#------------------------------------------------------------------------------ #$Date: 2015-07-09 01:06:54 +0300 (Thu, 09 Jul 2015) $ #$Revision: 141402 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/52/03/1520313.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_1520313 loop_ _publ_author_name 'Ro\&sbach, Jan' 'Harms, Klaus' 'Koert, Ulrich' _publ_section_title ; \a-Crotyl-\a-difluoroboranyloxy-amides: Structure and Reactivity of Isolable Intermediates in Stereospecific \a-Ketol Rearrangements. ; _journal_issue 12 _journal_name_full 'Organic letters' _journal_page_first 3122 _journal_page_last 3125 _journal_paper_doi 10.1021/acs.orglett.5b01427 _journal_volume 17 _journal_year 2015 _chemical_formula_moiety 'C10 H16 B F2 N O4' _chemical_formula_sum 'C10 H16 B F2 N O4' _chemical_formula_weight 263.05 _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 geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _cell_angle_alpha 83.232(2) _cell_angle_beta 83.476(2) _cell_angle_gamma 76.265(2) _cell_formula_units_Z 2 _cell_length_a 7.0022(3) _cell_length_b 7.7079(4) _cell_length_c 12.3657(6) _cell_measurement_reflns_used 6410 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.2551 _cell_measurement_theta_min 2.7325 _cell_volume 641.26(5) _computing_cell_refinement 'BRUKER SAINT' _computing_data_collection 'BRUKER APEX2 2014.9-0' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_molecular_graphics 'DIAMOND (Crystal Impact)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT V2014/1 (Bruker AXS Inc., 2014)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker D8 QUEST area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_unetI/netI 0.0170 _diffrn_reflns_laue_measured_fraction_full 0.999 _diffrn_reflns_laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_number 10712 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.296 _diffrn_reflns_theta_min 2.732 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.120 _exptl_absorpt_correction_T_max 0.99 _exptl_absorpt_correction_T_min 0.96 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 276 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.11 _refine_diff_density_max 0.335 _refine_diff_density_min -0.171 _refine_diff_density_rms 0.037 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 168 _refine_ls_number_reflns 2327 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.063 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0297 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.2528P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.0763 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2121 _reflns_number_total 2327 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ol5b01427_si_002.cif _cod_data_source_block JR2103A_0m _cod_depositor_comments 'Adding full bibliography for 1520305--1520319.cif.' _cod_database_code 1520313 _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 0.971 _shelx_estimated_absorpt_t_max 0.987 _shelx_res_file ; JR2103A_0m.res created by SHELXL-2014/7 TITL JR2103A_0m_a.res in P-1 REM Old TITL JR2103A_0m in P-1 REM SHELXT solution in P-1 REM R1 0.109, Rweak 0.006, Alpha 0.028, Orientation as input REM Formula found by SHELXT: C9 B N O5 F2 CELL 0.71073 7.0022 7.7079 12.3657 83.232 83.476 76.265 ZERR 2.000 0.0003 0.0004 0.0006 0.002 0.002 0.002 LATT 1 SFAC C H B N O F UNIT 20 32 2 2 8 4 TEMP -173.150 SIZE 0.11 0.24 0.25 L.S. 10 BOND $H conf LIST 4 FMAP 2 PLAN 10 acta REM ##### WGHT 0.034300 0.252800 FVAR 1.13853 0.52985 F1 6 0.826661 0.134697 0.157361 11.00000 0.01795 0.01663 = 0.03757 -0.00133 -0.00241 0.00086 O1 5 0.484168 0.226484 0.204831 11.00000 0.01882 0.01097 = 0.01780 -0.00298 0.00012 -0.00319 N1 4 0.494480 0.681165 0.222591 11.00000 0.01658 0.01230 = 0.01970 -0.00163 -0.00039 -0.00179 C1 1 0.163702 0.200369 0.496788 11.00000 0.04075 0.02520 = 0.03179 0.00209 0.00650 -0.00839 AFIX 93 H1A 2 0.097217 0.311976 0.522936 11.00000 -1.20000 H1B 2 0.116642 0.095304 0.521312 11.00000 -1.20000 AFIX 0 B1 3 0.652627 0.246865 0.129327 11.00000 0.01773 0.01216 = 0.02141 -0.00281 -0.00029 -0.00249 F2 6 0.625417 0.234001 0.022032 11.00000 0.02781 0.02553 = 0.01915 -0.00656 0.00237 -0.00737 O2 5 0.049572 0.518752 0.291937 11.00000 0.01879 0.02439 = 0.02579 -0.00397 0.00202 -0.00140 C2 1 0.320565 0.191330 0.426782 11.00000 0.03165 0.01648 = 0.01671 0.00066 -0.00387 -0.00366 AFIX 43 H2 2 0.383150 0.077462 0.402455 11.00000 -1.20000 AFIX 0 O3 5 0.663579 0.442805 0.139138 11.00000 0.01518 0.01337 = 0.02102 -0.00138 0.00048 -0.00235 C3 1 0.408435 0.348145 