#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:26:48 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227263 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035851.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_4035851 loop_ _publ_author_name 'Vila, Carlos' 'Rostoll-Berenguer, Jaume' 'S\'anchez-Garc\'ia, Rub\'en' 'Blay, Gonzalo' 'Fern\'andez, Isabel' 'Mu\~noz, M Carmen' 'Pedro, Jos\'e R' _publ_section_title ; Enantioselective Synthesis of 2-Amino-1,1-diarylalkanes Bearing a Carbocyclic Ring Substituted Indole through Asymmetric Catalytic Reaction of Hydroxyindoles with Nitroalkenes. ; _journal_issue 12 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 6397 _journal_page_last 6407 _journal_paper_doi 10.1021/acs.joc.8b00612 _journal_volume 83 _journal_year 2018 _chemical_absolute_configuration ad _chemical_formula_sum 'C16 H13 Br N2 O3' _chemical_formula_weight 361.19 _space_group_crystal_system monoclinic _space_group_IT_number 5 _space_group_name_Hall 'C 2y' _space_group_name_H-M_alt 'C 1 2 1' _atom_sites_solution_hydrogens difmap _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 122.965(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 16.3130(7) _cell_length_b 11.6843(5) _cell_length_c 9.3275(4) _cell_measurement_reflns_used 1763 _cell_measurement_temperature 200(1) _cell_measurement_theta_max 24.5150 _cell_measurement_theta_min 4.0170 _cell_volume 1491.64(12) _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-2014 (Sheldrick, 2014)' _diffrn_ambient_temperature 200(1) _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.902 _diffrn_measurement_device_type 'SuperNova Sapphire3' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0330 _diffrn_reflns_av_unetI/netI 0.0669 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.902 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_number 6190 _diffrn_reflns_point_group_measured_fraction_full 0.913 _diffrn_reflns_point_group_measured_fraction_max 0.789 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.854 _diffrn_reflns_theta_min 3.487 _exptl_absorpt_coefficient_mu 2.770 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.94120 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Empirical absorption correction' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.608 _exptl_crystal_description prismatic _exptl_crystal_F_000 728 _exptl_crystal_size_max 0.080 _exptl_crystal_size_mid 0.060 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.303 _refine_diff_density_min -0.408 _refine_diff_density_rms 0.063 _refine_ls_abs_structure_details ; Flack x determined using 846 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.016(8) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.893 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 251 _refine_ls_number_reflns 3387 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.893 _refine_ls_R_factor_all 0.0708 _refine_ls_R_factor_gt 0.0464 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1040 _refine_ls_wR_factor_ref 0.1246 _reflns_Friedel_coverage 0.673 _reflns_Friedel_fraction_full 0.821 _reflns_Friedel_fraction_max 0.665 _reflns_number_gt 2537 _reflns_number_total 3387 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b00612_si_002.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'C 2' _cod_database_code 4035851 _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 0.809 _shelx_estimated_absorpt_t_max 0.874 _shelxl_version_number 2014-1 _shelx_res_file ; TITL carlos17 in I2 REM transformed to space group : C121:b1 CELL 0.71073 16.3130 11.6843 9.3275 90.000 122.965 90.000 ZERR 4 0.0007 0.0005 0.0004 0.000 0.003 0.000 LATT -7 SYMM -X,+Y,-Z SFAC C H N O BR UNIT 64 52 8 12 4 MERG 2 FMAP 2 omit -3 180 PLAN 30 SIZE 0.050 0.060 0.080 ACTA 50.00 BOND L.S. 8 size 0.05 0.06 0.08 WGHT 0.072000 FVAR 3.97465 BR 5 -0.934858 0.695820 -0.217097 11.00000 0.04616 0.07999 = 0.06587 -0.01530 0.02769 0.02323 O1 4 -1.165797 1.241593 -0.271625 11.00000 0.06220 0.03501 = 0.03898 0.00360 0.02908 -0.01145 O2 4 -1.408323 0.911341 -0.503485 11.00000 0.08168 0.15084 = 0.03607 -0.01602 0.02424 -0.08436 O3 4 -1.374469 0.971020 -0.680714 11.00000 0.07798 0.03985 = 0.03753 -0.00867 0.03635 -0.00397 N1 3 -1.212873 0.998087 0.100187 11.00000 0.03388 0.03858 = 0.03124 -0.00070 0.02145 0.00037 N2 3 -1.368764 0.977821 -0.545172 11.00000 0.03151 0.04895 = 0.03111 -0.00286 0.01228 -0.00633 C1 1 -1.241738 1.024216 -0.247713 11.00000 0.02439 0.03188 = 0.02813 -0.00243 0.01362 -0.00191 C2 1 -1.194411 1.114130 -0.107569 11.00000 0.02513 0.03138 = 0.02590 -0.00179 0.01377 0.00309 C3 1 -1.156344 1.217974 -0.119076 11.00000 0.03427 0.02891 = 0.03030 0.00085 0.01957 0.00091 C4 1 -1.110105 1.294277 0.017343 11.00000 0.03800 0.02902 = 0.04891 -0.00462 0.02332 -0.00173 C5 1 -1.099275 1.269709 0.170613 11.00000 0.03244 0.04496 = 0.03701 -0.01860 0.01592 -0.00316 C6 1 -1.135593 1.167004 0.189964 11.00000 0.02424 0.04275 = 0.03159 -0.00488 0.01610 0.00533 C7 1 -1.183126 1.091819 0.049780 11.00000 0.02285 0.03544 = 0.02861 0.00028 0.01705 0.00627 C8 1 -1.137787 1.114487 0.327296 11.00000 0.04125 0.05524 = 0.03142 -0.01067 0.02103 0.00196 C9 1 -1.184438 1.013427 0.268301 11.00000 0.04124 0.05666 = 0.03345 0.00351 0.02447 0.00383 C10 1 -1.167024 0.942590 -0.242285 11.00000 0.02719 0.02761 = 0.02259 -0.00432 0.01464 -0.00111 