#------------------------------------------------------------------------------ #$Date: 2015-07-09 01:06:54 +0300 (Thu, 09 Jul 2015) $ #$Revision: 141402 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/52/03/1520314.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_1520314 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 H17 N O4' _chemical_formula_sum 'C10 H17 N O4' _chemical_formula_weight 215.24 _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 106.191(4) _cell_angle_beta 106.585(4) _cell_angle_gamma 104.538(4) _cell_formula_units_Z 2 _cell_length_a 7.8792(10) _cell_length_b 8.1476(11) _cell_length_c 10.2749(13) _cell_measurement_reflns_used 3821 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.1454 _cell_measurement_theta_min 2.7894 _cell_volume 566.58(13) _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 'SHELXS-97 (Sheldrick, 2008)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 7.9 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.994 _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 0.0575 _diffrn_reflns_av_unetI/netI 0.0408 _diffrn_reflns_laue_measured_fraction_full 0.997 _diffrn_reflns_laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 10007 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.331 _diffrn_reflns_theta_min 2.234 _diffrn_source 'microfocus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.097 _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.5910 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/4 (Bruker AXS Inc.)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 232 _exptl_crystal_size_max 0.330 _exptl_crystal_size_mid 0.287 _exptl_crystal_size_min 0.064 _refine_diff_density_max 0.347 _refine_diff_density_min -0.243 _refine_diff_density_rms 0.060 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 144 _refine_ls_number_reflns 2064 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0492 _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^)+(0.0793P)^2^+0.1719P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1247 _refine_ls_wR_factor_ref 0.1358 _reflns_Friedel_coverage 0.000 _reflns_number_gt 1661 _reflns_number_total 2064 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ol5b01427_si_002.cif _cod_data_source_block JR2095A_0m _cod_depositor_comments 'Adding full bibliography for 1520305--1520319.cif.' _cod_database_code 1520314 _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_res_file ; JR2095A_0m.res created by SHELXL-2014/7 TITL JR2095A_0m in P-1 CELL 0.71073 7.8792 8.1476 10.2749 106.191 106.585 104.538 ZERR 2.00 0.0010 0.0011 0.0013 0.004 0.004 0.004 LATT 1 SFAC C H O N UNIT 20 34 8 2 LIST 4 ! automatically inserted. Change 6 to 4 for CHECKCIF!! TEMP -173.150 ACTA L.S. 12 FMAP 2 PLAN -3 0 0.00 HTAB HTAB O1 O2 EQIV $1 -x+1, -y+1, -z+1 HTAB O1 O2_$1 BOND $H CONF REM ##### WGHT 0.079300 0.171900 FVAR 1.21696 O1 3 0.330561 0.669773 0.444853 11.00000 0.03005 0.01885 = 0.01374 0.00274 0.00044 0.01137 H1 2 0.397017 0.612362 0.481522 11.00000 0.03776 N1 4 0.446434 0.861342 0.269247 11.00000 0.02144 0.01576 = 0.02660 0.00811 0.00338 0.00647 C1 1 -0.042495 0.121003 0.169033 11.00000 0.03174 0.01866 = 0.03589 0.00907 0.00877 0.00645 AFIX 93 H1A 2 -0.096979 0.099073 0.067720 11.00000 -1.20000 H1B 2 -0.042679 0.021178 0.199618 11.00000 -1.20000 AFIX 0 O2 3 0.466119 0.426311 0.327693 11.00000 0.02771 0.01903 = 0.02229 0.00723 0.00252 0.01183 C2 1 0.033353 0.289934 0.267163 11.00000 0.02865 0.02218 = 0.02559 0.01037 0.01060 0.00861 AFIX 43 H2 2 0.086351 0.306063 0.367325 11.00000 -1.20000 AFIX 0 O3 3 0.130665 0.758466 0.151468 11.00000 0.02607 0.01938 = 0.02325 0.00756 -0.00053 0.00793 C3 1 0.042650 0.459234 0.233122 11.00000 0.02277 0.01455 = 0.01908 0.00374 0.00409 0.00456 AFIX 13 H3 2 -0.014736 0.422069 0.124310 11.00000 -1.20000 AFIX 0 O4 3 0.596653 0.800065 0.311051 11.00000 0.02063 0.01504 = 0.02754 0.00209 0.00155 0.00676 C4 1 0.253752 0.586256 0.290105 11.00000 0.02172 0.01521 = 0.01271 0.00296 0.00079 0.00615 C5 1 0.363151 0.466583 0.239259 11.00000 0.01936 0.01085 = 0.02103 0.00387 0.00315 0.00216 C6 1 0.328791 0.397198 0.079975 11.00000 0.02520 0.01998 = 0.02014 0.00344 0.00539 