#------------------------------------------------------------------------------ #$Date: 2019-11-11 20:38:22 +0200 (Mon, 11 Nov 2019) $ #$Revision: 227288 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/03/58/4035880.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_4035880 loop_ _publ_author_name 'Mart\'inez-Pardo, Pablo' 'Blay, Gonzalo' 'Vila, Carlos' 'Sanz-Marco, Amparo' 'Mu\~noz, M Carmen' 'Pedro, Jos\'e R' _publ_section_title ; Enantioselective Synthesis of 5-Trifluoromethyl-2-oxazolines under Dual Silver/Organocatalysis. ; _journal_issue 1 _journal_name_full 'The Journal of organic chemistry' _journal_page_first 314 _journal_page_last 325 _journal_paper_doi 10.1021/acs.joc.8b02808 _journal_volume 84 _journal_year 2019 _chemical_absolute_configuration ad _chemical_formula_sum 'C15 H15 Br F3 N O3' _chemical_formula_weight 394.19 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens difmap _audit_creation_method SHELXL-2014 _cell_angle_alpha 90 _cell_angle_beta 118.539(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 8.7236(5) _cell_length_b 11.9043(4) _cell_length_c 8.7256(4) _cell_measurement_reflns_used 3336 _cell_measurement_temperature 200(1) _cell_measurement_theta_max 27.5770 _cell_measurement_theta_min 4.3230 _cell_volume 796.04(8) _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 0.901 _diffrn_measurement_device_type 'SuperNova Sapphire3' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_unetI/netI 0.0573 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.901 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_number 6958 _diffrn_reflns_point_group_measured_fraction_full 0.895 _diffrn_reflns_point_group_measured_fraction_max 0.771 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 29.808 _diffrn_reflns_theta_min 3.423 _exptl_absorpt_coefficient_mu 2.626 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.76962 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Empirical absorption correction' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.645 _exptl_crystal_description prismatic _exptl_crystal_F_000 396 _exptl_crystal_size_max 0.120 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.080 _refine_diff_density_max 0.612 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.064 _refine_ls_abs_structure_details ; Flack x determined using 1144 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.030(7) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.813 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 268 _refine_ls_number_reflns 3533 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 0.812 _refine_ls_R_factor_all 0.0395 _refine_ls_R_factor_gt 0.0336 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0566P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0766 _refine_ls_wR_factor_ref 0.0835 _reflns_Friedel_coverage 0.639 _reflns_Friedel_fraction_full 0.783 _reflns_Friedel_fraction_max 0.630 _reflns_number_gt 3225 _reflns_number_total 3533 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file jo8b02808_si_003.cif _cod_data_source_block shelx _cod_original_cell_volume 796.03(8) _cod_original_sg_symbol_H-M 'P 21' _cod_database_code 4035880 _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 0.743 _shelx_estimated_absorpt_t_max 0.817 _shelxl_version_number 2014-1 _shelx_res_file ; TITL gon34 in P2(1)/m CELL 0.71073 8.723629 11.904253 8.725586 90.0000 118.5391 90.0000 zerr 2 0.000453 0.000367 0.000421 0.0000 0.0066 0.0000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H N O F BR UNIT 30 30 2 6 6 2 MERG 2 OMIT -3.00 180.00 FMAP 2 PLAN 25 SIZE 0.080 0.100 0.120 ACTA 50.00 L.S. 