C11 1 -1.094259 0.984482 -0.264048 11.00000 0.03888 0.03657 = 0.05336 -0.00215 0.03226 -0.00429 C12 1 -1.026340 0.910265 -0.260008 11.00000 0.02888 0.05116 = 0.04881 -0.00740 0.02442 -0.00357 C13 1 -1.170409 0.827119 -0.216746 11.00000 0.02958 0.03422 = 0.03236 -0.00188 0.01531 -0.00464 C14 1 -1.101957 0.752802 -0.209179 11.00000 0.03937 0.03712 = 0.03839 -0.00081 0.01901 0.00412 C15 1 -1.031610 0.795604 -0.232347 11.00000 0.02959 0.04694 = 0.03045 -0.01066 0.01308 0.00627 C16 1 -1.309294 1.073441 -0.425459 11.00000 0.03361 0.04077 = 0.02904 -0.00039 0.01410 0.00134 H1 2 -1.287568 0.980942 -0.242162 11.00000 0.01684 H4 2 -1.088092 1.375445 -0.005219 11.00000 0.02664 H14 2 -1.113176 0.668000 -0.195332 11.00000 0.03380 H12 2 -0.982592 0.931747 -0.305502 11.00000 0.04240 H16A 2 -1.279755 1.101149 -0.468553 11.00000 0.05068 H8 2 -1.110466 1.149998 0.433454 11.00000 0.05091 H11 2 -1.092267 1.069608 -0.286439 11.00000 0.05165 H13 2 -1.224657 0.803696 -0.206939 11.00000 0.04494 H5 2 -1.065563 1.319246 0.254946 11.00000 0.03845 H16B 2 -1.361713 1.131581 -0.445823 11.00000 0.05274 H9 2 -1.198699 0.947196 0.322858 11.00000 0.06418 H1O 2 -1.145696 1.300539 -0.270671 11.00000 0.02968 H1N 2 -1.237345 0.936063 0.036560 11.00000 0.08102 HKLF 4 REM carlos17 in I2 REM R1 = 0.0464 for 2537 Fo > 4sig(Fo) and 0.0708 for all 3387 data REM 251 parameters refined using 1 restraints END WGHT 0.0271 0.0000 REM Highest difference peak 0.303, deepest hole -0.408, 1-sigma level 0.063 Q1 1 -0.9508 0.6404 -0.1524 11.00000 0.05 0.30 Q2 1 -0.9653 0.7284 -0.1492 11.00000 0.05 0.27 Q3 1 -0.9596 0.9540 -0.1603 11.00000 0.05 0.24 Q4 1 -1.1924 1.1789 0.4476 11.00000 0.05 0.24 Q5 1 -1.5000 1.1870 -0.5000 10.50000 0.05 0.23 Q6 1 -1.0830 0.6395 -0.2318 11.00000 0.05 0.23 Q7 1 -1.0590 0.6802 -0.1355 11.00000 0.05 0.23 Q8 1 -0.8987 0.7547 -0.0614 11.00000 0.05 0.22 Q9 1 -0.9499 1.0259 -0.0665 11.00000 0.05 0.22 Q10 1 -1.4355 1.1242 -0.4659 11.00000 0.05 0.22 Q11 1 -1.1992 0.5650 -0.2598 11.00000 0.05 0.21 Q12 1 -1.2903 0.8647 -0.0744 11.00000 0.05 0.21 Q13 1 -1.2401 1.0501 -0.5641 11.00000 0.05 0.21 Q14 1 -1.3370 0.9076 -0.3862 11.00000 0.05 0.21 Q15 1 -1.2028 1.3412 -0.4052 11.00000 0.05 0.21 Q16 1 -1.0267 0.7048 -0.2535 11.00000 0.05 0.20 Q17 1 -1.4523 0.9773 -0.5522 11.00000 0.05 0.20 Q18 1 -1.0759 0.7646 -0.2480 11.00000 0.05 0.20 Q19 1 -1.1791 0.7626 0.0110 11.00000 0.05 0.20 Q20 1 -1.1175 0.8641 0.3186 11.00000 0.05 0.19 Q21 1 -1.1914 0.9905 -0.1992 11.00000 0.05 0.19 Q22 1 -1.1417 0.9207 -0.3214 11.00000 0.05 0.19 Q23 1 -1.1504 0.6540 -0.2693 11.00000 0.05 0.19 Q24 1 -1.1434 0.7956 -0.2534 11.00000 0.05 0.19 Q25 1 -1.1937 1.1740 -0.1190 11.00000 0.05 0.19 Q26 1 -1.2595 0.9900 0.1338 11.00000 0.05 0.19 Q27 1 -1.1215 1.2244 0.1976 11.00000 0.05 0.19 Q28 1 -0.9597 0.9907 -0.2272 11.00000 0.05 0.19 Q29 1 -1.2782 1.2016 -0.4943 11.00000 0.05 0.19 Q30 1 -1.0863 0.8401 0.0198 11.00000 0.05 0.19 ; _shelx_res_checksum 40765 _shelx_hkl_file ; 0 -16 0 1269.87 852.226 4 2 -16 0 999.744 779.582 4 -2 -16 0-266.523 744.126 6 -1 -15 0 1452.09 911.375 4 1 -15 0-669.513 662.738 4 -1 -15 0 2020.42 918.813 6 3 -15 0 631.414 648.652 4 -3 -15 0-466.562 774.148 6 -3 -15 0-103.327 592.319 4 -5 -15 0 598.481 811.558 4 0 -14 0 117.675 436.016 6 0 -14 0 790.943 724.997 4 -2 -14 0 766.371 712.193 4 -2 -14 0 300.196 644.902 6 2 -14 0 1614.02 802.368 4 -4 -14 0-739.760 820.491 4 4 -14 0-263.321 599.240 4 6 -14 0 1281.97 737.111 4 -6 -14 0 2122.26 1028.09 4 1 -13 0 3454.73 1049.24 4 1 -13 0 3398.14 989.954 6 -1 -13 0 1464.55 821.547 6 -1 -13 0 3859.54 1114.63 4 3 -13 0 1065.88 653.709 4 -3 -13 0 1526.94 847.758 4 -5 -13 0 636.024 728.467 4 5 -13 0 1283.16 730.198 4 7 -13 0 220.905 542.350 4 -7 -13 0 483.058 584.076 4 -9 -13 0 979.556 781.297 4 0 -12 0 476.601 430.188 6 0 -12 0 1435.88 667.026 4 -2 -12 0 2198.61 834.125 4 2 -12 0 913.968 469.474 6 2 -12 0 862.379 671.953 4 4 -12 0 2600.34 867.367 4 -4 -12 0 1446.68 719.163 4 -6 -12 0 2977.13 1083.39 4 6 -12 0 3739.07 1032.13 4 8 -12 0 3555.02 1036.64 4 -8 -12 0 2796.81 1018.91 4 -10 -12 0 1391.70 864.225 4 -1 -11 0 809.931 480.328 4 1 -11 0 862.522 570.103 4 1 -11 0 667.564 497.937 6 3 -11 0 9371.23 1433.67 4 3 -11 0 11974.7 1424.06 6 -3 -11 0 10228.5 1563.92 4 5 -11 0 1570.32 644.030 4 -5 -11 0 1314.91 693.733 4 -7 -11 0 4256.69 1175.36 4 7 -11 0 3871.50 1030.78 4 -9 -11 0 5734.95 1310.56 4 9 -11 0 7309.89 1386.48 4 11 -11 0 902.136 745.580 4 -11 -11 0 1958.50 1005.09 4 0 -10 0 24182.2 2149.59 4 2 -10 0 7127.32 1151.57 4 -2 -10 0 7159.13 1207.16 4 2 -10 0 7902.26 1126.03 6 4 -10 0 1923.65 608.286 6 4 -10 0 2484.05 763.793 4 -4 -10 0 2759.48 862.723 4 -6 -10 0 9058.21 1490.52 4 6 -10 0 8274.90 1320.69 4 8 -10 0 4136.76 959.813 4 -8 -10 0 4761.76 1237.48 4 -10 -10 0 782.059 614.340 4 10 -10 0 161.282 508.163 4 -12 -10 0 5297.84 1438.34 4 -14 -10 0 1718.91 878.289 3 -1 -9 0 26773.4 2140.33 4 1 -9 0 28017.7 2158.97 4 3 -9 0 124.667 328.619 6 -3 -9 0 676.512 408.890 4 3 -9 0-190.918 436.621 4 5 -9 0 10900.2 1090.87 6 -5 -9 0 12295.6 1605.72 4 5 -9 0 8708.87 1248.74 4 7 -9 0 3154.15 818.888 4 -7 -9 0 3839.04 1018.34 4 -9 -9 0 10427.7 1681.39 4 -11 -9 0 4954.40 1361.39 4 -13 -9 0 2113.52 1070.04 4 -15 -9 0 3144.58 1119.44 3 0 -8 0 22313.4 1815.10 4 -2 -8 0 29615.5 2132.74 4 2 -8 0 26456.9 1789.50 6 2 -8 0 28857.3 2060.32 4 4 -8 0 13158.0 