9) N1 C1 H1 115.9(10) P1 C1 H1 132.1(10) C1 N1 N2 111.56(10) N3 N2 N1 114.90(10) N2 N3 P1 111.97(8) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance S1 N30 1.6212(10) S1 N20 1.6224(10) S1 N10 1.6943(10) N10 C12 1.4844(14) N10 C11 1.4848(14) C11 H11A 0.9800 C11 H11B 0.9800 C11 H11C 0.9800 C12 H12A 0.9800 C12 H12B 0.9800 C12 H12C 0.9800 N20 C22 1.4717(14) N20 C21 1.4730(14) C21 H21A 0.9800 C21 H21B 0.9800 C21 H21C 0.9800 C22 H22A 0.9800 C22 H22B 0.9800 C22 H22C 0.9800 N30 C31 1.4722(14) N30 C32 1.4743(14) C31 H31A 0.9800 C31 H31B 0.9800 C31 H31C 0.9800 C32 H32A 0.9800 C32 H32B 0.9800 C32 H32C 0.9800 P1 N3 1.6838(11) P1 C1 1.7216(12) C1 N1 1.3400(16) C1 H1 0.940(13) N1 N2 1.3465(15) N2 N3 1.3279(15)