8 WGHT 0.056600 FVAR 9.37287 BR 6 0.679123 0.662094 0.778763 11.00000 0.02920 0.02698 = 0.03392 -0.00014 0.01027 -0.00850 O1 4 0.925546 0.975630 0.643924 11.00000 0.03239 0.03397 = 0.02414 0.00224 0.01328 -0.00972 O2 4 0.403316 0.885820 0.593044 11.00000 0.02096 0.06282 = 0.03406 -0.01130 0.01098 -0.00337 O3 4 0.650636 0.971421 0.792419 11.00000 0.02367 0.03287 = 0.02040 -0.00191 0.01108 0.00180 N 3 0.636743 0.988874 0.449180 11.00000 0.04149 0.03485 = 0.02315 0.00646 0.01601 0.00634 C1 1 0.856752 0.867622 0.661733 11.00000 0.02547 0.02215 = 0.02039 -0.00336 0.01086 -0.00209 C2 1 0.940351 0.835044 0.852586 11.00000 0.02048 0.02007 = 0.02080 -0.00209 0.00981 0.00057 C3 1 0.879632 0.750454 0.920664 11.00000 0.02062 0.02179 = 0.02637 -0.00210 0.01037 -0.00254 C4 1 0.963025 0.725927 1.096585 11.00000 0.03022 0.02708 = 0.02935 0.00260 0.01437 -0.00053 C5 1 1.110225 0.785116 1.210631 11.00000 0.03371 0.03345 = 0.02065 0.00079 0.00880 0.00011 C6 1 1.174275 0.868829 1.146248 11.00000 0.02842 0.03118 = 0.02523 -0.00036 0.00422 -0.00218 C7 1 1.090608 0.892869 0.970998 11.00000 0.02262 0.02565 = 0.02595 -0.00007 0.00882 -0.00443 C8 1 0.920571 0.786534 0.565127 11.00000 0.02926 0.04412 = 0.02630 -0.00504 0.01547 0.00309 C9 1 0.786858 1.030371 0.512782 11.00000 0.04945 0.03019 = 0.02292 0.00570 0.01774 0.00184 C10 1 0.655391 0.885567 0.552183 11.00000 0.02096 0.02932 = 0.01698 -0.00203 0.00674 0.00122 C11 1 0.553185 0.911537 0.650615 11.00000 0.02257 0.02869 = 0.02144 0.00327 0.00946 0.00510 C12 1 0.580582 1.011975 0.908397 11.00000 0.02609 0.03821 = 0.02505 -0.00287 0.01387 0.00171 C13 1 0.431329 1.091316 0.808179 11.00000 0.05946 0.05360 = 0.04587 0.00729 0.02600 0.02887 C14 1 0.528034 0.912446 0.980895 11.00000 0.04504 0.04551 = 0.03775 -0.00233 0.02516 -0.00501 C15 1 0.737177 1.071825 1.051316 11.00000 0.05384 0.05419 = 0.03541 -0.01564 0.02862 -0.01620 F1 5 0.881100 0.681013 0.573326 11.00000 0.05181 0.03218 = 0.04942 -0.01510 0.02915 0.00060 F2 5 1.094142 0.791626 0.633008 11.00000 0.02829 0.06670 = 0.04784 -0.00869 0.02342 0.00620 F3 5 0.853168 0.813360 0.396643 11.00000 0.05338 0.06874 = 0.02851 -0.00306 0.02596 0.01270 H10 2 0.596085 0.824465 0.476670 11.00000 0.01067 H4 2 0.910428 0.673898 1.134184 11.00000 0.04377 H14C 2 0.438264 0.877501 0.898537 11.00000 0.04251 H14A 2 0.492189 0.946288 1.073637 11.00000 0.04544 H5 2 1.165828 0.766863 1.327693 11.00000 0.04011 H6 2 1.267460 0.900079 1.219428 11.00000 0.04660 H13C 2 0.482453 1.153290 0.759041 11.00000 0.07665 H7 2 1.139964 0.940994 0.925359 11.00000 0.06068 H13B 2 0.403636 1.128542 0.902122 11.00000 0.06921 H14B 2 0.610888 0.863025 1.039340 11.00000 0.06170 H13A 2 0.329371 1.058107 0.720537 11.00000 0.06307 H9 2 0.810169 1.102578 0.477597 11.00000 0.06408 H15A 2 0.817852 1.022946 1.110140 11.00000 0.05256 H15B 2 0.763167 1.128677 0.993342 11.00000 0.05981 H15C 2 0.697195 1.102884 1.145943 11.00000 0.07870 HKLF 4 REM gon34 in P2(1)/m REM R1 = 0.0336 for 3225 Fo > 4sig(Fo) and 0.0395 for all 3533 data REM 268 parameters refined using 1 restraints END WGHT 0.0216 0.0000 REM Highest difference peak 0.612, deepest hole -0.331, 1-sigma level 0.064 Q1 1 0.7827 0.6594 0.7750 11.00000 0.05 0.61 Q2 1 0.5471 0.6664 0.7580 11.00000 0.05 0.52 Q3 1 0.6560 0.6640 0.6639 11.00000 0.05 0.49 Q4 1 0.6994 0.6569 0.9127 11.00000 0.05 0.41 Q5 1 0.7749 0.6640 0.8955 11.00000 0.05 0.31 Q6 1 0.2251 1.1598 0.7117 11.00000 0.05 0.29 Q7 1 0.7384 0.8718 0.6436 11.00000 0.05 0.29 Q8 1 0.4318 0.6570 0.6807 11.00000 0.05 0.26 Q9 1 0.8843 0.6637 0.8547 11.00000 0.05 0.25 Q10 1 0.6023 0.6693 0.5023 11.00000 0.05 0.24 Q11 1 0.4666 1.1614 