1410.79 4 4 -8 0 14983.9 1229.82 6 -4 -8 0 13635.5 1499.78 4 6 -8 0 3776.93 826.588 4 6 -8 0 4574.57 607.700 6 -8 -8 0 24244.8 2342.44 4 -10 -8 0 11396.0 1722.16 4 -12 -8 0 2974.65 997.806 4 -14 -8 0 3225.24 1084.18 3 1 -7 0 39706.2 2240.54 4 -1 -7 0 40460.2 2306.46 4 -3 -7 0 720.941 388.362 4 3 -7 0 609.681 361.363 4 3 -7 0 1188.79 420.473 6 -5 -7 0 11888.2 1415.93 4 5 -7 0 13496.8 1009.38 6 -7 -7 0 58966.8 3342.28 4 -7 -7 0 55947.1 1948.61 1 7 -7 0 57811.4 1770.41 6 -9 -7 0 29126.4 2548.94 4 -9 -7 0 29727.2 1663.26 1 -11 -7 0 6427.27 1396.66 4 -13 -7 0 1407.01 859.690 3 -15 -7 0 4544.42 1329.07 3 0 -6 0 8793.77 975.062 4 2 -6 0 11851.9 1128.88 4 -2 -6 0 11361.3 1161.75 4 -4 -6 0 10828.7 1224.90 4 4 -6 0 10598.9 838.876 6 6 -6 0 33945.7 1288.93 6 -6 -6 0 35215.1 2377.03 4 -6 -6 0 33111.3 1390.62 1 -8 -6 0 22204.6 2025.41 4 -8 -6 0 20132.4 1317.00 1 -10 -6 0 13938.1 1787.12 4 -10 -6 0 18908.8 1483.86 1 -12 -6 0 8160.78 1118.08 1 -12 -6 0 8117.20 1397.17 3 -14 -6 0 9610.69 1699.04 3 -16 -6 0 6008.31 1542.65 3 1 -5 0 93222.5 3010.75 4 -1 -5 0 90919.8 3062.83 4 3 -5 0 13956.1 910.126 6 -3 -5 0 13749.0 1208.89 4 5 -5 0 42071.8 1399.30 6 -5 -5 0 43134.3 1497.76 1 -5 -5 0 44325.0 2413.73 4 -7 -5 0 15461.0 1532.61 4 7 -5 0 16005.7 687.385 6 -7 -5 0 17167.9 1144.97 1 -9 -5 0 21477.7 2039.90 4 -9 -5 0 18446.6 1391.61 1 -11 -5 0 3918.13 958.414 3 -11 -5 0 2833.34 665.975 1 -11 -5 0 2958.21 849.474 4 -13 -5 0 406.274 520.787 3 -13 -5 0 424.425 385.264 1 -15 -5 0 10189.7 1802.94 3 -15 -5 0 9006.09 1402.76 1 -17 -5 0 7701.97 1737.87 3 0 -4 0 300943. 5740.60 4 2 -4 0 121177. 3220.14 4 -2 -4 0 118194. 3331.23 4 -4 -4 0 42244.4 2111.59 4 4 -4 0 46424.4 1355.30 6 -4 -4 0 44716.9 1396.02 1 -6 -4 0 54072.3 1939.64 1 -6 -4 0 54393.6 2679.70 4 6 -4 0 52634.5 1306.49 6 -8 -4 0 24738.8 1983.67 4 -8 -4 0 22463.1 1451.73 1 -10 -4 0 30269.4 2448.58 4 -10 -4 0 29851.2 2347.41 3 -10 -4 0 29936.9 1919.11 1 -12 -4 0 4097.91 1057.48 3 -12 -4 0 2929.53 729.835 1 -14 -4 0 17214.6 2166.66 3 -14 -4 0 18919.4 1933.27 1 -16 -4 0 1141.56 791.802 3 -16 -4 0 2157.63 737.786 1 1 -3 0 100110. 2543.77 4 -1 -3 0 97013.5 2601.27 4 -3 -3 0 57929.0 1452.02 1 3 -3 0 55663.7 1406.12 6 -3 -3 0 55323.6 2116.82 4 5 -3 0 56794.6 1294.47 6 -5 -3 0 54960.1 2414.75 4 -5 -3 0 54687.8 1807.49 1 5 -3 0 59154.5 1930.30 5 7 -3 0 219328. 4402.58 5 -7 -3 0 217110. 5848.21 4 -7 -3 0 214886. 4845.61 1 -9 -3 0 11465.2 1135.24 1 -9 -3 0 9315.13 1248.01 3 -11 -3 0 114.632 342.781 1 -11 -3 0 593.469 540.275 3 -13 -3 0 4361.08 1091.77 3 -13 -3 0 4296.25 932.200 1 -15 -3 0 5980.76 1154.73 1 -15 -3 0 3314.75 1093.15 3 -17 -3 0 3227.61 944.442 1 -17 -3 0 3293.21 1181.05 3 0 -2 0 106604. 2263.43 4 -2 -2 0 227937. 4312.16 4 2 -2 0 232493. 3428.24 6 2 -2 0 234264. 4167.25 2 -2 -2 0 233610. 3455.79 1 -4 -2 0 29780.3 1189.90 1 4 -2 0 32619.6 1184.01 5 -4 -2 0 29177.1 1490.48 4 6 -2 0 25183.6 1090.46 5 -6 -2 0 29190.5 1471.32 1 -6 -2 0 27095.0 1707.66 4 -8 -2 0 78692.3 3346.71 3 -8 -2 0 77201.5 2922.02 1 -10 -2 0 21595.5 1707.64 1 -10 -2 0 19975.1 1885.31 3 -12 -2 0 4155.23 641.219 5 -12 -2 0 3820.61 882.781 1 -12 -2 0 3670.75 871.043 3 -14 -2 0 10158.2 1655.28 3 -14 -2 0 11263.2 1538.09 1 -16 -2 0 11947.9 1749.27 1 -16 -2 0 17986.8 2418.99 3 -18 -2 0 2444.36 1086.29 1 -3 -1 0 334919. 5203.36 1 3 -1 0 334039. 5415.45 2 -3 -1 0 323960. 5630.56 4 3 -1 0 339343. 5622.54 3 3 -1 0 346371. 4839.55 5 -5 -1 0 161485. 4078.00 3 -5 -1 0 170185. 3754.07 1 -7 -1 0 123360. 4000.62 3 -7 -1 0 121227. 3590.22 1 -9 -1 0 38714.2 2235.00 1 -9 -1 0 39730.6 2465.45 3 -11 -1 0 4706.04 913.299 1 -11 -1 0 4439.45 975.875 3 -11 -1 0 4967.35 630.920 5 -13 -1 0 2624.58 769.209 1 -13 -1 0 4107.46 1078.09 3 -15 -1 0 7686.07 1572.26 3 -15 -1 0 7752.32 1363.32 1 -17 -1 0 3788.10 1113.14 1 4 0 0 306729. 5062.09 2 -4 0 0 301915. 5332.47 1 4 0 0 298184. 5472.54 4 -4 0 0 295459. 5541.12 3 -6 0 0 14105.0 756.897 5 -6 0 0 15116.9 1114.64 1 -6 0 0 16933.4 1295.07 3 -8 0 0 65551.2 1987.21 5 -8 0 0 68112.6 3082.16 3 -8 0 0 66844.1 2818.87 1 -10 0 0 2761.59 431.253 5 -10 0 0 5027.46 908.685 1 -10 0 0 3474.00 760.627 3 -12 0 0 384.267 464.051 1 -12 0 0 828.744 501.623 3 -14 0 0 1195.98 656.941 1 -16 0 0 7198.92 1446.47 1 -18 0 0-1003.17 714.961 1 -3 1 0 339322. 5441.76 2 -3 1 0 336234. 4599.28 6 -3 1 0 337830. 5507.57 1 3 1 0 335802. 5205.93 1 3 1 0 338178. 5707.37 4 -3 1 0 334468. 4869.86 5 -5 1 0 142213. 2733.26 6 -5 1 0 137832. 3701.71 3 -5 1 0 143604. 2756.89 5 -5 1 0 141281. 3568.85 1 -7 1 0 125760. 2795.49 5 -7 1 0 125124. 2915.81 6 -7 1 0 127226. 4090.08 3 -7 1 0 125949. 