0.382276 11.00000 0.02436 0.01529 = 0.01481 -0.00143 -0.00230 -0.00280 AFIX 13 H3 2 0.331094 0.457022 0.417154 11.00000 -1.20000 AFIX 0 O4 5 0.336650 0.750190 0.296012 11.00000 0.02165 0.01454 = 0.01753 -0.00233 0.00072 0.00081 C4 1 0.395256 0.382503 0.257281 11.00000 0.01770 0.00996 = 0.01622 -0.00160 -0.00073 -0.00240 C5 1 0.178732 0.449698 0.226886 11.00000 0.01739 0.01230 = 0.01953 0.00223 -0.00011 -0.00571 C6 1 0.144165 0.423266 0.113472 11.00000 0.01737 0.03103 = 0.02013 0.00069 -0.00367 -0.00574 AFIX 137 H6A 2 0.018999 0.502570 0.093735 11.00000 -1.50000 H6B 2 0.138571 0.298180 0.110160 11.00000 -1.50000 H6C 2 0.252265 0.451721 0.062172 11.00000 -1.50000 AFIX 0 C7 1 0.623934 0.312461 0.409735 11.00000 0.03027 0.02573 = 0.02023 0.00142 -0.00857 -0.00521 AFIX 137 H7A 2 0.703776 0.212644 0.370624 11.00000 -1.50000 H7B 2 0.630157 0.281736 0.488644 11.00000 -1.50000 H7C 2 0.675189 0.420262 0.387434 11.00000 -1.50000 AFIX 0 C8 1 0.518979 0.514381 0.204597 11.00000 0.01460 0.01437 = 0.01418 0.00054 -0.00550 -0.00134 C9 1 0.629709 0.796616 0.180502 11.00000 0.02073 0.01471 = 0.03431 -0.00219 -0.00106 -0.00616 PART 1 AFIX 137 H9A 2 0.570697 0.884214 0.122581 21.00000 -1.50000 H9B 2 0.754557 0.723190 0.150816 21.00000 -1.50000 H9C 2 0.654500 0.859817 0.239900 21.00000 -1.50000 AFIX 137 PART 2 H9D 2 0.624733 0.822989 0.101249 -21.00000 -1.50000 H9E 2 0.764370 0.735331 0.196527 -21.00000 -1.50000 H9F 2 0.590650 0.908900 0.215522 -21.00000 -1.50000 AFIX 0 PART 0 C10 1 0.191490 0.886241 0.238970 11.00000 0.02122 0.01544 = 0.02644 -0.00001 -0.00097 0.00255 AFIX 137 H10A 2 0.246074 0.991620 0.214551 11.00000 -1.50000 H10B 2 0.072145 0.920850 0.288457 11.00000 -1.50000 H10C 2 0.158382 0.837980 0.175445 11.00000 -1.50000 AFIX 0 HKLF 4 REM JR2103A_0m_a.res in P-1 REM R1 = 0.0297 for 2121 Fo > 4sig(Fo) and 0.0333 for all 2327 data REM 168 parameters refined using 0 restraints END WGHT 0.0347 0.2533 REM Highest difference peak 0.335, deepest hole -0.171, 1-sigma level 0.037 Q1 1 0.4027 0.3675 0.3223 11.00000 0.05 0.34 Q2 1 0.2913 0.4146 0.2407 11.00000 0.05 0.31 Q3 1 0.4425 0.4594 0.2356 11.00000 0.05 0.29 Q4 1 0.3645 0.2755 0.4007 11.00000 0.05 0.23 Q5 1 0.4411 0.3061 0.2324 11.00000 0.05 0.21 Q6 1 0.5027 0.3353 0.3952 11.00000 0.05 0.20 Q7 1 0.2030 0.2162 0.4232 11.00000 0.05 0.19 Q8 1 0.7222 0.3820 0.4136 11.00000 0.05 0.18 Q9 1 0.5648 0.7390 0.2048 11.00000 0.05 0.18 Q10 1 0.1773 0.4456 0.1682 11.00000 0.05 0.18 ; _shelx_res_checksum 1725 _shelx_hkl_file ; -1 0 0 5409.59 126.674 3 -1 0 0 5681.42 128.220 1 1 0 0 5255.98 126.027 2 1 0 0 5443.94 128.067 1 1 0 0 5069.76 126.616 3 -2 0 0 6.28616 0.86900 1 -2 0 0 5.67418 0.35063 2 2 0 0 6.77295 0.58674 3 2 0 0 5.37682 0.41869 2 2 0 0 4.33661 0.72497 1 -3 0 0 12.5551 0.61152 2 -4 0 0 1000.41 25.5190 1 -4 0 0 1047.83 24.1253 2 -4 0 0 1024.95 24.5917 3 4 0 0 1008.32 25.7136 1 4 0 0 1020.59 24.3196 2 4 0 0 1008.05 24.8020 3 -5 0 0 53.1918 1.70556 2 -5 0 0 53.2483 2.22661 3 -5 0 0 49.8731 3.02159 1 5 0 0 49.2417 2.47519 3 5 0 0 50.3504 3.32344 1 -6 0 0 1093.73 25.6258 2 -6 0 0 1069.96 26.4020 3 -6 0 0 1085.85 27.8699 1 6 0 0 1069.74 26.8710 3 6 0 0 1057.63 28.2958 1 -7 0 0 279.937 9.73757 1 -7 0 0 278.894 7.09999 2 -7 0 0 275.626 8.15190 3 7 0 0 293.595 10.5404 1 7 0 0 272.902 8.68721 3 -8 0 0 3.94782 3.02730 1 -8 0 0 5.93824 1.90327 3 8 0 0 3.68421 2.29768 3 7 -1 0 6.21181 2.82137 1 7 -1 0 3.36759 1.72035 3 -7 1 0 2.62893 2.31695 1 -7 1 0 4.24061 1.36129 3 -7 1 0 4.13966 0.88351 2 6 -1 0 150.825 6.67232 1 6 -1 0 158.338 5.30902 3 6 -1 0 150.273 4.38807 2 -6 1 0 151.960 5.04595 3 -6 1 0 151.290 4.30302 2 -6 1 0 152.489 6.20712 1 5 -1 0 420.480 12.3546 1 5 -1 0 421.549 10.9648 3 5 -1 0 410.051 10.3239 2 -5 1 0 404.601 11.9381 1 -5 1 0 418.413 10.8652 3 -5 1 0 412.808 10.3191 2 4 -1 0 104.672 2.88785 2 4 -1 0 102.276 3.32927 3 -4 1 0 100.474 3.25788 3 -4 1 0 99.5039 4.02361 1 -4 1 0 100.780 2.92990 2 3 -1 0 79.2437 3.29149 1 3 -1 0 84.8443 2.31104 2 3 -1 0 81.0113 2.59070 3 -3 1 0 83.8637 2.39333 2 -3 1 0 84.9313 3.24852 1 -3 1 0 81.4994 2.62556 3 2 -1 0 82.8086 3.01525 1 2 -1 0 87.9145 2.35882 2 2 -1 0 82.0717 2.51631 3 -2 1 0 83.4081 2.95346 1 -2 1 0 88.1728 2.44709 2 -2 1 0 87.7226 2.59197 3 1 -1 0 19.4080 0.83505 3 1 -1 0 19.5938 1.01445 1 1 -1 0 19.6198 0.77532 2 -1 1 0 19.0712 0.79760 2 -1 1 0 19.6659 0.98887 1 -1 1 0 19.7869 0.86354 3 0 -1 0 3077.08 74.6702 3 0 -1 0 3137.17 74.6395 2 0 -1 0 3049.26 74.0134 1 0 1 0 3168.16 74.8526 3 0 1 0 3165.41 74.9208 2 0 1 0 3150.96 74.0339 1 -1 -1 0 1213.39 28.7258 2 -2 -1 0 2061.79 46.9020 1 -2 -1 0 2005.21 47.0998 3 2 1 0 1927.27 46.8990 1 2 1 0 1907.74 46.7404 3 -3 -1 0 323.123 8.12464 2 -3 -1 0 326.564 8.85878 1 -3 -1 0 339.545 8.43537 3 3 1 0 325.170 8.54739 3 3 1 0 324.684 8.95088 1 -4 -1 0 158.842 4.65353 3 -4 -1 0 159.740 5.32476 1 -4 -1 0 159.490 4.23235 2 4 1 0 163.826 4.92865 3 4 1 0 164.433 5.47960 1 -5 -1 0 79.4008 3.88691 1 -5 -1 0 85.8993 3.01955 3 -5 -1 0 85.9533 2.50333 2 5 1 0 91.1673 4.23087 1 5 1 0 91.3320 3.51654 3 -6 -1 0 90.5535 3.38405 3 -6 -1 0 89.5140 4.51923 1 -6 -1 0 89.7895 2.62505 2 6 1 0 88.7162 3.95112 3 -7 -1 0 57.5415 4.43740 1 -7 -1 0 58.6879 2.00565 2 -7 -1 0 52.8821 2.37847 2 -7 -1 0 60.1508 3.00648 3 7 1 0 60.3089 3.77053 3 -8 -1 0 67.5546 5.65438 1 -8 -1 0 66.7654 3.72514 3 7 -2 0 65.8821 5.99315 1 7 -2 0 57.5283 2.57182 2 -7 2 0 55.0245 2.59265 2 -7 2 0 51.2362 4.89151 1 6 -2 0 113.130 5.84921 1 6 -2 0 98.5239 3.32829 2 6 -2 0 106.269 4.16804 3 -6 2 0 102.367 5.33446 1 -6 2 0 108.484 4.27956 3 -6 2 0 108.734 3.58000 2 5 -2 0 7.45011 1.90109 1 5 -2 0 10.2325 1.03559 2 5 -2 0 8.73086 1.14852 3 -5 2 0 11.9222 1.13802 2 -5 2 0 8.46763 1.27897 3 -5 2 0 8.23157 1.68281 1 4 -2 0 1695.62 39.7052 2 4 -2 0 1646.68 41.4578 1 4 -2 0 1660.68 40.1492 3 -4 2 0 1707.60 40.0071 2 -4 2 0 1650.23 41.1400 1 -4 2 0 1707.18 40.3660 3 3 -2 0 142.610 4.99713 1 3 -2 0 145.025 4.23583 3 3 -2 0 150.593 3.98127 2 -3 2 0 148.542 4.40762 3 -3 2 0 144.500 4.18235 2 -3 2 0 147.894 4.90159 1 2 -2 0 626.047 14.8880 2 2 -2 0 603.864 15.5286 1 2 -2 0 608.560 15.0259 3 -2 2 0 615.601 15.1771 3 -2 2 0 608.331 15.4394 1 -2 2 0 618.017 15.0314 2 1 -2 0 1489.30 35.3405 1 1 -2 0 1479.68 35.2372 3 1 -2 0 1518.37 35.1693 2 -1 2 0 1494.81 35.3092 3 -1 2 0 1462.15 35.2165 2 -1 2 0 1443.13 35.2411 1 0 -2 0 2204.14 50.7962 1 0 -2 0 2069.83 50.5469 2 0 -2 0 2184.68 51.1100 3 0 2 0 2125.46 50.6764 1 0 2 0 2114.82 51.1219 3 0 2 0 2143.14 50.6122 2 -1 -2 0 7234.60 169.927 2 -1 -2 0 7049.52 170.619 3 -1 -2 0 7247.10 168.288 1 1 2 0 6972.22 169.338 2 1 2 0 7131.76 168.728 1 -2 -2 0 1470.95 35.0662 2 -3 -2 0 174.125 5.11629 3 -3 -2 0 176.451 5.27002 1 -3 -2 0 177.774 4.93825 2 -4 -2 0 154.875 4.54982 2 -4 -2 0 152.367 5.13777 1 -4 -2 0 159.278 4.49399 2 -4 -2 0 158.679 4.81814 3 -5 -2 0 14.0215 1.38190 2 -5 -2 0 14.2988 1.46340 3 -5 -2 0 12.4578 1.82144 1 -5 -2 0 14.3636 1.17779 2 -6 -2 0 20.5783 1.75957 2 -6 -2 0 26.3264 2.81760 1 -6 -2 0 24.0499 1.94733 3 -6 -2 0 24.9580 1.38182 2 -7 -2 0 57.5935 3.04118 3 -7 -2 0 56.1792 2.62795 2 -7 -2 0 61.2566 4.57246 1 -7 -2 0 60.6857 2.13096 2 -8 -2 0 0.43159 1.13184 2 -8 -2 0 -0.2342 1.51945 3 -8 -2 0 -1.2455 2.87789 1 -8 -2 0 0.11091 0.72190 2 7 -3 0 15.3506 3.98289 1 7 -3 0 13.5758 1.53268 2 7 -3 0 14.4744 2.16635 3 -7 3 0 16.9798 2.58628 3 -7 3 0 19.8737 1.85387 2 -7 3 0 20.4198 3.81524 1 6 -3 0 133.928 4.12168 2 6 -3 0 136.610 4.96153 3 6 -3 0 124.220 6.88696 1 -6 3 0 136.145 5.29295 3 -6 3 0 131.980 6.21917 1 -6 3 0 128.153 4.60391 2 5 -3 0 56.4243 2.71996 3 5 -3 0 48.3367 3.96488 1 5 -3 0 51.9025 2.10385 2 -5 3 0 54.4774 3.02138 3 -5 3 0 52.9311 2.64282 2 -5 3 0 53.5480 3.62047 1 4 -3 0 7.83814 1.07437 3 4 -3 0 8.77633 1.67950 1 4 -3 0 7.87950 0.86433 2 -4 3 0 9.73823 1.64325 1 -4 3 0 8.71276 1.14693 2 -4 3 0 6.84283 1.17879 3 3 -3 0 286.136 7.47178 2 3 -3 0 288.483 7.73833 3 3 -3 0 287.138 8.57817 1 -3 3 0 280.503 7.99542 3 -3 3 0 280.646 8.30202 1 -3 3 0 291.372 7.80751 2 2 -3 0 154.106 4.37133 2 2 -3 0 154.753 4.89820 1 2 -3 0 141.346 4.45077 3 -2 3 0 153.627 4.74075 1 -2 3 0 148.179 4.65831 3 -2 3 0 150.538 4.55258 2 1 -3 0 112.315 3.55396 1 1 -3 0 110.487 3.46784 2 1 -3 0 107.958 3.54012 3 -1 3 0 115.608 3.70831 3 -1 3 0 107.626 3.55464 2 -1 3 0 113.145 3.44117 1 0 -3 0 2359.94 55.5158 1 0 -3 0 2362.51 55.6326 3 0 -3 0 2310.46 55.5107 2 0 3 0 2368.57 56.0740 1 0 3 0 2297.95 55.6484 3 0 3 0 2336.85 55.6108 2 -1 -3 0 979.750 23.1087 1 -1 -3 0 986.227 23.7473 2 -1 -3 0 965.003 23.8558 3 1 3 0 989.588 23.2278 1 1 3 0 947.085 23.7793 2 -2 -3 0 1838.52 43.6918 2 -2 -3 0 1876.68 43.3064 1 -2 -3 0 1765.12 43.8310 3 -3 -3 0 101.702 3.50643 1 -3 -3 0 102.492 3.45002 2 -4 -3 0 3.25753 0.93006 1 -4 -3 0 2.10074 0.76122 2 -4 -3 0 1.80025 0.81082 3 -5 -3 0 114.119 4.58841 1 -5 -3 0 114.810 3.89924 2 -5 -3 0 113.574 4.21566 3 -5 -3 0 118.298 3.99348 2 -6 -3 0 495.431 12.9414 2 -6 -3 0 491.865 12.7151 2 -6 -3 0 498.711 14.0964 1 -6 -3 0 500.978 13.3307 3 -7 -3 0 197.955 5.95613 2 -7 -3 0 169.501 6.94320 3 -7 -3 0 190.992 5.44228 2 -7 -3 0 190.667 7.53870 1 -8 -3 0 30.7441 2.74011 2 -8 -3 0 27.5235 3.06293 3 -8 -3 0 28.1845 