1.1147 11.00000 0.05 0.23 Q12 1 0.8669 0.6690 0.7037 11.00000 0.05 0.23 Q13 1 0.8716 0.8241 0.6153 11.00000 0.05 0.23 Q14 1 0.2976 1.1595 0.9853 11.00000 0.05 0.23 Q15 1 0.9934 0.6182 0.9696 11.00000 0.05 0.23 Q16 1 0.9272 0.7651 0.8797 11.00000 0.05 0.22 Q17 1 0.6191 0.9398 0.3670 11.00000 0.05 0.22 Q18 1 0.6024 0.9035 0.5804 11.00000 0.05 0.22 Q19 1 0.4093 1.1210 0.7118 11.00000 0.05 0.22 Q20 1 0.8790 0.8614 0.7593 11.00000 0.05 0.22 Q21 1 0.5947 0.9033 0.4608 11.00000 0.05 0.22 Q22 1 1.2611 0.9510 1.3468 11.00000 0.05 0.21 Q23 1 0.6981 0.7973 0.9541 11.00000 0.05 0.21 Q24 1 1.3920 0.9164 1.4070 11.00000 0.05 0.21 Q25 1 1.2952 0.6629 1.3835 11.00000 0.05 0.21 ; _shelx_res_checksum 91583 _shelx_hkl_file ; 0 0 -2 9870.90 858.848 6 0 0 -2 9897.16 861.185 5 0 0 2 9203.44 859.387 4 0 0 2 9005.97 834.359 5 0 0 3 61951.5 2938.70 5 0 0 3 55334.7 2862.01 4 0 0 3 59487.3 2867.99 3 0 0 4 1895.92 530.671 3 0 0 4 1948.33 579.080 4 0 0 4 2367.61 633.460 5 0 0 -5 214809. 7819.78 1 0 0 5 213259. 8386.24 5 0 0 5 215907. 8338.06 4 0 0 5 234892. 8490.61 3 0 0 -6 25018.4 2177.11 1 0 0 6 23261.3 2449.11 4 0 0 6 26670.3 2580.21 5 0 0 6 29473.5 2612.36 3 0 0 7 71878.1 4970.86 5 0 0 7 79940.6 4995.44 3 0 0 -7 72825.7 4290.30 1 0 0 8 173.367 559.735 5 0 0 -8-419.408 550.070 1 0 0 8 954.349 628.838 3 0 0 9 35632.9 3831.44 3 0 0 9 35767.2 3956.69 5 0 0 10-3315.90 1482.81 3 0 -1 2 87026.0 3000.58 4 0 1 2 73635.6 2992.39 5 0 1 2 73537.5 3113.82 6 0 -1 -2 95628.1 3379.08 6 0 1 2 70656.2 3225.97 4 0 -1 -2 92550.2 3263.63 3 0 1 2 74751.4 3119.17 3 0 -1 2 86188.0 3235.24 5 0 1 -2 75474.2 3110.15 5 0 -1 -2 92780.4 3206.14 5 0 1 -2 73905.7 3101.39 1 0 -1 3 75309.0 3159.46 5 0 1 -3 48362.8 2557.84 1 0 1 3 47866.4 2652.15 3 0 -1 3 73650.0 2902.75 4 0 1 3 47817.8 2697.41 6 0 1 3 45004.8 2727.72 4 0 1 3 47942.6 2589.97 5 0 -1 4 68538.3 3354.31 4 0 1 4 63133.7 3513.36 6 0 1 4 62892.0 3456.58 3 0 1 -4 60871.3 3262.57 1 0 -1 4 71347.2 3649.63 5 0 1 4 63070.3 3384.09 5 0 1 4 66085.5 3618.08 4 0 -1 5 85704.6 4256.34 4 0 1 5 81045.7 4522.34 4 0 1 5 83070.8 4413.10 5 0 1 5 86938.6 4541.14 3 0 -1 5 87461.4 4596.83 5 0 1 -5 81742.7 4199.96 1 0 1 6 46060.0 3391.52 5 0 1 6 48626.0 3487.28 3 0 1 -6 45104.1 3126.89 1 0 1 6 45509.7 3468.21 4 0 -1 -6 33780.0 2499.45 1 0 -1 6 35147.6 3091.08 5 0 -1 6 40236.8 3087.58 3 0 1 7 3431.08 945.669 5 0 -1 -7 5293.70 1014.37 1 0 1 7 5243.49 1236.98 3 0 -1 7 6416.08 1442.49 5 0 -1 7 4949.54 1001.06 3 0 1 -7 3212.01 928.231 1 0 -1 8 17074.1 2438.94 3 0 1 8 18259.8 2512.04 3 0 -1 8 15625.8 2408.59 5 0 1 8 21170.3 2763.95 5 0 1 -8 19888.9 2338.41 1 0 1 9 1091.50 1086.81 5 0 -1 9 1103.47 816.388 5 0 -1 9 2878.92 1213.17 3 0 1 9 4.22053 821.580 3 0 1 10 9140.30 2123.38 3 0 -1 10 9029.03 2134.07 3 0 1 10 12150.1 2457.29 5 0 2 0 146413. 3641.31 2 0 2 0 161744. 3612.61 4 0 2 0 151939. 3858.50 1 0 2 1 91879.2 3458.72 6 0 2 -1 90054.1 3063.48 5 0 2 1 87872.3 2852.57 5 0 -2 -1 93512.2 2832.92 1 0 2 1 89085.4 2736.23 1 0 -2 -1 96563.6 3540.34 6 0 2 -1 86203.9 3406.01 1 0 -2 -1 98575.1 2924.92 5 0 2 1 88173.4 3365.06 4 0 -2 1 99290.1 3492.65 1 0 -2 1 92552.2 3110.16 5 0 2 1 90536.9 2715.35 2 0 -2 -1 97832.8 2752.10 2 0 -2 2 281982. 8625.80 5 0 -2 -2 300620. 7809.59 1 0 -2 -2 285741. 8728.10 3 0 -2 -2 270696. 7595.00 2 0 2 2 287975. 9039.56 4 0 2 2 281031. 8376.11 5 0 2 2 274775. 8819.60 3 0 2 2 296316. 8908.33 6 0 -2 -2 286392. 8921.14 6 0 2 -2 299129. 8689.63 5 0 2 -2 279919. 8802.54 1 0 -2 2 278267. 7943.90 4 0 -2 -2 294059. 8379.05 5 0 2 3 151470. 6073.71 4 0 2 3 156152. 5904.26 3 0 2 3 153829. 5543.65 5 0 2 3 153878. 5830.21 6 0 2 -3 152452. 5840.54 1 0 -2 3 157932. 