3850.92 1 -9 1 0 46034.8 1692.16 5 -9 1 0 49329.2 2754.56 3 -9 1 0 48127.7 2579.82 1 -11 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1029.73 1 -10 4 -3 7208.82 1418.71 1 -8 4 -3 2770.12 839.380 1 -6 4 -3 1494.77 557.507 1 -4 4 -3 5050.77 827.406 1 -2 4 -3 83196.0 3073.58 1 0 4 -3 47026.3 1971.39 1 -2 4 3 14385.6 925.306 4 2 4 -3 14305.8 894.559 1 -4 4 3 84789.5 1930.23 4 -10 4 3 7379.76 1028.26 2 -10 4 3 6253.43 958.236 5 -12 4 3 23428.3 1909.27 2 -12 4 3 22978.4 1886.02 5 -14 4 3 31520.5 2367.46 2 -16 4 3 6119.36 1248.60 1 -16 4 3 6441.37 1202.33 2 -18 4 3 10419.0 1817.12 1 -13 5 -3-12.2448 495.597 1 -11 5 -3 1829.08 816.033 1 -9 5 -3 7948.88 1387.47 1 -7 5 -3 7864.32 1239.70 1 -5 5 -3 17777.4 1680.56 1 -3 5 -3 52454.5 2575.90 1 -1 5 -3 34112.0 1806.32 1 1 5 -3 23166.2 1274.55 1 3 5 -3 1171.46 232.268 1 -3 5 3 655.973 218.055 4 -11 5 3 17839.4 1721.15 2 -13 5 3 29458.7 2349.30 2 -15 5 3 5442.97 1140.53 2 -17 5 3 2044.95 971.690 1 -17 5 3 2989.70 971.013 2 -19 5 3 2150.53 959.355 1 -12 6 -3 1886.99 897.616 1 -10 6 -3 14348.9 1929.56 1 -8 6 -3 472.890 501.185 1 -6 6 -3 4805.78 937.797 1 -4 6 -3 6038.20 944.826 1 -2 6 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3512.21 1188.23 2 -11 13 3 1164.07 891.304 2 -13 13 3 1435.30 842.068 1 -2 14 3 847.874 689.100 2 -4 14 3 606.713 645.045 2 -6 14 3 2416.60 921.349 2 -8 14 3 1778.02 821.254 2 -3 15 3 599.235 719.281 2 -5 15 3-1120.46 748.472 2 3 -15 -4-884.221 698.130 6 5 -15 -4 1015.95 821.074 6 -4 -14 -4 1642.58 822.374 4 0 -14 -4 1252.82 793.823 6 0 -14 4-1032.32 952.378 4 2 -14 -4 2040.31 1004.98 6 -2 -14 4 2921.48 1080.71 4 4 -14 -4 2580.39 1010.09 6 -4 -14 4-252.242 741.900 4 6 -14 -4-398.683 543.790 6 -6 -14 4 1061.79 991.748 4 -5 -13 -4 1250.52 809.037 4 -3 -13 -4 847.318 698.507 4 -3 -13 -4 1916.18 1117.03 6 3 -13 4 1922.15 1002.46 4 -1 -13 -4 2016.53 800.552 4 -1 -13 -4 2098.42 1089.16 6 1 -13 4 2324.54 1136.89 4 -1 -13 4 1763.71 954.170 4 1 -13 -4 2057.94 1045.28 6 -3 -13 4 2675.29 1144.13 4 3 -13 -4 323.186 594.865 6 5 -13 -4 687.768 549.464 6 -5 -13 4 779.355 825.144 4 -7 -13 4 1209.86 831.383 4 7 -13 -4 893.497 599.460 6 -9 -13 4 3356.25 1198.27 4 6 -12 4 2937.28 1294.07 4 -4 -12 -4 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1791.77 4 4 -8 -4 12719.9 1578.52 6 6 -8 -4 2643.08 482.075 4 -6 -8 4 2411.29 800.638 4 6 -8 -4 3051.81 772.378 6 8 -8 -4 29448.9 1462.18 4 -8 -8 4 31665.9 2605.51 4 8 -8 -4 36019.8 2463.75 6 -10 -8 4 8904.01 1452.22 4 10 -8 -4 6434.23 999.871 6 -12 -8 4 16138.6 2026.32 4 12 -8 -4 13144.2 1418.46 6 -14 -8 4 8117.13 1527.53 4 -16 -8 4 5266.43 1364.38 4 -18 -8 4 5587.22 1440.17 4 -11 -7 -4-108.345 687.415 6 -9 -7 -4 560.023 560.230 1 -9 -7 -4 444.606 492.629 6 -9 -7 -4-331.155 518.822 3 -7 -7 -4 2218.56 709.508 3 -7 -7 -4 2451.42 832.446 1 -7 -7 -4 1738.18 773.552 6 -5 -7 -4 20065.1 2177.43 6 -5 -7 -4 16359.8 1549.66 3 -5 -7 -4 13969.6 1561.14 1 -3 -7 -4 6661.95 1044.57 1 -3 -7 -4 4644.20 1056.04 6 -3 -7 -4 5762.00 810.931 3 -1 -7 -4 2597.37 673.897 4 -1 -7 -4 1935.04 707.562 6 -1 -7 -4 2612.21 459.260 3 1 -7 -4 16984.2 1457.54 4 -1 -7 4 16315.4 1795.38 4 1 -7 -4 15249.4 1723.74 6 3 -7 -4 17961.1 1292.54 4 -3 -7 4 19394.0 1903.66 4 3 -7 -4 19633.7 1863.70 6 5 -7 -4 21596.2 1247.27 4 -5 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2421.69 4 4 -6 -4 33965.4 2331.02 6 -4 -6 4 32699.8 1413.70 1 -6 -6 4 6049.07 578.934 2 6 -6 -4 6538.82 528.115 4 -6 -6 4 6555.60 1041.71 4 6 -6 -4 6960.93 1045.53 6 -6 -6 4 6133.27 494.328 1 -8 -6 4 7171.13 1169.19 4 8 -6 -4 7097.44 495.605 4 8 -6 -4 7762.94 1059.41 6 -8 -6 4 5665.08 467.697 1 10 -6 -4 16356.5 921.107 4 -10 -6 4 12847.6 1586.71 4 10 -6 -4 16884.4 1530.53 6 -12 -6 4 12205.5 1618.61 4 12 -6 -4 11433.6 1274.96 6 -14 -6 4 8109.12 1408.00 4 14 -6 -4 7877.08 1075.48 6 -16 -6 4 21793.2 2431.65 4 -18 -6 4 4005.43 1148.35 4 -13 -5 -4 279.140 485.434 1 -11 -5 -4 72.6945 526.938 1 -9 -5 -4 592.067 489.865 6 -9 -5 -4 557.754 586.374 1 -7 -5 -4 2503.71 831.220 6 -7 -5 -4 3369.48 870.452 1 -5 -5 -4 20346.0 2042.62 6 -5 -5 -4 22483.4 1776.13 3 -5 -5 -4 20172.0 1818.56 1 -3 -5 -4 8447.42 951.751 3 -3 -5 -4 9774.73 1208.81 1 -3 -5 -4 8169.46 1255.70 6 -1 -5 -4 4406.40 897.941 6 -1 -5 -4 4050.45 747.543 1 1 -5 4 2805.54 404.035 6 -1 -5 -4 3809.82 508.491 3 1 -5 -4 17388.0 1644.06 6 -3 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1459.59 4 3 5 -4 31339.7 1493.25 1 -5 5 4 53998.7 1576.40 4 -13 5 4 918.066 485.002 2 -15 5 4 9136.20 1371.69 2 -17 5 4 3782.43 990.955 2 -19 5 4 6629.28 1566.03 1 -19 5 4 7590.33 1490.88 2 -10 6 -4 658.964 914.778 1 -8 6 -4 6392.58 1337.07 1 -6 6 -4 13044.9 1629.14 1 -4 6 -4 6088.79 1031.43 1 -2 6 -4 5023.92 856.869 1 0 6 -4 7063.93 909.982 1 2 6 -4 24378.6 1423.52 1 -4 6 4 30480.7 1482.32 4 4 6 -4 32883.6 1402.04 1 -12 6 4 15431.5 1706.07 2 -14 6 4 6966.68 1213.85 2 -16 6 4 12582.0 1766.15 2 -18 6 4 2731.11 901.895 2 -18 6 4 3017.75 1002.52 1 -11 7 -4 76.8443 796.214 1 -9 7 -4-232.841 678.508 1 -7 7 -4 1887.58 738.965 1 -5 7 -4 16095.3 1774.00 1 -3 7 -4 6368.07 1058.58 1 -1 7 -4 1170.83 425.557 1 1 7 -4 17251.4 1295.79 1 3 7 -4 18748.7 1105.48 1 -11 7 4 3980.93 900.953 2 -13 7 4 5287.87 1108.87 2 -15 7 4 3778.13 1034.76 2 -17 7 4 8812.25 1572.83 2 -19 7 4 1742.70 837.325 2 -10 8 -4 809.185 680.254 1 -8 8 -4 719.891 693.746 1 -6 8 -4 1128.74 613.938 1 -4 8 -4 5868.89 1051.21 1 -2 8 -4 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1 8 2097.56 952.027 3 -21 1 8 849.786 804.348 5 -4 2 -8-75.0488 510.811 1 -2 2 -8 5247.78 1304.73 1 0 2 -8 4397.91 1048.88 1 0 2 -8 3354.31 731.721 6 2 2 -8 4978.30 1114.33 1 2 2 -8 4144.86 841.008 6 4 2 -8 9003.89 1349.69 1 4 2 -8 11296.1 1371.89 6 -4 2 8 9112.18 1266.85 5 6 2 -8 10843.2 1398.48 6 -6 2 8 10727.6 1442.11 5 8 2 -8 6068.87 1108.56 6 -8 2 8 4842.35 1062.90 5 10 2 -8 29093.8 2473.47 6 -10 2 8 25100.6 2405.62 5 -12 2 8 27410.9 2581.81 5 -14 2 8 3945.70 1112.30 5 -14 2 8 2914.25 719.256 3 -16 2 8 2351.27 924.556 5 -16 2 8 1109.86 561.496 3 -18 2 8 11634.1 1914.26 5 -20 2 8 6764.51 1581.02 5 -22 2 8 75.0712 710.085 5 -5 3 -8 704.561 654.082 1 -3 3 -8 3774.02 1113.79 1 -1 3 -8 627.509 