1.82218 2 -8 -3 0 22.9715 3.51087 1 6 -4 0 90.0222 4.12165 3 6 -4 0 91.5833 6.72412 1 6 -4 0 88.6429 3.41103 2 -6 4 0 90.3283 4.20875 2 -6 4 0 86.6887 4.87784 3 -6 4 0 90.6653 5.85893 1 5 -4 0 68.9803 3.38802 3 5 -4 0 73.9350 2.84201 2 5 -4 0 66.7627 4.95677 1 -5 4 0 73.4098 3.55854 2 -5 4 0 73.5241 4.52309 1 -5 4 0 72.5267 4.02746 3 4 -4 0 174.875 5.11560 2 4 -4 0 170.440 5.45122 3 4 -4 0 167.504 6.72573 1 -4 4 0 176.720 5.70765 2 -4 4 0 173.952 6.33880 1 -4 4 0 174.519 5.98231 3 3 -4 0 392.799 10.3576 2 3 -4 0 391.721 11.4533 1 3 -4 0 406.354 10.6508 3 -3 4 0 404.095 11.1470 1 -3 4 0 400.578 10.8318 2 -3 4 0 392.006 11.0190 3 2 -4 0 53.9190 2.33045 2 2 -4 0 53.4639 2.72254 1 2 -4 0 52.4054 2.46109 3 -2 4 0 53.8526 2.58574 2 -2 4 0 52.2472 2.65853 3 -2 4 0 50.0700 2.47919 1 1 -4 0 786.346 19.8635 2 1 -4 0 758.649 19.9733 3 1 -4 0 806.849 19.9000 1 -1 4 0 813.741 20.1151 2 -1 4 0 820.997 19.7139 1 -1 4 0 809.388 20.2053 3 0 -4 0 543.031 14.5925 3 0 -4 0 569.351 14.0645 1 0 -4 0 571.672 14.5032 2 0 4 0 585.533 14.6791 2 0 4 0 560.723 14.6940 3 0 4 0 571.592 13.9161 1 -1 -4 0 73.4750 2.24873 1 -1 -4 0 71.7556 3.03112 3 -1 -4 0 71.0798 2.84045 2 1 4 0 70.0894 3.00984 3 1 4 0 72.0661 2.28615 1 1 4 0 69.6469 2.96930 2 -2 -4 0 444.644 10.5517 1 -2 -4 0 436.003 11.5530 3 -2 -4 0 411.289 11.2651 2 2 4 0 412.469 11.3696 2 -3 -4 0 563.386 14.1238 1 -3 -4 0 559.097 14.8613 3 -3 -4 0 563.394 14.5645 2 -4 -4 0 80.2241 3.62878 3 -4 -4 0 86.0431 3.41455 2 -4 -4 0 88.5469 3.50784 1 -4 -4 0 85.6909 3.43925 1 -5 -4 0 460.239 12.7592 3 -5 -4 0 454.371 12.4022 2 -5 -4 0 476.101 12.8723 1 -6 -4 0 34.8964 2.57688 2 -6 -4 0 40.9534 3.37583 1 -6 -4 0 41.0722 2.97555 3 -6 -4 0 35.8863 2.72087 2 -7 -4 0 121.012 5.10138 3 -7 -4 0 122.361 4.80278 2 -7 -4 0 121.022 4.50750 2 -7 -4 0 119.135 5.88972 1 -8 -4 0 32.0614 4.14871 1 -8 -4 0 35.3401 3.25344 2 -8 -4 0 30.8371 2.57815 2 -8 -4 0 33.8652 3.65972 3 5 -5 0 17.1929 1.79475 2 5 -5 0 15.2463 3.30753 1 5 -5 0 16.6300 2.12072 3 -5 5 0 19.5632 3.03226 1 -5 5 0 18.6440 2.32145 2 -5 5 0 18.8649 2.70024 3 4 -5 0 945.314 25.6323 1 4 -5 0 980.710 24.2312 3 4 -5 0 951.893 23.7374 2 -4 5 0 959.370 24.4874 2 -4 5 0 951.856 24.8140 3 -4 5 0 978.907 25.0088 1 3 -5 0 2.91097 1.42076 1 3 -5 0 -0.1472 0.85359 2 3 -5 0 -1.4612 0.90394 3 -3 5 0 1.80436 1.27400 3 -3 5 0 -0.0534 1.23358 2 -3 5 0 -0.9864 1.15696 1 2 -5 0 534.610 14.0099 2 2 -5 0 532.784 14.2345 3 2 -5 0 544.656 14.5087 1 -2 5 0 542.521 14.0908 1 -2 5 0 535.959 14.5900 3 -2 5 0 532.810 14.4142 2 1 -5 0 284.246 8.51606 3 1 -5 0 299.262 8.35796 1 1 -5 0 293.923 8.39734 2 -1 5 0 306.910 8.85942 3 -1 5 0 290.387 8.66266 2 -1 5 0 291.405 8.00291 1 0 -5 0 6.21508 1.14558 3 0 -5 0 6.92728 0.92797 1 0 -5 0 4.38136 0.96230 2 0 5 0 4.29163 1.18643 2 0 5 0 5.14231 0.68720 1 0 5 0 6.27713 1.27955 3 -1 -5 0 7.26168 1.23050 2 -1 -5 0 3.44398 1.16224 3 -1 -5 0 4.60500 0.66640 1 1 5 0 4.86686 0.67620 1 1 5 0 6.47693 1.36764 2 -2 -5 0 2579.58 62.6221 2 -2 -5 0 2649.92 61.8737 1 -2 -5 0 2576.87 62.9048 3 2 5 0 2642.25 62.8608 2 -3 -5 0 637.317 16.9678 2 -3 -5 0 660.422 16.0486 1 -3 -5 0 659.915 17.3523 3 -4 -5 0 128.433 5.28916 3 -4 -5 0 127.352 4.27618 1 -4 -5 0 130.853 4.60460 1 -4 -5 0 133.822 4.83078 2 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37.7693 2.96882 3 0 6 0 32.4304 1.73295 1 0 6 0 30.9013 2.84999 2 -1 -6 0 196.526 6.78294 3 -1 -6 0 194.159 6.51599 2 -1 -6 0 198.669 5.61903 1 1 6 0 195.751 5.58949 1 1 6 0 202.647 6.87940 2 -2 -6 0 334.780 9.91819 2 -2 -6 0 340.211 10.2721 3 -2 -6 0 339.590 8.73492 1 2 6 0 340.741 9.13676 1 2 6 0 339.112 10.1785 2 -3 -6 0 344.007 8.82158 1 -3 -6 0 358.675 10.6114 3 -3 -6 0 331.477 10.0566 2 -4 -6 0 191.742 5.57562 1 -4 -6 0 197.901 6.64420 2 -4 -6 0 198.447 7.23051 3 -4 -6 0 191.860 6.11149 1 -5 -6 0 30.6437 2.21641 1 -5 -6 0 31.3411 2.92002 1 -5 -6 0 33.9887 3.39222 3 -5 -6 0 25.4077 2.97083 2 -5 -6 0 33.4807 3.50174 3 -6 -6 0 163.175 6.33102 1 -6 -6 0 162.107 7.34893 3 -6 -6 0 155.554 5.92608 1 -6 -6 0 179.807 6.36613 2 -6 -6 0 158.205 6.81070 3 -7 -6 0 0.20143 2.03597 2 -7 -6 0 8.12916 2.51232 1 -7 -6 0 11.0941 3.62759 3 -7 -6 0 7.57900 2.37565 1 -7 -6 0 4.15948 2.45165 3 -7 -6 0 3.67743 2.25779 2 3 -7 0 75.9886 4.23297 2 3 -7 0 77.4275 4.66387 3 3 -7 0 82.6403 5.59154 1 -3 7 0 83.6125 5.61707 3 -3 7 0 81.8493 5.28596 2 -3 7 0 80.5481 4.54213 1 2 -7 0 201.820 7.04692 2 2 -7 0 192.480 7.30160 1 2 -7 0 205.619 7.36039 3 -2 7 0 200.132 7.82146 3 -2 7 0 217.729 7.98907 2 -2 7 0 202.284 6.64149 1 1 -7 0 635.227 17.0012 1 1 -7 0 635.609 17.1915 2 1 -7 0 657.298 