5219.58 4 0 -2 3 165127. 5882.86 5 0 2 4 183110. 7230.30 6 0 -2 4 213091. 7476.37 5 0 -2 4 205668. 6742.29 4 0 2 4 180021. 7461.90 4 0 2 4 180604. 6918.24 5 0 2 4 188121. 7279.49 3 0 2 -4 183789. 7056.12 1 0 2 5 33253.1 2821.84 4 0 2 5 30210.5 2591.45 6 0 2 5 37411.8 2827.40 3 0 2 5 30704.0 2456.72 5 0 2 -5 34221.5 2558.37 1 0 -2 6 52134.7 3832.78 5 0 2 6 56907.7 3934.58 3 0 -2 -6 52533.2 2994.21 1 0 2 -6 52531.0 3613.97 1 0 2 6 49675.2 3839.72 4 0 2 6 52157.3 3675.35 5 0 2 6 51563.6 3812.97 6 0 2 7 35091.5 3299.98 3 0 -2 7 44689.2 3793.71 5 0 -2 -7 40085.8 2763.36 1 0 2 7 34434.3 3279.75 5 0 2 -7 34699.1 3107.26 1 0 -2 7 46632.6 3640.29 3 0 2 -8 100.371 538.292 1 0 -2 8-560.329 688.427 3 0 -2 8 701.244 631.387 5 0 2 8-142.114 470.955 3 0 2 8 333.940 433.749 5 0 2 9 6984.54 1775.03 5 0 2 9 8382.50 1815.09 3 0 -2 9 6331.39 1408.45 3 0 -2 9 7322.91 1728.98 5 0 2 10 5637.78 1617.81 5 0 -2 10 7084.05 1892.31 3 0 2 10 5828.33 1630.64 3 0 3 0 69.4443 95.2352 2 0 3 0 4.88422 105.780 1 0 3 0-59.7381 76.0542 4 0 -3 0 218.710 193.526 1 0 3 1 473370. 12729.5 2 0 3 -1 464542. 12939.9 5 0 3 1 451019. 12799.4 1 0 -3 -1 469183. 12740.6 2 0 -3 1 500901. 13850.1 1 0 3 1 455366. 13468.2 4 0 -3 -1 484224. 12956.7 1 0 3 -1 470114. 13696.4 1 0 3 1 459917. 12574.6 5 0 -3 1 478097. 12978.5 5 0 3 -1 453732. 13345.2 2 0 3 1 460196. 13799.2 6 0 -3 -1 502490. 12737.6 5 0 -3 -2 42482.6 1970.23 5 0 3 -2 48699.2 2282.24 5 0 3 2 45881.8 2570.06 4 0 3 -2 47228.1 2601.41 1 0 3 2 44522.4 1992.32 5 0 -3 2 39648.4 2149.16 5 0 3 2 49899.5 1680.06 1 0 -3 -2 42194.2 1531.88 2 0 -3 -2 36973.0 1627.50 1 0 3 2 44810.2 2528.97 6 0 -3 -3 187108. 5316.78 2 0 -3 3 181211. 6722.47 5 0 3 3 199334. 7066.46 6 0 3 3 194284. 7298.90 4 0 3 -3 198798. 7100.85 1 0 3 3 185534. 6416.52 5 0 -3 -3 188198. 5568.35 1 0 3 4 96347.7 4250.43 5 0 -3 4 86558.4 4409.13 5 0 3 -4 97194.8 4624.03 1 0 -3 -4 85528.5 3170.13 1 0 3 4 94244.2 4715.71 3 0 3 4 96808.1 4907.26 4 0 3 4 94251.8 4562.92 6 0 3 5 30941.0 2850.06 4 0 3 5 36408.7 2908.36 3 0 3 5 33481.1 2563.39 5 0 3 -5 33096.0 2691.50 1 0 3 5 34746.9 2819.99 6 0 -3 5 37340.1 2915.82 5 0 3 6 103156. 5793.12 3 0 -3 6 119035. 6078.01 5 0 3 6 104119. 6024.92 4 0 3 6 101930. 5707.17 6 0 3 6 105476. 5526.91 5 0 3 -6 100379. 5499.74 1 0 3 7 13071.1 2031.61 3 0 3 7 11713.9 1837.95 5 0 -3 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3 -4 1 -4 42529.3 2915.19 1 4 1 5 2199.99 1049.70 3 4 -1 5 1117.79 684.862 3 4 1 6 8762.72 1960.02 3 4 -1 6 7030.05 1818.47 3 4 1 7 6166.87 1937.94 3 4 -1 7 10154.7 2298.11 3 -4 2 11 2733.32 1272.25 4 4 2 -11 3847.10 1406.55 1 -4 -2 11 266.176 854.590 5 -4 2 11 3977.12 1438.86 5 -4 -2 10 8803.58 1892.61 4 -4 2 10 8958.75 2041.12 4 -4 -2 10 9182.77 2058.80 5 -4 2 10 11976.2 2274.83 5 -4 -2 9 2177.68 1079.30 5 -4 2 9-40.7277 710.083 5 -4 -2 8 34249.4 3419.29 5 -4 2 8 31133.7 3256.73 5 -4 -2 7 533.915 378.265 2 -4 -2 7 246.043 347.796 5 -4 2 7 1366.80 766.745 5 -4 -2 7 1601.15 419.413 3 -4 2 6 72896.8 3112.91 2 -4 -2 6 80700.5 4120.18 2 4 2 -6 71487.8 2954.99 6 -4 -2 6 91271.2 4797.87 5 -4 2 6 83941.4 4804.64 5 4 -2 -5 34031.3 1557.77 3 -4 2 5 36246.2 1547.22 6 -4 -2 5 31684.5 2409.74 2 -4 2 5 37927.8 1939.46 2 -4 -2 5 30525.0 2555.15 5 -4 2 5 37900.2 2866.07 5 -4 2 4 60171.1 2496.86 2 4 2 -4 48878.4 2046.68 6 -4 -2 4 53834.0 2982.57 2 -4 -2 4 54632.2 3216.61 5 -4 2 4 63036.3 3599.58 5 -4 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1779.01 2 -9 -4 10 278.558 662.155 2 -9 -4 10 509.339 734.441 5 -9 -4 9 10974.8 2013.61 2 -9 -4 9 9998.52 2079.90 5 -9 4 9 8131.72 1995.75 5 -9 -4 8 4091.39 1330.89 2 -9 -4 8 6862.44 1674.17 5 -9 4 8 9461.91 