0.00782 AFIX 137 H6A 2 0.193113 0.328016 0.022630 11.00000 -1.50000 H6B 2 0.400651 0.317150 0.061295 11.00000 -1.50000 H6C 2 0.370038 0.500851 0.051369 11.00000 -1.50000 AFIX 0 REM ##### REM ##### REM ##### REM ##### C7 1 -0.071801 0.556551 0.301859 11.00000 0.02794 0.02467 = 0.02940 0.00736 0.01030 0.00924 AFIX 137 H7A 2 -0.071789 0.662530 0.274458 11.00000 -1.50000 H7B 2 -0.014161 0.597734 0.408866 11.00000 -1.50000 H7C 2 -0.202604 0.471588 0.266186 11.00000 -1.50000 AFIX 0 C8 1 0.269099 0.740170 0.228631 11.00000 0.02303 0.01180 = 0.01590 0.00134 0.00304 0.00710 C9 1 0.482048 0.998283 0.205150 11.00000 0.03410 0.01819 = 0.03355 0.01251 0.00882 0.00620 AFIX 137 H9A 2 0.380760 1.048986 0.194220 11.00000 -1.50000 H9B 2 0.485108 0.941392 0.108712 11.00000 -1.50000 H9C 2 0.604272 1.096742 0.269329 11.00000 -1.50000 AFIX 0 C10 1 0.725160 0.914698 0.460202 11.00000 0.02238 0.02133 = 0.03056 0.00158 -0.00298 0.00541 AFIX 137 H10A 2 0.833020 0.874501 0.486452 11.00000 -1.50000 H10B 2 0.658525 0.905132 0.526579 11.00000 -1.50000 H10C 2 0.771103 1.042218 0.468747 11.00000 -1.50000 REM ##### AFIX 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM JR2095A_0m in P-1 REM R1 = 0.0492 for 1661 Fo > 4sig(Fo) and 0.0649 for all 2064 data REM 144 parameters refined using 0 restraints END WGHT 0.0793 0.1719 REM Instructions for potential hydrogen bonds HTAB O1 O2 HTAB O1 O2_$1 EQIV $2 -x, -y+1, -z HTAB C3 O3_$2 HTAB C6 O3_$2 HTAB C10 O1 REM Highest difference peak 0.347, deepest hole -0.243, 1-sigma level 0.060 Q1 1 0.3243 0.5427 0.2620 11.00000 0.05 0.35 Q2 1 0.2316 0.6664 0.4819 11.00000 0.05 0.33 Q3 1 0.6861 0.8067 0.2559 11.00000 0.05 0.31 ; _shelx_res_checksum 56828 _shelx_hkl_file ; -1 0 0 533.265 27.6034 2 -1 0 0 495.520 27.6126 1 1 0 0 499.434 27.5998 2 1 0 0 474.188 27.6035 1 1 0 0 421.877 27.6514 2 -2 0 0 981.829 53.1258 2 -2 0 0 887.407 53.0745 2 -2 0 0 970.459 53.1569 1 2 0 0 884.138 53.3421 2 2 0 0 955.168 53.1533 1 2 0 0 936.229 53.1311 2 -3 0 0 646.321 34.3263 2 -3 0 0 615.978 34.3713 1 -3 0 0 573.837 34.2400 2 3 0 0 596.922 34.3414 1 3 0 0 573.855 34.3889 2 3 0 0 595.817 34.3262 2 -4 0 0 33.9107 2.76774 2 -4 0 0 32.9028 3.22923 1 -4 0 0 31.3650 2.53563 2 4 0 0 29.4502 3.32619 2 4 0 0 28.4914 3.21129 1 4 0 0 29.2194 3.09129 2 -5 0 0 82.8185 5.68174 1 -5 0 0 70.6739 5.06179 2 -5 0 0 71.4578 4.80264 2 5 0 0 63.4814 6.29180 2 5 0 0 66.5397 5.55516 1 5 0 0 67.7984 5.38551 2 -6 0 0 12.9169 2.97486 1 -6 0 0 4.83762 2.19523 2 -6 0 0 0.22822 2.04608 2 6 0 0 5.39942 3.23492 1 6 0 0 3.93202 2.98979 2 6 0 0 4.97149 4.05287 2 -7 0 0 5.83221 4.09917 1 -7 0 0 3.93623 2.91068 2 -7 0 0 -3.3602 3.13474 2 7 0 0 2.48513 4.29870 2 7 0 0 0.66923 4.53181 1 7 0 0 -1.3656 6.63743 2 -8 0 0 -13.695 5.66844 1 -8 0 0 -0.2548 3.78356 2 -8 0 0 -2.8590 3.98719 2 8 0 0 3.20475 5.90537 2 8 0 0 -5.1066 6.27419 1 8 0 0 5.30047 9.26204 2 8 -1 0 6.60617 4.74629 1 8 -1 0 1.57215 7.39986 2 8 -1 0 15.9442 6.15426 2 -8 1 0 1.63353 4.60626 1 -8 1 0 11.2128 3.82420 2 -8 1 0 12.2117 3.81875 2 7 -1 0 84.4996 8.63085 2 7 -1 0 86.1482 8.30856 2 7 -1 0 91.6175 7.79665 1 -7 1 0 101.148 7.79661 1 -7 1 0 90.0048 7.08768 2 -7 1 0 102.790 6.90439 2 6 -1 0 70.3512 5.81412 1 6 -1 0 63.1964 6.12316 2 6 -1 0 64.6462 6.10026 2 -6 1 0 67.0614 5.05799 2 -6 1 0 65.5693 5.50251 2 -6 1 0 78.0824 5.71695 1 5 -1 0 56.0331 4.71843 2 5 -1 0 56.2925 4.58349 1 5 -1 0 58.0434 4.75152 2 -5 1 0 65.5181 4.50088 1 -5 1 0 57.2800 4.32226 2 -5 1 0 57.5252 4.25669 2 4 -1 0 0.36942 1.24791 1 4 -1 0 -1.1354 1.60877 2 4 -1 0 3.74347 1.33338 2 -4 1 0 1.78235 1.11617 1 -4 1 0 3.23958 1.39554 2 -4 1 0 2.99081 1.14905 2 3 -1 0 75.4652 4.91984 2 3 -1 0 68.3332 4.53055 1 -3 1 0 77.8169 4.56977 1 -3 1 0 73.3698 4.62922 2 -3 1 0 76.8736 4.74235 2 2 -1 0 79.3436 4.99479 2 2 -1 0 79.2935 5.26692 2 -2 1 0 87.2735 5.12867 2 1 -1 0 951.777 53.4395 2 1 -1 0 919.118 53.5786 2 -1 1 0 956.410 53.5518 2 0 -1 0 1587.48 90.8652 1 0 -1 0 1521.30 91.0678 2 0 -1 0 1515.45 90.8890 2 0 1 0 1583.76 90.8583 1 0 1 0 1833.40 91.1390 2 0 1 0 1591.27 90.9140 2 -1 -1 0 1.31142 1.12014 1 -1 -1 0 2.85230 0.90311 2 1 1 0 2.41434 1.02310 2 1 1 0 1.64563 1.50698 2 1 1 0 1.78269 1.12476 1 -2 -1 0 