17.5462 3 -1 7 0 629.994 16.3734 1 -1 7 0 647.566 17.9417 3 -1 7 0 636.379 17.8121 2 0 -7 0 60.7217 3.07058 1 0 -7 0 59.2430 3.86887 3 0 -7 0 50.4261 3.37372 2 0 7 0 65.4971 4.15266 2 0 7 0 58.1850 2.59930 1 0 7 0 59.3203 4.19803 3 -1 -7 0 1.92439 1.50429 3 -1 -7 0 0.09624 0.85828 1 -1 -7 0 0.70262 1.33562 2 1 7 0 -0.4281 0.81430 1 1 7 0 0.64560 1.33029 2 -2 -7 0 167.182 6.23837 2 -2 -7 0 165.934 4.87803 1 -2 -7 0 162.309 6.49450 3 2 7 0 162.126 5.25044 1 2 7 0 166.716 6.52320 2 -3 -7 0 3.42919 0.79376 1 -3 -7 0 5.16401 1.78772 2 -3 -7 0 5.30610 1.96987 3 -4 -7 0 -2.6134 1.90632 3 -4 -7 0 -1.1367 1.23848 1 -4 -7 0 0.86019 0.73115 1 -4 -7 0 0.07940 1.59093 2 -5 -7 0 166.336 6.74788 2 -5 -7 0 174.131 6.19197 1 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62.2759 2.63089 1 -5 -8 0 32.8115 3.47609 2 -5 -8 0 29.8823 3.17658 1 -5 -8 0 32.5814 4.23381 3 -5 -8 0 28.4981 2.14709 1 -1 -9 0 42.0686 3.30235 1 -1 -9 0 28.2912 3.23749 2 -1 -9 0 36.0696 3.99697 3 1 9 0 39.9843 3.20077 1 -2 -9 0 2.84436 1.46117 1 -2 -9 0 0.76686 2.41390 2 -2 -9 0 9.72463 3.01609 3 -3 -9 0 28.7624 4.12521 3 -3 -9 0 21.6567 3.28138 2 -3 -9 0 20.7333 2.10813 1 -3 -9 1 3.49240 2.56665 2 -3 -9 1 3.62714 3.33793 3 -2 -9 1 12.3601 3.35441 3 -2 -9 1 3.92150 2.33278 2 1 9 -1 17.6893 1.79378 1 1 9 -1 12.9535 3.49257 2 -1 -9 1 13.1394 3.22704 3 -1 -9 1 13.9512 1.84835 1 -1 -9 1 17.1095 2.73965 2 -5 -8 1 36.0001 3.62632 2 -5 -8 1 47.7198 5.28602 3 -5 -8 1 47.2139 2.82457 1 -5 -8 1 39.5098 2.01416 1 -5 -8 1 50.0008 4.93342 3 -4 -8 1 3.97249 2.41281 2 -4 -8 1 7.57586 1.21039 1 -4 -8 1 12.3088 1.32554 1 -4 -8 1 10.8663 2.72037 3 -3 -8 1 3.18088 1.83245 2 -3 -8 1 5.24737 1.06575 1 -3 -8 1 4.65328 0.79459 1 -3 -8 1 6.88957 2.69442 3 2 8 -1 75.6750 5.14835 2 -2 -8 1 73.2480 4.37023 2 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4.91694 2.13269 3 -3 -1 13 8.05706 2.12403 1 -3 -1 13 5.21292 1.85511 2 2 1 -13 75.7264 5.22230 3 2 1 -13 63.6080 4.19043 1 2 1 -13 70.0798 3.70506 2 -2 -1 13 66.0199 4.10139 3 -2 -1 13 60.9344 3.87923 2 -2 -1 13 70.6281 4.22328 1 1 1 -13 16.9014 1.89432 2 1 1 -13 19.4135 2.36073 1 1 1 -13 17.6785 2.69206 3 -1 -1 13 16.8407 2.02555 3 -1 -1 13 17.7367 3.05818 1 -1 -1 13 15.8478 2.14947 2 0 1 -13 9.97715 1.77540 1 0 1 -13 12.3073 2.23422 3 0 1 -13 9.27252 1.77288 2 0 -1 13 11.0706 1.92515 2 0 -1 13 10.5718 1.67741 3 0 -1 13 10.4922 2.65775 1 -1 1 -13 20.0252 2.22124 2 -1 1 -13 24.4831 2.64951 1 1 -1 13 20.4148 2.36394 2 1 -1 13 24.3317 2.28635 3 -2 1 -13 76.3365 4.00328 1 -2 1 -13 69.9035 4.07412 2 2 -1 13 82.0265 4.54552 2 2 -1 13 79.9534 3.12869 3 -3 1 -13 0.42889 1.67679 2 -3 1 -13 0.03582 1.76646 1 3 -1 13 3.01908 2.00944 2 3 0 -13 49.6061 4.60065 1 3 0 -13 52.6532 5.01224 3 3 0 -13 50.5795 3.15304 2 -3 0 13 45.4448 4.31518 1 -3 0 13 52.8687 4.13216 3 -3 0 13 48.5251 3.85870 2 2 0 -13 0.67807 1.94036 3 2 0 -13 0.71639 1.77259 1 2 0 -13 1.21958 2.56356 2 -2 0 13 -0.8172 1.68621 1 -2 0 13 0.01093 3.51024 2 -2 0 13 1.74279 1.56092 3 1 0 -13 -1.5478 1.17337 2 1 0 -13 -0.5100 1.67208 3 1 0 -13 -3.6778 1.46061 1 -1 0 13 -0.8564 1.76276 1 -1 0 13 -3.2847 1.51279 2 -1 0 13 -0.1582 1.40844 3 0 0 -13 2.05377 1.42784 1 0 0 -13 -0.1533 1.08496 2 0 0 -13 -0.1678 1.44025 3 0 0 13 1.84615 1.30057 3 0 0 13 -2.3144 1.73721 1 0 0 13 -0.3555 1.45685 2 -1 0 -13 39.8632 2.82090 2 -1 0 -13 38.2774 3.16107 3 -1 0 -13 32.3301 2.83116 1 1 0 13 37.1450 4.11060 1 1 0 13 37.3829 2.70088 3 1 0 13 31.8733 3.01342 2 -2 0 -13 20.8659 2.07816 2 -2 0 -13 23.7165 2.33897 1 2 0 13 29.9871 3.09336 2 2 0 13 26.4906 2.13131 3 -3 0 -13 -2.0357 1.25558 2 -3 0 -13 3.78489 1.75066 1 3 0 13 0.21892 0.89007 3 3 0 13 1.29647 1.73183 2 -4 0 -13 22.7027 2.87560 1 -4 0 -13 28.9924 2.97821 2 4 0 13 21.0350 2.95667 2 3 -1 -13 38.6221 3.70141 3 3 -1 -13 35.8213 3.89302 1 3 -1 -13 37.5347 2.63703 2 -3 1 13 39.7244 4.15272 3 -3 1 13 40.9228 4.22300 1 2 -1 -13 9.32870 1.45880 2 2 -1 -13 7.71872 2.20426 3 2 -1 -13 10.6735 2.38822 1 -2 1 13 11.9144 2.25994 2 -2 1 13 8.29469 2.16049 1 -2 1 13 8.46660 2.06052 3 1 -1 -13 21.9136 2.57983 1 1 -1 -13 21.9086 2.28609 2 1 -1 -13 28.5631 3.20004 3 -1 1 13 22.8310 2.66036 2 -1 1 13 27.7637 3.15337 3 -1 1 13 22.2064 2.63509 1 0 -1 -13 21.3887 2.49776 3 0 -1 -13 21.4249 2.44092 1 0 -1 -13 29.3627 2.41744 2 0 1 13 23.3449 2.50896 2 0 1 13 24.4957 2.79918 1 0 1 13 19.8535 3.34039 3 -1 -1 -13 164.749 5.92129 3 -1 -1 -13 182.760 5.89913 2 -1 -1 -13 170.741 6.25545 1 1 1 13 167.565 5.84608 3 1 1 13 176.726 7.35152 1 1 1 13 174.450 6.80401 2 -2 -1 -13 13.7322 1.92499 1 -2 -1 -13 18.6308 2.05761 