2055.54 5 -9 -4 7 373.558 516.503 2 -9 -4 7-761.804 696.554 5 -9 4 7 71.3215 421.578 2 -9 -4 6 20558.3 2581.44 2 -9 4 6 16383.1 1879.07 2 -9 -4 6 21536.7 2682.73 5 -9 4 5 11970.9 1667.46 2 -9 4 5 12572.4 1942.44 1 -9 -4 5 13441.3 2150.14 2 -9 -4 5 11146.7 1859.45 5 -9 4 4 17465.3 2224.48 1 -9 -4 4 21019.2 2540.21 2 -9 4 3 20676.0 2406.50 1 -9 -4 3 21931.9 2611.64 2 -9 4 2 19271.0 2309.93 1 -9 -4 2 22535.6 2682.36 2 9 -4 -1 3692.65 1101.80 3 -9 4 1 2859.11 887.618 1 -9 -4 1 3718.91 1163.93 2 9 -4 0 10358.1 2154.60 3 -9 4 0 13260.9 1991.44 1 -9 -4 0 11207.3 1927.94 2 9 -4 1 3076.46 1441.58 3 -9 -4 -1 3859.77 1234.49 2 -9 -4 -2 2765.78 1080.12 2 -9 -5 10 12854.5 2329.56 2 -9 -5 10 11215.7 2330.91 5 -9 -5 9 5956.94 1593.15 2 -9 -5 9 3621.04 1238.13 5 -9 5 9 4353.49 1469.87 5 -9 -5 8 3399.24 1368.53 2 -9 -5 8 3269.80 1146.63 5 -9 5 8 3879.22 1330.60 5 -9 -5 7 9675.32 1802.74 2 -9 -5 7 11586.2 2008.74 5 -9 5 7 10095.3 2004.43 5 -9 5 6 1438.16 998.564 1 -9 -5 6 1091.51 512.299 2 -9 -5 6 1099.19 666.483 5 -9 5 6 1025.93 552.982 2 -9 5 5 20750.2 2521.63 1 -9 5 5 19040.0 2084.60 2 -9 -5 5 18535.1 2401.65 5 -9 -5 5 19891.0 2558.20 2 -9 5 4 2275.30 919.345 1 -9 -5 4 2980.70 1130.00 2 -9 5 3 31113.8 3092.62 1 -9 -5 3 33414.6 3325.70 2 -9 5 2 7533.04 1513.68 1 9 5 -2 6420.41 1448.97 6 -9 -5 2 4746.08 1318.50 2 -9 5 1 15319.1 2260.63 1 9 5 -1 16338.1 2555.17 6 -9 -5 1 20168.1 2630.63 2 -9 5 0 6193.92 1458.77 1 -9 -5 0 6919.12 1528.75 2 9 -5 1 3687.45 1316.64 3 -9 5 -1 7708.00 1719.56 1 -9 -5 -1 5323.46 1446.19 2 -9 -6 10-38.9297 733.385 2 -9 -6 10 2195.96 883.067 5 -9 -6 9 2400.41 1160.42 2 -9 -6 9 2297.01 1099.04 5 -9 6 9 3997.86 1477.01 5 -9 -6 8 1459.24 1006.21 2 -9 -6 8 2996.58 1141.35 5 -9 6 8 2270.77 946.432 5 -9 -6 7 7545.10 1872.19 2 -9 -6 7 8341.27 1737.90 5 -9 6 7 5583.92 1583.12 5 -9 6 6 25995.6 2951.52 1 -9 6 6 22480.1 2196.00 2 -9 -6 6 24747.8 2742.42 5 -9 -6 6 20094.0 2740.74 2 -9 6 5 2496.14 962.951 1 -9 -6 5 2686.21 991.306 2 -9 6 4 21605.6 2606.03 1 -9 -6 4 26655.1 3138.35 2 -9 6 3 1671.88 889.827 1 -9 -6 3 1837.71 877.814 2 -9 6 2 13860.5 2133.64 1 9 6 -2 13740.8 2197.35 6 -9 -6 2 17203.5 2477.99 2 -9 6 1 10197.1 1937.42 1 9 6 -1 9983.04 2054.51 6 -9 -6 1 9968.22 2010.03 2 -9 6 0 3596.05 1269.10 1 9 6 0 2057.07 1048.35 6 -9 -6 0 4538.74 1422.68 2 -9 6 -1 8919.86 1813.68 1 -9 -6 -1 9591.33 1977.99 2 -9 -7 9 12965.8 2573.99 2 -9 -7 8 2669.59 1139.53 2 -9 7 8 2971.89 1355.22 5 -9 -7 7 7007.03 1933.86 2 -9 7 7 7517.06 1887.74 5 -9 7 6 11096.7 1968.79 1 -9 -7 6 9895.86 1871.06 2 -9 7 5 10509.0 1887.35 1 -9 -7 5 5016.15 1474.31 2 -9 7 4 7903.51 1668.57 1 -9 -7 4 8080.16 1816.87 2 -9 7 3 15569.3 2303.86 1 -9 -7 3 15496.9 2449.69 2 -9 7 2 7572.66 1734.72 1 9 7 -2 6564.83 1581.27 6 -9 -7 2 8285.27 1790.92 2 -9 7 1 10986.0 2005.79 1 9 7 -1 9324.88 1979.64 6 -9 -7 1 8026.23 1758.35 2 9 7 0 9903.66 2164.07 6 -9 7 0 10699.7 2063.58 1 -9 -7 0 8431.96 1766.14 2 -9 7 -1 4035.74 1380.91 1 -9 8 8 10010.5 2148.77 5 -9 8 7 6317.10 1607.30 1 -9 -8 7 5565.21 1722.15 2 -9 8 7 3642.86 1365.26 5 -9 8 6 2868.07 1107.21 1 -9 -8 6 3554.25 1450.75 2 -9 8 6 6056.46 1652.92 5 -9 8 5 2058.76 1017.97 1 -9 -8 5 437.584 655.088 2 -9 8 4 12151.3 2040.62 1 -9 -8 4 16663.3 2569.18 2 -9 8 3 6814.88 1684.40 1 -9 -8 3 4283.88 1274.23 2 -9 8 2 13575.3 2262.46 1 -9 -8 2 14084.1 2284.73 2 9 8 -1 5269.32 1451.20 6 -9 8 1 3369.46 1255.38 1 -9 -8 1 2295.03 987.498 2 9 8 0 11623.5 2449.07 6 -9 -8 0 14779.6 2393.01 2 -9 9 7 4594.23 1516.28 5 -9 9 6 1249.80 885.738 1 -9 -9 6 2139.10 1205.28 2 -9 9 6-214.055 680.835 5 -9 9 5 9758.71 1965.22 1 -9 -9 5 15020.9 2683.49 2 -9 9 4 2303.27 1115.52 1 -9 -9 4-480.455 868.522 2 -9 9 3 11524.5 2272.43 1 -9 -9 3 6081.22 1628.07 2 -9 -9 2 960.878 532.109 2 9 9 -1 15990.6 2659.93 6 9 10 -7 423.999 507.458 1 -9 10 6 18548.9 2920.47 5 9 10 -1 3296.43 1251.97 6 -10 0 9 3082.08 1323.37 5 -10 0 8 11806.6 1929.33 2 -10 0 8 9154.47 1976.37 5 -10 0 7 2851.99 1055.85 2 -10 0 7 1790.82 1012.32 5 -10 0 6 3710.63 1014.85 2 -10 0 5 27247.4 2860.66 2 -10 0 4 570.520 467.081 2 -10 0 3 5867.08 1328.03 2 -10 0 2 2807.25 1022.01 2 -10 0 1 14418.2 2209.49 2 -10 0 0 937.187 743.332 2 10 0 0-918.127 907.904 3 10 0 1 4802.41 1496.07 3 -10 -1 9 8859.72 1654.27 2 -10 -1 9 9245.91 1991.21 5 -10 1 9 9570.06 2151.53 5 -10 -1 8 4038.85 1173.60 2 -10 1 8 2933.63 1005.17 2 -10 1 8 2637.46 1184.02 5 -10 -1 7 7274.90 1498.98 2 -10 1 7 7067.63 1620.98 2 -10 -1 7 5836.23 1549.24 5 -10 1 7 7706.65 1798.96 5 -10 -1 6 13997.7 2095.79 2 -10 -1 6 14920.8 2406.92 5 -10 1 6 12911.5 1874.03 2 -10 -1 5 13211.3 2042.32 2 -10 1 5 11103.4 1756.50 2 -10 -1 4 10314.4 1734.06 2 -10 1 4 8404.70 1556.91 2 -10 1 3 6334.72 1516.82 2 -10 -1 3 4663.73 1259.42 2 -10 1 2 10333.7 1770.07 2 -10 -1 2 8919.96 1703.09 2 -10 1 1 3063.65 1082.95 2 -10 -1 1 1951.78 671.183 2 10 1 0 18827.9 2969.66 3 10 -1 0 15186.8 2686.18 3 -10 -1 0 14538.8 2318.63 2 10 1 1 1949.97 943.396 3 10 -1 1 4215.86 1248.25 3 -10 -2 9 3012.13 1007.32 2 -10 -2 9 5358.60 1616.08 5 -10 2 9 3885.40 1410.60 5 -10 -2 8 5077.97 1308.42 2 -10 -2 8 5903.09 1692.19 5 -10 2 8 7853.69 1932.95 5 -10 -2 7 8255.66 1695.41 2 -10 -2 7 5799.63 1577.39 5 -10 2 7 7568.50 1680.81 5 -10 2 7 5965.73 1259.49 2 -10 -2 6 18626.7 2462.89 2 -10 2 6 20374.9 2339.33 2 -10 -2 6 20504.4 2780.22 5 -10 -2 5 6798.31 1536.74 2 -10 2 5 7087.06 1445.26 2 -10 -2 4 7954.14 1662.49 2 -10 2 4 4814.26 1222.35 2 -10 2 3 13716.3 2065.83 2 -10 2 3 13941.5 2064.28 1 -10 -2 3 14882.1 2202.21 2 -10 2 2 880.756 523.120 1 -10 -2 2 914.546 527.402 2 -10 2 1 8536.79 1585.68 1 -10 -2 1 10333.7 1913.05 2 10 2 0 5973.00 1756.90 3 10 -2 0 2332.74 1410.93 3 10 2 1 11136.2 2584.78 3 10 -2 1 14080.7 2807.81 3 -10 -3 9 7883.87 1825.47 2 -10 -3 9 5293.69 1595.88 5 -10 3 9 4161.49 1562.95 5 -10 -3 8 5621.74 1481.66 2 -10 -3 8 4284.07 1373.33 5 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1910.63 2 -10 4 3 14957.9 2238.66 1 -10 -4 3 14752.6 2270.88 2 -10 4 2 2956.39 1067.75 1 -10 -4 2 1514.76 606.378 2 -10 4 1 16282.6 2325.53 1 -10 -4 1 15780.1 2385.85 2 10 -4 0 837.808 927.526 3 -10 -5 9 17510.7 2793.74 2 -10 -5 9 16904.5 2712.53 5 -10 -5 8 4438.07 1573.91 2 -10 -5 8 4204.66 1439.43 5 -10 5 8 6788.96 1766.92 5 -10 -5 7 4218.54 1333.41 2 -10 -5 7 2232.07 1053.45 5 -10 5 7 1993.07 1215.15 5 -10 -5 6 10119.3 1973.34 2 -10 -5 6 12348.7 2064.25 5 -10 5 6 9190.47 1532.85 2 -10 5 5 3705.97 1057.11 2 -10 5 5 3551.58 1153.27 1 -10 -5 5 4367.89 1377.03 2 -10 -5 5 4196.27 1221.12 5 -10 5 4 15573.1 2310.46 1 -10 -5 4 18302.4 2583.46 2 -10 5 3 620.627 552.117 1 -10 -5 3 1039.51 990.499 2 -10 5 2 21550.0 2716.00 1 -10 -5 2 18150.5 2665.82 2 -10 5 1 1717.90 773.468 1 -10 -5 1 975.262 669.137 2 10 -5 0 8905.65 2149.38 3 -10 5 0 14688.1 2307.80 1 -10 -6 8 7282.95 1962.15 2 -10 -6 7 9796.43 2016.67 2 -10 6 7 8437.46 1977.17 5 -10 6 6 3526.74 1142.88 1 -10 -6 6 5061.80 1373.84 2 -10 6 5 8111.49 1480.50 2 -10 6 5 6916.76 1617.67 1 -10 -6 5 5588.22 1597.17 2 -10 6 4 7910.71 1715.00 1 -10 -6 4 6915.63 1744.44 2 -10 6 3 6511.23 1564.58 1 -10 -6 3 8575.24 1855.65 2 -10 6 2-586.711 811.857 1 -10 -6 2 2108.59 1150.26 2 -10 6 1 6480.64 1662.52 1 10 -6 0 2392.01 1128.88 3 -10 7 6 3260.15 1345.18 1 -10 -7 6 1064.76 739.844 2 -10 7 5 10180.4 1945.43 1 -10 -7 5 12727.2 2297.45 2 -10 7 4 10631.4 1969.72 1 -10 -7 4 10311.0 2145.04 2 -10 7 3 1503.19 833.996 1 -11 0 8 1539.02 843.506 2 -11 0 8 2582.24 1188.78 5 -11 0 7 5662.36 1451.57 2 -11 0 7 3708.11 1391.99 5 -11 0 6 6785.02 1504.15 2 -11 0 5 227.278 478.799 2 -11 0 4-815.753 780.190 2 -11 0 3 4174.61 1232.47 2 -11 -1 8 7313.88 1614.23 2 -11 1 8 6792.09 1480.61 2 -11 -1 8 8704.21 2040.71 5 -11 -1 7 1350.70 833.448 2 -11 1 7 530.166 813.265 2 -11 -1 7 1133.90 869.092 5 -11 1 7 1680.75 974.081 5 -11 -1 6 5942.69 1556.83 2 -11 1 6 3504.11 1079.14 2 -11 -1 5 187.351 464.072 2 -11 1 5 1257.91 907.873 2 -11 -1 4 10177.9 1946.79 2 -11 1 4 7528.64 1574.00 2 -11 -1 3 7536.62 1601.25 2 -11 1 3 7052.18 1601.57 2 -11 -2 9 4589.41 1302.74 2 -11 -2 8 423.135 480.719 2 -11 -2 8 1517.95 895.106 5 -11 -2 7 13707.6 2247.01 2 -11 -2 7 12145.7 2258.12 5 -11 2 7 11064.9 1876.63 2 -11 2 7 8369.62 1998.87 5 -11 -2 6 2471.27 1145.41 2 -11 -2 6 1376.59 923.584 5 -11 2 6 812.050 659.228 2 -11 -2 5 8099.89 1783.46 2 -11 2 5 10386.4 1859.63 2 -11 -2 4 9230.24 1860.27 2 -11 2 4 10506.2 1886.10 2 -11 2 3 10728.3 1986.42 2 -11 -3 9-463.067 872.937 2 -11 -3 8 5921.13 1508.00 2 -11 -3 8 3449.52 1273.06 5 -11 -3 7 956.400 536.072 2 -11 -3 7 1714.73 830.808 5 -11 3 7 2088.23 860.230 2 -11 -3 6 4907.55 1468.26 2 -11 -3 6 5462.33 1571.34 5 -11 3 6 7185.83 1479.58 2 -11 -3 5 6842.61 1577.25 2 -11 3 5 5952.95 1339.13 2 -11 3 4 7599.33 1637.82 2 -11 -3 4 9961.54 1999.74 2 -11 3 3 2295.60 1024.59 1 -11 3 2 5143.73 1425.65 1 -11 -4 8 2291.54 1228.06 5 -11 -4 7 3792.34 1281.46 2 -11 -4 7 3450.07 1160.50 5 -11 -4 6 2524.51 1129.81 2 -11 -4 6 1705.81 966.293 5 -11 4 6 2023.68 926.874 2 -11 4 5 10331.1 1822.03 2 -11 4 4 1902.13 928.938 2 -11 4 4 1606.46 777.998 1 -11 4 3 4300.58 1333.10 1 -11 4 2 10287.8 1953.99 1 -11 5 6 9077.45 1654.63 2 -11 5 5 1713.83 848.226 2 -11 5 4 8725.29 1786.81 2 -11 6 5 4429.94 1254.48 2 -11 7 5 2964.24 1017.53 2 0 0 0 0.00 0.00 0 TITL gon34 in P2(1)/m REM P2(1)/m (#11 in standard setting) CELL 0.71073 8.723629 11.904253 8.725586 90.0000 118.5391 90.0000 ZERR 7.00 0.000453 0.000368 0.000421 0.0000 0.0066 0.0000 LATT 1 SYMM -x, y+1/2,-z SFAC C H N O UNIT 77.00 70.00 7.00 7.00 TREF HKLF 4 END ; _shelx_hkl_checksum 50272 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, 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 0.67912(5) 0.66209(4) 0.77876(5) 0.03202(13) Uani 1 1 d O1 O 0.9255(4) 0.9756(3) 0.6439(4) 0.0303(7) Uani 1 1 d O2 O 0.4033(4) 0.8858(4) 0.5930(5) 0.0402(9) Uani 1 1 d O3 O 0.6506(4) 0.9714(3) 0.7924(3) 0.0254(6) Uani 1 1 d N N 0.6367(6) 0.9889(4) 0.4492(5) 0.0329(9) Uani 1 1 d C1 C 0.8568(5) 0.8676(4) 0.6617(5) 0.0227(8) Uani 1 1 d C2 C 0.9404(5) 0.8350(3) 0.8526(5) 0.0205(8) Uani 1 1 d C3 C 0.8796(5) 0.7505(4) 0.9207(5) 0.0233(8) Uani 1 1 d C4 C 0.9630(6) 0.7259(4) 1.0966(6) 0.0288(9) Uani 1 1 d C5 C 1.1102(6) 0.7851(4) 1.2106(6) 0.0310(10) Uani 1 1 d C6 C 1.1743(6) 0.8688(4) 1.1462(6) 0.0318(10) Uani 1 1 d C7 C 1.0906(5) 0.8929(4) 0.9710(6) 0.0259(9) Uani 1 1 d C8 C 0.9206(6) 0.7865(5) 0.5651(6) 0.0323(10) Uani 1 1 d C9 C 0.7869(7) 1.0304(4) 0.5128(6) 0.0340(11) Uani 1 1 d C10 C 0.6554(5) 0.8856(4) 0.5522(5) 0.0234(8) Uani 1 1 d C11 C 0.5532(5) 0.9115(4) 0.6506(5) 0.0247(8) Uani 1 1 d C12 C 0.5806(6) 1.0120(4) 0.9084(6) 0.0291(9) Uani 1 1 d C13 C 0.4313(10) 1.0913(6) 0.8082(9) 0.0526(16) Uani 1 1 d C14 C 0.5280(9) 0.9124(6) 0.9809(8) 0.0405(12) Uani 1 1 d C15 C 0.7372(9) 1.0718(6) 1.0513(8) 0.0448(14) Uani 1 1 d F1 F 0.8811(4) 0.6810(3) 0.5733(4) 0.0424(8) Uani 1 1 d F2 F 1.0941(4) 0.7916(3) 0.6330(4) 0.0454(8) Uani 1 1 d F3 F 0.8532(4) 0.8134(3) 0.3966(4) 0.0476(8) Uani 