275.137 17.0902 1 -2 -1 0 306.461 17.0298 2 -2 -1 0 298.571 17.0692 2 2 1 0 306.292 17.0449 2 2 1 0 279.311 17.0964 1 -3 -1 0 1248.12 64.5713 2 -3 -1 0 1091.50 64.4311 2 -3 -1 0 1138.80 64.6346 1 3 1 0 1124.47 64.4949 2 3 1 0 1072.10 64.5849 1 3 1 0 1121.32 64.8457 2 -4 -1 0 30.1057 2.91511 2 -4 -1 0 32.5559 3.77506 1 -4 -1 0 24.7042 2.64340 2 4 1 0 28.8112 4.07826 2 4 1 0 28.5032 3.01548 2 4 1 0 28.3620 3.97276 1 -5 -1 0 3.99986 2.73553 1 -5 -1 0 0.86454 2.29675 2 -5 -1 0 1.53432 1.73145 2 5 1 0 0.72936 2.95862 1 5 1 0 0.55186 4.08041 2 5 1 0 -0.9061 2.23222 2 -6 -1 0 227.326 14.2373 1 -6 -1 0 215.210 13.4403 2 -6 -1 0 216.434 13.0606 2 6 1 0 206.496 13.7431 2 6 1 0 202.253 14.2455 1 -7 -1 0 34.5103 4.52292 2 -7 -1 0 40.5658 5.19453 2 -7 -1 0 47.2158 6.21517 1 7 1 0 40.4566 6.38869 1 7 1 0 28.4894 5.78755 2 7 1 0 19.7446 8.41623 2 -8 -1 0 11.7701 4.89744 2 -8 -1 0 7.46017 4.55213 2 -8 -1 0 -9.2039 7.23353 1 8 1 0 3.07966 7.61536 2 8 1 0 -26.403 12.1480 2 8 1 0 -5.4300 8.37062 1 8 -2 0 14.0158 6.25394 2 8 -2 0 4.32415 6.64652 2 -8 2 0 13.5986 3.58334 2 -8 2 0 18.8527 4.21961 2 7 -2 0 857.613 46.3475 2 7 -2 0 761.308 45.5589 2 -7 2 0 738.767 45.1110 2 6 -2 0 6.46198 2.84766 2 6 -2 0 -4.7611 3.43288 2 -6 2 0 5.29613 1.98690 2 5 -2 0 364.450 22.4014 2 5 -2 0 354.174 22.2940 2 -5 2 0 380.901 21.9643 2 -5 2 0 404.692 22.0086 2 4 -2 0 394.046 23.9644 2 4 -2 0 424.497 24.4095 2 -4 2 0 427.211 24.0917 2 3 -2 0 1822.05 111.362 2 3 -2 0 1939.51 111.084 2 -3 2 0 2115.68 111.256 2 2 -2 0 4.66962 2.06054 2 -2 2 0 4.63904 1.64604 2 -2 2 0 3.43075 1.25221 2 1 -2 0 61.7789 4.25098 2 1 -2 0 66.7471 4.15822 1 1 -2 0 72.3378 5.40106 2 -1 2 0 63.4809 4.15145 1 -1 2 0 62.9863 4.82167 2 -1 2 0 58.9603 4.33834 2 0 -2 0 98.4992 6.50716 2 0 -2 0 105.831 7.25224 2 0 -2 0 102.699 6.47334 1 0 2 0 105.851 6.50884 1 0 2 0 118.772 7.36060 2 0 2 0 102.049 6.57253 2 -1 -2 0 421.403 24.3907 2 -1 -2 0 408.037 24.4127 1 1 2 0 386.418 24.3764 1 1 2 0 443.236 24.4886 2 1 2 0 452.820 24.9597 2 -2 -2 0 893.888 48.5133 2 -2 -2 0 808.393 48.5426 1 2 2 0 844.875 48.9879 2 2 2 0 881.480 48.5506 2 2 2 0 806.631 48.5239 1 -3 -2 0 870.035 52.3713 1 -3 -2 0 938.648 52.2711 2 -3 -2 0 863.194 52.2599 2 3 2 0 910.480 52.2878 2 3 2 0 901.218 52.4128 1 3 2 0 1004.05 54.7186 2 -4 -2 0 157.327 9.66837 2 -4 -2 0 152.566 9.65360 2 -4 -2 0 148.679 10.0506 1 4 2 0 135.283 11.3172 2 4 2 0 143.198 9.69008 2 4 2 0 161.142 10.4211 1 -5 -2 0 20.7282 2.98816 2 -5 -2 0 28.5217 4.10121 1 -5 -2 0 24.4099 3.01558 2 5 2 0 14.3133 6.11891 2 5 2 0 22.5869 3.43956 2 5 2 0 17.7292 4.32725 1 -6 -2 0 21.2916 5.41617 1 -6 -2 0 24.1724 3.56001 2 -6 -2 0 21.5777 3.36917 2 6 2 0 12.1242 6.49907 1 6 2 0 20.8450 4.41103 2 6 2 0 8.32915 8.02098 2 -7 -2 0 5.10532 3.69725 2 -7 -2 0 13.1952 6.64915 1 -7 -2 0 1.64966 4.42282 2 7 2 0 -5.8405 5.45519 2 7 2 0 10.3053 6.95752 1 7 2 0 -0.4001 11.0562 2 9 -3 0 68.5373 11.6728 2 9 -3 0 29.8971 8.67981 2 -9 3 0 29.6714 5.04831 2 -9 3 0 42.5258 6.85115 2 8 -3 0 20.5289 7.67399 2 8 -3 0 -3.0775 5.60449 2 -8 3 0 15.4821 4.84248 2 -8 3 0 14.0308 3.77281 2 7 -3 0 -9.1851 4.11161 2 7 -3 0 -13.739 5.73894 2 -7 3 0 -2.4437 3.13990 2 6 -3 0 -1.6364 2.43690 2 6 -3 0 4.90791 4.30529 2 -6 3 0 -1.6439 1.97358 2 -6 3 0 1.35203 2.52609 2 5 -3 0 438.163 26.8800 2 5 -3 0 464.796 26.1494 2 -5 3 0 444.314 26.2145 2 4 -3 0 530.219 32.2668 2 4 -3 0 531.437 31.5271 2 -4 3 0 577.269 31.7650 2 3 -3 0 36.0978 4.11063 2 3 -3 0 33.8173 3.01291 2 -3 3 0 32.4141 3.71450 2 -3 3 0 37.4605 3.66088 2 2 -3 0 172.257 11.1189 2 2 -3 0 161.401 9.73986 1 2 -3 0 174.664 10.0638 2 -2 3 0 158.870 10.5018 2 -2 3 0 158.091 9.66257 1 -2 3 0 158.648 10.1361 2 1 -3 0 633.428 34.8311 1 1 -3 0 618.692 35.6638 2 1 -3 0 574.055 34.9386 2 -1 3 0 621.465 35.5670 2 -1 3 0 588.464 35.0392 2 -1 3 0 607.179 34.7752 1 0 -3 0 128.273 7.76429 1 0 -3 0 107.287 7.64207 2 0 -3 0 121.159 8.77834 2 0 3 0 131.405 8.95255 2 0 3 0 122.553 7.72184 1 0 3 0 117.706 7.89119 2 -1 -3 0 535.281 31.5300 2 -1 -3 0 530.690 30.8717 2 -1 -3 0 486.676 30.8245 1 1 3 0 515.216 30.8632 1 1 3 0 587.902 31.8529 2 1 3 0 542.431 30.9936 2 -2 -3 0 294.023 16.5517 2 -2 -3 0 272.613 16.6470 1 2 3 0 279.455 16.7202 