2 -2 -1 -13 18.8791 1.85487 3 2 1 13 15.4812 1.79456 3 2 1 13 15.8888 2.59754 2 -3 -1 -13 75.4511 3.06079 3 -3 -1 -13 78.5925 3.82412 2 -3 -1 -13 74.0261 4.29247 1 3 1 13 75.5478 4.84609 2 3 1 13 66.8590 3.03879 3 -4 -1 -13 18.9228 2.80249 1 -4 -1 -13 15.4773 2.13263 2 4 1 13 13.7699 2.63683 2 2 -2 -13 137.546 6.23493 3 2 -2 -13 142.834 6.58373 1 2 -2 -13 139.573 4.82512 2 -2 2 13 145.071 6.52218 1 -2 2 13 146.948 6.24292 3 1 -2 -13 1.45474 1.74950 3 1 -2 -13 -0.8395 1.73726 1 1 -2 -13 1.84250 1.20418 2 -1 2 13 4.78437 2.03128 1 -1 2 13 3.63682 1.72736 3 0 -2 -13 101.701 4.20457 2 0 -2 -13 107.169 4.71755 3 0 -2 -13 98.5460 4.85347 1 0 2 13 103.496 5.58683 1 0 2 13 113.801 5.31136 2 0 2 13 100.315 4.81873 3 -1 -2 -13 12.7730 1.60062 2 -1 -2 -13 14.2825 1.96272 1 -1 -2 -13 15.8132 1.89364 3 1 2 13 15.4336 2.76347 1 1 2 13 14.3113 2.03267 3 1 2 13 11.4728 2.47966 2 -2 -2 -13 171.984 5.58835 3 -2 -2 -13 163.305 6.25141 1 -2 -2 -13 170.694 5.86799 2 2 2 13 164.234 7.59851 1 2 2 13 166.577 7.00354 2 2 2 13 169.636 5.82868 3 -3 -2 -13 9.87583 1.68489 2 -3 -2 -13 13.1509 1.46565 3 -3 -2 -13 14.2197 2.17469 1 3 2 13 13.0988 1.68653 3 3 2 13 14.3504 2.60016 2 -4 -2 -13 32.1750 1.72557 3 -4 -2 -13 31.2299 3.12970 2 -4 -2 -13 34.4569 3.31706 1 4 2 13 30.9848 3.49899 2 2 -3 -13 4.32316 1.57859 2 2 -3 -13 3.02237 2.41962 1 2 -3 -13 6.66633 2.31433 3 -2 3 13 7.25076 2.77220 1 -2 3 13 6.31526 2.67965 3 1 -3 -13 71.8573 4.35236 3 1 -3 -13 73.0272 4.80990 1 1 -3 -13 67.2425 3.43097 2 -1 3 13 71.9969 4.69924 3 -1 3 13 69.0656 4.77788 1 0 -3 -13 36.9502 3.52535 1 0 -3 -13 39.3552 2.88707 2 0 -3 -13 41.2015 3.25132 3 0 3 13 35.0373 3.63428 1 0 3 13 41.3920 3.98373 3 -1 -3 -13 62.5259 3.41152 2 -1 -3 -13 62.2315 3.47259 3 -1 -3 -13 58.7362 3.72770 1 1 3 13 56.5711 4.01120 3 1 3 13 54.9070 4.76483 1 -2 -3 -13 0.95401 1.28059 3 -2 -3 -13 0.82156 1.38940 1 -2 -3 -13 -0.4680 1.39552 2 2 3 13 -0.0454 2.11351 1 2 3 13 1.93772 1.72379 3 -3 -3 -13 24.7815 2.84597 1 -3 -3 -13 24.3584 2.26513 3 -3 -3 -13 21.7476 2.32703 2 3 3 13 23.3000 2.40379 3 3 3 13 28.6799 3.53069 2 -4 -3 -13 31.9419 2.12022 3 -4 -3 -13 36.5240 3.21054 2 -4 -3 -13 25.7557 2.90789 1 4 3 13 32.7416 3.99115 2 4 3 13 30.3527 2.87114 3 1 -4 -13 81.7051 5.24046 1 1 -4 -13 80.5848 3.97870 2 1 -4 -13 81.6973 4.69742 3 -1 4 13 81.4870 5.62351 1 -1 4 13 87.8606 5.81850 3 0 -4 -13 114.851 4.76884 2 0 -4 -13 103.500 5.62658 1 0 -4 -13 120.843 5.29034 3 0 4 13 111.311 6.22544 1 0 4 13 108.543 5.95262 3 -1 -4 -13 83.5695 4.14458 2 -1 -4 -13 84.3219 4.69130 1 -1 -4 -13 79.1222 4.19382 3 1 4 13 86.3510 5.06210 3 1 4 13 82.8720 5.39264 1 -2 -4 -13 1.54825 1.49426 3 -2 -4 -13 2.00329 1.76078 1 -2 -4 -13 2.60539 1.62259 2 2 4 13 0.27781 2.64756 1 2 4 13 -0.5616 1.95471 3 -3 -4 -13 18.5831 1.94417 3 -3 -4 -13 18.1197 2.40053 2 -3 -4 -13 15.9010 2.45992 1 3 4 13 18.7854 2.67024 3 3 4 13 15.6300 3.18129 1 -4 -4 -13 4.22125 1.80191 2 -4 -4 -13 1.30474 2.07891 1 -4 -4 -13 3.02097 1.33979 3 4 4 13 4.71300 1.87769 3 -1 -5 -13 6.15482 2.10160 1 -1 -5 -13 8.08223 2.17218 3 -1 -5 -13 14.1123 2.40885 2 1 5 13 15.6736 3.12281 1 1 5 13 11.7141 2.93243 3 -2 -5 -13 21.7122 2.63562 2 -2 -5 -13 26.2657 2.67019 3 -2 -5 -13 24.9015 2.90409 1 2 5 13 24.1312 3.95396 1 2 5 13 20.4125 3.25851 3 -3 -5 -13 6.32325 2.35082 2 -3 -5 -13 5.14233 1.99159 1 -3 -5 -13 5.18836 1.81494 3 3 5 13 4.86053 2.57510 3 3 5 13 4.82734 3.27798 1 0 2 -14 0.35245 1.91817 2 0 2 -14 2.04888 2.03695 1 0 -2 14 2.27695 1.63908 3 0 -2 14 4.99953 2.20796 2 1 1 -14 5.21625 1.95765 1 1 1 -14 2.82596 1.81562 2 1 1 -14 7.54056 2.77045 3 -1 -1 14 4.19358 1.94542 3 -1 -1 14 1.40801 1.98521 2 -1 -1 14 7.77738 2.40688 1 0 1 -14 69.6989 4.14752 1 0 1 -14 65.2577 4.03816 2 0 1 -14 81.0476 5.05379 3 0 -1 14 75.3147 3.89929 3 0 -1 14 69.3588 4.41377 2 -1 1 -14 38.6051 3.56884 2 -1 1 -14 28.1653 3.13800 1 1 -1 14 43.2920 2.98585 3 1 -1 14 34.7752 3.16149 2 -2 1 -14 -0.2637 1.86361 2 -2 1 -14 -0.4924 1.52386 1 2 -1 14 0.52663 2.18632 2 2 -1 14 -1.1277 1.22916 3 1 0 -14 1.41105 1.94530 1 1 0 -14 0.00332 2.23891 3 1 0 -14 3.99522 1.54660 2 -1 0 14 3.37932 1.73984 3 -1 0 14 4.20393 2.35773 1 -1 0 14 6.95344 2.16598 2 0 0 -14 75.9299 3.91896 2 0 0 -14 69.4171 4.62475 3 0 0 -14 66.6526 4.23186 1 0 0 14 74.7198 4.10131 3 0 0 14 72.9805 5.09510 1 0 0 14 69.4961 4.63017 2 -1 0 -14 42.3516 3.71212 3 -1 0 -14 40.2348 3.19594 2 -1 0 -14 42.3181 3.38214 1 1 0 14 38.4133 4.11977 2 1 0 14 41.2624 2.98448 3 -2 0 -14 27.2025 2.66290 1 -2 0 -14 22.4688 2.27856 2 2 0 14 20.6100 2.79940 2 2 0 14 29.4113 2.65307 3 -3 