1 1 d H10 H 0.596(5) 0.824(4) 0.477(5) 0.011(10) Uiso 1 1 d H4 H 0.910(6) 0.674(6) 1.134(6) 0.044(14) Uiso 1 1 d H14C H 0.438(8) 0.878(6) 0.899(8) 0.043(17) Uiso 1 1 d H14A H 0.492(8) 0.946(5) 1.074(9) 0.045(18) Uiso 1 1 d H5 H 1.166(7) 0.767(5) 1.328(7) 0.040(15) Uiso 1 1 d H6 H 1.267(8) 0.900(6) 1.219(7) 0.047(17) Uiso 1 1 d H13C H 0.482(8) 1.153(9) 0.759(8) 0.08(2) Uiso 1 1 d H7 H 1.140(8) 0.941(6) 0.925(8) 0.06(2) Uiso 1 1 d H13B H 0.404(8) 1.129(6) 0.902(8) 0.07(2) Uiso 1 1 d H14B H 0.611(9) 0.863(6) 1.039(9) 0.06(2) Uiso 1 1 d H13A H 0.329(9) 1.058(7) 0.721(8) 0.06(2) Uiso 1 1 d H9 H 0.810(9) 1.103(6) 0.478(9) 0.06(2) Uiso 1 1 d H15A H 0.818(10) 1.023(6) 1.110(9) 0.05(2) Uiso 1 1 d H15B H 0.763(8) 1.129(6) 0.993(8) 0.06(2) Uiso 1 1 d H15C H 0.697(10) 1.103(6) 1.146(9) 0.08(2) 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 0.0292(2) 0.0270(2) 0.0339(2) -0.0001(2) 0.01027(16) -0.0085(2) O1 0.0324(16) 0.0340(18) 0.0241(15) 0.0022(13) 0.0133(13) -0.0097(14) O2 0.0210(16) 0.063(3) 0.0341(18) -0.0113(18) 0.0110(14) -0.0034(17) O3 0.0237(14) 0.0329(17) 0.0204(14) -0.0019(12) 0.0111(12) 0.0018(13) N 0.041(2) 0.035(2) 0.0232(18) 0.0065(17) 0.0160(18) 0.0063(19) C1 0.0255(19) 0.022(2) 0.0204(18) -0.0034(15) 0.0109(16) -0.0021(16) C2 0.0205(18) 0.0201(19) 0.0208(18) -0.0021(15) 0.0098(15) 0.0006(15) C3 0.0206(19) 0.022(2) 0.026(2) -0.0021(16) 0.0104(17) -0.0025(16) C4 0.030(2) 0.027(2) 0.029(2) 0.0026(18) 0.0144(19) -0.0005(18) C5 0.034(2) 0.033(3) 0.0207(19) 0.0008(18) 0.0088(19) 0.0001(19) C6 0.028(2) 0.031(3) 0.025(2) -0.0004(19) 0.0042(19) -0.0022(19) C7 0.023(2) 0.026(2) 0.026(2) -0.0001(17) 0.0088(17) -0.0044(17) C8 0.029(2) 0.044(3) 0.026(2) -0.0050(19) 0.0155(19) 0.003(2) C9 0.049(3) 0.030(2) 0.023(2) 0.0057(19) 0.018(2) 0.002(2) C10 0.0210(19) 0.029(2) 0.0170(17) -0.0020(16) 0.0067(16) 0.0012(17) C11 0.0226(19) 0.029(2) 0.0214(19) 0.0033(17) 0.0095(17) 0.0051(16) C12 0.026(2) 0.038(3) 0.025(2) -0.0029(18) 0.0139(18) 0.0017(18) C13 0.059(4) 0.054(4) 0.046(3) 0.007(3) 0.026(3) 0.029(3) C14 0.045(4) 0.046(3) 0.038(3) -0.002(3) 0.025(3) -0.005(3) C15 0.054(4) 0.054(4) 0.035(3) -0.016(3) 0.029(3) -0.016(3) F1 0.0518(16) 0.032(2) 0.0494(15) -0.0151(14) 0.0292(14) 0.0006(14) F2 0.0283(14) 0.067(2) 0.0478(17) -0.0087(15) 0.0234(13) 0.0062(14) F3 0.0534(19) 0.069(2) 0.0285(14) -0.0031(14) 0.0260(14) 0.0127(17) 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' F F 0.0171 0.0103 '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 C9 O1 C1 105.3(3) C11 O3 C12 121.3(3) C9 N C10 105.6(4) O1 C1 C2 109.7(3) O1 C1 C8 102.6(3) C2 C1 C8 109.2(3) O1 C1 C10 102.4(3) C2 C1 C10 121.2(3) C8 C1 C10 110.1(3) C3 C2 C7 116.9(4) C3 C2 C1 124.8(4) C7 C2 C1 118.3(4) C4 C3 C2 121.4(4) C4 C3 Br 116.0(3) C2 C3 Br 122.6(3) C3 C4 C5 120.5(4) C4 C5 C6 119.3(4) C7 C6 C5 119.9(4) C6 C7 C2 122.0(4) F1 C8 F3 107.4(4) F1 C8 F2 106.9(4) F3 C8 F2 106.6(4) F1 C8 C1 113.2(4) F3 C8 C1 111.5(4) F2 C8 C1 110.8(4) N C9 O1 120.1(4) N C10 C11 104.3(3) N C10 C1 104.4(4) C11 C10 C1 118.0(3) O2 C11 O3 128.0(4) O2 C11 C10 121.6(4) O3 C11 C10 110.2(3) O3 C12 C13 109.3(4) O3 C12 C14 109.5(4) C13 C12 C14 112.5(5) O3 C12 C15 102.1(4) C13 C12 C15 111.9(5) C14 C12 C15 111.0(5) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Br C3 1.905(4) O1 C9 1.369(6) O1 C1 1.458(5) O2 C11 1.195(5) O3 C11 1.325(5) O3 C12 1.490(5) N C9 1.254(7) N C10 1.486(6) C1 C2 1.515(5) C1 C8 1.549(6) C1 C10 1.562(6) C2 C3 1.396(6) C2 C7 1.402(6) C3 C4 1.380(6) C4 C5 1.384(7) C5 C6 1.386(7) C6 C7 1.373(6) C8 F1 1.313(6) C8 F3 1.335(5) C8 F2 1.338(5) C10 C11 1.536(6) C12 C13 1.505(7) C12 C14 1.514(7) C12 C15 1.517(7)