2 2 3 0 262.508 17.3924 2 2 3 0 266.640 16.6256 1 -3 -3 0 5.82732 2.09648 2 -3 -3 0 4.70354 2.92441 2 -3 -3 0 3.52429 2.24978 1 3 3 0 9.48005 2.77298 1 3 3 0 -1.2730 4.48561 2 3 3 0 3.16839 2.67606 2 -4 -3 0 0.23126 2.67373 2 -4 -3 0 0.50299 2.93146 2 -4 -3 0 4.16835 3.15850 1 4 3 0 2.03728 3.50151 1 4 3 0 5.02259 2.99575 2 4 3 0 11.3102 6.72027 2 -5 -3 0 13.9429 3.24239 2 -5 -3 0 15.1056 3.61800 2 5 3 0 12.4391 5.39358 1 5 3 0 11.8576 4.08960 2 5 3 0 8.07241 8.31864 2 -6 -3 0 252.837 17.2741 1 -6 -3 0 243.864 15.7857 2 -6 -3 0 231.367 15.3708 2 6 3 0 257.914 17.6149 1 6 3 0 232.497 16.2778 2 9 -4 0 1.02470 11.8514 2 -9 4 0 12.4304 5.08555 2 -9 4 0 14.4125 6.27944 2 8 -4 0 220.921 19.8025 2 8 -4 0 270.852 16.9044 2 -8 4 0 272.327 16.9383 2 -8 4 0 251.315 16.1551 2 7 -4 0 63.9070 6.01500 2 7 -4 0 59.8248 8.78327 2 -7 4 0 53.4862 6.32178 2 -7 4 0 49.6636 5.59702 2 6 -4 0 25.5960 3.06282 2 6 -4 0 27.8241 6.38990 2 -6 4 0 9.96503 3.00586 2 -6 4 0 23.7354 3.74555 2 5 -4 0 11.7113 2.44108 2 5 -4 0 15.9273 4.69923 2 -5 4 0 11.2102 3.05123 2 4 -4 0 103.389 9.71996 2 4 -4 0 133.220 8.36421 2 -4 4 0 133.012 8.79290 2 -4 4 0 141.389 9.04266 2 3 -4 0 1030.76 68.1468 2 3 -4 0 1177.11 67.0219 1 3 -4 0 1166.40 67.4019 2 -3 4 0 1172.47 66.9046 1 -3 4 0 1274.87 67.9634 2 -3 4 0 1249.35 67.6170 2 2 -4 0 625.620 35.9381 1 2 -4 0 707.239 37.4765 2 2 -4 0 617.699 36.2166 2 -2 4 0 616.565 36.8187 2 -2 4 0 574.086 36.2749 2 -2 4 0 617.309 35.8175 1 1 -4 0 7.21033 4.12462 2 1 -4 0 5.52880 1.77450 2 1 -4 0 6.40903 1.89655 1 -1 4 0 6.55502 3.27626 2 -1 4 0 4.43041 1.92133 1 -1 4 0 6.60213 2.52456 2 0 -4 0 11.2957 4.16402 2 0 -4 0 4.81166 1.79532 2 0 -4 0 7.82312 1.96930 1 0 4 0 7.35037 2.06091 1 0 4 0 9.19562 2.30310 2 0 4 0 4.56154 3.26774 2 -1 -4 0 430.519 25.6016 2 -1 -4 0 433.071 26.5910 2 -1 -4 0 416.129 25.5787 1 1 4 0 416.156 25.5359 1 1 4 0 430.193 25.8130 2 1 4 0 485.847 26.9662 2 -2 -4 0 153.975 11.0450 1 -2 -4 0 189.056 11.1355 2 2 4 0 184.283 11.6465 2 2 4 0 162.470 13.1691 2 2 4 0 166.783 11.5003 1 -3 -4 0 102.262 8.95388 2 -3 -4 0 108.426 7.99227 2 -3 -4 0 104.561 8.36013 1 3 4 0 101.531 10.9173 2 3 4 0 109.706 8.65778 1 3 4 0 117.790 8.80503 2 -4 -4 0 0.71605 3.32813 2 -4 -4 0 -1.3151 4.03931 2 -4 -4 0 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2 1 -3 10 134.843 12.3780 1 1 -3 10 135.213 8.96244 2 2 -3 10 76.0689 8.78958 1 3 -3 10 12.6405 9.91802 1 7 2 -10 63.9836 9.78644 1 7 2 -10 50.9869 14.6781 2 7 2 -10 53.8828 11.3595 2 -7 -2 10 46.8893 8.14370 2 -7 -2 10 76.7623 8.98037 1 -7 -2 10 69.6205 7.77809 2 6 2 -10 38.2054 8.62852 1 6 2 -10 41.9323 11.1011 2 6 2 -10 42.1236 8.80392 2 -6 -2 10 34.9057 6.58883 1 -6 -2 10 40.1981 5.78020 2 -6 -2 10 42.1005 6.83241 2 5 2 -10 107.806 13.5003 2 5 2 -10 90.7789 11.5478 2 5 2 -10 118.060 11.2903 1 -5 -2 10 98.4639 10.6139 1 -5 -2 10 114.872 9.81024 2 -5 -2 10 117.357 9.16175 2 4 2 -10 10.3003 5.58532 2 4 2 -10 7.08934 5.46642 1 4 2 -10 19.4806 6.56190 2 -4 -2 10 4.67828 4.07011 1 -4 -2 10 11.3597 4.04700 2 -4 -2 10 13.2068 4.34861 2 3 2 -10 35.7713 6.17718 1 3 2 -10 25.2380 5.60324 2 3 2 -10 19.0672 6.45345 2 -3 -2 10 40.3299 5.03875 2 -3 -2 10 34.1036 4.91898 2 -3 -2 10 24.5734 5.04546 1 2 2 -10 30.0324 5.79923 2 2 2 -10 11.5275 4.81080 2 -2 -2 10 18.9235 4.47951 1 -2 -2 10 17.8093 4.06824 2 -2 -2 10 17.5677 2.94778 2 -1 -2 10 8.51913 4.53200 1 -1 -2 10 6.55749 2.34085 2 -1 -2 10 0.37178 3.65090 2 0 -2 10 29.7156 3.83757 2 0 -2 10 20.3702 5.84770 1 0 -2 10 29.0294 4.17158 2 1 -2 10 -0.2227 2.83246 2 1 -2 10 -2.8778 5.97765 1 1 -2 10 -0.4044 2.23122 2 2 -2 10 0.75243 6.43322 1 2 -2 10 15.5145 8.77041 1 7 1 -10 33.5816 9.47834 1 7 1 -10 16.1181 11.4118 2 7 1 -10 27.4980 11.2848 2 -7 -1 10 21.3112 6.75974 1 -7 -1 10 21.7118 6.02996 2 -7 -1 10 24.9883 7.02352 2 6 1 -10 66.6666 8.65178 1 6 1 -10 74.7329 10.7877 2 6 1 -10 74.0441 11.3406 2 -6 -1 10 68.3951 8.03601 2 -6 -1 10 85.9151 9.30696 2 -6 -1 10 78.8825 10.3879 1 5 1 -10 28.2781 6.54196 1 5 1 -10 6.69143 7.66140 2 -5 -1 10 24.5074 4.35050 2 -5 -1 10 22.9444 4.63708 2 -5 -1 10 6.60367 5.02064 1 4 1 -10 10.6559 6.01631 2 4 1 -10 4.92171 5.57841 2 -4 -1 10 -3.4202 3.96391 2 -4 -1 10 3.34872 4.66283 