0 -14 3.17703 1.73617 2 -3 0 -14 -1.5867 1.80535 1 3 0 14 -1.3737 2.28428 2 3 0 14 -1.5963 1.02650 3 1 -1 -14 76.1879 3.77102 2 1 -1 -14 67.4424 4.85877 3 1 -1 -14 70.6534 4.81635 1 -1 1 14 84.9074 5.17616 1 -1 1 14 77.6817 4.76437 3 -1 1 14 77.1117 5.04865 2 0 -1 -14 6.23367 1.53078 2 0 -1 -14 8.80828 2.08418 3 0 -1 -14 9.34668 2.06216 1 0 1 14 12.4589 2.06896 3 0 1 14 5.31357 2.52224 1 0 1 14 10.6326 2.46915 2 -1 -1 -14 2.42980 1.68698 1 -1 -1 -14 2.46211 1.36691 2 -1 -1 -14 -0.1497 1.58745 3 1 1 14 -0.5555 2.38648 1 1 1 14 -1.1097 2.12034 2 1 1 14 2.88202 1.67415 3 -2 -1 -14 27.0005 3.08472 3 -2 -1 -14 29.5423 3.32313 1 -2 -1 -14 36.6278 3.03105 2 2 1 14 36.3366 3.65626 2 2 1 14 35.0383 2.97458 3 -3 -1 -14 33.9028 3.62843 1 -3 -1 -14 37.3982 3.31262 2 3 1 14 35.0220 3.88184 2 3 1 14 31.9322 2.55866 3 1 -2 -14 79.7270 5.16607 1 1 -2 -14 82.1411 3.87107 2 1 -2 -14 78.8114 4.94621 3 -1 2 14 79.9667 5.43537 1 -1 2 14 83.7045 5.04533 3 0 -2 -14 13.5195 2.36035 3 0 -2 -14 10.4272 2.08506 1 0 -2 -14 12.8783 1.87280 2 0 2 14 7.90617 2.16012 3 0 2 14 14.0285 2.60545 2 0 2 14 10.6144 2.70991 1 -1 -2 -14 17.7337 2.41338 3 -1 -2 -14 19.6356 2.19159 2 -1 -2 -14 19.7679 2.40384 1 1 2 14 16.9461 3.29056 1 1 2 14 21.9146 2.66100 3 1 2 14 19.4995 3.07544 2 -2 -2 -14 -1.0968 1.57161 2 -2 -2 -14 1.40422 1.59184 3 -2 -2 -14 -0.4404 1.71778 1 2 2 14 1.31312 1.72465 3 2 2 14 2.33202 2.97283 1 2 2 14 1.23059 2.51252 2 -3 -2 -14 7.43724 1.50215 3 -3 -2 -14 8.27727 1.99473 2 -3 -2 -14 1.54314 1.98025 1 3 2 14 3.88072 2.90054 2 3 2 14 9.48893 1.82185 3 0 -3 -14 138.208 5.83931 3 0 -3 -14 135.533 5.19486 2 0 -3 -14 129.463 6.26966 1 0 3 14 132.980 7.09762 1 0 3 14 139.072 6.54808 3 -1 -3 -14 23.4555 2.46833 3 -1 -3 -14 24.6874 2.95622 1 -1 -3 -14 30.6441 3.06065 2 1 3 14 26.4085 2.97478 3 1 3 14 19.1048 3.31923 1 -2 -3 -14 2.20287 1.54003 2 -2 -3 -14 -0.2378 1.83837 1 -2 -3 -14 2.41527 1.57579 3 2 3 14 4.88009 2.10647 3 2 3 14 4.41749 2.89890 1 -3 -3 -14 6.37074 1.94865 2 -3 -3 -14 5.99629 1.65697 3 -3 -3 -14 2.41684 1.92689 1 3 3 14 4.27837 1.96021 3 -1 -4 -14 73.9142 4.27852 3 -1 -4 -14 71.4442 4.24363 2 -1 -4 -14 59.1882 4.70843 1 1 4 14 64.0122 5.82686 1 1 4 14 78.8003 5.43962 3 -2 -4 -14 1.90715 1.71614 3 -2 -4 -14 0.81273 1.86505 2 -2 -4 -14 -0.7201 2.13035 1 2 4 14 1.55472 3.09926 1 2 4 14 -4.6279 2.22994 3 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/4' _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.9690 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 0.71092 7.007 7.712 12.376 83.272 83.505 76.313 ) ; _shelx_hkl_checksum 92718 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 F1 F 0.82666(10) 0.13470(9) 0.15736(6) 0.02496(19) Uani 1 1 d . . . . . O1 O 0.48417(12) 0.22648(10) 0.20483(6) 0.01590(19) Uani 1 1 d . . . . . N1 N 0.49448(14) 0.68117(13) 0.22259(8) 0.0165(2) Uani 1 1 d . . . . . C1 C 0.1637(2) 0.2004(2) 0.49679(12) 0.0336(3) Uani 1 1 d . . . . . H1A H 0.0972 0.3120 0.5229 0.040 Uiso 1 1 calc R U . . . H1B H 0.1166 0.0953 0.5213 0.040 Uiso 1 1 calc R U . . . B1 B 0.6526(2) 0.24686(18) 0.12933(11) 0.0173(3) Uani 1 1 d . . . . . F2 F 0.62542(11) 0.23400(10) 0.02203(6) 0.02393(19) Uani 1 1 d . . . . . O2 O 0.04957(13) 0.51875(12) 0.29194(7) 0.0238(2) Uani 1 1 d . . . . . C2 C 0.3206(2) 0.19133(17) 0.42678(10) 0.0220(3) Uani 1 1 d . . . . . H2 H 0.3831 0.0775 0.4025 0.026 Uiso 1 1 calc R U . . . O3 O 0.66358(12) 0.44280(11) 0.13914(7) 0.01686(19) Uani 1 1 d . . . . . C3 C 0.40844(18) 0.34815(16) 0.38228(9) 0.0184(3) Uani 1 1 d . . . . . H3 H 0.3311 0.4570 0.4172 0.022 Uiso 1 1 calc R U . . . O4 O 0.33665(12) 0.75019(11) 0.29601(7) 0.0189(2) Uani 1 1 d . . . . . C4 C 0.39526(17) 0.38250(15) 0.25728(9) 0.0148(2) Uani 1 1 d . . . . . C5 C 0.17873(17) 0.44970(15) 0.22689(10) 0.0164(3) Uani 1 1 d . . . . . C6 C 0.14417(18) 0.42327(19) 0.11347(10) 0.0229(3) Uani 1 1 d . . . . . H6A H 0.0190 0.5026 0.0937 0.034 Uiso 1 1 calc R U . . . H6B H 0.1386 0.2982 0.1102 0.034 Uiso 1 1 calc R U . . . H6C H 0.2523 0.4517 0.0622 0.034 Uiso 1 1 calc R U . . . C7 C 0.6239(2) 0.31246(18) 0.40974(11) 0.0254(3) Uani 1 1 d . . . . . H7A H 0.7038 0.2126 0.3706 0.038 Uiso 1 1 calc R U . . . H7B H 0.6302 0.2817 0.4886 0.038 Uiso 1 1 calc R U . . . H7C H 0.6752 0.4203 0.3874 0.038 Uiso 1 1 calc R U . . . C8 C 0.51898(17) 0.51438(15) 0.20460(9) 0.0145(2) Uani 1 1 d . . . . . C9 C 0.62971(19) 0.79662(17) 0.18050(11) 0.0230(3) Uani 1 1 d . . . . . H9A H 0.5707 0.8842 0.1226 0.035 Uiso 0.53(4) 1 calc R U P A 1 H9B H 0.7546 0.7232 0.1508 0.035 Uiso 0.53(4) 1 calc R U P A 1 H9C H 