723.761 1 1 3 -8 6054.10 1235.17 1 1 3 -8 6677.68 998.982 6 3 3 -8 8990.20 1217.03 6 3 3 -8 9846.20 1422.93 1 5 3 -8 3710.48 856.517 1 5 3 -8 5578.85 1023.56 6 7 3 -8 17019.9 1787.06 6 -7 3 8 18689.6 1952.66 5 -9 3 8 277.598 459.142 5 -11 3 8 9188.94 1510.56 5 -13 3 8 14810.9 2015.25 5 -15 3 8 2255.76 930.550 5 -17 3 8 462.427 619.346 5 -19 3 8 816.556 651.213 5 -21 3 8 3915.99 1234.83 5 -4 4 -8 2012.08 853.232 1 -2 4 -8 4878.56 1156.40 1 0 4 -8 253.314 495.483 1 2 4 -8 4082.66 962.691 1 4 4 -8 5855.76 1071.77 1 6 4 -8 33315.3 2389.88 1 -8 4 8 10130.5 1553.20 5 -10 4 8 25619.9 2474.20 5 -12 4 8 537.448 574.054 5 -14 4 8 3877.78 1103.58 5 -16 4 8 3162.57 1088.58 5 -18 4 8 3556.68 1090.21 5 -20 4 8 1320.08 772.657 5 -3 5 -8 211.501 511.806 1 -1 5 -8 1094.39 684.716 1 1 5 -8 1391.74 637.535 1 3 5 -8 10251.5 1416.33 1 5 5 -8 10648.4 1382.61 1 -11 5 8 11760.0 1802.20 5 -13 5 8 5076.61 1252.43 5 -15 5 8 1053.17 805.263 5 -17 5 8 5884.90 1458.70 5 -19 5 8 4068.95 1087.23 2 -19 5 8 4929.20 1408.15 5 -4 6 -8 1363.10 840.509 1 -2 6 -8 4585.57 1139.48 1 0 6 -8 356.886 494.597 1 2 6 -8 4352.58 969.146 1 4 6 -8 5653.37 1066.38 1 6 6 -8 2234.38 694.573 1 -18 6 8 3680.12 1025.71 2 -20 6 8 4004.17 1090.34 2 -3 7 -8 2890.46 1117.45 1 -1 7 -8 1354.93 808.147 1 1 7 -8 445.341 492.611 1 3 7 -8 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5 7 -3 -9 12192.4 1726.83 6 -7 -3 9 11694.7 1570.20 4 -7 -3 9 13715.3 1683.88 5 -9 -3 9 5003.14 1091.56 5 -9 -3 9 7149.34 1187.64 4 9 -3 -9 7622.21 1436.19 6 -11 -3 9 7964.12 1417.62 5 -11 -3 9 7134.62 1142.88 4 11 -3 -9 9517.55 1574.84 6 -13 -3 9 3999.36 1110.41 5 13 -3 -9 4561.00 1174.39 6 -15 -3 9 3652.28 1113.45 5 15 -3 -9 5822.46 1271.07 6 -17 -3 9 983.546 862.525 5 17 -3 -9 277.340 553.788 6 -19 -3 9 2043.45 1037.29 5 -2 -2 -9 176.446 519.932 1 0 -2 -9 4782.11 1306.88 1 0 -2 -9 2393.29 778.763 6 2 -2 -9 4615.43 1174.28 1 2 -2 -9 5454.21 1162.05 6 4 -2 -9 548.124 483.345 6 -4 -2 9 433.552 449.000 5 6 -2 -9 10354.1 1515.36 6 -6 -2 9 8197.02 1292.34 5 -8 -2 9 7311.88 1184.76 4 8 -2 -9 5151.37 1079.72 6 -8 -2 9 7493.22 1326.31 5 -10 -2 9 2093.77 703.931 4 10 -2 -9 1364.62 787.928 6 -10 -2 9 388.690 485.458 5 12 -2 -9 4822.66 1171.59 6 -12 -2 9 2868.66 950.477 5 14 -2 -9 1182.09 710.103 6 -14 -2 9 1548.00 885.394 5 16 -2 -9 3701.00 1094.55 6 -16 -2 9 4924.62 1379.77 5 -18 -2 9 158.247 568.173 5 -20 -2 9 1317.42 879.772 5 -22 -2 9 96.3825 698.228 3 -3 -1 -9 161.892 631.754 1 -1 -1 -9 4350.95 1258.56 1 1 -1 -9 5025.66 1353.32 1 1 -1 -9 5096.85 1149.51 6 3 -1 -9-331.586 646.190 1 3 -1 -9 1341.95 675.218 6 5 -1 -9 107.506 490.103 6 -5 -1 9-129.124 414.266 5 7 -1 -9 3093.14 941.195 6 -7 -1 9 4163.97 1047.41 5 -9 -1 9 19751.3 1705.57 4 9 -1 -9 17834.8 1997.99 6 -9 -1 9 15895.6 1892.95 5 11 -1 -9 3084.39 936.298 6 -11 -1 9 1774.31 787.845 5 13 -1 -9 2956.74 955.526 6 -13 -1 9 2454.08 914.362 5 15 -1 -9-201.612 465.204 6 -15 -1 9 86.8722 492.053 5 -17 -1 9 9878.15 1770.71 5 -19 -1 9 796.888 681.764 5 -21 -1 9 1133.47 916.315 5 -21 -1 9 598.007 610.626 3 -2 0 -9 325.070 612.554 1 0 0 -9 8657.95 1597.79 1 2 0 -9 3960.05 1055.59 1 2 0 -9 5306.48 1069.57 6 4 0 -9-46.0986 447.217 6 4 0 -9-187.862 650.136 1 -4 0 9 901.542 585.861 5 6 0 -9-137.785 463.015 6 -6 0 9 160.165 442.691 5 -8 0 9 852.406 446.207 4 8 0 -9-249.761 555.807 6 -8 0 9-192.145 504.460 5 10 0 -9 5521.92 1154.26 6 -10 0 9 7235.45 1377.23 5 12 0 -9 11950.0 1689.46 6 -12 0 9 11362.9 1702.55 5 14 0 -9 14560.9 1990.64 6 -14 0 9 20061.7 2384.98 5 -16 0 9 9238.65 1738.11 5 -18 0 9 1518.92 916.400 5 -20 0 9 1232.04 976.362 5 -3 1 -9 1677.56 917.067 1 -1 1 -9 4441.00 1203.87 1 1 1 -9 4388.21 940.417 6 1 1 -9 3584.50 1096.39 1 3 1 -9 1361.28 711.087 1 3 1 -9 492.467 371.115 6 5 1 -9 1189.89 586.607 1 5 1 -9 707.218 492.052 6 -5 1 9 338.974 342.831 5 7 1 -9 6071.33 1147.70 6 -7 1 9 5387.38 1115.70 5 9 1 -9 14802.1 1830.47 6 -9 1 9 16815.2 1972.10 5 11 1 -9 1629.88 710.771 6 -11 1 9 1780.45 845.531 5 13 1 -9 3594.82 1084.13 6 -13 1 9 5299.93 1304.15 5 -15 1 9 44.3332 527.960 5 -17 1 9 8940.37 1701.10 5 -19 1 9 5435.61 1562.71 5 -21 1 9 1743.91 1083.48 5 -2 2 -9 2353.47 1047.05 1 0 2 -9 1279.38 828.342 1 2 2 -9 5412.65 1032.12 6 2 2 -9 4468.60 1166.34 1 4 2 -9 127.895 469.956 6 4 2 -9 256.550 604.716 1 6 2 -9 9102.19 1359.83 6 -6 2 9 8851.31 1409.18 5 8 2 -9 5191.16 1110.83 6 -8 2 9 5825.99 1154.06 5 10 2 -9 1074.82 682.112 6 -10 2 9 2272.59 785.781 5 -12 2 9 6512.16 1388.93 5 -14 2 9 1205.90 690.434 5 -16 2 9 4803.24 1279.85 5 -18 2 9 843.739 723.339 5 -20 2 9-23.8305 844.780 5 -3 3 -9 1836.10 886.987 1 -1 3 -9 7901.00 1586.03 1 1 3 -9 907.429 644.284 1 3 3 -9 1943.08 772.121 1 3 3 -9 1013.09 606.532 6 5 3 -9 1873.72 725.605 1 5 3 -9 1037.08 568.856 6 7 3 -9 13362.2 1690.48 6 -7 3 9 11799.3 1670.33 5 -9 3 9 4123.28 1076.42 5 -11 3 9 6893.60 1441.33 5 -13 3 9 4856.53 1319.83 5 -15 3 9 3851.42 1168.15 5 -17 3 9 217.811 498.824 5 -19 3 9 1804.29 962.058 5 -2 4 -9 1462.96 911.034 1 0 4 -9 1252.30 791.445 1 2 4 -9 4289.47 1142.90 1 4 4 -9 375.891 446.876 1 6 4 -9 2418.52 751.542 1 -10 4 9 8973.89 1550.10 5 -12 4 9 1728.62 849.257 5 -14 4 9 9531.59 1748.39 5 -16 4 9 3936.45 1270.02 5 -18 4 9 2658.64 1048.24 5 -20 4 9 1690.08 927.463 5 -1 5 -9 4219.09 1174.94 1 1 5 -9 781.895 576.096 1 3 5 -9 816.367 606.736 1 5 5 -9 4225.36 1029.31 1 -13 5 9-906.111 869.331 5 -15 5 