1 -4 -1 10 1.27585 3.19109 2 3 1 -10 282.635 20.5170 2 3 1 -10 309.146 20.4056 2 -3 -1 10 313.916 20.2510 1 -3 -1 10 347.150 19.3280 2 -3 -1 10 338.186 19.8444 2 2 1 -10 97.8442 9.31162 2 2 1 -10 90.3271 9.17982 2 -2 -1 10 85.4426 8.84606 1 -2 -1 10 92.8255 7.77176 2 -2 -1 10 98.7714 6.76384 2 -1 -1 10 144.983 8.99852 2 -1 -1 10 117.952 11.3745 1 -1 -1 10 146.506 9.72895 2 0 -1 10 3.92722 3.26022 2 0 -1 10 -12.483 5.18352 1 0 -1 10 2.70941 2.63712 2 1 -1 10 19.9278 7.28111 1 2 -1 10 -8.7254 8.53883 1 2 -1 10 22.3777 9.83764 1 7 0 -10 -4.5863 9.91875 2 7 0 -10 9.43489 10.8760 2 -7 0 10 1.54820 6.23792 2 -7 0 10 7.06041 5.18792 2 -7 0 10 -5.2463 6.19799 1 6 0 -10 31.0252 9.37320 2 6 0 -10 34.9694 9.47330 2 -6 0 10 41.2870 6.51359 1 -6 0 10 40.6488 5.52140 2 -6 0 10 45.5802 6.43952 2 5 0 -10 24.7889 6.97724 2 5 0 -10 -1.2084 10.6659 2 -5 0 10 11.7274 5.56246 1 -5 0 10 18.2318 4.68845 2 -5 0 10 20.3340 4.18557 2 4 0 -10 36.9587 7.56971 2 4 0 -10 36.8874 6.33999 2 -4 0 10 38.9295 5.83282 1 -4 0 10 37.0526 5.39226 2 -4 0 10 53.0708 5.49590 2 3 0 -10 39.9033 7.65726 2 3 0 -10 45.1783 6.15620 2 -3 0 10 40.3698 5.21246 2 -3 0 10 43.1125 5.76878 1 -3 0 10 51.5666 5.05090 2 2 0 -10 12.3637 6.74284 2 2 0 -10 23.5569 4.97396 2 -2 0 10 7.22620 3.26479 2 -2 0 10 17.8842 4.84134 1 -2 0 10 18.9934 4.31371 2 -1 0 10 -3.4351 3.95250 2 -1 0 10 3.36644 2.88192 2 -1 0 10 2.87149 5.05553 1 0 0 10 38.4490 4.45856 2 0 0 10 33.9216 4.39745 2 0 0 10 40.0647 7.84614 1 0 0 10 29.8030 6.89157 1 1 0 10 1.96520 7.35632 1 1 0 10 11.3208 8.75057 1 7 -1 -10 31.0167 12.8864 2 7 -1 -10 8.41204 9.70778 2 -7 1 10 26.6308 7.74419 1 -7 1 10 19.9018 6.06444 2 -7 1 10 22.7577 7.60350 2 6 -1 -10 14.0472 8.46484 2 6 -1 -10 22.8155 11.1965 2 -6 1 10 21.5606 5.93202 2 -6 1 10 25.0752 5.24811 2 -6 1 10 19.6815 6.63633 1 5 -1 -10 11.3308 6.48355 2 5 -1 -10 23.6512 9.45226 2 -5 1 10 15.4709 5.33456 2 -5 1 10 4.20024 5.35619 1 -5 1 10 8.04625 4.64008 2 4 -1 -10 -9.2806 8.57167 2 4 -1 -10 3.61240 5.37134 2 -4 1 10 -1.7329 3.69748 2 -4 1 10 9.14913 4.88652 2 -4 1 10 -8.3550 5.17511 1 3 -1 -10 57.5313 9.45866 2 3 -1 -10 45.9678 6.21015 2 -3 1 10 53.0307 6.62294 2 -3 1 10 54.3833 6.59606 1 -3 1 10 55.4572 6.00704 2 2 -1 -10 3.34811 7.13740 2 2 -1 -10 6.15805 5.17279 2 -2 1 10 10.6442 3.62616 2 -2 1 10 -1.2024 4.72510 2 -2 1 10 -6.5830 5.23362 1 -1 1 10 12.0076 4.85833 2 -1 1 10 19.4262 6.27820 1 -1 1 10 15.0080 4.30552 2 -1 1 10 14.0147 7.23371 1 0 1 10 32.3394 5.09453 2 0 1 10 18.4896 5.23812 2 0 1 10 19.8446 7.58886 1 0 1 10 31.0341 8.58837 1 6 -2 -10 7.79170 12.5146 2 6 -2 -10 14.0319 8.29418 2 -6 2 10 21.7928 6.05265 2 -6 2 10 21.4959 7.26086 1 -6 2 10 20.1218 6.49594 2 5 -2 -10 -2.1391 6.74520 2 5 -2 -10 18.2023 10.6202 2 -5 2 10 17.3851 5.10394 2 -5 2 10 6.59384 6.19795 2 -5 2 10 3.93563 6.13796 1 4 -2 -10 4.37576 11.0097 2 4 -2 -10 5.26573 5.34953 2 -4 2 10 6.79714 4.79171 2 -4 2 10 16.8817 6.30997 2 -4 2 10 1.23198 5.75837 1 3 -2 -10 23.1623 5.52883 2 3 -2 -10 24.2907 10.8791 2 -3 2 10 16.6716 6.34875 1 -3 2 10 24.8090 5.89820 2 2 -2 -10 9.96232 10.3675 2 2 -2 -10 10.3707 5.43981 2 -2 2 10 12.0363 6.08299 1 -2 2 10 13.7880 4.86271 2 -2 2 10 8.48272 6.71843 2 -2 2 10 9.63044 7.59162 1 -1 2 10 11.7569 8.57298 1 -1 2 10 9.06188 6.13900 2 -1 2 10 10.9057 5.42004 2 -1 2 10 14.4624 7.15152 1 5 -3 -10 -9.0366 7.14840 2 5 -3 -10 -3.8410 14.4504 2 -5 3 10 0.56518 7.43438 2 -5 3 10 -14.851 7.28965 1 4 -3 -10 66.5529 14.7461 2 4 -3 -10 45.7783 6.61435 2 -4 3 10 44.9487 7.28735 2 -4 3 10 63.1409 10.0364 1 -4 3 10 60.9230 8.25793 1 -4 3 10 39.3091 8.69241 2 3 -3 -10 -5.0063 5.49658 2 3 -3 -10 -18.996 12.1440 2 -3 3 10 8.31216 8.43165 1 -3 3 10 -3.8279 6.97415 1 -3 3 10 -5.7640 7.06788 2 -3 3 10 3.09792 6.36011 2 3 6 -11 5.72701 7.31082 2 3 6 -11 7.01889 12.5051 2 3 6 -11 -5.3556 8.72059 1 -3 -6 11 1.38798 8.61613 2 -3 -6 11 -7.6729 6.95823 2 -3 -6 11 3.87581 6.37954 1 2 6 -11 59.7846 9.64245 1 2 6 -11 69.0079 10.9951 2 2 6 -11 56.2656 8.01195 2 -2 -6 11 59.2827 7.54237 1 -2 -6 11 85.5818 10.4874 2 -2 -6 11 55.4687 9.41469 2 1 6 -11 8.26881 6.09527 2 1 6 -11 -7.0287 8.89824 2 1 6 -11 3.30780 7.93198 1 -1 -6 11 3.19951 6.91540 2 -1 -6 11 -3.8053 