0.6545 0.8598 0.2399 0.035 Uiso 0.53(4) 1 calc R U P A 1 H9D H 0.6247 0.8230 0.1012 0.035 Uiso 0.47(4) 1 calc R U P A 2 H9E H 0.7644 0.7353 0.1965 0.035 Uiso 0.47(4) 1 calc R U P A 2 H9F H 0.5906 0.9089 0.2155 0.035 Uiso 0.47(4) 1 calc R U P A 2 C10 C 0.19149(19) 0.88624(17) 0.23897(11) 0.0224(3) Uani 1 1 d . . . . . H10A H 0.2461 0.9916 0.2146 0.034 Uiso 1 1 calc R U . . . H10B H 0.0721 0.9208 0.2885 0.034 Uiso 1 1 calc R U . . . H10C H 0.1584 0.8380 0.1754 0.034 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F1 0.0179(4) 0.0166(4) 0.0376(4) -0.0013(3) -0.0024(3) 0.0009(3) O1 0.0188(4) 0.0110(4) 0.0178(4) -0.0030(3) 0.0001(3) -0.0032(3) N1 0.0166(5) 0.0123(5) 0.0197(5) -0.0016(4) -0.0004(4) -0.0018(4) C1 0.0408(8) 0.0252(7) 0.0318(8) 0.0021(6) 0.0065(6) -0.0084(6) B1 0.0177(7) 0.0122(6) 0.0214(7) -0.0028(5) -0.0003(5) -0.0025(5) F2 0.0278(4) 0.0255(4) 0.0192(4) -0.0066(3) 0.0024(3) -0.0074(3) O2 0.0188(4) 0.0244(5) 0.0258(5) -0.0040(4) 0.0020(4) -0.0014(4) C2 0.0317(7) 0.0165(6) 0.0167(6) 0.0007(5) -0.0039(5) -0.0037(5) O3 0.0152(4) 0.0134(4) 0.0210(4) -0.0014(3) 0.0005(3) -0.0023(3) C3 0.0244(6) 0.0153(6) 0.0148(6) -0.0014(4) -0.0023(5) -0.0028(5) O4 0.0217(4) 0.0145(4) 0.0175(4) -0.0023(3) 0.0007(3) 0.0008(3) C4 0.0177(6) 0.0100(5) 0.0162(6) -0.0016(4) -0.0007(4) -0.0024(4) C5 0.0174(6) 0.0123(6) 0.0195(6) 0.0022(4) -0.0001(5) -0.0057(5) C6 0.0174(6) 0.0310(7) 0.0201(6) 0.0007(5) -0.0037(5) -0.0057(5) C7 0.0303(7) 0.0257(7) 0.0202(6) 0.0014(5) -0.0086(5) -0.0052(6) C8 0.0146(5) 0.0144(6) 0.0142(5) 0.0005(4) -0.0055(4) -0.0013(4) C9 0.0207(6) 0.0147(6) 0.0343(7) -0.0022(5) -0.0011(5) -0.0062(5) C10 0.0212(6) 0.0154(6) 0.0264(7) 0.0000(5) -0.0010(5) 0.0026(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' B B 0.0013 0.0007 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 C4 O1 B1 113.23(9) C8 N1 O4 117.09(10) C8 N1 C9 125.30(10) O4 N1 C9 117.33(9) C2 C1 H1A 120.0 C2 C1 H1B 120.0 H1A C1 H1B 120.0 F1 B1 F2 110.30(10) F1 B1 O1 113.81(10) F2 B1 O1 113.40(10) F1 B1 O3 108.67(10) F2 B1 O3 107.62(10) O1 B1 O3 102.48(9) C1 C2 C3 124.75(12) C1 C2 H2 117.6 C3 C2 H2 117.6 C8 O3 B1 109.00(9) C2 C3 C7 110.17(10) C2 C3 C4 109.76(10) C7 C3 C4 110.78(10) C2 C3 H3 108.7 C7 C3 H3 108.7 C4 C3 H3 108.7 N1 O4 C10 109.92(8) O1 C4 C8 102.11(9) O1 C4 C3 111.18(9) C8 C4 C3 111.76(9) O1 C4 C5 109.01(9) C8 C4 C5 109.92(9) C3 C4 C5 112.37(9) O2 C5 C6 123.29(11) O2 C5 C4 121.03(11) C6 C5 C4 115.68(10) C5 C6 H6A 109.5 C5 C6 H6B 109.5 H6A C6 H6B 109.5 C5 C6 H6C 109.5 H6A C6 H6C 109.5 H6B C6 H6C 109.5 C3 C7 H7A 109.5 C3 C7 H7B 109.5 H7A C7 H7B 109.5 C3 C7 H7C 109.5 H7A C7 H7C 109.5 H7B C7 H7C 109.5 O3 C8 N1 119.85(11) O3 C8 C4 113.00(10) N1 C8 C4 127.11(10) N1 C9 H9A 109.5 N1 C9 H9B 109.5 H9A C9 H9B 109.5 N1 C9 H9C 109.5 H9A C9 H9C 109.5 H9B C9 H9C 109.5 N1 C9 H9D 109.5 N1 C9 H9E 109.5 H9D C9 H9E 109.5 N1 C9 H9F 109.5 H9D C9 H9F 109.5 H9E C9 H9F 109.5 O4 C10 H10A 109.5 O4 C10 H10B 109.5 H10A C10 H10B 109.5 O4 C10 H10C 109.5 H10A C10 H10C 109.5 H10B C10 H10C 109.5 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance F1 B1 1.3703(15) O1 C4 1.4110(13) O1 B1 1.4460(16) N1 C8 1.2983(15) N1 O4 1.3912(12) N1 C9 1.4623(16) C1 C2 1.312(2) C1 H1A 0.9500 C1 H1B 0.9500 B1 F2 1.3798(16) B1 O3 1.5498(15) O2 C5 1.2064(15) C2 C3 1.5040(17) C2 H2 0.9500 O3 C8 1.2800(14) C3 C7 1.5379(18) C3 C4 1.5466(16) C3 H3 1.0000 O4 C10 1.4535(15) C4 C8 1.5304(16) C4 C5 1.5553(16) C5 C6 1.4949(17) C6 H6A 0.9800 C6 H6B 0.9800 C6 H6C 0.9800 C7 H7A 0.9800 C7 H7B 0.9800 C7 H7C 0.9800 C9 H9A 0.9800 C9 H9B 0.9800 C9 H9C 0.9800 C9 H9D 0.9800 C9 H9E 0.9800 C9 H9F 0.9800 C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 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 C4 O1 B1 F1 117.14(11) C4 O1 B1 F2 -115.69(11) C4 O1 B1 O3 0.01(12) F1 B1 O3 C8 -123.52(10) F2 B1 O3 C8 117.03(10) O1 B1 O3 C8 -2.77(12) C1 C2 C3 C7 121.29(15) C1 C2 C3 C4 -116.46(14) C8 N1 O4 C10 -113.44(11) C9 N1 O4 C10 72.39(12) B1 O1 C4 C8 2.23(12) B1 O1 C4 C3 -117.09(11) B1 O1 C4 C5 118.50(10) C2 C3 C4 O1 -54.99(13) C7 C3 C4 O1 66.90(12) C2 C3 C4 C8 -168.37(10) C7 C3 C4 C8 -46.48(13) C2 C3 C4 C5 67.50(12) C7 C3 C4 C5 -170.61(10) O1 C4 C5 O2 145.26(11) C8 C4 C5 O2 -103.59(12) C3 C4 C5 O2 21.56(15) O1 C4 C5 C6 -34.93(13) C8 C4 C5 C6 76.22(12) C3 C4 C5 C6 -158.64(10) B1 O3 C8 N1 -177.75(10) B1 O3 C8 C4 4.39(12) O4 N1 C8 O3 -178.90(9) C9 N1 C8 O3 -5.25(17) O4 N1 C8 C4 -1.38(16) C9 N1 C8 C4 172.27(11) O1 C4 C8 O3 -4.24(12) C3 C4 C8 O3 114.67(11) C5 C4 C8 O3 -119.84(10) O1 C4 C8 N1 178.09(11) C3 C4 C8 N1 -63.00(15) C5 C4 C8 N1 62.49(15)