9 6874.26 1509.74 5 -17 5 9 3997.24 1220.36 5 -19 5 9 840.117 836.597 5 -2 6 -9 330.683 649.839 1 0 6 -9 1783.59 850.458 1 2 6 -9 2053.14 779.313 1 4 6 -9 1724.91 684.307 1 6 6 -9 4354.80 1035.84 1 -20 6 9 240.552 589.691 2 -1 7 -9-1295.55 771.416 1 1 7 -9-174.017 539.530 1 3 7 -9 1600.61 699.150 1 5 7 -9 855.574 547.034 1 0 8 -9 1235.57 755.080 1 -7 -9 10 2740.80 1127.38 4 -9 -9 10 276.441 589.269 4 -11 -9 10 4294.01 1292.11 4 -13 -9 10 744.387 732.031 4 -15 -9 10 662.902 707.865 4 -4 -8 10-12.9764 597.411 4 -6 -8 10 5391.67 1433.18 4 6 -8 -10 2352.15 951.500 6 -8 -8 10 1557.07 944.547 4 8 -8 -10 1933.70 996.613 6 -10 -8 10 2821.27 1180.29 4 10 -8 -10 429.891 682.429 6 -12 -8 10 806.226 788.555 4 12 -8 -10 811.463 821.073 6 -14 -8 10 2498.73 983.565 4 14 -8 -10 3701.98 1207.83 6 3 -7 -10 3323.43 1134.74 6 -3 -7 10 2841.59 1224.49 4 5 -7 -10-478.479 603.506 6 -5 -7 10 97.4308 526.546 4 -7 -7 10 1244.25 744.256 5 -7 -7 10 1488.27 762.067 4 7 -7 -10 161.829 640.176 6 -9 -7 10 402.675 647.590 5 -9 -7 10 1081.14 663.200 4 9 -7 -10-316.445 639.241 6 -11 -7 10 266.216 561.054 5 -11 -7 10 262.638 583.763 4 11 -7 -10 1648.70 893.453 6 -13 -7 10 3654.62 1143.12 5 -13 -7 10 2192.11 878.169 4 13 -7 -10 3703.75 1164.89 6 -15 -7 10 1134.99 781.469 5 15 -7 -10 2036.27 1050.00 6 17 -7 -10 129.468 646.281 6 0 -6 -10 1639.06 999.605 6 2 -6 -10-508.618 634.741 6 4 -6 -10 2527.00 1007.49 6 -4 -6 10 5388.90 1412.14 4 6 -6 -10 1369.90 938.848 6 -6 -6 10 2322.24 869.678 4 -8 -6 10 732.755 665.833 5 -8 -6 10 1502.77 788.835 4 8 -6 -10-437.290 701.897 6 -10 -6 10 359.688 658.522 5 -10 -6 10 2075.88 920.584 4 10 -6 -10 1650.35 925.067 6 -12 -6 10 1003.42 762.820 5 -12 -6 10 652.442 564.006 4 12 -6 -10 2288.23 1063.17 6 -14 -6 10 1241.65 737.778 5 14 -6 -10 2197.11 981.260 6 -16 -6 10 582.001 672.662 5 16 -6 -10 1420.86 884.944 6 18 -6 -10 3358.45 1147.46 6 -1 -5 -10 1038.46 864.735 6 1 -5 -10 974.399 802.463 6 3 -5 -10 13.5012 461.890 6 5 -5 -10 1519.74 856.472 6 -5 -5 10 486.169 632.033 4 -7 -5 10 3578.22 958.006 5 -7 -5 10 2001.78 842.795 4 7 -5 -10 1296.45 843.681 6 -9 -5 10 3626.94 1123.36 5 -9 -5 10 3705.35 1076.76 4 9 -5 -10 2607.84 1005.78 6 -11 -5 10 5058.97 1207.36 5 -11 -5 10 3240.27 944.727 4 11 -5 -10 2010.50 853.850 6 -13 -5 10 2487.77 1034.02 5 13 -5 -10 5215.09 1372.65 6 -15 -5 10 2898.24 1057.02 5 15 -5 -10 670.677 639.533 6 -17 -5 10 2196.97 1137.81 5 17 -5 -10 524.521 556.663 6 19 -5 -10 2477.48 1031.21 6 0 -4 -10 498.815 674.406 6 2 -4 -10 601.406 595.327 6 4 -4 -10 2312.01 882.440 6 6 -4 -10 7588.14 1520.04 6 -6 -4 10 8173.14 1544.46 4 -6 -4 10 5505.83 1147.18 5 -8 -4 10 777.209 776.844 4 8 -4 -10 608.954 671.267 6 -8 -4 10 1649.90 759.470 5 -10 -4 10 5130.58 1216.94 5 -10 -4 10 4560.20 1071.98 4 10 -4 -10 3191.15 1022.14 6 -12 -4 10 1280.93 828.711 5 12 -4 -10-1.55877 788.711 6 -14 -4 10 1664.56 957.161 5 14 -4 -10 707.928 614.425 6 -16 -4 10 1623.31 803.511 5 16 -4 -10 1985.81 916.198 6 -18 -4 10 2466.72 1133.73 5 18 -4 -10 1039.18 699.722 6 1 -3 -10 1315.46 812.218 6 1 -3 -10 74.0412 653.968 1 3 -3 -10 919.947 613.156 6 5 -3 -10 941.162 658.428 6 7 -3 -10 1408.15 822.817 6 -7 -3 10 2145.75 840.852 4 -7 -3 10 2495.96 859.591 5 -9 -3 10-121.893 383.633 4 9 -3 -10 112.060 474.795 6 -9 -3 10 206.246 521.814 5 11 -3 -10 6882.04 1461.61 6 -11 -3 10 9692.65 1668.75 5 13 -3 -10 1840.32 801.748 6 -13 -3 10 3193.39 1063.93 5 15 -3 -10 5141.44 1352.09 6 -15 -3 10 1535.71 770.274 5 17 -3 -10 737.469 747.994 6 -17 -3 10 1706.61 878.591 5 -19 -3 10-295.645 935.846 5 0 -2 -10 2424.02 1028.79 1 2 -2 -10 293.456 641.462 6 2 -2 -10 1013.80 849.115 1 4 -2 -10 1344.31 784.572 6 6 -2 -10 739.722 672.642 6 -6 -2 10 147.045 461.491 5 -8 -2 10 1313.51 694.022 4 8 -2 -10 1958.90 931.489 6 -8 -2 10 18.4939 438.388 5 10 -2 -10 1019.55 745.404 6 -10 -2 10 1752.19 905.339 5 12 -2 -10 5980.67 1308.40 6 -12 -2 10 6240.46 1398.38 5 14 -2 -10 3374.66 1125.55 6 -14 -2 10 2356.94 985.392 5 16 -2 -10 1423.94 732.388 6 -16 -2 10 453.069 704.242 5 -18 -2 10 3205.87 1212.13 5 1 -1 -10-672.018 764.971 1 3 -1 -10 612.129 584.119 6 3 -1 -10 808.277 631.224 1 5 -1 -10 1909.92 799.320 6 7 -1 -10 4152.60 1100.11 6 -7 -1 10 2316.60 839.353 5 9 -1 -10 339.859 523.211 6 -9 -1 10 292.190 531.230 5 11 -1 -10 7119.62 1412.34 6 -11 -1 10 6277.76 1398.26 5 13 -1 -10 3921.97 1093.85 6 -13 -1 10 2553.89 908.596 5 15 -1 -10 231.503 795.520 6 -15 -1 10-516.928 751.635 5 -17 -1 10-55.8251 726.920 5 -19 -1 10 3793.58 1339.85 5 0 0 -10-160.055 789.810 1 2 0 -10-651.343 706.341 1 2 0 -10 196.273 358.667 6 4 0 -10 2810.38 991.546 1 4 0 -10 4091.45 1040.38 6 6 0 -10 4450.39 1074.43 6 -6 0 10 4650.09 1066.05 5 8 0 -10 129.366 626.303 6 -8 0 10 454.278 566.128 5 10 0 -10 4459.89 1079.46 6 -10 0 10 4389.89 1186.37 5 12 0 -10 727.904 757.450 6 -12 0 10 93.8356 512.100 5 14 0 -10 10102.7 1727.63 6 -14 0 10 9627.47 1754.07 5 -16 0 10 1490.40 862.172 5 -18 0 10 365.244 694.223 5 1 1 -10 743.825 880.290 1 3 1 -10 955.659 615.313 6 3 1 -10 1080.53 706.171 1 5 1 -10 4640.13 1055.43 6 -5 1 10 2376.77 747.507 5 5 1 -10 4014.09 1129.70 1 7 1 -10 3201.85 929.102 6 -7 1 10 5452.62 1215.27 5 9 1 -10-231.512 633.668 6 -9 1 10 816.113 712.356 5 11 1 -10 6575.36 1365.36 6 -11 1 10 3724.96 1161.77 5 13 1 -10 9779.34 1716.12 6 -13 1 10 4926.74 1367.50 5 -15 1 10 1061.83 739.126 5 -17 1 10 995.515 855.906 5 -19 1 10 751.539 981.083 5 0 2 -10 1627.60 1057.10 1 2 2 -10-398.310 601.182 1 4 2 -10 1157.98 673.575 1 4 2 -10 1431.39 669.626 6 6 2 -10-420.220 516.327 6 -6 2 10 1870.33 767.096 5 8 2 -10 1003.17 653.897 6 -8 2 10-221.358 516.480 5 10 2 -10 68.4341 499.699 6 -10 2 10-1056.16 837.943 5 -12 2 10 8740.94 1707.77 5 -14 2 10 2423.93 968.949 5 -16 2 10 1699.17 1045.35 5 -18 2 10 5926.79 1524.57 5 1 3 -10 6.81078 622.084 1 3 3 -10 1930.83 922.892 1 5 3 -10 1829.75 933.310 1 5 3 -10 618.707 445.991 6 7 3 -10 1383.35 678.152 6 -9 3 10-436.926 488.754 5 -11 3 10 9742.69 1717.85 5 -13 3 10 4165.96 1195.54 5 -15 3 10 5866.56 1405.49 5 -17 3 10 2314.62 992.793 5 -19 3 10 1509.34 1054.17 5 0 4 -10 733.330 500.898 1 2 4 -10-442.506 790.080 1 4 4 -10 1706.38 860.219 1 -10 4 10 4568.19 1194.95 5 -12 4 10-246.499 752.249 5 -14 4 10 1088.79 684.002 5 -16 4 10 2573.06 1102.77 5 -18 4 10 33.1068 771.491 5 1 5 -10-15.3164 519.560 1 3 5 -10 1737.92 781.604 1 5 5 -10 643.190 576.240 1 -15 5 10 281.609 613.035 5 -17 5 10-22.6469 714.322 5 2 6 -10 793.193 500.380 1 4 6 -10 5202.14 1227.97 1 1 7 -10-1032.48 719.427 1 3 7 -10 2912.20 975.405 1 -8 -8 11 1780.32 994.735 4 -10 -8 11-330.537 637.318 5 -10 -8 11-529.826 722.372 4 -12 -8 11 559.423 622.824 4 -7 -7 11 48.2765 611.241 4 -9 -7 11 2914.38 941.855 5 -9 -7 11 1111.79 831.207 4 -11 -7 11 1905.59 950.048 5 -11 -7 11 1912.16 988.105 4 -13 -7 11 1865.55 1048.91 5 -6 -6 11 652.051 532.214 4 -8 -6 11 3158.37 1179.52 4 8 -6 -11 3822.71 1292.30 6 -10 -6 11 497.653 701.986 5 -10 -6 11 1194.25 704.393 4 10 -6 -11 1340.75 717.088 6 -12 -6 11 907.448 867.526 5 12 -6 -11 2853.17 1218.37 6 -14 -6 11 243.356 578.975 5 5 -5 -11-132.219 695.703 6 -5 -5 11-531.641 648.418 4 -7 -5 11-45.6248 517.729 4 7 -5 -11 1415.11 869.916 6 -9 -5 11 1742.96 806.039 4 9 -5 -11 124.210 843.065 6 -9 -5 11 1391.51 755.418 5 -11 -5 11 985.499 706.860 5 11 -5 -11 469.141 604.420 6 -13 -5 11 2692.98 1035.42 5 13 -5 -11 1757.06 943.984 6 -15 -5 11 1086.53 949.670 5 15 -5 -11 2698.54 997.032 6 2 -4 -11 1298.72 723.252 6 4 -4 -11-28.1935 653.592 6 6 -4 -11 1496.44 958.280 6 -6 -4 11 802.476 583.652 4 8 -4 -11 732.141 837.185 6 -8 -4 11-240.598 526.750 5 10 -4 -11 2144.65 1056.19 6 -10 -4 11 2479.88 963.631 5 12 -4 -11 431.112 710.864 6 -12 -4 11-590.926 618.952 5 14 -4 -11-107.659 544.314 6 -14 -4 11 946.483 703.951 5 16 -4 -11 1873.41 926.654 6 -16 -4 11 1091.27 873.614 5 3 -3 -11 908.023 733.610 6 5 -3 -11 1251.58 727.655 6 7 -3 -11 804.584 701.217 6 9 -3 -11 1726.56 840.891 6 -9 -3 11 2561.51 876.371 5 11 -3 -11 5212.96 1355.44 6 -11 -3 11 4268.96 1210.81 5 13 -3 -11 1048.54 906.999 6 -13 -3 11 1038.64 938.413 5 15 -3 -11 2326.66 1023.94 6 -15 -3 11 2648.31 1158.67 5 17 -3 -11 939.386 761.490 6 -17 -3 11-584.177 659.339 5 4 -2 -11 4599.97 1176.53 6 6 -2 -11 43.2415 480.454 6 8 -2 -11 2088.26 966.872 6 -8 -2 11 3185.86 955.550 5 10 -2 -11 974.788 764.243 6 -10 -2 11-909.442 664.576 5 12 -2 -11 2890.59 1188.63 6 -12 -2 11 1296.37 738.918 5 14 -2 -11 1596.54 917.102 6 -14 -2 11 1936.33 913.501 5 16 -2 -11 1716.90 979.658 6 -16 -2 11 179.504 526.310 5 3 -1 -11 491.177 614.002 6 3 -1 -11-215.236 788.963 1 5 -1 -11 10.5507 547.019 6 7 -1 -11 1542.05 761.714 6 -7 -1 11 539.859 587.121 5 9 -1 -11 964.007 825.860 6 -9 -1 11 1807.65 889.187 5 11 -1 -11 1522.08 747.624 6 -11 -1 11 880.668 870.782 5 13 -1 -11 814.637 599.747 6 -13 -1 11 1872.78 931.746 5 15 -1 -11 1190.15 821.493 6 -15 -1 11-383.025 897.220 5 17 -1 -11 898.197 871.787 6 -17 -1 11 1784.50 1002.32 5 4 0 -11 2796.47 1117.73 1 4 0 -11 656.594 659.673 6 6 0 -11-75.6645 516.034 6 8 0 -11 1198.84 720.215 6 -8 0 11 1106.55 692.707 5 10 0 -11 263.656 495.557 6 -10 0 11-312.108 484.881 5 12 0 -11 2000.20 1058.99 6 -12 0 11 984.954 868.571 5 14 0 -11 253.784 718.469 6 -14 0 11 192.968 519.345 5 -16 0 11 684.323 790.696 5 3 1 -11 1543.94 871.238 1 5 1 -11 593.282 517.640 6 7 1 -11 359.607 497.291 6 -7 1 11 1021.20 655.038 5 9 1 -11 2930.39 1006.07 6 -9 1 11 2645.91 956.592 5 11 1 -11 3216.56 1118.73 6 -11 1 11 1633.95 771.609 5 13 1 -11 1459.77 848.176 6 -13 1 11 906.755 815.630 5 -15 1 11 385.060 662.276 5 -17 1 11-391.235 1030.12 5 4 2 -11 2092.02 1049.86 1 6 2 -11-406.445 643.040 6 8 2 -11 416.370 667.413 6 -8 2 11 1688.64 786.155 5 10 2 -11-411.362 634.091 6 -10 2 11-526.714 705.655 5 -12 2 11 648.740 699.229 5 -14 2 11 791.089 709.004 5 -16 2 11 659.875 958.102 5 3 3 -11 115.460 587.412 1 5 3 -11-528.194 554.603 1 7 3 -11 721.638 670.998 6 -9 3 11 667.935 647.245 5 -11 3 11 2607.47 1074.76 5 -13 3 11-515.480 776.730 5 -15 3 11 201.591 561.027 5 -17 3 11 3039.35 1297.51 5 4 4 -11-135.937 512.702 1 -12 4 11 406.723 830.965 5 -14 4 11-1222.41 883.471 5 -16 4 11 31.4583 798.915 5 3 5 -11 139.128 643.688 1 5 5 -11 262.073 604.872 1 4 6 -11 1233.30 799.947 1 -11 -5 12-788.020 609.350 5 -10 -4 12-1175.16 737.726 5 -12 -4 12-380.180 661.452 5 7 -3 -12 891.392 956.833 6 9 -3 -12 2553.87 1024.28 6 11 -3 -12 257.300 501.206 6 -11 -3 12 1851.48 928.589 5 -13 -3 12 52.0957 632.281 5 6 -2 -12-148.121 502.636 6 8 -2 -12 1436.90 826.409 6 10 -2 -12 1200.60 924.271 6 -10 -2 12-87.6223 576.559 5 12 -2 -12 1616.66 933.862 6 -12 -2 12 3241.80 1313.35 5 -14 -2 12-145.340 488.265 5 5 -1 -12 2735.67 999.085 6 7 -1 -12 572.157 815.222 6 9 -1 -12 661.134 701.454 6 11 -1 -12 553.822 834.487 6 -11 -1 12 2784.80 