6.16229 1 -1 -6 11 1.15739 6.73598 2 0 6 -11 60.9623 9.12106 1 0 6 -11 68.1767 9.66663 2 0 6 -11 60.4779 7.82989 2 0 -6 11 79.8998 10.1926 2 0 -6 11 62.1223 8.42413 2 0 -6 11 88.0585 11.3943 1 4 5 -11 -0.6105 7.98793 1 4 5 -11 -7.3914 12.2795 2 -4 -5 11 0.46964 6.82436 2 -4 -5 11 6.72225 7.44402 2 -4 -5 11 6.31486 5.80250 1 3 5 -11 7.56178 7.30453 1 3 5 -11 9.89934 10.4789 2 3 5 -11 9.84593 6.73549 2 -3 -5 11 15.8660 6.72974 2 -3 -5 11 8.80704 6.96352 2 -3 -5 11 8.09284 5.58695 1 2 5 -11 31.6454 9.63959 2 2 5 -11 32.5520 6.36969 2 2 5 -11 24.1115 7.84125 1 -2 -5 11 30.1572 7.07283 2 -2 -5 11 41.8966 6.88669 2 -2 -5 11 43.3333 6.29546 1 1 5 -11 1.33312 7.78983 2 1 5 -11 9.78819 4.94055 2 1 5 -11 3.03045 6.97843 1 -1 -5 11 5.38513 5.58083 2 -1 -5 11 3.37839 5.76212 1 -1 -5 11 12.2015 5.35679 2 0 -5 11 114.337 10.3976 2 0 -5 11 95.7987 11.6819 1 0 -5 11 126.275 11.2596 2 1 -5 11 53.8850 6.47604 2 1 -5 11 42.7173 7.81055 1 1 -5 11 41.5241 6.53571 2 5 4 -11 61.7037 9.45163 1 5 4 -11 33.5003 13.0178 2 5 4 -11 49.3107 10.2687 2 -5 -4 11 74.2370 9.83939 1 -5 -4 11 65.6047 8.00040 2 -5 -4 11 52.7028 8.42058 2 4 4 -11 0.49154 6.95599 1 4 4 -11 0.48059 6.62462 2 4 4 -11 22.6135 10.2390 2 -4 -4 11 2.43425 5.45878 2 -4 -4 11 -6.9160 5.20372 1 -4 -4 11 0.27291 5.90950 2 3 4 -11 39.8642 9.30687 2 3 4 -11 47.4520 6.74424 2 3 4 -11 44.1882 7.31413 1 -3 -4 11 31.7939 6.01308 2 -3 -4 11 37.3403 6.01308 2 -3 -4 11 40.6315 5.96314 1 2 4 -11 25.4459 7.59603 2 2 4 -11 -1.3041 6.10195 1 2 4 -11 0.97389 5.07055 2 -2 -4 11 3.93107 4.51501 2 -2 -4 11 4.53799 5.31763 2 -2 -4 11 3.50837 5.24311 1 1 4 -11 35.1327 7.07584 2 1 4 -11 31.0577 5.25651 2 -1 -4 11 54.9554 6.45054 2 -1 -4 11 41.9227 6.12820 1 -1 -4 11 45.5709 6.40070 2 0 -4 11 4.35769 4.24452 2 0 -4 11 5.62408 5.10515 2 0 -4 11 19.6083 6.19726 1 1 -4 11 21.7314 4.30729 2 1 -4 11 13.8738 7.57386 1 1 -4 11 16.8966 5.00658 2 6 3 -11 15.0071 10.7382 2 6 3 -11 5.47401 12.5373 2 6 3 -11 6.98647 9.01287 1 -6 -3 11 8.25883 7.18892 1 -6 -3 11 10.5864 7.13613 2 -6 -3 11 22.3108 6.82125 2 5 3 -11 222.278 17.8312 1 5 3 -11 199.042 20.1222 2 -5 -3 11 219.147 15.9560 2 -5 -3 11 237.368 15.6970 2 -5 -3 11 198.964 15.9525 1 4 3 -11 29.0998 7.42351 2 4 3 -11 41.9196 9.52224 2 4 3 -11 36.1291 7.47805 1 -4 -3 11 48.8902 5.64413 2 -4 -3 11 29.8927 5.87276 1 -4 -3 11 27.4813 6.07616 2 3 3 -11 166.389 13.5747 2 3 3 -11 182.485 14.6639 1 3 3 -11 186.288 16.1096 2 -3 -3 11 158.755 12.6645 1 -3 -3 11 196.040 13.8205 2 -3 -3 11 194.065 12.6197 2 2 3 -11 9.26180 7.09381 2 2 3 -11 15.2414 5.42245 2 -2 -3 11 11.9500 5.13483 1 -2 -3 11 25.7647 5.40195 2 -2 -3 11 20.2524 3.78269 2 -1 -3 11 13.6245 5.98917 1 -1 -3 11 12.5578 5.15689 2 -1 -3 11 8.72853 3.60571 2 0 -3 11 23.9944 3.75938 2 0 -3 11 22.8370 6.73062 1 0 -3 11 17.8647 4.80077 2 1 -3 11 15.1885 7.35715 1 1 -3 11 9.95663 4.42937 2 1 -3 11 24.5252 3.36365 2 6 2 -11 70.7886 10.4988 1 6 2 -11 54.6911 12.5116 2 6 2 -11 67.9271 12.0922 2 -6 -2 11 56.8789 8.62520 2 -6 -2 11 78.6334 8.86677 2 -6 -2 11 84.5547 11.7385 1 5 2 -11 -6.6540 7.01006 1 5 2 -11 3.13145 8.51331 2 5 2 -11 13.0644 10.4024 2 -5 -2 11 4.37010 5.19052 2 -5 -2 11 14.3278 5.45086 2 -5 -2 11 -5.1262 6.42961 1 4 2 -11 14.9278 6.16195 1 4 2 -11 13.9208 6.49995 2 4 2 -11 20.5469 7.52948 2 -4 -2 11 13.6257 4.66718 2 -4 -2 11 0.58338 5.16265 1 -4 -2 11 11.5793 4.69046 2 3 2 -11 -0.8414 5.99743 2 3 2 -11 -4.1043 6.96117 2 -3 -2 11 -1.5107 5.03414 2 -3 -2 11 3.90166 3.81328 2 -3 -2 11 0.39471 4.49684 1 2 2 -11 44.4871 6.50624 2 2 2 -11 49.1552 7.22326 2 -2 -2 11 25.8435 5.86334 1 -2 -2 11 49.1247 4.93121 2 -2 -2 11 37.6002 6.12293 2 -1 -2 11 6.53426 5.39746 1 -1 -2 11 11.6279 3.06422 2 -1 -2 11 4.23155 4.34461 2 0 -2 11 2.64818 2.79848 2 0 -2 11 8.85466 6.82244 1 0 -2 11 11.7803 4.52445 2 1 -2 11 -8.2047 7.32808 1 6 1 -11 10.0149 10.5345 2 6 1 -11 22.7133 8.80418 1 6 1 -11 8.85320 9.91358 2 -6 -1 11 17.6053 6.59887 2 -6 -1 11 8.55769 6.93585 1 -6 -1 11 7.76391 5.52387 2 5 1 -11 -1.9621 8.49912 2 5 1 -11 8.36315 7.87619 2 -5 -1 11 -12.111 5.67723 1 -5 -1 11 10.5049 6.18244 2 -5 -1 11 7.68706 4.69315 2 4 1 -11 7.70949 7.50185 2 4 1 -11 -6.7831 7.39670 2 -4 -1 11 5.84432 4.98316 2 -4 -1 11 -6.2071 5.71026 1 -4 -1 11 3.20772 3.90594 2 3 1 -11 93.4306 10.5826 2 3 1 -11 66.2305 9.27289 2 -3 -1 11 74.5442 6.67029 2 -3 -1 11 75.2350 8.52782 2 -3 -1 11 66.9205 9.15883 1 2 1 -11 18.0323 6.20043 2 2 1 -11 14.8416 6.96175 2 -2 -1 11 0.08195 5.25212 1 -2 -1 11 12.6001 3.30667 2 -2 -1 11 10.1497 4.71232 2 -1 -1 11 -2.1232 6.06005 1 -1 -1 11 15.3459 3.38979 2 -1 -1 11 7.88474 4.43199 2 0 -1 11 5.64931 6.99229 1 0 -1 11 -3.5600 4.03266 2 0 -1 11 -0.0129 3.45975 2 6 0 -11 26.1639 10.2043 2 -6 0 11 6.19732 5.25358 2 -6 0 11 24.9941 6.51829 2 -6 0 11 19.6662 7.14608 1 5 0 -11 12.3452 9.30977 2 5 0 -11 1.99502 7.82821 2 -5 0 11 2.40532 5.19495 2 -5 0 11 -6.6761 6.69149 1 -5 0 11 3.10022 4.43977 2 4 0 -11 3.67190 6.64078 2 4 0 -11 0.25437 9.21593 2 -4 0 11 4.31385 4.35417 2 -4 0 11 13.0438 5.73217 1 -4 0 11 4.59716 6.68348 2 3 0 -11 29.1513 8.62559 2 3 0 -11 22.9482 6.66405 2 -3 0 11 5.29807 5.49551 2 -3 0 11 4.96935 3.92410 2 -3 0 11 9.92847 5.10420 1 -2 0 11 -2.5512 5.96811 1 -2 0 11 -0.8153 5.03781 2 -2 0 11 4.04230 3.83675 2 -1 0 11 32.9030 7.51425 1 -1 0 11 35.6710 5.40024 2 5 -1 -11 7.49925 7.96528 2 5 -1 -11 -10.640 10.4630 2 -5 1 11 2.20293 6.39496 2 -5 1 11 3.95787 5.33950 2 -5 1 11 1.39463 6.61683 1 4 -1 -11 147.405 13.8065 2 4 -1 -11 161.812 18.4725 2 -4 1 11 143.866 14.0644 1 -4 1 11 173.124 13.5956 2 -4 1 11 168.826 12.0100 2 3 -1 -11 18.0860 7.62251 2 3 -1 -11 -2.1606 10.4875 2 -3 1 11 10.9883 6.16359 1 -3 1 11 11.9967 4.65758 2 -3 1 11 8.57770 6.25402 2 -2 1 11 81.1205 10.6111 2 -2 1 11 110.118 12.4238 1 3 4 -12 -18.639 10.2097 2 3 4 -12 -9.8118 7.70120 1 3 4 -12 0.20590 7.50978 2 -3 -4 12 -11.149 5.42019 2 -3 -4 12 9.74340 6.18598 1 -3 -4 12 0.02689 6.91208 2 2 4 -12 26.0681 9.89823 2 2 4 -12 11.7809 6.39906 2 -2 -4 12 25.4415 6.63930 1 -2 -4 12 14.3372 6.85643 2 -2 -4 12 11.2839 5.18424 2 -1 -4 12 0.03869 4.88678 2 -1 -4 12 6.29826 6.88195 1 -1 -4 12 11.0514 6.94125 2 4 3 -12 37.6822 8.85904 1 4 3 -12 37.9509 10.6930 2 4 3 -12 27.6370 9.11764 2 -4 -3 12 22.5246 6.79276 1 -4 -3 12 36.4078 7.09921 2 -4 -3 12 26.6691 5.91334 2 3 3 -12 -3.4128 7.43038 2 3 3 -12 14.1334 9.00667 2 -3 -3 12 -2.4164 5.01851 2 -3 -3 12 1.95601 6.31121 2 -3 -3 12 0.91678 5.82886 1 2 3 -12 14.7817 8.78398 2 -2 -3 12 -9.7844 6.88649 1 -2 -3 12 4.60175 6.73129 2 -2 -3 12 -0.3404 4.11647 2 -1 -3 12 4.52905 4.08362 2 -1 -3 12 0.81247 5.86703 2 -1 -3 12 0.69277 7.44019 1 4 2 -12 -5.4643 8.07061 2 4 2 -12 18.0626 9.19537 2 -4 -2 12 10.5828 5.02597 2 -4 -2 12 5.20512 6.20707 1 3 2 -12 -14.761 8.95065 2 3 2 -12 3.27443 7.77402 2 -3 -2 12 -4.7473 4.57847 2 -3 -2 12 1.68620 6.38953 1 -3 -2 12 -8.9285 6.58796 2 -2 -2 12 2.81795 5.60967 2 -2 -2 12 -1.5833 3.88122 2 -2 -2 12 11.9502 6.80645 1 -1 -2 12 7.28664 5.91851 2 -1 -2 12 1.61200 3.83555 2 -1 -2 12 4.12885 7.16011 1 4 1 -12 19.1921 8.84968 2 4 1 -12 17.2261 10.8177 2 -4 -1 12 2.25756 6.86853 1 -4 -1 12 5.16278 4.83743 2 -4 -1 12 2.07293 6.52749 2 3 1 -12 22.0000 9.62858 2 3 1 -12 18.7473 8.72743 2 -3 -1 12 23.4964 6.73305 1 -3 -1 12 20.6537 4.61918 2 -3 -1 12 12.0114 6.52794 2 -2 -1 12 1.87407 5.96481 2 -2 -1 12 3.91962 4.37185 2 -2 -1 12 -9.1018 6.38025 1 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details 'SADABS 2014/4' _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_max 0.7452 _exptl_absorpt_correction_T_min 0.5910 _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 0.71088 7.890 8.153 10.283 106.143 106.624 104.510 ) ; _shelx_hkl_checksum 77509 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 O1 O 0.33056(19) 0.66977(17) 0.44485(14) 0.0230(3) Uani 1 1 d . . H1 H 0.397(3) 0.612(3) 0.482(3) 0.038(7) Uiso 1 1 d . . N1 N 0.4464(2) 0.8613(2) 0.26925(18) 0.0227(4) Uani 1 1 d . . C1 C -0.0425(3) 0.1210(3) 0.1690(2) 0.0306(5) Uani 1 1 d . . H1A H -0.0970 0.0991 0.0677 0.037 Uiso 1 1 calc R U H1B H -0.0427 0.0212 0.1996 0.037 Uiso 1 1 calc R U O2 O 0.46612(18) 0.42631(17) 0.32769(14) 0.0241(3) Uani 1 1 d . . C2 C 0.0334(3) 0.2899(3) 0.2672(2) 0.0252(5) Uani 1 1 d . . H2 H 0.0864 0.3061 0.3673 0.030 Uiso 1 1 calc R U O3 O 0.13067(18) 0.75847(17) 0.15147(14) 0.0254(4) Uani 1 1 d . . C3 C 0.0427(3) 0.4592(2) 0.2331(2) 