1220.01 5 13 -1 -12 1510.37 910.946 6 -13 -1 12 3472.76 1232.92 5 -15 -1 12 42.0457 566.902 5 6 0 -12 233.170 566.157 6 8 0 -12 1219.76 685.760 6 10 0 -12-792.404 808.592 6 -10 0 12 749.501 628.562 5 12 0 -12-123.431 690.655 6 -12 0 12 606.788 780.988 5 14 0 -12-693.879 808.906 6 -14 0 12 1029.83 969.188 5 7 1 -12-358.073 551.163 6 9 1 -12-454.474 632.896 6 -9 1 12-326.925 685.090 5 11 1 -12-421.395 657.030 6 -11 1 12 101.735 587.004 5 13 1 -12 1356.95 918.045 6 -13 1 12 2889.32 1124.46 5 -15 1 12 1301.62 1043.82 5 8 2 -12 2489.64 1026.62 6 10 2 -12-914.500 925.521 6 -10 2 12-1039.81 880.237 5 -12 2 12 1625.54 956.334 5 -14 2 12-1101.56 942.817 5 -11 3 12 259.295 739.073 5 -13 3 12 472.929 563.085 5 -11 1 13 353.486 588.870 5 0 0 0 0.00 0.00 0 ; _shelx_hkl_checksum 86903 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag Br Br -0.93486(5) 0.69582(7) -0.21710(10) 0.0654(3) Uani 1 1 d O1 O -1.1658(4) 1.2416(4) -0.2716(6) 0.0446(12) Uani 1 1 d O2 O -1.4083(5) 0.9113(8) -0.5035(7) 0.094(3) Uani 1 1 d O3 O -1.3745(4) 0.9710(4) -0.6807(6) 0.0492(13) Uani 1 1 d N1 N -1.2129(4) 0.9981(5) 0.1002(7) 0.0326(11) Uani 1 1 d N2 N -1.3688(4) 0.9778(5) -0.5452(7) 0.0396(13) Uani 1 1 d C1 C -1.2417(4) 1.0242(5) -0.2477(7) 0.0285(12) Uani 1 1 d C2 C -1.1944(4) 1.1141(5) -0.1076(7) 0.0275(12) Uani 1 1 d C3 C -1.1563(4) 1.2180(5) -0.1191(7) 0.0301(12) Uani 1 1 d C4 C -1.1101(5) 1.2943(5) 0.0173(9) 0.0388(14) Uani 1 1 d C5 C -1.0993(5) 1.2697(6) 0.1706(9) 0.0397(15) Uani 1 1 d C6 C -1.1356(4) 1.1670(5) 0.1900(7) 0.0324(14) Uani 1 1 d C7 C -1.1831(4) 1.0918(5) 0.0498(7) 0.0274(11) Uani 1 1 d C8 C -1.1378(5) 1.1145(7) 0.3273(9) 0.0420(16) Uani 1 1 d C9 C -1.1844(5) 1.0134(7) 0.2683(8) 0.0416(16) Uani 1 1 d C10 C -1.1670(4) 0.9426(5) -0.2423(7) 0.0252(11) Uani 1 1 d C11 C -1.0943(5) 0.9845(6) -0.2640(9) 0.0392(15) Uani 1 1 d C12 C -1.0263(5) 0.9103(7) -0.2600(9) 0.0413(16) Uani 1 1 d C13 C -1.1704(4) 0.8271(5) -0.2167(8) 0.0329(13) Uani 1 1 d C14 C -1.1020(5) 0.7528(6) -0.2092(9) 0.0394(15) Uani 1 1 d C15 C -1.0316(4) 0.7956(6) -0.2323(8) 0.0373(15) Uani 1 1 d C16 C -1.3093(5) 1.0734(6) -0.4255(8) 0.0360(14) Uani 1 1 d H1 H -1.288(4) 0.981(5) -0.242(7) 0.017(14) Uiso 1 1 d H4 H -1.088(4) 1.375(5) -0.005(7) 0.027(15) Uiso 1 1 d H14 H -1.113(5) 0.668(6) -0.195(8) 0.034(18) Uiso 1 1 d H12 H -0.983(5) 0.932(6) -0.306(9) 0.042(19) Uiso 1 1 d H16A H -1.280(6) 1.101(7) -0.469(10) 0.05(2) Uiso 1 1 d H8 H -1.110(5) 1.150(6) 0.433(10) 0.05(2) Uiso 1 1 d H11 H -1.092(6) 1.070(7) -0.286(10) 0.05(2) Uiso 1 1 d H13 H -1.225(6) 0.804(6) -0.207(9) 0.045(19) Uiso 1 1 d H5 H -1.066(5) 1.319(6) 0.255(9) 0.038(18) Uiso 1 1 d H16B H -1.362(6) 1.132(7) -0.446(9) 0.05(2) Uiso 1 1 d H9 H -1.199(6) 0.947(8) 0.323(11) 0.06(3) Uiso 1 1 d H1O H -1.146(5) 1.301(6) -0.271(9) 0.030(18) Uiso 1 1 d H1N H -1.237(9) 0.936(10) 0.037(14) 0.08(3) Uiso 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 Br 0.0462(4) 0.0800(6) 0.0659(5) -0.0153(5) 0.0277(3) 0.0232(4) O1 0.062(3) 0.035(3) 0.039(3) 0.004(2) 0.029(2) -0.011(2) O2 0.082(4) 0.151(6) 0.036(3) -0.016(3) 0.024(3) -0.084(5) O3 0.078(4) 0.040(3) 0.038(3) -0.009(2) 0.036(3) -0.004(3) N1 0.034(3) 0.039(3) 0.031(3) -0.001(2) 0.021(2) 0.000(2) N2 0.032(3) 0.049(3) 0.031(3) -0.003(3) 0.012(2) -0.006(2) C1 0.024(3) 0.032(3) 0.028(3) -0.002(2) 0.014(2) -0.002(2) C2 0.025(3) 0.031(3) 0.026(3) -0.002(2) 0.014(2) 0.003(2) C3 0.034(3) 0.029(3) 0.030(3) 0.001(2) 0.020(2) 0.001(2) C4 0.038(3) 0.029(3) 0.049(4) -0.005(3) 0.023(3) -0.002(3) C5 0.032(3) 0.045(4) 0.037(3) -0.019(3) 0.016(3) -0.003(3) C6 0.024(2) 0.043(4) 0.032(3) -0.005(3) 0.016(2) 0.005(2) C7 0.023(3) 0.035(3) 0.029(3) 0.000(2) 0.017(2) 0.006(2) C8 0.041(4) 0.055(4) 0.031(3) -0.011(3) 0.021(3) 0.002(3) C9 0.041(3) 0.057(4) 0.033(3) 0.004(3) 0.024(3) 0.004(3) C10 0.027(3) 0.028(3) 0.023(3) -0.004(2) 0.015(2) -0.001(2) C11 0.039(3) 0.037(3) 0.053(4) -0.002(3) 0.032(3) -0.004(3) C12 0.029(3) 0.051(4) 0.049(4) -0.007(3) 0.024(3) -0.004(3) C13 0.030(3) 0.034(3) 0.032(3) -0.002(3) 0.015(3) -0.005(2) C14 0.039(3) 0.037(4) 0.038(4) -0.001(3) 0.019(3) 0.004(3) C15 0.030(3) 0.047(4) 0.030(3) -0.011(3) 0.013(3) 0.006(3) C16 0.034(3) 0.041(4) 0.029(3) 0.000(3) 0.014(3) 0.001(3) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 C7 N1 C9 108.7(6) O2 N2 O3 122.8(6) O2 N2 C16 118.9(5) O3 N2 C16 118.3(6) C10 C1 C2 112.4(4) C10 C1 C16 111.4(5) C2 C1 C16 113.9(5) C7 C2 C3 115.6(5) C7 C2 C1 119.2(5) C3 C2 C1 125.1(5) O1 C3 C4 121.2(5) O1 C3 C2 116.8(5) C4 C3 C2 122.0(5) C3 C4 C5 121.1(6) C6 C5 C4 119.5(6) C5 C6 C7 118.4(5) C5 C6 C8 134.5(6) C7 C6 C8 107.0(5) N1 C7 C2 129.4(5) N1 C7 C6 107.3(5) C2 C7 C6 123.3(5) C9 C8 C6 107.0(6) C8 C9 N1 110.0(6) C13 C10 C11 119.1(6) C13 C10 C1 120.8(5) C11 C10 C1 120.2(5) C12 C11 C10 120.3(7) C15 C12 C11 118.8(6) C10 C13 C14 121.1(6) C13 C14 C15 118.9(7) C12 C15 C14 121.8(6) C12 C15 Br 118.4(5) C14 C15 Br 119.7(5) N2 C16 C1 108.7(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br C15 1.904(6) O1 C3 1.373(7) O2 N2 1.202(7) O3 N2 1.219(7) N1 C7 1.380(8) N1 C9 1.384(8) N2 C16 1.502(8) C1 C10 1.527(8) C1 C2 1.520(8) C1 C16 1.518(9) C2 C7 1.401(8) C2 C3 1.394(8) C3 C4 1.392(8) C4 C5 1.372(9) C5 C6 1.393(10) C6 C7 1.407(8) C6 C8 1.438(9) C8 C9 1.349(11) C10 C13 1.376(9) C10 C11 1.397(8) C11 C12 1.391(10) C12 C15 1.376(10) C13 C14 1.386(9) C14 C15 1.372(9)