0.0208(4) Uani 1 1 d . . H3 H -0.0147 0.4221 0.1243 0.025 Uiso 1 1 calc R U O4 O 0.59665(17) 0.80006(17) 0.31105(15) 0.0242(3) Uani 1 1 d . . C4 C 0.2538(2) 0.5863(2) 0.29010(19) 0.0186(4) Uani 1 1 d . . C5 C 0.3632(2) 0.4666(2) 0.2393(2) 0.0194(4) Uani 1 1 d . . C6 C 0.3288(3) 0.3972(3) 0.0800(2) 0.0236(4) Uani 1 1 d . . H6A H 0.1931 0.3280 0.0226 0.035 Uiso 1 1 calc R U H6B H 0.4007 0.3172 0.0613 0.035 Uiso 1 1 calc R U H6C H 0.3700 0.5009 0.0514 0.035 Uiso 1 1 calc R U C7 C -0.0718(3) 0.5566(3) 0.3019(2) 0.0282(5) Uani 1 1 d . . H7A H -0.0718 0.6625 0.2745 0.042 Uiso 1 1 calc R U H7B H -0.0142 0.5977 0.4089 0.042 Uiso 1 1 calc R U H7C H -0.2026 0.4716 0.2662 0.042 Uiso 1 1 calc R U C8 C 0.2691(3) 0.7402(2) 0.22863(19) 0.0187(4) Uani 1 1 d . . C9 C 0.4820(3) 0.9983(3) 0.2051(2) 0.0296(5) Uani 1 1 d . . H9A H 0.3808 1.0490 0.1942 0.044 Uiso 1 1 calc R U H9B H 0.4851 0.9414 0.1087 0.044 Uiso 1 1 calc R U H9C H 0.6043 1.0967 0.2693 0.044 Uiso 1 1 calc R U C10 C 0.7252(3) 0.9147(3) 0.4602(2) 0.0303(5) Uani 1 1 d . . H10A H 0.8330 0.8745 0.4865 0.045 Uiso 1 1 calc R U H10B H 0.6585 0.9051 0.5266 0.045 Uiso 1 1 calc R U H10C H 0.7711 1.0422 0.4687 0.045 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0301(7) 0.0189(7) 0.0137(7) 0.0027(5) 0.0004(6) 0.0114(6) N1 0.0214(8) 0.0158(8) 0.0266(9) 0.0081(7) 0.0034(7) 0.0065(6) C1 0.0317(11) 0.0187(10) 0.0359(12) 0.0091(9) 0.0088(10) 0.0064(8) O2 0.0277(7) 0.0190(7) 0.0223(7) 0.0072(6) 0.0025(6) 0.0118(6) C2 0.0287(10) 0.0222(10) 0.0256(10) 0.0104(8) 0.0106(9) 0.0086(8) O3 0.0261(7) 0.0194(7) 0.0232(7) 0.0076(6) -0.0005(6) 0.0079(6) C3 0.0228(9) 0.0146(9) 0.0191(10) 0.0037(7) 0.0041(8) 0.0046(7) O4 0.0206(7) 0.0150(7) 0.0275(8) 0.0021(6) 0.0015(6) 0.0068(5) C4 0.0217(9) 0.0152(9) 0.0127(9) 0.0030(7) 0.0008(8) 0.0061(7) C5 0.0194(9) 0.0109(8) 0.0210(10) 0.0039(7) 0.0032(8) 0.0022(7) C6 0.0252(10) 0.0200(10) 0.0201(10) 0.0034(8) 0.0054(8) 0.0078(8) C7 0.0279(10) 0.0247(10) 0.0294(11) 0.0074(9) 0.0103(9) 0.0092(8) C8 0.0230(9) 0.0118(9) 0.0159(9) 0.0013(7) 0.0030(8) 0.0071(7) C9 0.0341(11) 0.0182(10) 0.0335(12) 0.0125(9) 0.0088(10) 0.0062(9) C10 0.0224(10) 0.0213(10) 0.0306(12) 0.0016(9) -0.0030(9) 0.0054(8) 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' O O 0.0106 0.0060 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle C4 O1 H1 109.8(16) C8 N1 O4 116.52(14) C8 N1 C9 121.71(16) O4 N1 C9 114.40(15) C2 C1 H1A 120.0 C2 C1 H1B 120.0 H1A C1 H1B 120.0 C1 C2 C3 125.18(19) C1 C2 H2 117.4 C3 C2 H2 117.4 C2 C3 C7 109.74(16) C2 C3 C4 109.44(16) C7 C3 C4 111.65(15) C2 C3 H3 108.7 C7 C3 H3 108.7 C4 C3 H3 108.7 N1 O4 C10 110.23(13) O1 C4 C5 109.95(14) O1 C4 C8 107.86(13) C5 C4 C8 110.83(14) O1 C4 C3 110.61(14) C5 C4 C3 107.42(14) C8 C4 C3 110.19(15) O2 C5 C6 123.01(16) O2 C5 C4 119.26(16) C6 C5 C4 117.65(15) 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 120.49(16) O3 C8 C4 122.94(16) N1 C8 C4 116.52(16) 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 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 O1 C4 1.414(2) O1 H1 0.86(3) N1 C8 1.359(2) N1 O4 1.400(2) N1 C9 1.454(2) C1 C2 1.318(3) C1 H1A 0.9500 C1 H1B 0.9500 O2 C5 1.213(2) C2 C3 1.504(3) C2 H2 0.9500 O3 C8 1.222(2) C3 C7 1.533(3) C3 C4 1.556(2) C3 H3 1.0000 O4 C10 1.445(2) C4 C5 1.537(3) C4 C8 1.548(2) C5 C6 1.492(3) 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 C10 H10A 0.9800 C10 H10B 0.9800 C10 H10C 0.9800 loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O2 0.86(3) 2.16(2) 2.6440(19) 115(2) . O1 H1 O2 0.86(3) 2.10(3) 2.8555(19) 146(2) 2_666 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 C1 C2 C3 C7 117.1(2) C1 C2 C3 C4 -120.0(2) C8 N1 O4 C10 -120.34(17) C9 N1 O4 C10 89.04(19) C2 C3 C4 O1 -72.56(18) C7 C3 C4 O1 49.1(2) C2 C3 C4 C5 47.44(19) C7 C3 C4 C5 169.14(16) C2 C3 C4 C8 168.27(14) C7 C3 C4 C8 -70.03(19) O1 C4 C5 O2 15.1(2) C8 C4 C5 O2 134.21(17) C3 C4 C5 O2 -105.37(18) O1 C4 C5 C6 -168.08(15) C8 C4 C5 C6 -48.9(2) C3 C4 C5 C6 71.49(19) O4 N1 C8 O3 -158.24(16) C9 N1 C8 O3 -9.9(3) O4 N1 C8 C4 24.1(2) C9 N1 C8 C4 172.45(16) O1 C4 C8 O3 -118.15(18) C5 C4 C8 O3 121.44(18) C3 C4 C8 O3 2.7(2) O1 C4 C8 N1 59.41(19) C5 C4 C8 N1 -61.0(2) C3 C4 C8 N1 -179.75(15)